Thermally and Electrically Conductive Polypropylene Based Resins for Fuel Cell Bipolar Plates By Beth A. Johnson A THESIS Submitted in partial fulfillment of the requirements for the degree of Master of Science in Chemical Engineering MICHIGAN TECHNOLOGICAL UNIVERSITY 2009 Copyright© Beth A. Johnson 2009 This thesis, “Thermally and Electrically Conductive Polypropylene Based Resins for Fuel Cell Bipolar Plates,” is hereby approved in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE in the field of Chemical Engineering. DEPARTMENT – Chemical Engineering Signatures: Thesis Advisor _______________________ Dr. Julia A. King Department Chair _______________________ Dr. S. Komar Kawatra Date: ______________________________ Abstract “Thermally and Electrically Conductive Polypropylene Based Resins for Fuel Cell Bipolar Plates” Adding different conductive carbon fillers to insulating thermoplastic resins increases the composite electrical and thermal conductivity. One potential market for these thermally and electrically conductive resins is for fuel cell bipolar plates. These bipolar plates are used in the fuel cell to transfer oxygen and hydrogen that are used to in the reaction, remove excess heat and water produced in the reaction, and to provide electrical contact between the cells. In this study, varying amounts of three different carbon fillers (carbon black, synthetic graphite particles, and carbon nanotubes) were added to polypropylene. The maximum single filler amounts that that could be extruded and injection molded were 15 wt% for carbon black, 80 wt% for synthetic graphite, and 15 wt% for FibrilTM carbon nanotubes. The in-plane and through plane thermal conductivity and the electrical resistivity (1/electrical conductivity) was measured for each polymer composites. The effects of single fillers and combinations of the different fillers were studied via a factorial design. From the thermal conductivity results, it was determined that each single filler caused a statistically significant increase in composite through-plane thermal conductivity, with synthetic graphite causing the largest increase. All of the composites containing combinations of the different fillers also caused a statistically significant increase in composite through-plane thermal conductivity. Composites containing 80 wt% synthetic graphite and the three fillers (2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes) had an in-plane thermal conductivity of 28.0 W/m K and 24.0 W/m K, both values are above 20 W/m.K which is the desired target for bipolar plates. From the electrical conductivity results the percolation thresholds for each filler was determined. The percolation threshold was 1.4 vol % for the composites containing only carbon black, 2.1 vol% for those containing only carbon nanotubes, and 13 vol % for those containing only synthetic graphite particles. The factorial results indicated that, for the composites containing only single fillers, synthetic graphite, followed closely by carbon nanotubes, and then carbon black, cause a statistically significant decrease in composite electrical resistivity. All composites containing combinations of different fillers had a statistically significant effect which increased the electrical resistivity. The composite closest to the US Department of Energy target of 100 S/cm is the 2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes formulation compression molded with an electrical conductivity result of 91 S/cm. i Acknowledgements First I would like to thank my advisor Dr. Julie King for all of her guidance and support throughout my time and Michigan Technological University. I would also like to thank Dr. Jason Keith, Dr. Tony Rogers, and Dr. Ibrahim Miskioglu for taking time out of their busy schedules to be on my committee. I would like to acknowledge the Department of Energy (Award Number DEFG36-08GO88104) and the National Science Foundation (DMI-0456537) for funding this project. I would also like to acknowledge Asbury Carbons and Akzo Nobel for providing carbon fillers and the Dow Chemical Company for providing the polypropylene polymer. I would like to thank all the undergraduate students at Michigan Technological University that helped me with this project. I would especially like to thank Michael Via, Charlie Ciarkowski, and Daniel R. Woldring for all their hard work and for starting the project while I was finishing up my bachelor’s degree. Without them I would not have been able to finish most of my research in the summer. Finally, I would like to thank my family for all their support throughout my entire college career. They helped me through tough decisions and supported me when I needed help. They are a large part of my success and without them this wouldn’t have been possible. ii Table of Contents Abstract ............................................................................................................................... i Acknowledgements ........................................................................................................... ii List of Figures .................................................................................................................. vii List of Tables ..................................................................................................................... x Nomenclature .............................................................................................................. xxvii Chapter 1: Introduction ................................................................................................... 1 1.1: Introduction .............................................................................................................. 1 1.2: Motivation ................................................................................................................ 2 1.3: Objectives ................................................................................................................. 4 1.4: References ................................................................................................................ 5 Chapter 2: Background .................................................................................................... 9 2.1: Fuel Cells ................................................................................................................. 9 2.1.1: Proton Exchange Membrane Fuel Cells ......................................................... 10 2.1.1.1: Proton Exchange Membrane/Catalyst Assembly .................................... 12 2.1.1.2: Bipolar Plates ........................................................................................... 14 2.1.1.3: The Backing Layers or Gas Diffusion Layers ......................................... 16 2.1.2: Thermal and Electrical Management in the Fuel Cell .................................... 17 2.2: Thermal Conductivity ............................................................................................ 17 2.3: Electrical Conductivity .......................................................................................... 20 2.4: References .............................................................................................................. 24 Chapter 3: Materials....................................................................................................... 28 3.1: Materials ................................................................................................................. 28 3.2: Matrix Material ...................................................................................................... 28 3.2.1: Semi-Crystalline Homopolymer Polypropylene Resin H7012-35RN ............ 28 3.3: Filler Materials ....................................................................................................... 29 3.3.1: Carbon Black .................................................................................................. 29 3.3.2: Synthetic Graphite .......................................................................................... 32 3.3.3: Hyperion Fibril Carbon Nanotubes................................................................. 34 3.4: Formulation Naming Convention ......................................................................... 36 3.5: References ............................................................................................................. 39 iii Chapter 4: Fabrication and Experimental Methods ................................................... 41 4.1: Fabrication Methods............................................................................................... 41 4.1.1: Extrusion ......................................................................................................... 41 4.1.2: Drying ............................................................................................................. 44 4.1.3: Injection Molding ........................................................................................... 45 4.1.4: Compression Molding..................................................................................... 47 4.2:Experimental Test Methods .................................................................................... 50 4.2.1: Through-Plane Electrical Resistivity Test Method ......................................... 50 4.2.2: In-Plane Electrical Resistivity Test Method ................................................... 51 4.2.3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Test Method .. 53 4.2.4: Thermal Conductivity: Guarded Heat Flow Meter Test Method ................... 56 4.2.5: Thermal Conductivity: Transient Plane Source Test Method ........................ 58 4.2.6: HotDisk Analyser: Specific Heat .................................................................... 62 4.2.7 Density: ASTM D792-66 ................................................................................. 64 4.2.8: Solvent Digestion – ASTM D5226-98 ........................................................... 65 4.2.9: Filler Length and Aspect Ratio ....................................................................... 67 4.2.10: Determination of Filler Orientation in a Polymer Composite ...................... 70 4.2.10.1: Sample Preparation and Polishing ......................................................... 70 4.2.10.2: Optical Imaging Methods ...................................................................... 76 4.2.10.3: Image Processing and Analysis ............................................................. 78 4.2.10.4 Microtoming ........................................................................................... 80 4.2-11: Field Emission Scanning Electron Microscope (FESEM) Test Method ...... 81 4.3: References ............................................................................................................. 81 Chapter 5: Miscellaneous Results.................................................................................. 84 5.1: Density Results....................................................................................................... 84 5.2: Solvent Digestion Results ...................................................................................... 85 5.3: Filler Length and Aspect Ratio Results ................................................................. 86 5.4: Orientation Results ................................................................................................. 87 5.5: Field Emission Scanning Electron Microscope (FESEM) Results ........................ 90 5.6: Conclusions ............................................................................................................ 91 5.7: References .............................................................................................................. 92 iv Chapter 6: Electrical Resistivity Results and Design of Experiment Analysis ......... 93 6.1: Single Filler Electrical Resistivity Results ............................................................. 93 6.2: Electrical Resistivity Factorial Design Results ...................................................... 99 6.3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Results ................ 104 6.4: Conclusions .......................................................................................................... 107 6.5: References ............................................................................................................ 108 Chapter 7: Thermal Conductivity Results and Design of Experiment Analysis .... 110 7.1: Through Plane Thermal Conductivity Results ..................................................... 110 7.2: Through Plane Thermal Conductivity Factorial Design Results ......................... 116 7.3: In-Plane Thermal Conductivity Results ............................................................... 121 7.4: Conclusions .......................................................................................................... 124 7.5: References ............................................................................................................ 125 Chapter 8: Summary, Conclusions, and Future Work ............................................. 126 8.1: Summary .............................................................................................................. 126 8.1.1: Effects of Single Conductive Fillers on Electrical Resistivity ..................... 126 8.1.2: Effects of Multiple Conductive Fillers on Electrical Resistivity .................. 127 8.1.3: Effects of Single Conductive Fillers on Thermal Conductivity ................... 129 8.1.4: Effects of Multiple Conductive Fillers on Through-Plane Thermal Conductivity............................................................................................................ 130 8.1.5: Miscellaneous Results................................................................................... 131 8.2: Conclusions .......................................................................................................... 131 8.3: Recommendations for Future Work ..................................................................... 133 8.4: References ............................................................................................................ 135 Appendix A: Screw Design and Extrusion Run Conditions ..................................... 136 Appendix B: Injection Mold Run Conditions ............................................................ 147 Appendix C: Electrical Resistivity .............................................................................. 156 Appendix D: US Fuel Cell Council Through Plane Electrical Resistivity Results . 195 Appendix E: TCA 300 Through-Plane Thermal Conductivity Results at 55°C ..... 298 Appendix F: Heat Capacity.......................................................................................... 321 Appendix G: Hot Disk Thermal Conductivity at 23°C ............................................. 329 Appendix H: Density..................................................................................................... 337 v Appendix I: Solvent Digestion Results ........................................................................ 355 Appendix J: Filler Length and Aspect Ratio Results ................................................ 356 Appendix K: Orientation Results and Photomicrographs ........................................ 357 Appendix L: Field Emission Scanning Electron Microscope Photomicrographs ... 366 Appendix M: Permission Letters ................................................................................. 369 vi List of Figures Figure 2.1-1: Proton Exchange Membrane Fuel Cell Schematic ..................................... 12 Figure 2.2-1: Two-Dimensional Array of Atoms in a Crystalline Structure .................... 18 Figure 2.3-1: Dependence of Electrical Conductivity on Filler Volume Fraction ........... 21 Figure 2.3-2: Definition of Percolation Theory in a Square Lattice ................................. 22 Figure 3.2-1: Chemical Structure for Polypropylene ........................................................ 29 Figure 3.3-1: Ketjenblack EC-600 JD Primary Aggregate ............................................... 31 Figure 3.3-2: Photomicrograph of Thermocarb TC-300 Synthetic Graphite ................... 34 Figure 4.1-1: American Leistritz Extruder Corporation Model ZSE 27 ........................... 42 Figure 4.1-2: Schenck AccuRate Flexwall Feeder ........................................................... 43 Figure 4.1-3: Schenck AccuRate Conisteel Feeder .......................................................... 43 Figure 4.1-4: Picture showing the Water Bath and Pelletizer........................................... 44 Figure 4.1-5: Bry Air Drying Oven System...................................................................... 45 Figure 4.1-6: Niigata Injection Molding Machine Model NE85UA4 ............................... 46 Figure 4.1-7: Four-Cavity Mold Used in Injection Molding ............................................ 47 Figure 4.1-8: Wabash Model V75H-18-CLX Compression Molding Press..................... 50 Figure 4.2-1: Diagram of Through Plane Electrical Resistivity Test ............................... 51 Figure 4.2-2: (A) Experimental Set-up for Four-Probe Test Method (B) Sample Dimensions ............................................................................................... 52 Figure 4.2-3: Setup for Through-Plane (US Fuel Cell Council) Electrical Resistivity Test Method ...................................................................................................... 53 Figure 4.2-4: Schematic of Through-Plane (US Fuel Cell Council) Electrical Resistivity Test Method .............................................................................................. 56 Figure 4.2-5: Holometrix Model TCA-300 Thermal Conductivity Analyzer .................. 57 Figure 4.2-6: Schematic of Through-Plane Thermal Conductivity Test Method ............. 58 Figure 4.2-7: Mathis Instruments Hot Disk Thermal Constants Analyzer ....................... 59 Figure 4.2-8: Schematic of Samples and Sensor for the Hot Disk. The insert at the lower left shows the double spiral heating element. ........................................... 60 Figure 4.2-9: Hot Disk Inc. Heat Capacity Cell................................................................ 63 Figure 4.2-10: Solvent Digestion Filtration Apparatus..................................................... 67 Figure 4.2-11: Filler Dispersion Apparatus ...................................................................... 68 Figure 4.2-12: Microscope Setup for Filler Length/Aspect Ratio Analysis ..................... 68 Figure 4.2-13: “Through Plane” and “XY Plane” Surface Samples Studied from Injection Molded Disk.............................................................................................. 70 Figure 4.2-14: “In Plane” Surface Samples Studied from Tensile Bar............................. 71 Figure 4.2-15: Top View of Epoxy Pucks “Through Plane” Sample (left) and “In Plane” Sample (right) ........................................................................................... 72 Figure 4.2-16: Oval Shaped Ground Epoxy Pucks ........................................................... 72 Figure 4.2-17: Prepared Puck with Both Slides Attached ................................................ 73 Figure 4.2-18: Cut-off Saw Used to Cut Samples to 0.2 mm ........................................... 74 Figure 4.2-19: 0.2 mm Thin Composite Samples Ready to be Polished .......................... 74 Figure 4.2-20: Buehler Ecomet 4 Grinder/Polisher .......................................................... 75 Figure 4.2-21: Olympus BX60 Reflected Light Microscope............................................ 77 vii Figure 4.2-22: Diagram of Images Taken on “In Plane” and “Through Plane” Surfaces 77 Figure 5.4-1: In-Plane Photomicrograph for Injection Molded 65 wt% Synthetic Graphite in Polypropylene at 200X Magnification .................................................. 89 Figure 5.4-2: Through-Plane Photomicrograph for Injection Molded 65 wt% Synthetic Graphite in Polypropylene at 200X Magnification ................................... 89 Figure 5.5-1: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion FIBRILTM Carbon Nanotubes in Polypropylene Composit ...................... 90 Figure 6.1-1: Single Filler Electrical Resistivity Results for FibrilTM Carbon Nanotubes and Carbon Black in Polypropylene and Carbon Black in Vectra............ 97 Figure 6.1-2: Single Filler Electrical Resistivity Results for Synthetic Graphite in Polypropylene and in Vectra ..................................................................... 98 Figure 7.1-1: Single Filler Through-Plane Thermal Conductivity Results for FibrilTM carbon nanotubes and Carbon Black in Polypropylene and Carbon Black in Vectra .................................................................................................. 114 Figure 7.1-2: Single Filler Through-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene and in Vectra................................................ 115 Figure 7.3-1: In-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene Composites ..................................................................... 123 Figure A.1: 5-14-2005 Extruder Screw Design .............................................................. 136 Figure K.1: In-Plane Photomicrograph for Injection Molded 30 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification ................................................ 358 Figure K.2: Through-Plane Photomicrograph for Injection Molded 20 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .................................. 358 Figure K.3: In-Plane Photomicrograph for Injection Molded 45 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification ................................................ 359 Figure K.4: Through-Plane Photomicrograph for Injection Molded 45 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .................................. 359 Figure K.5: In-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification ................................................ 360 Figure K.6: Through-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .................................. 360 Figure K.7: XY-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC300 in Polypropylene at 200X Magnification ......................................... 361 Figure K.8: In-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .................................. 362 Figure K.9: Through-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .............. 362 Figure K.10: XY-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .................................. 363 viii Figure K.11: In-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .............. 364 Figure K.12: Through-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification ..... 364 Figure K.13: XY-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification .............. 365 Figure L.1: Field Emission Scanning Electron Microscope Photomicrograph of 15% wt Carbon Black in Polypropylene Composite............................................ 366 Figure L.2: Field Emission Scanning Electron Microscope Photomicrograph of 15% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite ........ 367 Figure L.3: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite .................................... 367 Figure L.4: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite .................................... 368 Figure M.1: Email from Matt Clingerman for Figures 4.2-1 and 4.2-2.......................... 369 Figure M.2: Email from Rebecca Hauser for Figures 2.1-1 ........................................... 369 Figure M.3: Email from Rebecca Hauser for Figures 4.2-4 and 4.2-11 ......................... 370 Figure M.4: Email from Asbury Carbon for Figures 3.3-2............................................. 370 ix List of Tables Table 1.1-1: Thermal Conductivity for Common Materials [1] ......................................... 2 Table 1.1-2: Electrical Conductivity for Common Materials [2] ....................................... 2 Table 1.1-3: Desired Bipolar Plate Properties .................................................................... 4 Table 2.1-1: Summary of the Different Types of Fuel Cells ............................................ 10 Table 2.1.-2: Desired Bipolar Plate Properties ................................................................. 14 Table 3.2-1: Properties of Dow H7012-35RN Polypropylene Resin/Molded Parts ........ 29 Table 3.3-1: Properties of Akzo Nobel Ketjenblack EC-600 JD ...................................... 31 Table 3.3-2: Properties of Thermocarb TC-300 Synthetic Graphite ................................ 33 Table 3.3-3: Properties of FIBRILTM Carbon Nanotubes ............................................... 36 Table 3.4-1: Single Filler Loading Levels ........................................................................ 38 Table 4.2-1: Buehler Polishing Procedure for Polypropylene .......................................... 76 Table 5.1-1: Density Results for Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ................................................................................................ 85 Table 5.1-2: Density Results for 30 wt% Synthetic Graphite in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................... 85 Table 5.2-1: Solvent Digestion Results for 45% wt Synthetic Graphite in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN.................................. 86 Table 5.3-1: Mean Length and Aspect Ratio Results for Single Filler Synthetic Graphite Formulations ................................................................................................ 87 Table 5.4-1: Orientation Results for a Formulation Containing 65 wt% Synthetic Graphite in Polypropylene .......................................................................................... 88 Table 6.1-1: Electrical Resistivity Results for Carbon Black in Polypropylene .............. 94 Table 6.1-2: Electrical Resistivity Results for FibrilTM Carbon Nanotubes in Polypropylene .............................................................................................. 95 Table 6.1-3: Electrical Resistivity Results for Synthetic Graphite in Polypropylene ...... 96 Table 6.2-1: Filler Loadings in Factorial Design Formulations ..................................... 100 Table 6.2-2: Filler Loadings in Factorial Design Formulation and Electrical Resistivity Results (IM= Injection Molded, CM=Compression Molded) ................... 102 Table 6.2-3: Factorial Design Analysis for Log (Electrical Resistivity, ohm-cm) ......... 103 Table 6.3-1: Single Filler Through-Plane Electrical Resistivity (US Fuel Cell Council) Results ........................................................................................................ 105 Table 6.3-2: Multiple Filler Through-Plane Electrical Resistivity (US Fuel Cell Council) Results ........................................................................................................ 106 Table 6.3-3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Results from Dana Corporation [12] ............................................................................... 106 Table 7.1-1: Through Plane Thermal Conductivity at 55º C for Carbon Black in Polypropylene ............................................................................................ 111 Table 7.1-2: Through Plane Thermal Conductivity at 55º C for FibrilTM carbon nanotubes in Polypropylene ........................................................................................ 112 Table 7.1-3: Through Plane Thermal Conductivity at 55º C for Synthetic Graphite in Polypropylene ............................................................................................ 113 Table 7.2-1: Filler Loadings in Factorial Design Formulations ..................................... 117 x Table 7.2-2: Filler Loadings in Factorial Design Formulations and Through-Plane Thermal Conductivity Results ................................................................... 119 Table 7.2-3: Factorial Design Analysis for Through-Plane Thermal Conductivity ....... 120 Table 7.3-1: In-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene Composites ........................................................................ 122 Table 7.3-2: In-Plane Thermal Conductivity Results for Composites Containing Combinations of Different Fillers in Polypropylene ................................. 123 Table 8.1-1: Filler Loadings in Factorial Design Formulations ..................................... 127 Table A.1: Purge Conditions Using Dow H7012-35RN Polypropylene Homopolymer Only............................................................................................................ 137 Table A.2: Ketjenblack EC-600 JD Carbon Black Formulations ................................... 138 Table A.3a: Thermocarb TC-300 Synthetic Graphite Formulations .............................. 139 Table A.3b: Thermocarb TC-300 Synthetic Graphite Formulations .............................. 140 Table A.4a: Hyperion Fibril Carbon Nanotube Formulations ........................................ 141 Table A.4b: Hyperion Fibril Carbon Nanotube Formulations ........................................ 142 Table A.5: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite Combinations .............................................................................. 143 Table A.6: Ketjenblack EC-600 JD Carbon Black/Hyperion Fibril Carbon Nanotube Combinations ............................................................................................. 144 Table A.7: Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations ............................................................................................. 145 Table A.8: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations ...................... 146 Table B.1: Ketjenblack EC-600 JD Carbon Black Formulations ................................... 147 Table B.2a: Thermocarb TC-300 Synthetic Graphite Formulations .............................. 148 Table B.2b: Thermocarb TC-300 Synthetic Graphite Formulations .............................. 149 Table B.3a: Hyperion Fibril Carbon Nanotube Formulations ........................................ 150 Table B.3b: Hyperion Fibril Carbon Nanotube Formulations ........................................ 151 Table B.4: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite Combinations .............................................................................. 152 Table B.5: Ketjenblack EC-600 JD Carbon Black/Hyperion Fibril Carbon Nanotube Combinations ............................................................................................. 153 Table B.6: Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations ............................................................................................. 154 Table B.7:Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations ...................... 155 Table C.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN .......... 156 Table C.2:Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................................... 156 Table C.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 157 Table C.4: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 157 xi Table C.5: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 158 Table C.6: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 158 Table C.7: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 159 Table C.8: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 159 Table C.9: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 160 Table C.10: 1.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 161 Table C.11: 2.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 161 Table C.12: 4 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 162 Table C.13: 5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 162 Table C.14: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 164 Table C.15: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 165 Table C.16: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 166 Table C.17: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 167 Table C.18: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 168 Table C.19: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 169 Table C.20: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 170 Table C.21: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 171 Table C.22: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 172 Table C.23: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 173 Table C.24: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 174 Table C.25: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 175 Table C.26: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 176 xii Table C.27: 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 178 Table C.28: 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 179 Table C.29: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 180 Table C.30: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 181 Table C.31: 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 182 Table C.32: 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 183 Table C.33: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ... 184 Table C.34: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 185 Table C.35: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 186 Table C.36: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 187 Table C.37: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 188 Table C.38a: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 189 Table C.38b: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 190 Table C.39: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN .......................................................... 191 Table C.40: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 192 Table C.41a: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded ....................... 193 Table C.41b: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded ........................ 194 Table D.1: Poco Reference June 23, 2008 ...................................................................... 195 xiii Table D.2: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results ................................. 195 Table D.3: EA4P Disk 10 Results .................................................................................. 196 Table D.4: EA4P Disk 5 Results .................................................................................... 196 Table D.5: EA4P Disk 25 Results .................................................................................. 197 Table D.6: EA4P Disk 6 Results .................................................................................... 197 Table D.7: Overall Results for 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 198 Table D.8: Poco Reference June 23, 2008 ...................................................................... 199 Table D.9: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results ................................. 199 Table D.10: EA5P Disk 23 Results ................................................................................ 200 Table D.11: EA5P Disk 5 Results .................................................................................. 200 Table D.12: EA5P Disk 6 Results .................................................................................. 201 Table D.13: EA5P Disk 13 Results ................................................................................ 201 Table D.14: Overall Results for 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 202 Table D.15: Poco Reference 6-23-08.............................................................................. 203 Table D.16: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 22 Results ................................. 203 Table D.17: EA6P Disk 8 Results .................................................................................. 204 Table D.18: EA6P Disk 33 Results ................................................................................ 204 Table D.19: EA6P Disk 23 Results ................................................................................ 205 Table D.20: EA6P Disk 12 Results ................................................................................ 205 Table D.21: Overall Results for 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 206 Table D.22: Poco Reference 6-25-08.............................................................................. 207 Table D.23: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 8 Results ................................... 207 Table D.24: EA7.5P Disk 27 Results ............................................................................. 208 Table D.25: EA7.5P Disk 26 Results ............................................................................. 208 Table D.26: EA7.5P Disk 6 Results ............................................................................... 209 Table D.27: EA7.5P Disk 5 Results ............................................................................... 209 Table D.28: Overall Results for 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 210 Table D.29: Poco Reference 6/26/08 .............................................................................. 211 Table D.30: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 20 Results ................................. 211 Table D.31: EB65P Disk 30 Results ............................................................................... 212 Table D.32: EB65P Disk 6 Results ................................................................................. 212 Table D.33: EB65P Disk 19 Results ............................................................................... 213 Table D.34: EB65P Disk 21 Results ............................................................................... 213 Table D.35: Poco Reference 6/27/08 .............................................................................. 214 Table D.36: EB65P Disk 7 Results ................................................................................. 214 xiv Table D.37: Overall Results for 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 215 Table D.38: Poco Reference 6/26/08 .............................................................................. 216 Table D.39: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 24 Results ................. 216 Table D.40: EB65PR Disk 30 Results ............................................................................ 217 Table D.41: EB65PR Disk 23 Results ............................................................................ 217 Table D.42: EB65PR Disk 13 Results ............................................................................ 218 Table D.43: EB65PR Disk 19 Results ............................................................................ 218 Table D.44: Overall Results for 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate......................... 219 Table D.45: Poco Reference 6/26/08 .............................................................................. 220 Table D.46: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 7 Results ................................... 220 Table D.47: EB70P Disk 6 Results ................................................................................. 221 Table D.48: EB70P Disk 18 Results ............................................................................... 221 Table D.49: EB70P Disk 15 Results ............................................................................... 222 Table D.50: EB70P Disk 30 Results ............................................................................... 222 Table D.51: Overall Results for 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 223 Table D.52: Poco Reference 6/26/08 .............................................................................. 224 Table D.53: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 19 Results ................................. 224 Table D.54: EB75P Disk 8 Results ................................................................................. 225 Table D.55: EB75P Disk 14 Results ............................................................................... 225 Table D.56: EB75P Disk 15 Results ............................................................................... 226 Table D.57: EB75P Disk 18 Results ............................................................................... 226 Table D.58: Poco Reference 7/1/08 ................................................................................ 227 Table D.59: EB75P Disk 7 Results ................................................................................. 227 Table D.60: EB75P Disk 25 Results ............................................................................... 228 Table D.61: EB75P Disk 14 Results ............................................................................... 228 Table D.62: Overall Results for 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 229 Table D.63: Poco Reference 7/2/08 ............................................................................... 230 Table D.64: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 15 Results ................................. 230 Table D.65: EB80P Disk 18 Results ............................................................................... 231 Table D.66: EB80P Disk 24 Results ............................................................................... 231 Table D.67: EB80P Disk 12 Results ............................................................................... 232 Table D.68: EB80P Disk 30 Results ............................................................................... 232 Table D.69: Overall Results for 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ......................................... 233 Table D.70: Poco Reference 6/30/08 .............................................................................. 234 xv Table D.71: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 19 Results ................................. 234 Table D.72: EQ7.5P Disk 32 Results ............................................................................. 235 Table D.73: Poco Reference 7/11/08 .............................................................................. 235 Table D.74: EQ7.5P Disk 20 Results ............................................................................. 236 Table D.75: EQ7.5P Disk 24 Results ............................................................................. 236 Table D.76: EQ7.5P Disk 13 Results ............................................................................. 237 Table D.77: EQ7.5P Disk 17 Results ............................................................................. 237 Table D.78: EQ7.5P Disk 15 Results ............................................................................. 238 Table D.79: EQ7.5P Disk 12 Results ............................................................................. 238 Table D.80: Overall Results for 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 239 Table D.81: Poco Reference 6/30/08 .............................................................................. 240 Table D.82: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 29 Results ................. 240 Table D.83: EQ7.5PR Disk 6 Results ............................................................................. 241 Table D.84: EQ7.5PR Disk 17 Results ........................................................................... 241 Table D.85: Poco Reference 7/11/08 .............................................................................. 242 Table D.86: EQ7.5PR Disk 22 Results ........................................................................... 242 Table D.87: EQ7.5PR Disk 17 Results ........................................................................... 243 Table D.88: EQ7.5PR Disk 32 Results ........................................................................... 243 Table D.89: EQ7.5PR Disk 27 Results ........................................................................... 244 Table D.90: EQ7.5PR Disk 24 Results ........................................................................... 244 Table D.91: Overall Results for 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 245 Table D.92: Poco Reference 7/1/08 ................................................................................ 246 Table D.93: 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 11 Results ................................. 246 Table D.94: EQ10P Disk 12 Results .............................................................................. 247 Table D.95: EQ10P Disk 18 Results .............................................................................. 247 Table D.96: EQ10P Disk 24 Results .............................................................................. 248 Table D.97: EQ10P Disk 16 Results .............................................................................. 248 Table D.98: EQ10P Disk 23 Results .............................................................................. 249 Table D.99: Overall Results for 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 249 Table D.100: Poco Reference 6/26/08 ............................................................................ 250 Table D.101: 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 32 Results ................................. 250 Table D.102: EQ15P Disk 34 Results ............................................................................ 251 Table D.103: EQ15P Disk 23 Results ............................................................................ 251 Table D.104: EQ15P Disk 29 Results ............................................................................ 252 Table D.105: EQ15P Disk 19 Results ............................................................................ 252 xvi Table D.106: Overall Results for 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 253 Table D.107: Poco Reference 6/27/08 ............................................................................ 254 Table D.108: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 15 Results ........................................................................................................ 254 Table D.109: EA2.5B65P Disk 31 Results ..................................................................... 255 Table D.110: EA2.5B65P Disk 36 Results ..................................................................... 255 Table D.111: EA2.5B65P Disk 30 Results ..................................................................... 256 Table D.112: EA2.5B65P Disk 17 Results ..................................................................... 256 Table D.113: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN.................................................................................... 257 Table D.114: Poco Reference 6/27/08 ............................................................................ 258 Table D.115: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 10 Results .......................................................................... 258 Table D.116: Poco Reference 6/26/08 ............................................................................ 259 Table D.117: EA2.5B65PR Disk 7 Results .................................................................... 259 Table D.118: EA2.5B65PR Disk 17 Results .................................................................. 260 Table D.119: EA2.5B65PR Disk 30 Results .................................................................. 260 Table D.120: EA2.5B65PR Disk 19 Results .................................................................. 261 Table D.121: EA2.5B65PR Disk 16 Results .................................................................. 261 Table D.122: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate.................................................................... 262 Table D.123: Poco Reference 7/3/08 .............................................................................. 263 Table D.124: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Disk 29 Results............................................................................... 263 Table D.125: EA2.5Q6P Disk 17 Results....................................................................... 264 Table D.126: EA2.5Q6P Disk 32 Results....................................................................... 264 Table D.127: EA2.5Q6P Disk 39 Results....................................................................... 265 Table D.128: EA2.5Q6P Disk 34 Results....................................................................... 265 Table D.129: EA2.5Q6P Disk 26 Results....................................................................... 266 Table D.130: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN.................................................................................... 266 Table D.131: Poco Reference 7/7/08 .............................................................................. 267 Table D.132: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Replicate Disk 20 Results................................................................ 267 Table D.133: EA2.5Q6PR Disk 27 Results .................................................................... 268 Table D.134: EA2.5Q6PR Disk 31 Results .................................................................... 268 xvii Table D.135: EA2.5Q6PR Disk 22 Results .................................................................... 269 Table D.136: EA2.5Q6PR Disk 18 Results .................................................................... 269 Table D.137: EA2.5Q6PR Disk 26 Results .................................................................... 270 Table D.138: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate.................................................................... 270 Table D.139: Poco Reference 7/7/08 .............................................................................. 271 Table D.140: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results ........................................................................................................ 271 Table D.141: EB65Q6P Disk 16 Results ........................................................................ 272 Table D.142: EB65Q6P Disk 17 Results ........................................................................ 272 Table D.143: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN.................................................................................... 273 Table D.144: Dana Corporation Poco Reference 7/18/08 .............................................. 274 Table D.145: Dana Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 16 ...................................................................... 274 Table D.146: Dana Results for EB65Q6P Disk 17 ......................................................... 275 Table D.147: Dana Results for EB65Q6P Disk 18 ......................................................... 275 Table D.148: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN from Dana Corporation ............................................. 276 Table D.149: Poco Reference 7/8/08 .............................................................................. 277 Table D.150: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 25 Results .......................................................................... 277 Table D.151: EB65Q6PR Disk 15 Results ..................................................................... 278 Table D.152: EB65Q6PR Disk 38 Results ..................................................................... 278 Table D.153: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate.................................................................... 279 Table D.154: Poco Reference 7/7/08 .............................................................................. 280 Table D.155: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Disk 40 Results .... 280 Table D.156: Poco Reference 7/21/08 ............................................................................ 281 Table D.157: EA2.5B65Q6P Disk 25 Results ................................................................ 281 Table D.158: EA2.5B65Q6P Disk 46 Results ................................................................ 282 Table D.159: EA2.5B65Q6P Disk 43 Results ................................................................ 282 Table D.160: EA2.5B65Q6P Disk 16 Results ................................................................ 283 xviii Table D.161: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded ... 283 Table D.162: Dana Corporation Poco Reference 7/18/08 .............................................. 284 Table D.163: Dana Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Disk 14................................................................................................................ 284 Table D.164: Dana Results for EA2.5B65Q6P Injection Molded Disk 36 .................... 285 Table D.165: Dana Results for EA2.5B65Q6P Injection Molded Disk 57 .................... 285 Table D.166: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded from Dana Corporation ....................................................................................... 286 Table D.167: Poco Reference 7/8/08 .............................................................................. 287 Table D.168: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded Disk 47 Results ........................................................................................................ 287 Table D.169: EA2.5B65Q6PR Disk 16 Results ............................................................. 288 Table D.170: EA2.5B65Q6PR Disk 41 Results ............................................................. 288 Table D.171: EA2.5B65Q6PR Disk 12 Results ............................................................. 289 Table D.172: EA2.5B65Q6PR Disk 19 Results ............................................................. 289 Table D.173: EA2.5B65Q6PR Disk 22 Results ............................................................. 290 Table D.174: EA2.5B65Q6PR Disk 41 Results ............................................................. 290 Table D.175: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded ....................................................................................................... 291 Table D.176: Poco Reference 7/21/08 ............................................................................ 292 Table D.177: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Disk 8C Results .................................................................................................................... 292 Table D.178: Poco Reference 7/9/08 .............................................................................. 293 Table D.179: EA2.5B65Q6P Disk 1C Results ............................................................... 293 Table D.180: EA2.5B65Q6P Disk 3C Results ............................................................... 294 Table D.181: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded .................................................................................................................... 294 Table D.182: Dana Corporation Poco Reference 7/18/08 .............................................. 295 Table D.183: Dana Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene xix Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Disk 1C ...................................................................................................... 295 Table D.184: Dana Results for EA2.5B65Q6P Disk 2C ................................................ 296 Table D.185: Dana Results for EA2.5B65Q6P Disk 3C ................................................ 296 Table D.186: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded from Dana Corporation .............................................................................. 297 Table E.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN........... 298 Table E.2: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN........... 298 Table E.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 299 Table E.4: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 299 Table E.5: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 300 Table E.6: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 300 Table E.7: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 301 Table E.8: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 301 Table E.9: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 301 Table E.10: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 302 Table E.11: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 303 Table E.12: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 303 Table E.13: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 304 Table E.14: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 304 Table E.15: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 305 Table E.16: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 305 Table E.17: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 306 Table E.18: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 306 Table E.19: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 307 xx Table E.20: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 307 Table E.21: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 308 Table E.22: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 308 Table E.23: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 309 Table E.24: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 309 Table E.25: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 310 Table E.26: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 310 Table E.27: 1.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 311 Table E.28: 2.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 311 Table E.29: 4 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 312 Table E.30: 5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 312 Table E.31: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 313 Table E.32: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 313 Table E.33: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 314 Table E.34: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 314 Table E.35: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 315 Table E.36: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 315 Table E.37: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 316 Table E.38: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 316 Table E.39: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ... 317 Table E.40: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 317 xxi Table E.41: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 318 Table E.42: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 318 Table E.43: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded ............................... 319 Table E.44: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded............... 319 Table E.45: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded ........................ 320 Table F.1: Density and Specific Heat Values for Each Component Used [1] ................ 321 Table F.2: Theoretical Specific Heat, Density, and Volumetric Specific Heat for Thermocarb TC-300 Synthetic Graphite, Ketjenblack EC-600 JD Carbon Black, and Hyperion FIBRILTM Nanotubes Formulations ........................ 323 Table F.3: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........... 324 Table F.4: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 325 Table F.5: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 326 Table F.6: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 326 Table F.7: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 327 Table F.8: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 327 Table F.9: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 327 Table G.1: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 329 Table G.2: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 329 Table G.3: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 330 Table G.4: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 330 Table G.5: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 331 Table G.6: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 331 xxii Table G.7: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 332 Table G.8: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 332 Table G.9: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 333 Table G.10: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 333 Table G.11: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 334 Table G.12: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 334 Table G.13: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 335 Table G.14: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 335 Table G.15: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded ............................... 336 Table G.16: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded ........................ 336 Table H.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN .......... 337 Table H.2: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 338 Table H.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 338 Table H.4: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 339 Table H.5: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 339 Table H.6: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 340 Table H.7: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 340 Table H.8: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 341 Table H.9: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 341 Table H.10: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 342 Table H.11: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 342 xxiii Table H.12: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 342 Table H.13: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 343 Table H.14: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 343 Table H.15: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 343 Table H.16: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 344 Table H.17: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 344 Table H.19: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 345 Table H.20: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 345 Table H.21: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 346 Table H.221: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 346 Table H.23: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 347 Table H.24: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 347 Table H.25: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 347 Table H.26: 1.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 348 Table H.27: 2.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 348 Table H.28: 4 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 349 Table H.29: 5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 349 Table H.30: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 349 Table H.31: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 350 Table H.32: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 350 Table H.33: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 350 Table H.34: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 351 xxiv Table H.35: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 351 Table H.36: 20 wt% Hyperion FIBRILTM nanotubes in Polypropylene Masterbatch MB3020-01 ................................................................................................ 351 Table H.37: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 352 Table H.38: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 352 Table H.39: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ... 352 Table H.40: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 353 Table H.41: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 353 Table H.42: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate .................................................................................................... 353 Table H.43: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ........................................................... 354 Table H.44: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate ........................................... 354 Table I.1: Solvent Digestion Results for 25 wt% and 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN ....... 355 Table J.1: Filler Length and Aspect Ratio Results for Single Filler Thermocarb TC-300 Formulations .............................................................................................. 356 Table K.1: Orientation Results – Single Filler Thermocarb TC-300 Formulations and Three Filler Formulation ............................................................................ 357 xxv xxvi Nomenclature A ASample Cp Cpc Cpi c D ER ERpoco ERsample i K k kc kin kthru L l m mi P p Q Qr q R RCircuit RContact RMeasured RPOCO RSample Rn Rno r' T t u V w wcomposite wfilter Area (cm2) Area of sample (cm2) Heat capacity (J/kg·K) Heat capacity of individual formulation (J/kg·K) Heat capacity of individual component (J/kg·K) Volumetric heat capacity (J/m3·K) Sample diameter (cm) Electrical resistivity (ohm-cm) Electrical resistivity of POCO graphite (mΩ-cm) Electrical resistivity of sample (mΩ-cm) Current (A) Thermal conductivity of composite (W/m·K) Thermal conductivity (W/m·K) Thermal conductivity of composite (W/m·K) In-plane thermal conductivity (W/m·K) Through-plane thermal conductivity (W/m·K) Length over which change in volts measured (cm) Ring number Number of rings Mass of component (kg) Power (W) Mean free path (m) Total power (W) Power per unit length (W/m) Heat flux (W/m2) Radius of outermost ring source (m) Circuit resistance (mΩ) Contact resistance (mΩ) Resistance measured by the test (mΩ) Resistance of POCO graphite (mΩ) Resistance of test sample (mΩ) Resistance at time n (Ω) Resistance at time 0 (Ω) Radius of sensor ‘ring’ (m) Temperature (K) Time (s) Velocity of molecules (m/s) Voltage (V) Sample width (cm) Original composite sample weight (g) Filter paper weight (g) xxvii wfinal wPetridish x xpoco xi yi Final weight (g) Petri dish weight (g) Sample thickness (cm) Poco thickness (cm) Particle count parameter Particle count parameter α β ∆T δ δΤ/δxi φi ρ ρι ρtheo ρfluid σ τ Θ Thermal diffusivity (m2/s) Temperature coefficient of resistance (1/K) Change in temperature (K) Dirac delta function Temperature gradient (K/m) Weight fraction of component Density (kg/m3) Density of component (g/cm3) Theoretical density of composite (g/cm3) Density of fluid (g/cm3) Integration variable Hot Disk equation parameter Moment angle xxviii Chapter 1: Introduction 1.1: Introduction Most polymer resins are thermally and electrically insulating. Increasing the thermal and electrical conductivity of these resins allows them to be used in other applications. Over the past 20 year thermoplastics have been replacing metal parts in many different applications [1]. Thermoplastics have high impact resistance, are non corrosive, are lighter, and are often more cost effective than metals [2]. Thermoplastics can be tailored for specific applications and properties depending on what resin and additives are used in the material. One example for using conductive thermoplastics is in computer chips, where thousands of circuits are placed onto one chip. The conductive thermoplastic resin can be used to help protect the circuits on the chip from electrostatic discharge and from overheating [1-2]. Typical thermal conductivity values (W/m•K) are listed in Table 1.1-1 [1] and electrical conductivity values (S-cm) are listed in Table 1.1-2 [2] for some common materials. One way to increase the thermal and electrical conductivity of thermoplastics is to add fillers to the polymer resin. There are three main categories of fillers; carbon (carbon black, carbon nanotubes, graphite, or carbon fibers), ceramics (aluminum boride, aluminum nitride, boron nitride), and metals (copper flakes and fibers, silver flakes, stainless steel fibers, aluminum fibers, flakes, and powder); that are added to thermoplastics to increase the conductivity of the material [1-16]. 1 Table 1.1-1: Thermal Conductivity for Common Materials [1] Materials Thermal Conductivity (W/m·K) 0.2 to 0.3 400 225 60 105 45 Polymers Copper Aluminum (extruded) Aluminum (cast) Brass Steel Table 1.1-2: Electrical Conductivity for Common Materials [2] Materials Electrical Conductivity (S-cm) 10-7 to 10-14 5.9 x 105 6.3 x 105 3.6 x 105 1.5 x 105 300 Polymers Copper Silver Aluminum Nickel Carbon (amphorous) 1.2: Motivation One emerging market for thermally conductive resins is for bipolar plates for use in Proton Exchange Membrane (PEM) fuel cells. The proton membrane fuel cell is one of the most promising fuel cells being looked at for uses in transportation, distributed power, and portable electrical devices [17]. The PEM fuel cell creates DC electricity from the reaction between hydrogen and oxygen, which can be used to power a motor. The byproducts produced from a PEM fuel cell is water and heat, which is much more 2 environmentally friendly compared to byproducts produced from the standard internal combustion engine [17-19]. Currently, the cost of a PEM fuel cell is the limiting factor for fuel cells being used in automobiles. So many researchers are trying to develop new materials that are less expensive to reduce the fuel cell costs. The bipolar plates used in a PEM fuel cell account for approximately 80% of the total weight and 45% of the total cost [20]. The bipolar plates are used to distribute the oxygen to the cathode and the hydrogen to the anode, remove water and heat from the reaction, provide electrical contact between the plates to carry the current from cell to cell, and to keep the reactants separated [17,20]. To meet all of these functions bipolar plates need to be thermal and electrically conductive, be made of a gas impermeable material, need to be resistant to corrosion in acidic conditions, and need to have high structural strength [18, 21-22]. Bipolar plates also need to be light weight and need to be produced using low cost materials and manufacturing techniques [21, 22]. Traditional bipolar plates have been made from metal alloys and graphite. More recently researchers have been looking into conductive composites because they are lighter, cheaper, and easier to manufacture [17, 22]. Because of this trend in bipolar plate research, this project’s focuses will be on adding different carbon fillers to a thermoplastic matrix in order to obtain high electrical and thermal conductivities, as well to reduce the volume and the weight of a fuel cell. Table 1.1-3 shows some of the properties desired for bipolar plates used in PEM Fuel Cells. 3 Along with these properties, bipolar plates need have to have good thermal and dimensional stability at the typical fuel cell operating temperature of 80ºC [19, 25-26]. Table 1.1-3: Desired Bipolar Plate Properties [23-24] Property Cost Weight Thermal Conductivity Electrical Conductivity Hydrogen Permeation Rate Flexural Strength Corrosion Resistance Units $/kW kg/kW W/m·K S/cm cm3/sec·cm2 MPa µA/cm2 Target 5 < 0.4 > 20 > 100 < 2 x 10-6 > 25 <1 1.3: Objectives The goal of this M.S. research was to determine the effects and interactions of the carbon fillers on a composite’s electrical and thermal conductivity. These composite formulations could then potentially be used in bipolar plates for fuel cells. This project will involve fabricating the carbon/polymer composites, performing thermal and electrical conductivity tests, and analyzing the data to determine the effect and interaction of the fillers. Often, bipolar plates are being produced using a single type of graphite powder in a thermosetting resin (often a vinyl ester) [27-30]. Carbon filled thermoplastic resins (i.e., polypropylene, liquid crystalline polymer, polyphenylene sulfide, polyethylene, etc.) are currently being considered for fuel cell bipolar plates because the polymer can be remelted [20, 31-34]. In this research a thermoplastic resin (polypropylene) was used as the polymer matrix and the three carbon fillers investigated were synthetic graphite, carbon black, and carbon nanotubes. Other work has been done 4 in thermoplastic resins using some of the same fillers [35-37], so it may be possible to develop a new material for bipolar plates that can meet the desired bipolar plate properties (see Table 1.1-2). 1.4: References 1. J. M. Finan, Proceedings of the Society of Plastics Engineers Annual Technical Conference, May 2-6 1999, 1547-1550. 2. W.M. Wright, G.W. Woodham, Conductive Polymers and Plastics, J.M. Margolis (Ed), Chapman and Hall, New York, NY, 1989, 118-174. 3. Taipalus, T. Harmia, M. Q. Zhang, and K. Friedrich, Composite Science and Technology, 61, 801-814 (2001). 4. Y. Agari and T. Uno, Journal of Applied Polymer Science, 30, 2225-2236 (1985). 5. D. M. Bigg, Polymer Engineering and Science, 17, 842-847 (1977). 6. D. M. Bigg, Advanced Polymer Technology., 4, 255-266 (1984). 7. M. Narkis, G. Lidor, A. Vaxman, and L. Zuri, Journal of Electrostatics, 47, 201214 (1999). 8. K. Nagata, H. Iwabuki, and H. Nigo, Composite Interfaces, 6, 483-495 (1999). 9. A. Demain, “Thermal Conductivity of Polymer-Chopped Carbon Fibre Composites”, Ph.D. Dissertation, Universite Catholique de Louvain, Louvain- la-Neuve, Belgium (1994). 5 10. J. A. King, K. W. Tucker, J. D. Meyers, E. H. Weber, M. L. Clingerman, and K. R. Ambrosius, Polymer Composites., 22, 142-154 (2001). 11. M. V. Murthy, Proceedings of the Society of Plastics Engineers Annual Technical Conference, 1396-1400 (1994). 12. R.M. Simon, Polymer News, 11, 102-108 (1985). 13. P. Mapleston, Modern Plastics, 69, 80-83 (1992). 14. J.-B. Donnet, R. C. Bansal, and M.-J. Wang, Carbon Black, 2nd edition, Marcel Dekker, Inc, New York, 1993. 15. J.-C. Huang, Advanced Polymer Technology, 21, 299-313 (2002). 16. D. M. Bigg, Polymer Composites, 8, 1-7 (1987). 17. D.G. Baird, J. Huang, and J.E. McGrath, Plastics Engineering, 59, 46-55 (2003). 18. S. Thomas and M. Zalbowitz, Fuel Cells: Green Power, Los Alamos National Laboratory, LA-UR-99-3231, 1999. 19. L.E. Nunnery, Jr., Fuel Cell Technology, Society of Automotive Engineers (SAE) Conference, 1998. 20. A. Hermann, T. Chaudhuri, and P. Spagnol, International Journal of Hydrogen Energy, 30, 1297-1302 (2005). 21. G.O. Mepsted, and J.M. Moore, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, 6 W. Vielstick, H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003,286-293. 22. M.J. Ajersch, M.W. Fowler, K. Karan, B.A. Peppley, Fuel Cell Science, Engineering and Technology, Rochester, NY, April 2003: 253-260. 23. “2007 Technical Plan-Fuel Cells” United States Department of Energy, MultiYear Research, Development, and Demonstration Plan http://www1.eere.energy.gov/hydrogenandfuelcells/mypp/pdfs/fuel_cells.pdf (accessed November 2008). 24. J. Larminie, and A. Dicks, Fuel Cell Systems Explained, 2nd Edition, John Wiley & Sons, West Sussex, England, 2003, 1-119. 25. R. Leaversuch, “Fuel Cells Jolt Plastics Innovation”, Plastics Technology Online, November 2001, www.plasticstechnology.com/articles/200111fa2.html., accessed December 23, 2003. 26. N. Garland, “Materials for Bipolar www.eere.energy.gov/hydrogenandfuelcells /pdfs/nn0123s.pdf, Plates”, Department of Energy sponsored research presented May 9-10, 2002 in Golden, CO, accessed January 15, 2004. 27. M. S. Wilson and D. N. Busick, U.S. Patent Number 6,248,467: “Composite Bipolar Plate for Electrochemical Cells”, June 19, 2001. 28. R. O. Loutfy and M. Hecht, U.S. Patent Number 6,511,766: “Low Cost Molded Plastic Fuel Cell Separator Plate with Conductive Elements”, January 28, 2003. 7 29. J. C. Braun, J. E. Zabriskie, Jr., J. K. Neutzler, M. Fuchs, and R. C. Gustafson, U. S. Patent Number 6,180,275: “Fuel Cell Collector Plate and Method of Fabrication”, January 30, 2001. 30. V. Mehta and J. S. Cooper, Journal of Power Sources, 114, 32-53 (2003). 31. F. Migri, M. A. Huneault, and M. F. Champagne, Polymer Engineering Science, 44, 1755-1765 (2004). 32. J. Huang, D. G. Baird, and J. E. McGrath, Journal of Power Sources, 150, 110119 (2005). 33. H. Wolf, and M. Willert-Porada, Journal of Power Sources, 153, 41-46 (2006). 34. K. Robberg and V. Trapp, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, W. Vielstick, H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003, 308-314. 35. J. A. Heiser, J. A. King, J. P. Konell, I. Miskioglu, and L. L. Sutter, Advances in Polymer Technology, 23, 135-146 (2004). 36. J. A. King, R. L. Barton, R. A. Hauser, and J. M. Keith, Polymer Composites, 29, 421-428 (2008). 37. R. A. Hauser, J. A. King, R. M. Pagel, and J. M. Keith, Journal of Applied Polymer Science, 109, 2145-2155 (2008). 8 Chapter 2: Background 2.1: Fuel Cells The concept of fuel cells was first invented by William Grove, a lawyer/scientist in 1839. He set up a simple experiment where first an electric current is passed through water in order to electrolyze the water into hydrogen and oxygen. Once the hydrogen and oxygen are separated then the power source was replaced with an ammeter. This ammeter showed a current which means that the hydrogen and water were recombining to form water, thus reversing the electrolysis [1]. In a fuel cell, hydrogen gas is combined with oxygen to form water in the reaction is shown below. 2H2 + O2 → 2H2O There are six different types of fuel cells that have emerged as viable systems for the present and in the future. Usually each fuel cell type is distinguished by the electrode used with some other important differences used to classify them. Each fuel cell type runs best at different temperatures and is suited for specific applications. Proton exchange membrane fuel cells will be discussed further in later sections, because the research was conducted on materials that can be used in one component of the PEM fuel cell. 9 Table 2.1-1: Summary of the Different Types of Fuel Cells [1] Fuel Cell Type Mobile Ion Proton Exchange Membrane (PEMFC) Alkaline (AFC) H+ Operating Temperature 30 – 100ºC OH- 50 – 200ºC Direct Methanol (DMFC) H+ 20 – 90ºC Phosphoric Acid (PAFC) Molten Carbonate (MCFC) H+ ~220ºC CO32- ~650ºC O2- 500 – 1000ºC Solid Oxide (SOFC) Applications Vehicles and mobile applications and low power CHP* systems. Used in space vehicles, e.g. Apollo, Shuttle Suitable for portable electronic systems of low power, running for long times. Large number of 200kW CHP systems in use. Suitable for medium- to large-scale CHP systems, up to MW capacity. Suitable for all sizes of CHP systems, 2kW to multi-MW. *CHP – Combined Heat and Power 2.1.1: Proton Exchange Membrane Fuel Cells Proton exchange membrane (PEM) fuel cell, also known as solid polymer fuel cells (SPFC), were first invented by General Electric in the 1960’s to be used by NASA in the first manned space vehicle [1]. PEM fuel cells have shown the most promise as a versatile, portable, and environmentally friendly alternative fuel technology, especially in the transportation sector [2]. This is because they can operate at low temperatures and be configured to provide different combinations of voltage and current depending on the application [3]. In a PEM fuel cell hydrogen (fuel) reacts with oxygen to create DC 10 electricity, which can be used to power a motor. The byproducts produced from a PEM fuel cell is water and heat and they have no emissions while idling. They are also very simple and quiet because there are no moving parts. PEM fuel cells are also more efficient compared to an internal combustion engine [1, 3-5]. A schematic of a PEM fuel cell is shown in Figure 2-1.1 [6] (Permission letter shown in Appendix M). There are three main components of a fuel cell: the proton exchange membrane/electrode assembly, the bipolar plates, and the gas diffusion layer (discussed in more detail in later sections). In a fuel cell, hydrogen flows into the anode side, where it comes in contact with a platinum catalyst that helps the hydrogen separate into protons and electrons. Once the hydrogen is ionized, the protons go through the proton exchange membrane and the electrons go through an external circuit, creating the electricity needed to power a motor. Once the protons are in the proton exchange membrane, they react with oxygen that is coming in on the cathode side of the fuel cells and electrons, from the external circuit, to form water. To help the reaction in the proton exchange membrane a platinum catalyst is used. From each cell typically 0.7 volts is produced, so to get the power necessary to run a motor hundreds of fuel cells are stacked together. For example, a car motor will need 430 fuel cells stacked together to achieve 300 volts required to run the motor [4-5]. 11 Figure 2.1-1: Proton Exchange Membrane Fuel Cell Schematic (Reproduced with permission from Rebecca Hauser, Permission letter shown in Appendix M) 2.1.1.1: Proton Exchange Membrane/Catalyst Assembly The proton exchange membrane is made from a solid organic polymer usually a poly(perflourosulfonic) acid. A proton exchange membrane consists of three different regions: 1. A Teflon-like, fluorocarbon backbone consisting of hundreds of repeating –CF2-CF-CF2- units in length 2. Side chains consisting of –O- CF2-CF-O-CF2 -CF2- that connect the first region to the third region 3. Ion clusters consisting of sulfonic acid ions, SO3-, H+ In the membrane structure, when water is absorbed, the SO3- become attached permanently to the side chain and is unable to move. Instead only the positive, hydrogen ions, are free to move around inside the membrane between different SO3- locations. Thus, making a solid hydrated membrane that is an excellent conductor of hydrogen ions. 12 These hydrogen ions can only move in one direction through the membrane, anode to cathode, and this movement is essential to the operation of a fuel cell. While proton exchange membranes do conduct protons they do not conduct electrons. So since the electrons cannot pass through the membrane, in order for them to reach the other side of the fuel cell they need to go through an external wire. This movement of electrons through the external wire is what creates the electricity necessary to run a motor [5]. In a fuel cell, there is an electrochemical reaction occurring with two separate half-reactions, an oxidation and reduction reaction. Because these half reactions usually happen very slowly at 80ºC, the normal operating temperature of a fuel cell, catalyst is used at the anode and cathode to increase the rate of the half reactions. The catalyst that is found to work best in fuel cells is platinum. The two platinum catalysts are located on both sides of the proton exchange membrane in a fuel cell [5]. The reduction half reaction is occurring at the cathode catalyst and the oxidation half reaction at the anode catalyst. In the oxidation half reaction, hydrogen gas separates into hydrogen ions and electrons with the help of the platinum catalyst. The hydrogen ions separated travel through the proton exchange membrane and the electrons go through an external wire to the cathode catalyst. In the reduction half reaction, oxygen is reduced with the help of the platinum before reacting with electrons and hydrogen ions to form heat and water. Both half reactions and the overall reaction are shown below [5]. 2H2 → 4H+ + 4e- Oxidation half reaction occurring at anode O2 + 4H+ + 4e- → 2H2O Reduction half reaction occurring at cathode 2H2 + O2 Overall cell reaction → 2H2O 13 2.1.1.2: Bipolar Plates Bipolar plates are a very important component of a fuel cell. They can account for 70-80% of the stack weight and up to 45% of the costs [7-8]. Bipolar plates have multiple functions in a fuel cell. They are used to distribute the oxygen to the cathode and the hydrogen to the anode, to manage water and heat from the reaction by removing them, provide electrical contact between the plates to carry the current from cell to cell, and to keep the reactants separated [4,7]. Bipolar plates also need to be made from lightweight, inexpensive materials that can be easily processed when producing bipolar plates [2, 9]. Materials for bipolar plates need meet certain property requirements. Table 2.1-2 shows some of the properties desired for bipolar plates used in PEM Fuel Cells. Along with these properties, bipolar plates need have to have good thermal and dimensional stability at the typical fuel cell operating temperature of 80ºC [3, 10-11]. Table 2.1.-2: Desired Bipolar Plate Properties [1, 12] Property Cost Weight Thermal Conductivity Electrical Conductivity Hydrogen Permeation Rate Flexural Strength Corrosion Resistance Units $/kW kg/kW W/m·K S/cm 3 cm /sec·cm2 MPa µA/cm2 Target 5 < 0.4 > 20 > 100 < 2 x 10-6 > 25 <1 Bipolar plates can be made from many different materials, such as graphite, metal, or polymer composites with carbon or metal conductive fillers. Graphite is one of the more traditional materials used to produce bipolar plates. The graphite bipolar plates 14 have very good thermal and electrical conductivity, excellent chemical compatibility, and are corrosion resistant. Some problems with graphite bipolar plates are the cost, from machining the gas flow channels into the plate and making the raw graphite, and that graphite has low mechanical strength properties [4,7]. Metal bipolar plates have very good electrical and thermal conductivity, good mechanical stability, and can be easily made. The main problem is they are not very resistant to corrosion in the acidic conditions of a fuel cell. Aluminum, titanium, and nickel bipolar plates need to be coated with a protective layer to resist corrosion. Stainless steel is the only metal that has been studied that has the chemical stability to resist corrosion [4, 7]. Polymer composites are made from both thermosetting (phenolics, vinyl esters, and epoxies) or thermoplastic (polypropylene, polyethylene) resins with different carbon and metals conductive fillers [4, 13]. They are then compression or injection molded to create bipolar plates with the gas flow channels, thus reducing the costs associated with machining and other processing steps [4]. Compression molding is the method of choice for the production of bipolar plates because it has better precision, produces better electrical and thermal conductivities, and is able to handle compounds with higher filler loadings. However, bipolar plate production may eventually shift to injection molding because it is one of the fastest and least expensive ways to produce plastics [10]. Currently, bipolar plates used commercially are produced from a polymer composite comprised of a thermosetting resin and a single type of graphite. Two companies, BMCI and Quantum, have developed bipolar plates made from polymer 15 composites with 70-90 wt% graphite in a vinyl ester [10]. However, many different carbon filled thermoplastic resins are currently being studied by researchers for use in fuel cell bipolar plates [7-8, 14-16]. When comparing the two types of resins there are some advantages to thermoplastic resins. One is that they can be re-melted and used in other applications, while thermosetting resins cannot be reused. A second advantage is thermoplastics have better chemical stability compared to thermosetting resins [14]. 2.1.1.3: The Backing Layers or Gas Diffusion Layers The backing layers or gas diffusion layers are in between the bipolar plate and the catalyst on both the anode and cathode side of a fuel cell. The backing layer needs to be made of a material that has good conduction of electrons, so they are usually made from porous carbon cloth or carbon paper that is 100 to 300 microns thick. The backing layer is porous to ensure that the hydrogen gas will spread out as the gas goes from higher concentrated areas to lower concentration areas, thus insuring that the gas makes contact with the entire surface of the catalyst [5]. The backing layer also helps to manage the amount of water that is in a fuel. The backing material needs to retain the enough water vapor to keep the proton exchange membrane humidified. But it also needs to allow water created at the cathode to leave the cell, thus reducing the risk of the fuel cell flooding. To keep the water from clogging the pores in the carbon cloth or paper and preventing gas diffusion, the backing layer material is often wet-proofed with Teflon [5]. 16 2.1.2: Thermal and Electrical Management in the Fuel Cell One anode-cathode cell with an area of 100 cm2 operating at 80ºC and 1 atm of pressure produces 0.7 volts, and generates 1.7 kJ/min of excess heat and 2.5 kJ/min of electric energy. Because of the electric and heat output the bipolar plates need to be made of materials that have good electrical conductivity to allow the conduction of electricity and good thermal conductivity to remove the excess heat. These desired properties (from Table 2.1-2) for thermal conductivity are greater than 20 W/m K and for electrical conductivity greater than 100 S/cm. 2.2: Thermal Conductivity Heat is described as a change in energy (temperature) between two substances or within a substance. There are three ways to transfer heat convection, radiation, and conduction [17]. In solids, the main mechanism for heat transfer is through conduction, which is described using Fourier’s Law shown in Equation 2.1 [18]. q = −k ∂T ∂x (2.1) In Equation 2.1, q is the heat flux (the heat flow per unit area in units of W/m2) which is dependent on the k the thermal conductivity (W/m•K) and the temperature gradient (K/m) [18]. The negative sign in Equation 2.1 comes from the fact that heat will always flow from a hotter to a colder region [19]. Heat is transported through a material using free electrons or phonons. In metals, the heat is transported primarily using free electrons. In non-metals, such as polymers, heat is transported using phonons [20]. 17 A phonon is a quanta of thermal vibrational energy. Phonons transport energy by interacting with electrons, protons, neutrons, and other phonons present in the material [17]. In a two dimensional diagram, the atoms of a crystalline structure can be represented using balls and springs, as shown in Figure 2.2-1. So when there is a vibration at one end of the structure, the energy is transmitted through the springs to the other side of the structure [6]. Figure 2.2-1: Two-Dimensional Array of Atoms in a Crystalline Structure Phonon interactions are a very efficient way of transporting heat through a material. The scattering of these phonons as they move through a material greatly decreases the amount of heat transferred, thus increasing the thermal resistance of the material [17]. Phonons can be scattered when there are changes in the arrangement or the size of the atoms in a crystalline structure. The amount of scattering depends on the distances between the defects in the crystal structure. If there is a large distance between the defects then the phonons will continue through the material and not be scattered, thus increasing the thermal conductivity. If the distance is short between the defects the 18 phonons will be scattered more frequently, causing a higher thermal resistance and a lower thermal conductivity [6, 20-21]. The Debye model, shown in Equation 2.2, illustrates how heat is conducted in materials using phonons [19]. 1 k = ⋅c ⋅u ⋅ p 3 (2.2) In Equation 2.2, k is the thermal conductivity (W/m•K), c is the volumetric heat capacity (J/m3•K), u is the velocity of the molecules (m/s), and p is the mean free path (m), which is the rate energy is exchanged between phonons [19, 20]. For the materials being used in this study, polymers and carbon fillers, heat is primarily transferred using phonons. The thermal conductivity for the carbon fillers, polymers, and composites will follow the Debye model. Many carbon fillers have an electrical conductivity that comes from the transportation of electrons like metals but, because of their crystalline structure their thermal conductivity is from phonon interactions [20-22]. The thermal conductivity of a material is a bulk property compared to electrical conductivity which is path selective [17]. Previous work with carbon filler and polymer composites has shown that the thermal conductivity will increase as the filler concentration increases, compared to the electrical conductivity which will increase rapidly at the percolation threshold and stay near this value as the amount of filler is increases. This shows that thermal conductivity is not dependent on the where the fillers are located and if they are in contact with other filler particles [23, 24]. 19 2.3: Electrical Conductivity The electrical conductivity of a composite is dependent on the amount of filler used in the composite and is given in units of S/cm. There are three stages of electrical conductivity, illustrated in Figure 2.3-1. At low filler concentrations the electrical conductivity is close to the electrical conductivity of the polymer used in the composite. Polymers usually have electrical conductivities of 10-14 to 10-17 S/cm, making them very electrically resistant. At a critical volume concentration, known as the percolation threshold, the electrical conductivity of the composite will increase rapidly with only a small change in the amount of filler. After the percolation threshold has been reached the electrical conductivity will flatten and approach the electrical conductivity of the fillers used in the composite. Carbon fillers usually have electrical conductivities in the range 102 to 105 S/cm. The percolation threshold is the point where there is enough filler in the composite to start forming conductive networks. These conductive networks form a continuous path that allows electricity to pass easily through a composite, thus increasing the electrical conductivity. The formation of conductive networks is known as percolation theory [22, 25]. 20 Figure 2.3-1: Dependence of Electrical Conductivity on Filler Volume Fraction Percolation theory has its origins in World War II, where Flory and Stockmayer used it to describe why smaller branching molecules form larger macromolecules. However, the start of percolation theory is attributed to Broadbent and Hammersley, who in a 1957 paper gave the theory a name and explained it using geometry and probablilty. Stauffer explains percolation theory using a large array of squares also known as a square lattice, shown in Figure 2.3-2A. Figure 2.3-2B shows a square lattice with some squares filled with large dots while others are left blank and Figure 2.3-2C shows clusters, which are a group of squares that all have dots in them. Percolation theory deals with how many clusters are in a lattice and the properties of these clusters. Throughout the lattice dots are randomly distributed, with each square having a probability (p) of obtaining a dot. When the probablility of a square being occupied is large enough, then there are enough dots to create a cluster that entends through the entire square lattice from top to 21 bottom and from left to right. This cluster is known to be percolating through the system [26]. Figure 2.3-2: Definition of Percolation Theory in a Square Lattice Stauffer then used the idea of a forest fire to explain percolation theory. Stauffer used a square lattice like Figure 2.3-2 to represent the forest. There is a probability of p if there is a tree in a square and a probability of (1-p) if the square is empty. The fire can only spread if there is a tree next to the one that is burning and the fire will be extinguished if there is not another tree. If the trees on the left side of square lattice are allowed to burn, we need to determine if the fire can spread to the right side of the lattice. When at the percolation threshold, there are enough neighboring trees that the fire will spread through the lattice from left to right igniting the entire forest [26]. The properties of the fillers used in the composite are a major factor when determining the electrical conductivity. Fillers can come in many different forms and each form can have a different electrical conductivity. One example is carbon, it can be in a small particle, fibers, or as a nanotube. Some typical electrical conductivities for 22 different carbon fillers are: carbon black 102 S/cm, graphite 105 S/cm, and pitch based carbon fibers 103 S/cm [27-29]. The properties of the fillers can also affect the electrical conductivity of a composite. The electrical conductivity can be affected by fillers particle size and the morphology. In one study it was found that decreasing the particle size also decreased the electrical conductivity of the composite when using flake or spherical graphite particles, so particle size does affect the electrical conductivity of a composite. This study also showed that spherical graphite increased the electrical conductivity of the composite compared to flake graphite [30]. In another study it was found that a larger aspect ratio (length to width ratio) reduces the critical volume concentration in a polymer composite, thus allowing the composite to reach the percolation threshold using less filler in the composite [31]. The filler properties allow researchers to predict the electrical conductivity of the polymer composites, but other factors can cause the actual electrical conductivity to be different than the predicted values. Filler particles with high aspect ratios tend to align in the direction of the flow when compression and injection molded. So polymer composites manufactured using these techniques have an increased electrical conductivity along the axis of alignment [32]. Another factor that can affect the electrical conductivity is how well the polymer bonds with the fillers surface. If there is poor bonding between the filler surface and the polymer then the filler distribution will be segregated in the polymer composite [33]. In one study by Mamunya, he found that if the surface tensions of the polymer and filler are lower than there is less interface tension and 23 the polymer is able to form a bond with the fillers surface, thus increasing the electrical conductivity [34]. 2.4: References 1. J. Larminie, and A. Dicks, Fuel Cell Systems Explained, 2nd Edition, John Wiley & Sons, West Sussex, England, 2003, 1-119. 2. M.J. Ajersch, M.W. Fowler, K. Karan, B.A. Peppley, Fuel Cell Science, Engineering and Technology, Rochester, NY, April 2003: 253-260. 3. L.E. Nunnery, Jr., Fuel Cell Technology, Society of Automotive Engineers (SAE) Conference, 1998. 4. D.G. Baird, J. Huang, and J.E. McGrath, Plastics Engineering, 59, 46-55 (2003). 5. S. Thomas and M. Zalbowitz, Fuel Cells: Green Power, Los Alamos National Laboratory, LA-UR-99-3231, 1999. 6. R. A. Hauser, “Synergistic Effects and Modeling of Thermally Conductive Resins for Fuel Cell Bipolar Plate Applications.” PhD Dissertation. Michigan Technological University: US, 2008. 7. A. Hermann, T. Chaudhuri, and P. Spagnol, International Journal of Hydrogen Energy, 30, 1297-1302 (2005). 8. H. Wolf and M. Willert-Porada, Journal of Power Sources, 153, 41-46 (2006). 9. G.O. Mepsted, and J.M. Moore, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, 24 W. Vielstick, H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003,286-293. 10. R. Leaversuch, “Fuel Cells Jolt Plastics Innovation”, Plastics Technology Online, November 2001, www.plasticstechnology.com/articles/200111fa2.html., accessed December 23, 2003. 11. N. Garland, “Materials for Bipolar www.eere.energy.gov/hydrogenandfuelcells /pdfs/nn0123s.pdf, Plates”, Department of Energy sponsored research presented May 9-10, 2002 in Golden, CO, accessed January 15, 2004. 12. “2007 Technical Plan-Fuel Cells” United States Department of Energy, MultiYear Research, Development, and Demonstration Plan http://www1.eere.energy.gov/hydrogenandfuelcells/mypp/pdfs/fuel_cells.pdf, accessed November 2008. 13. V. Mehta and J. S. Cooper, Journal of Power Sources, 114, 32-53 (2003). 14. F. Migri, M. A. Huneault, and M. F. Champagne, Polymer Engineering Science, 44, 1755-1765 (2004). 15. J. Huang, D. G. Baird, and J. E. McGrath, Journal of Power Sources, 150, 110119 (2005). 16. K. Robberg and V. Trapp, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, W. Vielstick, 25 H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003, 308-314. 17. D. M. Bigg. Polymer Composites, 7, 125-139 (1986). 18. R. B. Bird, W.E. Stewart, and E.N. Lightfoot, Transport Phenomena, 2nd Edition, Wiley, New York, NY, 2002. 19. J. E. Parrott and A. D. Stuckes. Thermal Conductivity of Solids, Pion Limited, London, England, 1975. 20. R. Berman, Thermal Conduction in Solids, Clarendon Press, Oxford, NY, 1976. 21. E. H. Weber, “Development and Modeling of Thermally Conductive Polymer/Carbon Composites”, Ph.D. Dissertation, Michigan Technological University, Houghton, MI, 2001. 22. D. Bigg, Metal Filler Polymers: Properties and Applications, S. K. Bhattacharya (Ed), Marcel Dekker Inc, New York, 1986, 165-226. 23. Y. Agari, and T. Uno, Journal of Applied Polymer Science, 30, 2225-2236 (1985). 24. Y. Agari, A. Ueda, and S. Nagai, Journal of Applied Polymer Science, 42, 16551669 (1991). 25. M. L. Clingerman, E. H. Weber, J. A. King, K. H. Schulz. Journal of Applied Polymer Science, 88, 2280-2299 (2003). 26. D. Stauffer and A. Aharony, Introduction to Percolation Theory, 2nd Edition, Taylor and Francis Inc., Philadelphia, PA, 1994, 1-56. 26 27. M. L. Clingerman, “Development and Modeling of Electrically Conductive Composite Materials”, Ph.D. Dissertation, Michigan Technological University, Houghton, MI, 2001. 28. A. Demain and J-P. Issi, Journal of Composite Materials, 27, 668-683 (1993). 29. J.-B. Donnet, R. C. Bansal, and M.-J. Wang, Carbon Black, 2nd edition, Marcel Dekker, Inc, New York, 1993. 30. J. Zhang, Y. Zou, and J. He, Journal of Zhejiang University Science, 6A, 10801083 (2005). 31. J. Yi and G. Choi, Journal of Electroceramics, 3:4, 361-369 (1999). 32. R. H. Blunk, D. J. Lisi, Y. Yoo, and C, L, Tucker III, AIChE Journal, 49, 18-29 (2003). 33. G. R. Ruschau and R. E. Newnham, Journal of Composite Materials, 26, 27272735 (1992). 34. E. P. Mamunya, V. V. Davidenko, and E. V. Lebedev, Composite Interfaces, 4, 169-176 (1997). 27 Chapter 3: Materials 3.1: Materials For this study three different carbon fillers and one polymer matrix were used. The polymer matrix used was Dow’s Semi-Crystalline Homopolymer Polypropylene Resin H7012-35RN. The three different carbon fillers studied were Ketjenblack EC-600 JD carbon black from Akzo Nobel, Inc., Asbury Carbons’ Thermocarb TC-300 synthetic graphite, and Hyperion Catalysis International’s Fibril TM nanotubes. The following sections will discuss each material in more detail. 3.2: Matrix Material 3.2.1: Semi-Crystalline Homopolymer Polypropylene Resin H7012-35RN The polymer matrix used for this project was Dow’s Semi-Crystalline Homopolymer Polypropylene Resin H7012-35RN. This polypropylene resin is very good for injection molding because it has good process ability and mold filling, as well as containing a nucleating agent giving the polymer a short molding time. Polypropylene is a thermoplastic material that can be re-melted for other uses which is way it has been looked at in other research for use in bipolar plates [2-3]. Figure 3.2-1 shows the chemical structure of polypropylene and Table 3.2-1 [1] shows the properties for the polypropylene used in this project. 28 CH3 H3C n CH3 Figure 3.2-1: Chemical Structure for Polypropylene Table 3.2-1: Properties of Dow H7012-35RN Polypropylene Resin/Molded Parts[1] Resin Properties Density (g/cc) Melt Flow Rate (g/10 min) Melting Point (ºC) 0.9 35 163 Glass Transition Temperature (ºC) Crystalline Temperature (ºC) -6.6 127 Molded Parts Properties Tensile Strength at Yield, (MPa) Tensile Elongation at Yield, (%) Flexural Modulus, 1% Secant, (MPa) Notched Izod Impact@ 23°C , (J/m) Deflection Temperature Under Load @ 0.45 MPa, unannealed, (°C) 34 7 1,420 25 110 3.3: Filler Materials 3.3.1: Carbon Black Carbon black is a particulate form of carbon that is produced in industry using thermal cracking or thermal decomposition [5]. Carbon black is used in elastomers (rubber), plastics, inks, and paint, with the majority of the carbon black produced being used in tires. In plastics carbon black is used as a colorant, as a stabilizer to protect the polymer from UV radiation, reinforcement, and to improve the electrical conductivity of 29 the material [4]. Carbon black is produced using one of five different processes: furnace, thermal, impingement, lampblack, and acetylene. Today the majority of the world’s carbon black is produced using the furnace process. In the furnace method a feedstock, usually oil containing a large concentration of aromatic hydrocarbons, is preheated to 200 to 250 degrees Celsius [6]. After the feedstock is preheated it is then injected into a hot-flame zone, created by burning a fuel which is usually natural gas [4]. In the hot-flame zone the oil is vaporized and undergoes thermal decomposition to form the carbon. To stop the reaction water is applied in the reactor and then the gas stream is sent to filters, where the carbon is separated from the gas used in the reactor. To increase the bulk density of the carbon it is either mixed in pin machines with more water or tumbled in horizontal drums, where it forms small pellets before being dried in a rotary kiln dryer [4,7]. Carbon black can be sold as pellets or as a powder depending on the end use application [7]. The structure and size of the carbon black produced depends on many factors. Some of these factors are type and concentration of raw material, temperature in the reactor, and residence time in the reactor [6]. Carbon blacks that are have smaller aggregates, higher structures, and low concentrations of volatiles increase the conductivity in a polymer composite [6]. In this project the carbon black was Ketjenblack EC-600 JD from Akzo Nobel Inc. This particular carbon black has a high electrical conductivity even at low filler loading levels, which is why it was chosen for the project. In this carbon black, the reasoning behind this attribute is because the particle has a large surface area and is highly branched allowing it to contact a larger amount of polymer, thus increasing the 30 electrical conductivity. The carbon black comes in the form of pellets that range in size from 100 microns to 2 mm in size [8]. A small amount of force applied to the pellets causes the pellets to separate into agglomerates, ranging in size from 10 to 100 micrometers long [8]. If the agglomerates are exposed to a high shear force, when mixed in with the polymer, then they separate even further to form primary aggregates that range in size from 30 to 100 nanometers [8]. The properties of Ketjenblack EC-600 JD are in Table 3.3-1 [8] and Figure 3.3-1 is a picture of a carbon black aggregate. Table 3.3-1: Properties of Akzo Nobel Ketjenblack EC-600 JD [8] Electrical Resistivity Aggregate Size Specific Gravity Apparent Bulk Density max Ash Content, Moisture, max. BET Surface Area Pore Volume 0.01-0.1 Ohm-cm 30-100 nm 1.8 g/cm3 100-120 kg/m3 0.1wt% 0.5 wt% 1250 m2/g 480-510 cm3/100g Figure 3.3-1: Ketjenblack EC-600 JD Primary Aggregate 31 3.3.2: Synthetic Graphite Synthetic graphite is produced using a high temperature treatment on carbon materials, which contain highly graphitizable forms of carbon. The primary feedstock for producing synthetic graphite is calcined petroleum coke and coal tar pitches. To manufacture synthetic graphite it involves many different mixing, molding, and baking operations before being heat-treated at temperatures between 2500 and 3000 degrees Celsius. The high temperature treatment reduces the concentration of impurities in the synthetic graphite compared to the original carbon used in production, giving the synthetic graphite products a high purity of 99% or more. The reason for the reduction in impurities is because the high temperature vaporizes the volatile impurities. At these high temperatures impurities that are removed include sulfur, nitrogen, hydrogen, all the organic compounds in the original feedstock, and most metal oxides. Synthetic graphite has many uses in multiple applications of industry. Some examples of applications that use synthetic graphite are conductive fillers, rubber and plastic compounds, drilling, coatings, foundry, and fuel cell bipolar plates [9]. The synthetic graphite used for this project is Asbusy Carbons’ Thermocarb TC300, which is a primary synthetic graphite previously sold by Conoco [10, 11]. Thermocarb TC-300 is produced from a thermally treated highly aromatic petroleum feedstock and contains very few impurities. This synthetic graphite was chosen for this project because of its high thermal conductivity and low electrical resistivity. Table 3.3-2 shows the properties of Thermocarb TC-300 Synthetic Graphite [10, 11] and Figure 3.3-2 shows a photomicrograph of Thermocarb TC-300. 32 Table 3.3-2: Properties of Thermocarb TC-300 Synthetic Graphite [10, 11] Filler Thermocarb TC-300 Synthetic Graphite 99.91 <0.1 0.004 2.24 1.4 600. in “a” crystallographic direction 0.020 Carbon Content, wt% Ash, wt% Sulfur, wt% Density, g/cc BET Surface Area, m2/g Thermal Conductivity at 23oC, W/m.K Electrical Resistivity of bulk carbon powder at 150 psi, 23oC, parallel to pressing axis, ohm-cm Particle Shape Particle Aspect Ratio Acicular 1.7 Sieve Analysis +600 microns + 500 microns +300 microns + 212 microns +180 microns +150 microns +75 microns +44 microns -44 microns wt % 0.19 0.36 5.24 12.04 8.25 12.44 34.89 16.17 10.42 33 Figure 3.3-2: Photomicrograph of Thermocarb TC-300 Synthetic Graphite (Reproduced with permission from Asbury Carbon Permission letter shown in Appendix M) 3.3.3: Hyperion Fibril Carbon Nanotubes Carbon nanotubes are hollow tubes made from sheets of graphite. There are two types of nanotubes single walled and multi-walled. There are four ways to synthesis carbon nanotubes; arc discharge, laser ablation, floating methods, and chemical vapor disposition (CVD). The chemical vapor disposition method has been in use since 1959, and was used to produce carbon filaments and fibers. In the CVD method to grow a carbon nanotube a hydrocarbon vapor, one example benzene, is passed over a catalyst at a temperature around 1100 degrees Celsius. Changing the type of hydrocarbon vapor, type of catalyst and particle size, as well as the temperature allows different carbon nanotubes to be grown that vary in size, morphology, and quality. The elements usually used as catalysts are 3d transition elements; iron, cobalt, and nickel. The CVD process has a very high yield but the carbon purity is low compared with other methods. 34 In an industrial CVD operation the reaction takes place in a fluidized bed reactor. In the reactor the hydrocarbon comes in contact with the catalyst where it splits into carbon and hydrogen. The carbon attaches to the catalyst and a nanotube starts to grow. As the nanotube grows, it causes the catalyst to disintegrate and then be distributed over the carbon nanotube agglomerate coming out of the reactor. This carbon nanotube agglomerate contains more than 95 wt% carbon and has a high bulk density, making the material easier to handle [12, 13]. Carbon nanotubes can be used in multiple applications. In polymers they are used to increase electrical conductivity and improve the mechanical properties. Carbon nanotubes are better than conventional fillers in polymer composites because they improve electrical conductivity with a lower amount of filler and they do not degrade the mechanical properties of the composite. The disadvantage is that the carbon nanotubes have a higher cost compared to conventional fillers [13]. Some other applications of nanotubes are as field emitters for high power microwave transmitters, as nanoscale probe tips, in the electrostatic application of paints, and as low voltage electromechanical actuators [12]. In this study the carbon nanotubes used were Hyperion Catalysis International’s FIBRILTM nanotubes. This is a conductive, vapor grown, multi-walled carbon nanotube. They are produced from a high purity, low molecular weight hydrocarbons in a proprietary, continuous, gas phase, catalyzed reaction. The outside diameter of the tube is 10 nm and the length is 10 µm, which gives an aspect ratio (length/diameter) of 1000. Due to this high aspect ratio, very low concentrations of nanotubes are needed to produce 35 an electrically conductive composite. This material was provided by Hyperion Catalysis International in a 20 wt% FIBRILTM masterbatch MB3020-01. Table 3.3-3 shows the properties of this carbon filler [14]. Table 3.3-3: Properties of FIBRILTM Carbon Nanotubes [14] Composition Diameter Length Morphology Density Pure carbon with trace residual of metal oxide catalyst 0.01 µm 10 µm 8 graphitic sheets wrapped around a hollow 0.005 µm core 2.0 g/cc 3.4: Formulation Naming Convention In this project to be able to identify the test specimens easily and quickly all of the samples have a unique identification name and number assigned. Because all of the polymer composite look similar it is crucial that the samples be labeled properly so that it is known which formulation is being tested. Each sample had a label allowing that specified what filler is used, the weight percent of the filler, and the order that the sample was injection molded. The naming convention shown below was used for all the samples in this project. E w x P y – z – ## Where, E = project description (started as a Department of Energy project) w = filler type (A = carbon black, B = synthetic graphite, and Q=Carbon Nanotubes) x = weight percent of conductive filler in composite 36 P = polymer matrix (P for H7012-35RN Polypropylene) y = indicates replicate number (none for original, R for first replicate) z = specimen type (F for flex bar, T for tensile bar, and TC for thermal conductivity disks) ## = specimen number (indicative of the order it was injection molded) An example of the naming convention is EB10P-TC-12. This means the sample is a thermal conductivity disk containing 10 wt% synthetic graphite and was the 12th sample injection molded for this formulation. For a formulation that contains multiple conductive fillers an example of the label under the naming convention is EB65Q6P-TC-1. This label indicates that the sample is a thermal conductivity disk containing 65 wt% synthetic graphite and 10 wt% carbon nanotubes in polypropylene and was the 15th sample from the injection molding machine for this formulation. The concentrations (shown in wt% and the corresponding vol %) for all the single filler composites tested in this research are shown in Table 3.4-1. The concentrations for the multiple filler composites will be shown and discussed in later chapters. Some of the conductivity samples tested came from compression molded plates. These samples are labeled the same as the injection molded samples except the letter ‘C’ is added after the specimen number. This extra ‘C’ allows the compression molded samples to be distinguished from the injection molded samples. An example is shown below: EA2.5B65Q6P- 1C 37 This label indicates that this sample contains 2.5 wt% carbon black, 65 wt% synthetic graphite and 6 wt% carbon nanotubes and that it was the first conductivity disk cut from a compression molded plate. Table 3.4-1: Single Filler Loading Levels Filler wt % 5 Carbon Black Vol % N/A 1.3 2.0 2.6 Synthetic Graphite Vol % N/A N/A N/A N/A Carbon Nanotubes Vol % 0.68 1.1 1.8 2.3 6 3.1 N/A 2.8 7.5 3.9 N/A 3.52 10 5.3 4.3 4.8 15 8.1 6.6 7.4 20 N/A 9.1 N/A 25 N/A 11.8 N/A 30 N/A 14.7 N/A 35 N/A 17.8 N/A 40 N/A 21.1 N/A 45 N/A 24.7 N/A 50 N/A 28.7 N/A 55 N/A 32.9 N/A 60 N/A 37.6 N/A 65 N/A 42.7 N/A 70 N/A 48.4 N/A 75 N/A 54.7 N/A 80 N/A 61.6 N/A 1.5 2.5 4 38 3.5: References 1. Technical Information Dow H7012-35RN Polypropylene Resin, Dow, Midland, MI, 2005. 2. F. Migri, M. A. Huneault, and M. F. Champagne, Polymer Engineering Science, 44, 1755-1765 (2004). 3. Y. Wang, “Conductive Thermoplastic Composite Blends for Flow Field Plates for Use in Polymer Electrolyte Membrane Cells (PEMFC)”, M.S. Thesis, University of Waterloo, Waterloo, Ontario, Canada, 2006. 4. J.-B. Donnet, R. C. Bansal, and M.-J. Wang, Carbon Black, 2nd edition, Marcel Dekker, Inc, New York, 1993. 5. J. Accorsi, E. Romero. Plastics Engineering, 51, 29 (1995). 6. F. Spinelli, Plastics, Additives, and Modifiers Handbook. J. Edenbaum (Ed.) Chapman and Hall, New York, NY, 1996, 615-643. 7. K.A. Burgess and F. Lyon, Encyclopedia of Polymer Science and Technology 2nd Edition, H.F. Mark, N.M Bikales, C. G. Overberger, G. Menges (Eds), John Wiley and Sons Inc, New York, NY, 1985, 623-640. 8. Akzo Nobel Electrically Conductive Ketjenblack Product Literature, 300. S. Riverside Plaza, Chicago, IL, 1999. 9. http://www.asbury.com/Graphite.html#synthetic - Accessed October 5, 2008. 10. Asbury Carbons Product Information, Asbury, NJ, 2004. 11. Conoco Carbons Products Literature, Conoco, Inc., P.O. Box 2197, Houston, TX, 1999. 39 12. A. Ramirez, Bells Lab Technical Journal, 10, 171 (2005). 13. M. Bierdel, S.Buchholz, V. Michele, L. Mleczko, R. Rudolf, M. Voetz, and A. Wolf, Physica Status Solidi B, 244, 3939-3943 (2007). 14. Hyperion Catalysis International Fibril Product Literature, Hyperion Catalysis International, 38 Smith Place, Cambridge, MA, 2008. 40 Chapter 4: Fabrication and Experimental Methods 4.1: Fabrication Methods This section will discuss the details of test specimen fabrication. Specific information on conditions and screw design can be found in the Appendices. 4.1.1: Extrusion For this entire project, the fillers and polypropylene were used as received. The extruder used was an American Leistritz Extruder Corporation Model ZSE 27. A picture of the extruder is shown in Figure 4.1-1. This extruder has a 27 mm co-rotating intermeshing twin screw with 10 zones and a length/diameter ratio of 40. The screw design, shown in Appendix A, was chosen to obtain a minimum amount of filler degradation, while still dispersing the fillers well in the polymer. The pure polypropylene pellets and the Hyperion FIBRILTM masterbatch MB3020-01 (containing 20 wt% carbon nanotubes) were introduced in Zone 1, which is water cooled. For all the composites containing single fillers, synthetic graphite and carbon black were added into the polymer melt at Zone 5. For the composites containing combinations of fillers, carbon black was added into the polymer melt at Zone 7; synthetic graphite was added to the polymer melt at Zone 5. Fillers were added at two different zones in order to adequately mix the large amount of fillers. Schenck AccuRate gravimetric feeders were used to accurately control the amount of each material added to the extruder. A Schenck AccuRate Flexwall gravimetric feeder was used in Zone 1, 41 shown in Figure 4.1-2, and Schenck AccuRate Conisteel feeders were used in Zones 5 and 7, shown in Figure 4.1-3. After passing through the extruder, the polymer strands (3 mm in diameter) enter a water bath and then a ConAir Model 20402HP-14A pelletizer that produced nominally 3 mm long pellets. Figure 4.1-4 shows a picture of the water bath and the pelletizer. Typically for each formulation ten pounds of pellets were produced. Appendix A shows the extrusion run condition for the all the composite formulations. Figure 4.1-1: American Leistritz Extruder Corporation Model ZSE 27 42 Figure 4.1-2: Schenck AccuRate Flexwall Feeder Figure 4.1-3: Schenck AccuRate Conisteel Feeder 43 Figure 4.1-4: Picture showing the Water Bath and Pelletizer 4.1.2: Drying After extrusion, the polypropylene based composites were dried in a Bry Air System indirect heated dehumidifying drying oven at 80oC for 4 hours. Figure 4.1-5 shows a picture of the Bry air dryer. The polymer is dried to remove water that it may have acquired while in the water bath. Once the polymer is dry, it is stored in moisture barrier bags before being injection molded. 44 Figure 4.1-5: Bry Air Drying Oven System 4.1.3: Injection Molding A Niigata injection molding machine, model NE85UA4, was used to produce test specimens [1]. This machine has a 40 mm diameter single screw with a length/diameter ratio of 18. It also has a maximum injection pressure of 22,610 psi, a maximum screw speed of 320 rpm, and a maximum clamping force of 82.50 US tons The lengths of the feed, compression, and metering sections of the single screw are 396 mm, 180 mm, and 144 mm respectively [1] . Figure 4.1-6 shows a picture of the Niigata injection molding machine. A four-cavity mold was used to produce 3.2 mm thick 16.5 cm long ASTM Type I tensile bars (end gated), 3.2 mm thick 6.4 cm diameter disks (end gated) and 3.2 mm thick 12.7 cm long by 1.27 cm wide flex bars (end-gated) [2]. Figure 4.1-7 shows a picture of the four-cavity mold. Appendix B shows the conditions used to injection mold each composite formulation. 45 Figure 4.1-6: Niigata Injection Molding Machine Model NE85UA4 To begin the injection molding process the machine was first heated to the operating temperature. After the operating temperature is reached, then the machine is purged using Dow’s semi crystalline homopolymer polypropylene resin H7012-35RN to remove any contaminants. About four pounds of material is used to create 25-30 flex bars, 6.4 mm disks, and tensile bars for each composite formulation. For some formulations, more disks had to be made because the tensile and flex bars would not mold because of the high resin viscosity (highly filled materials). The conditions for each formulation were kept constant as long as the samples could be molded. Typically, the only parameters to change in between formulations were the temperatures, shot size, and the injection pressure. As the samples were injection molded they were labeled according to the labeling system outline in Chapter 3.4 and stored in Ziploc bags. 46 Figure 4.1-7: Four-Cavity Mold Used in Injection Molding When the required number of samples for a formulation is reached, then the next formulation was added to the hopper. The five samples produced in between formulations are discarded because they are transition material contaminated with the previous formulation. After all the formulations have been molded into specimens, the machine is purged with Dow’s semi crystalline homopolymer polypropylene resin H7012-35RN to remove all the contaminants. When the polymer melt is free from any black material the injection molding machine is clean and the machine is shut down. 4.1.4: Compression Molding The only composite formulation that was compression molded is the three filler formulation containing, 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM 47 nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN. This formulation is compression molded because of the high viscosity and other researchers have shown that composites produced by compression molding, as opposed to injection molding, have produced materials with higher conductivities [3]. The compression molding press used to produce 8.5 inches long, 7 inches wide, and 3.2 mm thick plates is the Wabash Model V75H-18-CLX, shown in Figure 4.1-8. The procedure for fabricating plates is discussed below. 1. The pellets made from the extruder are ground up using a coffee grinder. Once the grinding is complete the pellets are sifted use a size #65 Taylor mesh shifting tray to collect 222 grams of material with a particle size of 208 microns or less. 2. The press platen set point temperature is set to 230º C and then the platens are closed to heat to the set point. 3. The 7 inch by 8.5 inch mold is coated with Slide Biodegradable Mold Release, as well as the four shims used to get the desired plate thickness. The top and bottom caul plates were coated with 10% wt Dynamar 9316 (mold release) from 3M in an acetone solution. 4. To make up the mold, place the picture frame mold on top of the protective sheet metal. Then place the thinner caul plate with the smooth side up into the picture frame mold. After the caul plate is in the mold spread the 222 grams of material evenly over the plate in the mold. Once the material is in the 48 mold, place the thicker caul plate on top and then the second piece of protective sheet metal on top of that. 5. After the platen set point is reached, then the platens are opened and the mold prepared in step four is slid into the press. The guard door is then closed to protect the operators. 6. The platens are closed and 1 ton (34 psi) of force is applied to the mold for 25 minutes at 230º C. 7. After the 25 minutes, the force is increased from 1 ton to 30 tons (1008 psi). This new force is applied for 25 minutes at 230º C. 8. The mold is cooled until the platen temperature is 25º C at 30 tons of force. Air is used to cool the platens to 343º C, water/air is used to cool the platens to 177º C., and just water is used to cool the plate to 25º C. 9. The mold is removed from the press and the mold placed on the mold opening device with a piece of metal placed on top of the mold. Then the mold is placed back in the press where 1 ton of force is applied. This causes the compression molded plate to fall out of the picture frame. Everything is removed from the press and cleaned for next use. 10. After the plates are produced, then composite thermal and electrical conductivity samples are cut out of the compression molded plates. 49 Figure 4.1-8: Wabash Model V75H-18-CLX Compression Molding Press 4.2:Experimental Test Methods 4.2.1: Through-Plane Electrical Resistivity Test Method For samples with an electrical resistivity > 104 ohm-cm, through-plane (also called transverse), volumetric electrical conductivity test was conducted. In this method, a constant voltage (typically 100V) was applied to the as-molded test specimen, and the resistivity was measured according to ASTM D257 using a Keithley 6517A Electrometer/High Resistance Meter and an 8009 Resistivity Test Fixture [4]. The Keithley 6524 High Resistance Measurement Software was used to automate the 50 conductivity measurement. For each formulation, a minimum of six specimens were tested. Each test specimen was an injection molded disk that was 6.4 cm in diameter and 3.2 mm thick. Figure 4.2-1 shows a picture illustrating this apparatus [5] (Permission letter shown in Appendix M). All the results from this test are shown in Appendix C. Sample Current Meter Voltage Source Figure 4.2-1: Diagram of Through Plane Electrical Resistivity Test (Reproduced with permission from Matthew Clingerman, Permission letter shown in Appendix M) 4.2.2: In-Plane Electrical Resistivity Test Method The volumetric in-plane (also called longitudinal) electrical resistivity was measured on all samples with an electrical resistivity < 104 ohm-cm. Test specimens cut from the center gauge portion of a tensile bar were surface ground on all sides and then cut into sticks 1.8 mm wide by 1.8 mm thick by 25.4 mm long, Figure 4.2-2b shows a diagram of the sample size [5] (Permission letter shown in Appendix M). Typically for each formulation, a total of six specimens were cut from a single tensile bar, and three tensile bars were used to obtain a total of eighteen test specimens [6]. These samples were then tested using the four-probe technique. This technique measures resistivity by applying a constant current (typically 5 to 10 mA) and measuring the voltage drop over 51 the center 6 mm of the sample [7], Figure 4.2-2a shows a schematic of this test [5]. A Keithley 224 Programmable Current Source and Keithley 182 Digital Sensitive Voltmeter were used. Equation 4.1 below is then used to calculate the electrical resistivity. All the results from this test are shown in Appendix C. ER = ( ∆V )( w)( x ) ( i )( L ) (4.1) where: ER = Electrical Resistivity, ohm-cm ∆V = Voltage drop over center 0.6 cm of sample, volts w = sample width, cm x = sample thickness, cm i = current, amps L = length over which ∆V is measured (0.6 cm) Constant current out of sample 25mm Current Source ∆V from center 6mm 2mm Sample Volt Meter Constant current in through sample (A) 2mm (B) Figure 4.2-2: (A) Experimental Set-up for Four-Probe Test Method (B) Sample Dimensions (Reproduced with permission from Matthew Clingerman, Permission letter shown in Appendix M) 52 4.2.3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Test Method The transverse (through-plane) volumetric electrical resistivity of the 63.5 mm diameter injection molded disks was determined according to the US Fuel Cell Council [8]. In this test gold-plated copper electrodes are attached to the platens of a hydraulic press. Wires connect the electrodes to a Keithley 2400 Source Meter that provides the current to the sample and a Keithley 2182A Nano Voltmeter that reads the change in voltage. The setup is shown in Figure 4.2-3. For each formulation, at least 3 samples were tested. Figure 4.2-3: Setup for Through-Plane (US Fuel Cell Council) Electrical Resistivity Test Method 53 Before the samples are run, a reference material the same size as the unknown sample is run to determine the resistance of the circuit and the contact. The reference material used was POCO graphite DFP-1. Two different disk sizes, 2.5” or 2” inch diameter with a thickness of 3.25 mm, were used depending on the sample size being tested. The POCO graphite DFP-1 has an electrical resistivity of 1.500 mΩ·cm [9]. Using Equations 4.2 and 4.3 the resistance of the circuit and the contact may be measured [8]. In Equation 4.2 ERPOCO is the electrical resistivity (mΩ·cm) of the POCO reference, xpoco is the thickness (cm), A is the area (cm2), and RPOCO is the resistance of the POCO reference (mΩ). In Equation 4.3 the Rmeasured is the resistance of the sample measured in the test, Rcircuit is the resistance of the circuit, and Rcontact is the resistance of the contact with all the resistances being in mΩ. ERPOCO ⋅ xPOCO A (4.2) Rmeasured − RPOCO = Rcircuit + Rcontact (4.3) RPOCO = Equations 4.4 and 4.5 are used to calculate the electrical resistivity of the composite sample [7]. Equation 4.4 is very similar to Equation 4.3 except that the RSample, resistance of the sample (mΩ), is used instead of RPOCO. In Equation 4.5 ERSample is the electrical resistivity (mΩ·cm), Asample is the area of the composite sample (cm2) and x is the thickness of the composite sample (cm). Rmeasured = Rsample + Rcircuit + Rcontact ERSample = 54 RSample ⋅ ASample x (4.4) (4.5) Each test is done at 1000 psi to simulate actual conditions in a fuel cell. Equation 4.6 is used to calculate the amount of force that needs to be applied to the sample to achieve 1000 psi, with Asample being the area of the sample (cm2) Re quired Force (lb f ) = ASample ⋅1000 psi (4.6) The pounds force is applied to the sample by using the hydraulic press and taking a reading from pressure transducer attached to the hydraulic press. The procedure below is used to measure the electrical resistivity of a composite sample. 1. Two pieces of Toray carbon paper cut to the size of the sample are placed on each side of the reference material. 2. The sample is then placed in between the electrodes. The hydraulic press is pumped until the pressure transducer reaches 4900 lbsf (1000 psi) to precondition the material. The paper is preconditioned every time new sheets are used. 3. The hydraulic press is released and then the sample is rotated 30 degrees. The pressure is reapplied until it gets to 4900 lbsf (1000 psi). Then the current is applied and the voltage change recorded. Using Ohms Law, Resistance=Voltage/Current, then the resistance is calculated for the sample. 4. Step three is repeated 10 times for the reference material. After the sample is removed the electrodes are cleaned with alcohol and compressed air. 5. The composite samples are sanded before being tested to remove the resin rich layer. 55 6. Steps 1 and 3 are repeated on the composite sample. For each sample 5 measurements are taken. Figure 4.2-4 shows a schematic for the US Fuel Cell Council through plane electrical resistivity test method [20] (Permission letter shown in Appendix M). The results from this test are shown in Appendix D. Figure 4.2-4: Schematic of Through-Plane (US Fuel Cell Council) Electrical Resistivity Test Method (Reproduced with permission from Rebecca Hauser, Permission letter shown in Appendix M) 4.2.4: Thermal Conductivity: Guarded Heat Flow Meter Test Method The through-plane thermal conductivity of a 3.2 mm thick, 5 cm diameter disk shaped test specimen was measured at 55oC using a Holometrix Model TCA-300 Thermal Conductivity Analyzer, Figure 4.2-5, which uses the ASTM F433 guarded heat flow meter method [10]. The thermal conductivity was measured at 55°C because this 56 was as close to ambient temperature as could be measured, while still maintaining a temperature gradient in the apparatus. Figure 4.2-6 shows a schematic of the test method used to measure through plane thermal conductivity [11]. The samples used for this test were 5 cm diameter disks cut from the 6.4 cm diameter injection molded disks or from the compression molded plates using a hole saw. For each formulation, at least four samples were tested. The results from this test are seen in Appendix E. Figure 4.2-5: Holometrix Model TCA-300 Thermal Conductivity Analyzer 57 Figure 4.2-6: Schematic of Through-Plane Thermal Conductivity Test Method 4.2.5: Thermal Conductivity: Transient Plane Source Test Method The Mathis Instruments Hot Disk Thermal Constants Analyzer is an emerging technology that uses the transient plane source technique to measure the in-plane and through-plane thermal conductivity of an anisotropic material in the same test [12-16]. Figure 4.2-7 is a picture of the Hot Disk Thermal Constants Analyzer. The sensors used in this test method consisted of a 10µm thick nickel foil embedded between two 25.4 µm thick layers of Kapton polyimide film. The nickel foil was wound in a double spiral pattern and had a radius, R, of either 3.189 mm or 6.403 mm. For the more conductive samples the sensor with the larger radius was used. The thermal conductivities were measured at 23oC. Since the test specimens are anisotropic, this test method is useful for this project. 58 Figure 4.2-7: Mathis Instruments Hot Disk Thermal Constants Analyzer Figure 4.2-8 shows how the sensor is positioned between two samples of composite material. In this experiment, the samples tested were composite disks with a diameter, D of 6.4 cm and a thickness, x of 3.2 mm. To help ensure that the assumption of an infinite sample domain was met and that heat was not penetrating completely through the sample in the axial direction, two of these composite disks were stacked together above the sensor and two more stacked below it, giving us a double thickness of sample. This stacking of disks allowed the generation of more reproducible data. For each formulation, typically 5 different sets of 4 disks (a total of 20 disks) were tested. The sensor then had a constant electrical current (variable by sample from 0.08W – 1W) over a short period of time (variable by sample from 2.5s – 10s) passed through it. The generated heat dissipated within the double spiral was conducted through the Kapton 59 insulating layer and into the surrounding sample, causing a rise in the temperature of the sensor and the sample. Figure 4.2-8: Schematic of Samples and Sensor for the Hot Disk. The insert at the lower left shows the double spiral heating element. From a theoretical standpoint, the double spiral pattern can be approximated by a series of concentric, equally spaced ring sources. The characteristic heat conduction Equation, assuming radial symmetry in the sample, is then given as [12-16]: (ρC p ) ∂T = k in 1 ∂ r ∂T ∂t r ∂r ∂r ∂ 2T + k thru 2 + ∑ Qr δ (r − r ' )δ ( z ) ∂z rings 60 (4.7) where ρ is the density of the sample (kg/m3), Cp is the heat capacity of the sample (J/(kg·K)), T is the temperature of the sample (K), t is the time of the measurement (s), kin and kthru are the in-plane and through-plane thermal conductivities of the sample (W/m·K), δ is the Dirac delta function, r ' is the radius of one of the ring sources, and Qr is the power supplied to that ring per unit length of the ring (W/m). The total power for each ring is proportional to the circumference of the ring 2π r ' , such that the total power supplied for all of the rings is Q (W). This total power Q is an input parameter to the Hot Disk Thermal Constants Analyzer. The first term in Equation 4.7 represents accumulation of thermal energy, the second term radial (referred to as in-plane in our experiments) heat conduction, the third term axial (referred to as through-plane in our experiments) heat conduction, and the final term is a heat source. The sample can be approximated as an infinite domain if the experimental time is much less than the characteristic thermal diffusion time. For an anisotropic material in a cylindrical geometry, the experimental time must meet the following two criteria: t << (D / 2) / (α in ) and t << x 2 / (α thru ) , where x is the sample thickness and D is the 2 sample diameter. In these formulas, α = k /( ρC p ) , which is the thermal diffusivity of the composite material. The average transient temperature increase of the sensor is simultaneously measured by recording the change in electrical resistance of the nickel sensor [12-16] according to: 61 ∆T = 1 Rn − 1 β Rno (4.8) where ∆T is the change in temperature at time t (K), β is the temperature coefficient of resistance (TCR) of the material (1/K), Rn is the electrical resistance of the nickel at time t (Ω), and Rno is the electrical resistance of the nickel at time 0 (Ω). The temperature rise in Equation 4.8 is correlated with the in-plane and through-plane thermal conductivities through the solution of Equation 4.7 as: ∆T = P π 3/ 2 R k in k thru F (τ ) (4.9) where P is the power dissipation in the probe and F (τ ) is a dimensionless time dependent function of τ = α in t / R 2 given by an integral of a double series over the number of rings m: τ m m l2 + k2 F (τ ) = [m(m + 1)]− 2 ∫ σ − 2 ∑ l ∑ k exp − 2 2 4m σ 0 l =1 k =1 lk I 0 dσ 2 2 2m σ (4.10) A more detailed derivation of Equations 4.9 and 4.10 are given by He [17]. Equations 4.7 through 4.10 are used to determine the in-plane and through-plane thermal conductivity of the composite being tested. The results for the in-plane and throughplane thermal conductivity from the Hot Disk Thermal Constants Analyzer are shown in Appendix G. 4.2.6: Hot Disk Analyser: Specific Heat The specific heat of polymer composites was measured using the Hot Disk Inc. Heat Capacity Cell, shown in Figure 4.2-9. In this method, three 25 mm diameter disks are stacked in the heat capacity cell. The heat capacity cell has a copper cup surrounded 62 by polystyrene insulation with a stainless steel shell around the insulation [15]. A nickel sensor is attached to the bottom of the copper cup and with an adaptor that attaches to the Hot Disk Thermal Constants Analyzer. The 25 mm diameter disks are 3.2 mm thick and are cut from the 64 mm in diameter injection molded disks. Two samples are cut out of each injection molded disk. Before starting the test with a sample the copper cup is run empty to obtain a reference. Once the samples are in the cell, then a constant supply of power is applied to the sample over a specific time period. As the power is applied to the copper cup and composite sample, the rise in temperature is recorded by measuring the increase in the resistance of the sensor. The specific heat is calculated for a polymer composite by comparing the rise temperature of the reference to the rise in temperature of the copper cup with the composite sample. For each formulation at least three samples were tested. Specific heat results for composites and the individual components are shown in Appendix F. Figure 4.2-9: Hot Disk Inc. Heat Capacity Cell 63 4.2.7 Density: ASTM D792-66 The density of the polymer composites was found by using the ASTM D792-66 test method, Specific Gravity and Density of Plastics by Displacement [18]. In this test the samples that were tested are the 6.4 cm diameter injection molded disks. The samples are first weighed dry and then weighed when submerged in water or Isopar M, a high purity isoparaffinic solvent available with an initial boiling point of 223 º C from Exxon. Some of the samples had to be tested in Isopar M, density of 0.7859 g/ml, because polypropylene has a density of 0.9 g/ml which is less than water. So the samples with low filler loadings, densities less than 1g/ml, could not be tested in water. The water/Isopar M used was allowed to sit open overnight to remove an air bubbles and come to equilibrium with the room. Once the weights are known then the density is calculated using Equation 4.11, where ρfluid is the density of water or Isopar M. Equation 4.12 is used to calculate the theoretical density for each polymer composite formulation. In Equation 4.12, ρi is the density of each individual component, Фi is the weight fraction of each individual component, and ρtheo is the theoretical density. The complete density results are found in Appendix H. ρ= DryWeight ⋅ ρ Fluid (T ) DryWeight − WetWeight ρTheo = 1 (4.11) (4.12) φ ∑i ρi i 64 4.2.8: Solvent Digestion – ASTM D5226-98 In order to determine the length and aspect ratio (length/diameter) of the fillers in the injection molded test specimens, solvent digestion was used to dissolve the polymer matrix. The solvent digestion follows the ASTM D5226-98 method for digesting polymers [19]. In this test 0.2 g of a sample obtained from a flex bar is used for the digestion. For each polymer composite formulation, three samples underwent solvent digestion. Only samples containing synthetic graphite underwent solvent digestion because these particles are large enough not clog the filer. The procedure for the solvent digestion is outlined below. The results from the solvent digestion are shown in Appendix I. 1. After the 0.2 g sample is weighed it is placed in a labeled sample tube without the top. Then add between 20 and 25 ml of xylene to each tube. There needs to be enough solvent to completely dissolve the polymer matrix. 2. Place the test tube on a hot plate in a holding rack. Turn on the hotplate and increase the temperature until the xylene is boiling. Also place a beaker of approximately 30 extra ml of xylene on a second hot plate. This xylene will be used later when filtering the samples. 3. Allow the samples to dissolve for three to six hours at a minimum temperature of 120oC. 4. While the samples are dissolving, petri dishes for each sample are labeled and a Millipore .45 µm filter paper is placed on the bottom. Using a four-place Denver Instruments A-250 scale the weights of the Petri dishes and filter 65 paper are measured and recorded. Also set up the vacuum filtration apparatus, shown in Figure 4.2-10. The vacuum filtration apparatus has a vacuum flask, vacuum pump, and Fisher Brand 47 mm microanalysis filter assembly 5. After the polymer is completely dissolved, place the filter from the Petri dish in the vacuum filtration apparatus and turn on the vacuum. Pour solution over the filter. Wash the sample tube with 5-10 ml of hot xylene, around 120 º C, and pour liquid into the funnel. The hot xylene dissolves any polypropylene that came out of solution, thus keeping the filter from being clogged. 6. The vacuum is kept on until there is no liquid left on the filter paper. A spatula is used to remove the filter paper with the filler and place it in the corresponding Petri dish. The Petri dish is placed in the fume hood with the lid half on to allow air to circulate. This removes any remaining liquid. 7. Repeat steps 5 and 6 for all the samples. Allow the samples to dry for 48 hours. If samples appear clumpy or have curled sections this means there is still some polymer left in the sample. These samples need to be washed with hot xylene, around 120 º C, at least twice in the vacuum filtration apparatus. 8. After the samples are dry, weigh the Petri dish, filter paper, and filler to get a final weight. The weight percent is calculated using Equation 4.13. 66 Figure 4.2-10: Solvent Digestion Filtration Apparatus wt % = WFinal − WFilter ( s ) − WPetriDish WComposite (4.13) 4.2.9: Filler Length and Aspect Ratio In order to determine the length and aspect ratio (length/diameter) of the synthetic graphite in the injection molded test specimens, solvent digestion is used to dissolve the polymer matrix and liberate the fillers. The fillers are then dispersed onto a glass slide. Figure 4.2-11 shows the apparatus that is used to disperse the fillers onto the slide [20] (Permission letter shown in Appendix M). From the Petri dish, a small amount of filler (0.01 g or less) is removed with a micro spatula. Only a small amount is used so that there is no overlap of the fillers when the pictures are taken. The filler is placed in the crucible and the rubber stopper is put back in place. Then the flask is placed over a glass slide on a piece of paper. Then with a compressed air canister, a small amount of air is blown above the crucible causing the filler to disperse onto the slide below. After each run the devise is cleaned so there is no contamination and the paper is thrown away. 67 Compressed Gas One Hole Stopper Filler in Crucible Plastic Vacuum Flask with Bottom Removed Glass Slide Figure 4.2-11: Filler Dispersion Apparatus (Reproduced with permission from Rebecca Hauser, Permission letter shown in Appendix M) Once the glass slide had the fillers on it then it is placed on a Prior automatic stage for the microscope setup. Figure 4.2-12 shows a picture of this setup. The microscope used was an Olympus SZH10 optical microscope with an Optronics Engineering LX-750 video camera. The filler images (at 70X magnification) were collected using Scion Image Version 1.62 software. The macro used to take pictures was originally written by Dr. Larry Sutter of Michigan Technological University and was modified when used for this project. Figure 4.2-12: Microscope Setup for Filler Length/Aspect Ratio Analysis 68 The images were then processed using Adobe Photoshop 5.0 and the Image Processing Tool Kit version 3.0. Because between 50 and 100 pictures were collected for each sample a batch operation was used to determine the filler length and aspect ratio. For each formulation, approximately 1,000 particles were measured. The batch operation contained the following steps [21]: 1. Convert image from RGB to grayscale 2. Fit and remove the background to remove the uneven lighting of the image 3. Automatic leveling of the image, which standardizes the contrast of the image 4. Threshold, this converts the image to a binary image in which all the fillers are in black 5. Feature cutoff and threshold, this removed all the features that came in contact with the edge of image 6. Calibrate, this loaded a predetermined calibration based on the magnification and resolution of the image 7. Measure all, this measured 26 different items of each feature in the image and stored them in a text file that was appended to for each new image. To measure the length and aspect ratio an algorithm was used that measures the minimum and maximum thickness of each feature. Also the length and height of each feature is measured every 11.25°. From these measurements the maximum and minimum distance are calculated. The maximum is the length and the minimum is the breadth. The aspect 69 ratio is calculated by dividing the length by the breadth [21]. The filler length and aspect ratio results are shown in Appendix J. 4.2.10: Determination of Filler Orientation in a Polymer Composite 4.2.10.1: Sample Preparation and Polishing Samples are cut from two injection molded pieces. First, from the center of a 6.4 cm diameter four ½ inch square pieces are cut out using the scroll saw. These samples show the “through-plane” and the “xy plane” surfaces. Figure 4.2-13 shows a figure of how the samples are cut from the disk. The three samples with the zigzag line are the “through-plane” surfaces studied and the “xy plane” surface is the shown with the diagonal lines. Figure 4.2-13: “Through Plane” and “XY Plane” Surface Samples Studied from Injection Molded Disk 70 For the “in plane” surface samples three parts of the middle portion of a tensile bar were cut up or a matchstick was cut into three pieces. Figure 4.2-14 shows a picture of a tensile bar and shows the middle portion where the samples were cut from. Figure 4.2-14: “In Plane” Surface Samples Studied from Tensile Bar Once the samples were cut they were then placed in labeled mold cups that had been sprayed with mold release. Then an epoxy from MSI Mager Scientific was made by mixing Epoxide Cold Mounting Resin and Hardener. The epoxy was made up by weight with a ratio of 5 parts resin to 1 part hardener. After the epoxy is mixed, it was poured into the mold cup until the samples were covered. The samples are then allowed to dry for 48 hours before being removed from the mold cups. Figure 4.2-15 below shows a picture of the top view of the epoxy pucks with the “through plane” and “in plane” sample. 71 Figure 4.2-15: Top View of Epoxy Pucks “Through Plane” Sample (left) and “In Plane” Sample (right) After the epoxy samples are cured they need to be polished so that the fillers can be seen for image analysis. First the pucks are ground on both sides using a 12” abrasive pad that is 60 grit. Figure 4.2-16 shows a picture of what the pucks look like after the sides have been removed. Once the pucks are in the oval shape then they are attached to glass microscope slides using JB Kwik Weld and labeled. Figure 4.2-16: Oval Shaped Ground Epoxy Pucks After the JB Kwik Weld is dry, then a diamond surface grinder is used to remove the epoxy covering the sample’s surface. In the diamond surface grinder the sample is attached to a plate and secured using a vacuum, before being passed over a diamond 72 grinding wheel. Once the sample puck is flat and the surface’s exposed then the puck is washed with soap and water. Then another slide, with one slide frosted and one side clear is attached to the other side of the puck. The frosted side of slide is attached to the puck using Epotech 301 epoxy. Figure 4.2-17 shows a polymer puck with both slides attached. Figure 4.2-17: Prepared Puck with Both Slides Attached After the epoxy is dry, the slide frosted side of the slide is numbered with a roman number. The sample is then placed frosted side down in the cut off saw’s vacuum chuck and secured using a vacuum. The cut off saw then cuts the samples so they are 0.2 mm thick. Figure 4.2-18 shows the cut-off saw used to make the 0.2 mm samples. After the samples are cut they are ground again using the diamond surface grinder to make sure that the surfaces of the samples are flat. Figure 4.2-19 shows what the samples look like after being cut and ground again. 73 Figure 4.2-18: Cut-off Saw Used to Cut Samples to 0.2 mm Figure 4.2-19: 0.2 mm Thin Composite Samples Ready to be Polished Before polishing, the samples are placed in an ultrasonic bath for 5 minutes. This step is needed to remove any grit on the sample because the polypropylene scratches easily. All the polishing is done by hand using the Buehler Ecomet 4 Grinder/Polisher, shown in Figure 4.2-20. First the samples are polished on a Texmet P polishing cloth (PSA 12” diameter) with the 3 µm Metadi Supreme Polycrystalline Diamond suspension at 190 rpm for 2-3 minutes. Then the samples are washed and looked at under the microscope to see if all the scratches are gone and the filler visible. If there are still scratches the polishing is continued using 3 µm diamond suspension until they are removed. 74 Figure 4.2-20: Buehler Ecomet 4 Grinder/Polisher Once the scratches are gone, then the samples are polished with Master-Tex Master polishing cloth (PSA 12” diameter) with the Masterprep 0.05 µm polishing suspension at 190 rpm.. The sample is then viewed under the microscope aft after er a few minutes of polishing to see if the fillers can be seen clearly. The slide will continue to be polished with the Masterprep 0.05 µm polishing suspension until the fillers look clear. Once the polishing is complete then pictures of the surfaces ar aree ready to be taken to be used later in filler orientation analysis. Samples were sent to Buehler so that they could develop a preparation procedure. This was done because the polypropylene had a tendency to develop scratches very easily 75 that hindered the imaging process. The procedure developed by Buehler is shown in Table 4.2-1 for polypropylene composites [22]. All the samples prepared by Buehler had images taken under a microscope and the fillers were analyzed for filler orientation. Table 4.2-1: Buehler Polishing Procedure for Polypropylene Surface Lubricant Abrasive Time (Minutes) Force (lbs) RPM Direction CARBIMET® Water SiC - 320 grit Till plane 5 230 Contra CARBIMET® Water SiC - 600 grit 2:00 5 230 Contra CARBIMET® Water SiC - 800 grit 2:00 5 230 Contra METADI® Supreme - 3 µm MASTERPREP ® 5:00 5 130 Contra 3:00 5 130 Contra TEXMET® 1500 MICROCLOTH ® 4.2.10.2: Optical Imaging Methods After polishing the samples are viewed using an Olympus BX60 reflected light microscope at a magnification of 200x. Figure 4.2-21 shows an image of the microscope used. To collect images of the filler the program Scion Image Version 1.62 was used. For the “in plane” surface images were taken in the direction of conduction. For the “through plane” surface images were taken perpendicular to the direction of conduction. Figure 4.2-22 shows a diagram of where the images were taken for the “in plane” and “through plane” surfaces. Usually, 9-16 images were taken for each surface depending on how good the polishing job was. These images were then pieced together to form a large composite image that was then used for the filler orientation analysis. 76 Figure 4.2-21: Olympus BX60 Reflected Light Microscope Figure 4.2-22: Diagram of Images Taken on “In Plane” and “Through Plane” Surfaces 77 4.2.10.3: Image Processing and Analysis After the images are taken they are then processed using Adobe Photoshop 5.0 and the Image Processing Tool Kit version 3.0. First each individual image has the color and any background variation removed. This turns the image into an 8 bit gray scale image and also leveled out any uneven lighting. Next each image was pasted onto a new canvas where the images are placed together to form one composite image. The composite image then has brightness threshold run to turn the fillers black and the background white. Next, a Euclidean distance map (EDM) open operation was performed to remove any small particles in the picture and to help separate the fillers image from the polymer matrix image. What the EDM open operation does is shrink each feature a certain number of pixels and expands them by the same number of pixels. Compared to the standard morphological open, the EDM version of “open” command does a better job of keeping the shape of the particle. After the EDM, a cutoff operation is used to remove any features that are touching the edge of the picture and any features that are smaller than 50 pixels. For each filler particle the moment angle was measured, as a measure of the orientation. This angle measurement gives some indication of the filler’s orientation in the composites and is measured from the direction of conduction. To get the angle of each particle, a method similar to fitting a line to a set of data is used [23]. The angle is calculated using Equations 4.14-4.22 [23]. Equations 4.14-4.18 are summations that calculate the location of each pixel in each particle. The moment around the x and y axes 78 are calculated in Equations 4.19-4.21. Equation 4.22 calculates the angle of minimum momentum or the moment angle. S x = ∑ xi (4.14) S y = ∑ yi (4.15) S xx = ∑ xi2 (4.16) S yy = ∑ yi2 (4.17) S xy = ∑ xi ⋅ yi (4.18) M xx = S xx − M yy = S yy − M xy = S xy − S x2 Area S y2 (4.19) (4.20) Area Sx ⋅ S y (4.21) Area M − M + yy xx θ = tan −1 2 − M yy ) + 4 ⋅ M xy2 2 ⋅ M xy (M xx (4.22) The method used to calculate the moment angle is a robust method. This is because it uses the main axes to calculate the angle and it does not fit an ellipse to the outside of the particle. When an ellipse method is used, one pixel sticking out on a feature can cause the calculated angle to be dramatically different from the actual angle. Compared to the moment angle method, where one or two pixels sticking out on a feature does not cause the angle be changed significantly [21]. Adobe Photoshop 5.0 and the Image Processing Tool Kit version 3.0 were used to determine the moment angle of each particle. Appendix K shows the orientation results as well as photomicrographs of the through-plane and in-plane surfaces. 79 4.2.10.4 Microtoming Microtoming was used as an alternative to polishing because at low filler concentrations the polypropylene was scratched very easily. This procedure was developed with the help of Owen Mills (Electron Optics Engineer at Michigan Technological University). For microtoming the samples need to be no longer than 1 cm and the surface needs to be no larger than 2 mm by 2mm, so matchsticks were used. The samples are placed in flexible silicone side molds and then epoxy is poured in. The samples need 24 hours to dry and then they are removed from the mold. The samples do not need labels since the molds have labels that will be embedded into the epoxy. After the samples are removed, choose the samples with the sample closest to the front surface of the mold and then trim the epoxy until the polymer is exposed. Then have a Microtome technician mount the sample and begin the microtoming. A diamond blade is used to remove 2 micron thick sections from the sample until the surface is completely smooth. Once the microtoming is complete, polish the sample using Master-Tex polishing cloth (PSA 12” diameter) with the Masterprep 0.05 µm polishing suspension for 15 to 20 seconds at 190 rpm. Then place the sample on a piece of glass and use the Olympus BX60 reflected light microscope at a magnification of 200x to take images of the filler. Once the images are taken follow the same procedure discussed in the previous section. Appendix K shows the orientation results as well as photomicrographs of the throughplane and in-plane surfaces. 80 4.2-11: Field Emission Scanning Electron Microscope (FESEM) Test Method A Hitachi Cold Field Emission Scanning Electron Microscope (FESEM) was used to view the fracture surface polymer composites at 5kV. This method was used to view the smaller fillers, (carbon black and carbon nanotubes) that could not be seen in the optical microscope. The photomicrographs from the FESEM can be seen in Appendix L. 4.3: References 1. Niigata Engineering Co. Ltd., Nagaoka Works, Model NE85UA4, Machine No. 50031F. Nagaoka Works, Niigata, Japan. 2. Four Cavity Mold, Master Precision Molds, Inc., Greenville, MI, Phone No. 800632-8912. 3. R. Leaversuch, “Fuel Cells Jolt Plastics Innovation”, Plastics Technology Online, November 2001, www.plasticstechnology.com/articles/200111fa2.html., accessed December 23, 2003. 4. “Standard Test Methods for DC Resistance or Conductance of Insulating Materials”, ASTM Standard D257-91, American Society for Testing and Materials, Philadelphia, PA, 1998. 5. Clingerman, M.L., "Development and Modeling of Electrically Conductive Composite Materials", Ph.D. dissertation in Chemical Engineering, Michigan Technological University, December 2001. 6. J. A. Heiser, J. A. King, J. P. Konell, I. Miskioglu, and L. L. Sutter, Advances in Polymer Technology, 23, 135-146 (2004). 81 7. J. A. King, K. W. Tucker, J. D. Meyers, E. H. Weber, M. L. Clingerman, and K. R. Ambrosius, Polymer Composites, 22, 142-154 (2001). 8. “Through-Plane Electrical Conductivity Testing Protocol for Composite Materials”, Document No. 05-160, US Fuel Cell Council, 1100 H. Street, NW, Suite 800, Washington, DC, 2004. 9. “Poco Graphite-Graphite Materials- DFP-1” http://www.poco.com/us/Graphite/dfp.asp-Accessed July 2007 10. “Evaluating Thermal Conductivity of Gasket Materials”, ASTM Standard D43377 (Reapproved 1993), American Society for Testing and Materials, Philadelphia, 1996. 11. Holometrix Model TCA - 300 Thermal Conductivity Analyzer using Guarded Heat Flow Meter Method, 25 Wiggins Avenue, Bedford, Massachusetts. 12. M. Gustavsson, E. Karawacki, and S.E. Gustafsson, Review of Scientific Instruments, 65, 3856-3859 (1994). 13. T. Log and S.E. Gustafsson, Fire and Materials, 19, 43-49 (1995). 14. V. Bohac, M.K. Gustafsson, L. Kubicar, and S.E. Gustafsson, Review of Scientific Instruments, 71, 2452-2455 (2000). 15. Hot Disk Thermal Constants Analyzer Instruction Manual, Mathis Instruments, Ltd., Fredericton, New Brunswick, Canada, 2001. 82 16. Transient Plane Source-Gustafsson Hot Disk Technique, standards for Contact Transient Measurements of Thermal Properties. National Physical Laboratory, United Kingdom, http://www.npl.co.uk/thermal/ctm, accessed February 2006 17. Y. He, Thermochimica Acta, 436, 122-129 (2005). 18. “Specific Gravity and Density of Plastics by Displacement”, ASTM Standard D792 - 66 (Re-approved 1975), American Society for Testing and Materials, Philadelphia, Pennsylvania, 1986. 19. “Standard Practice for Dissolving Polymer Materials”, ASTM Standard D5226 98, American Society for Testing and Materials, Philadelphia, Pennsylvania, 1998. 20. R. A. Hauser (2008). “Synergistic Effects and Modeling of Thermally Conductive Resins for Fuel Cell Bipolar Plate Applications.” PhD Dissertation. Michigan Technological University. 21. Weber, E.H., “Development and Modeling of Thermally Conductive Polymer/Carbon Composites”, PhD Dissertation, Michigan Technological University, 2001. 22. N. Vahora “Lab Report LB0807020” Email to Julie King. 30 July 2008. 23. Russ, J.C., The Image Processing Handbook, 3rd ed. CRC and IEEE Press, Boca Raton, 1999. 83 Chapter 5: Miscellaneous Results 5.1: Density Results The densities for each individual injection molded formulation were measured and then compared to the theoretical density. The densities were compared to verify that the amount of filler in each compound matched the formulation target value used in the extrusion process. The theoretical density was calculated using Equation 5.1 shown below. In the Equation the symbol ρTheo represents the theoretical density with ρi representing the density of the individual components and Фi the weight fraction of each component used for each formulation. ρTheo = 1 Φi ∑ρ i (5.1) i Table 5.1-1 shows the density results for the polypropylene semi crystalline homopolymer resin H7012-35RN. Table 5.1-2 shows the density results for a single filler formulation, 30 wt% synthetic graphite in polypropylene. At least three samples for each formulation were tested for their density, and from these samples an average and the standard deviation were calculated. After looking at all the comparisons between the theoretical and the actual density for all of the formulations it can be concluded that the gravimetric feeders used to feed the extruder are accurately putting in the amount of filler specified for each compound. The density results for all the formulations are shown in Appendix H. 84 Table 5.1-1: Density Results for Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Theoretical Actual Number Density (g/ml) Density (g/ml) 6/2/2008 EP-TC-12 0.9000 0.9079 EP-TC-16 0.9000 0.9092 EP-TC-23 0.9000 0.9100 EP-TC-27 0.9000 0.9096 EP-TC-37 0.9000 0.9087 Average 0.9091 Standard Deviation 0.0008 Number of Samples 5 Table 5.1-2: Density Results for 30 wt% Synthetic Graphite in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Theoretical Actual Number Density (g/ml) Density (g/ml) 5/30/2008 EB30P-TC-7 1.0968 1.0958 EB30P-TC-11 1.0968 1.0960 EB30P-TC-15 1.0968 1.0960 EB30P-TC-20 1.0968 1.0956 EB30P-TC-23 1.0968 1.0966 Average 1.0960 Standard Deviation 0.0004 Number of Samples 5 5.2: Solvent Digestion Results Solvent digestion was performed on injection molded samples containing synthetic graphite as described in Chapter 4.2-8. Solvent digestion was only performed 85 on composites containing synthetic graphite because the particles are large enough not to clog the filter. The weight percent of the synthetic graphite is calculated using Equation 4.13 in Chapter 4.2-8. These results are also used to verify that the gravimetric feeders used in the extrusion process are accurately controlling the amount of filler being added for each polymer formulation. Table 5.2-1 shows the results for the polymer composite containing 45 wt % synthetic graphite. These results confirm that the gravimetric feeders are accurately feeding the filler into the polymer composite. Complete solvent digestion results are shown in Appendix I. Table 5.2-1: Solvent Digestion Results for 45% wt Synthetic Graphite in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Formulation Actual Weight Target Weight Fraction Fraction 6/3/2008 EB45P-1 0.47 0.45 6/3/2008 EB45P-3 0.49 0.45 5.3: Filler Length and Aspect Ratio Results The mean filler length and aspect ratio was determined for the synthetic graphite using the particles removed from the polymer using the solvent digestion process described in Chapter 4.2-8. The carbon black and Fibril carbon nanotubes were not tested because of their small size, carbon black being 30-100 nm and the Fibril carbon nanotubes having a diameter of 0.01 µm. The results for the three synthetic graphite samples that were analyzed as well as the “as received” results from Rebecca Hauser’s previous work are shown in Table 5.3-1 [1]. The “as received particles had a mean aspect ratio of 1.757 and mean length of 67 86 µm compared to the injection molded fillers that had a mean aspect ratio of approximately 1.67 and mean length of approximately 40 µm. The values reported in this analysis agree with previous studies values, and the similarity between the “as received” values and the values after the synthetic graphite is put into the polymer, also agrees with previous studies done on the material [2,3, 4]. The results are also shown in Appendix J. Table 5.3-1: Mean Length and Aspect Ratio Results for Single Filler Synthetic Graphite Formulations [1] Formulation Filler Fabrication Method As Received Thermocarb EB25P Thermocarb EB45P Thermocarb EB65P Thermocarb Injection Molded Injection Molded Injection Molded Injection Molded Mean Length (mm) 0.0670 Standard Deviation (mm) 0.0590 Mean Aspect Ratio 1.757 Standard Deviation n 0.412 3533 0.0411 0.0302 1.671 0.372 855 0.0379 0.0520 1.660 0.355 412 0.0379 0.0560 1.652 0.037 830 5.4: Orientation Results The orientation angle for the synthetic graphite in polypropylene was measured using the procedure described in Chapter 4.2-10. Table 5.4-1 shows the orientation results (average, standard deviation, and number of fillers included) for the formulation 65 wt% synthetic graphite in polypropylene. The in-plane and the XY plane surfaces have an orientation angle around 30 degrees compared to the through-plane surface having an orientation angle around 60 degrees. On surfaces with orientation angles closer to 0 degrees this indicates that the fillers are primarily oriented in the direction of conduction, the in-plane and xy-plane surfaces in this study. On surfaces with orientation 87 angles closer to 90 degrees this indicates that the fillers are primarily oriented perpendicular to the direction of conduction, the through-plane surface in this study. Table 5.4-1: Orientation Results for a Formulation Containing 65 wt% Synthetic Graphite in Polypropylene Formulation Fabrication Method Surface Studied EB65P Injection Molded Injection Molded Injection Molded In Plane EB65P EB65P XY Plane Through Plane Angle Mean ± Stdev (Degrees) 27.49± 25.7 29.17± 23.36 60.70± 27.1 n 609 1438 1438 Figure 5.4-1 is a photomicrograph showing an in-plane surface for the formulation containing 65 wt% synthetic graphite in polypropylene. This figure shows that most of the fillers are orientated with the direction of conduction. Figure 5.4-2 is a photomicrograph showing a through-plane surface for the formulation containing 65 wt% synthetic graphite in polypropylene. This figure shows that most of the fillers are orientated perpendicular to the direction of conduction. Both figures orientation results coincide with the results found for the through plane and in-plane surface in Table 5.4-1. These results are the same for all the injection molded and compression molded samples looked at in this study, and the results agree with other previous studies [3-7]. All the filler orientation results and photomicrographs are shown in Appendix K. 88 Figure 5.4-1: In-Plane Photomicrograph for Injection Molded 65 wt% Synthetic Graphite in Polypropylene at 200X Magnification Figure 5.4-2: Through-Plane Photomicrograph for Injection Molded 65 wt% Synthetic Graphite in Polypropylene at 200X Magnification 89 5.5: Field Emission Scanning Electron Microscope (FESEM) Results FESEM pictures were taken for to see all of the fillers but especially to see the carbon black and the Fibril carbon nanotubes because of their small size. Chapter 4.2-11 discusses the procedure for taking FESEM pictures. Multiple pictures were taken on three different samples. One with 15% wt carbon black in polypropylene, another with 15% wt Hyperion FIBRILTM Carbon Nanotubes in polypropylene, and a third containing all three fillers, 2.5% wt carbon black, 65% wt synthetic graphite, and 6% wt Hyperion FIBRILTM Carbon Nanotubes in polypropylene. In Figure 5.5-1, the carbon black is shown as the white spheres and the FIBRILTM Carbon Nanotubes are shown as the white fibers. This picture shows that the FIBRILTM Carbon Nanotubes are forming networks that could increase the conduction of the material. The remaining pictures taken with the FESEM are in Appendix L. Figure 5.5-1: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion FIBRILTM Carbon Nanotubes in Polypropylene Composit 90 5.6: Conclusions From the results above multiple conclusions can be drawn. • From the density and solvent digestion measurements it was concluded that the gravimetric feeders are accurately feeding the required amount of filler for each specific formulation into the polymer during the extrusion process. • The mean length and the mean aspect ratio for the synthetic graphite stayed the same even after being extruded and injection molded into samples and that these results agree with other studies. • From the orientation results on the synthetic graphite it can be concluded that, when looking at the in-plane surface, the fillers are primarily aligned in the conductivity measurement direction and when looking at the through plane surface, the fillers are primarily aligned perpendicular to the conductivity measurement direction. These results agree with other studies that have looked at the synthetic graphite as well as other types of carbon. • From the FESEM pictures it was concluded that the Fibrils Carbon Nanotubes are forming networks, and these networks could help to increase the conductivity of the material. 91 5.7: References 1. R. A. Hauser (2008). “Synergistic Effects and Modeling of Thermally Conductive 2. Resins for Fuel Cell Bipolar Plate Applications.” PhD Dissertation. Michigan Technological University: US. 3. J. A. King, R. L. Barton, R. A. Hauser, and J. M. Keith, Polymer Composites, 29, 421-428 (2008). 4. J. A. Heiser, J. A. King, J. P. Konell, I. Miskioglu, and L. L. Sutter, Journal of Applied Polymer Science, 91, 2881-2893 (2004). 5. J. P. Konell, J. A. King, and I. Miskioglu, Polymer Composites, 25, 172-185 (2004). 6. J. A. King, M. G. Miller, R. L. Barton, J. M, Keith, R. A. Hauser, K. R. Peterson, and L. L. Sutter, Journal of Applied Polymer Science, 99, 1552-1558 (2006). 7. J. M. Keith, J. A. King, P. W. Grant, A. J. Cole, B. M. Klett, and I. Miskioglu, Polymer Composites, 29, 15-21 (2008). 8. J. A. King, F. A. Morrison, J. M. Keith, M. G. Miller, R. C. Smith, M. Cruz, A. M. Neuhalfen, and R. L. Barton, Journal of Applied Polymer Science, 101, 2680-2688 (2006). 92 Chapter 6: Electrical Resistivity Results and Design of Experiment Analysis 6.1: Single Filler Electrical Resistivity Results Electrical resistivity tests were performed on all the formulations created. The electrical resistivity was tested using the procedures described in Chapter 4.2-1 to 4.2-3. Each formulation had different concentrations of Ketjenblack EC-600 JD carbon black (CB), Thermocarb TC-300 synthetic graphite (SG), and Hyperion FIBRILSTM nanotubes (CNT) in polypropylene semi crystalline homopolymer resin H7012-35RN. For polypropylene formulations it is noted that increasing the filler amount will also increase the composite’s melt viscosity. Because of the large increases in composite melt viscosity for carbon black and FibrilTM carbon nanotubes, these fillers are only used at low loading levels [1, 2]. The maximum single filler amounts that that could be extruded and injection molded were 15 wt% for carbon black, 80 wt% for synthetic graphite, and 15 wt% for FibrilTM carbon nanotubes. The mean, standard deviation, and number of samples test for each formulation containing varying amounts of single fillers are shown in Tables 6.1-1, 6.1-2 and 6.1-3. Figures 6.1-1 and 6.1-2 show the log (electrical resistivity in ohm-cm) for composites containing varying amounts of single fillers as a function of filler volume fraction. In these figures, all the data points have been plotted. Appendix C has the all the electrical resistivity results for the single filler polymer composites. Figures 6.1-1 and 6.1-2 follow the typical electrical resistivity curve. At low filler loadings, the electrical resistivity remains similar to that of the pure polymer. Then at a point called the percolation threshold, the resistivity decreases dramatically over a very narrow range of filler 93 concentrations. At higher filler loadings, the electrical resistivity begins to level out again at a value many orders of magnitude lower than that of the pure polymer [3, 4]. Table 6.1-1: Electrical Resistivity Results for Carbon Black in Polypropylene Formulation Filler wt % Filler vol% Electrical Resistivity (ohm-cm) Polypropylene (PP) 0.0 0.0 1.65 x 1017 ± 5.54 x 1016 n = 8 PP Replicate 0.0 0.0 1.42 x 1017 ± 3.30 x 1016 n = 6 2.5CB 2.5 1.27 1.10 x 1016 ± 4.53 x 1015 n = 9 2.5CB Replicate 2.5 1.27 1.31 x 1016 ± 3.93 x 1015 n = 6 4CB 4.0 2.04 6811.72 ± 828.53 n = 5 5CB 5.0 2.56 641.35 ± 50.96 n = 5 6CB 6.0 3.09 192.30 ± 31.33 n = 5 7.5CB 7.5 3.90 11.66 ± 0.43 n = 5 10CB 10.0 5.26 2.93 ± 0.16 n = 26 15CB 15.0 8.11 1.15 ± 0.03 n = 24 94 Table 6.1-2: Electrical Resistivity Results for FibrilTM Carbon Nanotubes in Polypropylene Formulation Filler wt % Filler vol% Electrical Resistivity (ohm-cm) Polypropylene (PP) 0.0 0.0 1.65 x 1017 ± 5.54 x 1016 n = 8 PP Replicate 0.0 0.0 1.42 x 1017 ± 3.30 x 1016 n = 6 1.5CNT 1.5 0.68 9.90 x 1016 ± 3.66 x 1015 n = 6 2.5CNT 2.5 1.14 1.36 x 1016 ± 5.02 x 1015 n = 9 4CNT 4.0 1.84 2.71 x 1015 ± 3.22 x 1014 n = 6 5CNT 5.0 2.31 5.22 x 107 ± 6.42 x 107 n = 6 6CNT 6.0 2.79 15.86 ± 1.65 n = 29 6CNT Replicate 6.0 2.79 18.29 ± 1.31 n = 29 7.5CNT 7.5 3.52 5.09 ± 0.37 n = 29 10CNT 10.0 4.76 1.56 ± 0.08 n = 30 15CNT 15.0 7.36 0.40 ± 0.02 n = 30 95 Table 6.1-3: Electrical Resistivity Results for Synthetic Graphite in Polypropylene Formulation Filler wt % Filler vol% Electrical Resistivity (ohm-cm) Polypropylene (PP) 0.0 0.0 1.65 x 1017 ± 5.54 x 1016 n = 8 PP Replicate 0.0 0.0 1.42 x 1017 ± 3.30 x 1016 n = 6 10SG 10.0 4.27 1.39 x 1017 ± 2.92 x 1016 n = 8 15SG 15.0 6.62 9.42 x 1016 ± 1.15 x 1016 n = 6 20SG 20.0 9.13 6.19 x 1016 ± 1.29 x 1016 n = 6 25SG 25.0 11.81 3.33 x 1016 ± 4.75 x 1015 n =6 30SG 30.0 14.69 1.07 x 108 ± 2.72 x 107 n = 6 35SG 35.0 17.79 5484.40 ± 1411.30 n = 15 40SG 40.0 21.13 394.12 ± 68.46 n = 19 45SG 45.0 24.74 98.89 ± 11.11 n = 27 50SG 50.0 28.66 39.18 ± 4.59 n = 22 55SG 55.0 32.93 17.89 ± 2.61 n = 24 60SG 60.0 37.60 8.40 ± 0.75 n = 21 65SG 65.0 42.70 3.43 ± 0.68 n = 27 65SG Replicate 65.0 42.70 3.34 ± 0.73 n = 30 70SG 70.0 48.40 1.31 ± 0.22 n = 29 75SG 75.0 54.66 0.38 ± 0.06 n = 22 80SG 80.0 61.64 0.09 ± 0.01 n = 20 96 Figure 6.1-1: Single Filler Electrical Resistivity Results for FibrilTM Carbon Nanotubes and Carbon Black in Polypropylene and Carbon Black in Vectra 97 Figure 6.1-2: Single Filler Electrical Resistivity Results for Synthetic Graphite in Polypropylene and in Vectra Figure 6.1-1 illustrates that the carbon black and carbon nanotubes are effective at decreasing the electrical resistivity (1/electrical conductivity) at low filler loadings. The pure polypropylene has a mean electrical resistivity of 1.5 x 1017 ohm-cm. The percolation threshold occurs at 1.4 vol% for carbon black and 2.1 vol% for carbon nanotubes. At the highest filler concentration, the carbon black produced a mean composite resistivity of 1 ohm-cm (15 wt%= 8.1 vol%), compared to 0.4 ohm-cm for the carbon nanotube composite (15 wt% = 7.4 vol). The percolation threshold is likely low for the carbon black composites due to the highly branched, high surface area carbon black structure, and for the carbon nanotube composites due to the filler high aspect ratio 98 of 1000. The electrical resistivity results for carbon black in Ticona’s Vectra A950 Liquid Crystal Polymer are also shown in Figure 6.1-1, which was previously reported by this research group [5]. For the carbon black/Vectra composites the percolation threshold is 3.7 vol% and the lowest electrical resistivity is 2 ohm-cm (15 wt%= 12.1 vol%). Other researchers have noted that carbon black/PP composites often have a lower percolation threshold [6, 7]. Figure 6.1-2 shows that the percolation threshold for Thermocarb synthetic graphite/PP composites occurs at 13 vol%. The reason why a higher filler amount is needed for the percolation threshold for composites containing Thermocarb is due to the different particle shape/structure and properties of synthetic graphite particles as compared to carbon black and carbon nanotubes (see Tables 3.3-1, 3.3-2, and 3.3-3 in Chapter 3). Thermocarb has a much smaller aspect ratio (1.7) compared to 1000 for carbon nanotubes and the highly branched carbon black structure. Thermocarb also has a much smaller surface area of 1.4 m2/g, compared to 1250 m2/g for carbon black and 250 m2/g for carbon nanotubes. The composites containing 80 wt% (61.6 vol%) Thermocarb had a mean electrical resistivity of 0.09 ohm-cm. Figure 6.1-2 also shows for the Thermocarb synthetic graphite/Vectra composites, the percolation threshold is 15 vol% and the lowest electrical resistivity for the 80 wt% (71.4 vol%) composite is 0.08 ohm-cm [5]. 6.2: Electrical Resistivity Factorial Design Results For this project the most efficient type of experiment that can be used to determine what effect an individual filler will have on the electrical resistivity and the possible 99 interactions between the fillers is a factorial design. A factorial design can determine what effect each filler has on the system by calculating a single value to quantify the change in electrical resistivity relative to the increases in the weight percent of the filler in a polymer composite. Once the effects are known they can be ranked to determine what fillers and combinations of fillers produce the greatest change in electrical resistivity [8]. For all three fillers the lowest loading was zero wt% but the high loading level varied depending on the filler. The high loading for carbon black was 2.5% wt, for synthetic graphite 65% wt, and for the FibrilTM carbon nanotubes 6 wt %. Table 6.2-1 shows the different filler loading for the factorial design. The loading levels were chosen so that the composite would be conductive as well as have a low enough viscosity so that it could be extruded and injection molded into samples for testing. Table 6.2-1: Filler Loadings in Factorial Design Formulations Formulations No filler 2.5CB 65SG 6CNT 2.5CB*65SG 2.5CB*6CNT 65SG*6CNT 2.5CB*65SG*6CNT Ketjenblack wt% 0 2.5 0 0 2.5 2.5 0 2.5 Thermocarb wt% 0 0 65 0 65 0 65 65 FIBRILTM wt% 0 0 0 6 0 6 6 6 Table 6.2-2 shows the mean, standard deviation, and number of specimens tested for the factorial design formulations (original and replicate). The complete results for the electrical resistivity values for the combinations are in Appendix C. Using these results, 100 an analysis of the factorial design was conducted using the log (mean electrical resistivity, ohm-cm) as the response for all of the injection molded samples (one formulation 2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes was also compression molded and these results will be discussed later). This analysis was performed using the Minitab version 13 Statistical Software package. For this analysis, the effects and P (sometimes designated as p) values for the electrical resistivity results were calculated. Small p values indicate that a factor (filler in this case) may have a significant effect on the composite electrical resistivity [8]. For all statistical calculations, the 95% confidence level was used. The effects and P values are given in Table 6.2-3, showing the values for all of the filler combinations. Further investigation of Table 6.2-3 yields some important information regarding the effects that fillers have on electrical resistivity. For the composites containing only single fillers, synthetic graphite, followed by carbon nanotubes, and then carbon black, cause a statistically significant decrease (negative effect term) in composite electrical resistivity (P< 0.05). Synthetic graphite causes the largest decrease in electrical resistivity (largest effect term), followed closely by carbon nanotubes. Synthetic graphite likely causes the largest decrease in electrical resistivity since it was added at the highest filler amount (65wt%= 42.7 vol%). Carbon nanotubes were added at 6 wt% (2.79 vol%) and these composites had almost as much of a reduction in electrical resistivity likely due to the high aspect ratio (1000), high surface area (250 m2/g), and conductive networks that carbon nanotubes are known to form [2]. 101 The composites containing 2.5 wt% (1.27 vol%) carbon black likely had the least reduction in electrical resistivity due to the small amount of carbon black used. Table 6.2-2: Filler Loadings in Factorial Design Formulation and Electrical Resistivity Results (IM= Injection Molded, CM=Compression Molded) Formulations Constituents Electrical Resistivity (ohm-cm) No filler (PP) Original Replicate 2.5CB Original Replicate 65SG Original Replicate 6CNT Original Replicate 2.5CB*65SG Original Replicate PP Wt% 100 Wt% CB 2.5 PP 97.5 Wt% SG 65 PP 35 Wt% CNT 6.0 PP 94.0 Wt% CB 2.5 SG 65 PP 32.5 2.5CB*6CNT Wt% Original CB 2.5 Replicate CNT 6 PP 91.5 65SG*6CNT Wt% Original SG 65 Replicate CNT 6 PP 29 2.5CB*65SG*6CNT Wt% Original CB 2.5 Replicate SG 65 CNT 6 PP 26.5 Vol% 100 Vol% 1.3 98.7 Vol% 42.7 57.3 Vol% 2.8 97.2 Vol% 2.1 43.6 54.3 Vol% 1.3 2.8 95.9 Vol% 45.2 4.7 50.1 Vol% 2.2 46.2 4.8 46.8 102 1.65 x 1017 ± 5.54 x 1016 n = 8 1.42 x 1017 ± 3.30 x 1016 n = 6 1.10 x 1016 ± 4.53 x 1015 n = 9 1.31 x 1016 ± 3.93 x 1015 n = 6 3.43 ± 0.68 n = 27 3.34 ± 0.73 n = 30 15.86 ± 1.65 n = 29 18.29 ± 1.31 n = 29 0.356 ± 0.026 n = 18 0.358 ± 0.031 n = 15 2.19 ± 0.18 n = 26 2.16 ± 0.12 n = 27 0.0559 ± 0.0098 n = 16 0.0558 ± 0.0090 n = 33 0.0261 ± 0.004 n = 21 IM 0.0268 ± 0.004 n = 19 IM 0.011 ± 0.0009 n = 34 CM Table 6.2-3: Factorial Design Analysis for Log (Electrical Resistivity, ohm-cm) Term Constant 2.5CB 65SG 6CNT 2.5CB*65SG 2.5CB*6CNT 65SG*6CNT 2.5CB*65SG*6CN Effect -0. 825 -9.396 -8.652 0.174 0.216 7.196 0.110 P 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 All the combinations of different fillers had a statistically significant effect on electrical resistivity (P<0.05). In every case, the effect term is positive, which means that the composite electrical resistivity increases when these two or three different fillers are used together. For example, when synthetic graphite and carbon nanotubes are combined into a composite, the composite electrical resistivity is higher than what would be expected from the additive effect of each single filler [8]. This statistically significant effect and positive effect term for different carbon fillers has been noted previously in nylon 6,6 based resins [9] and in Vectra based resins [5]. Table 6.2-2 shows that the electrical resistivity for the composite containing 2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes (designated 2.5CB/65SG/6CNT) in polypropylene (PP) is 0.0264 ohm-cm, which corresponds to an electrical conductivity (1/electrical resistivity) of 38 S/cm. The US Department of Energy electrical conductivity target for bipolar plates is 100 S/cm [10]. Other researchers have shown that composites produced by compression molding (CM), as opposed to injection molding (IM), have produced materials with higher electrical conductivity [11]. Hence, this three filler combination (2.5CB/65SG/6CNT in PP) was compression molded at 6.9 103 MPa at 230oC and tested. The mean electrical resistivity of these composites is 0.011 ohm-cm (standard deviation = 0.0009 ohm-cm for 34 samples tested), which gives an electrical conductivity result of 91 S/cm. This is near the target value. The higher electrical conductivity for compression molding, as compared to injection molding, is likely due to the fillers being more oriented in the ‘in-plane’ direction of measurement that is induced in the manufacturing process. Hence, further optimization of this CB/SG/CNT/PP material system will be the subject of future work and could achieve the electrical conductivity goal for bipolar plates. 6.3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Results The through plane electrical resistivity was tested on all of the multi-filler composites and on the single filler composites with lower electrical resistivity. These samples were tested using the test method that follows the US Fuel Cell Council’s guidelines to simulate actual conditions in a fuel cell. This test method is discussed in more detail in Chapter 4.4-3. Table 6.3-1 shows the through plane electrical resistivity results from the polymer composites with single fillers. The 80% wt synthetic graphite composite has the smallest electrical resistivity, 0.4276 ohm-cm, of the single filler polymer composites. The through plane electrical resistivity results are all higher than the in-plane electrical resistivity results, shown in Table 6.1-2 and 6.1-3. This difference is likely due to the filler being more oriented in the in-plane direction opposed to the through plane direction. 104 Table 6.3-1: Single Filler Through-Plane Electrical Resistivity (US Fuel Cell Council) Results Formulation Filler wt % Filler vol% Electrical Resistivity (ohm-cm) 65SG 65.0 42.70 28.194 ± 5.56 n = 6 65SG Replicate 65.0 42.70 23.300 ± 2.390 n =5 70SG 70.0 48.40 13.440 ± 0.951 n = 5 75SG 75.0 54.66 5.377 ± 0.629 n = 8 80SG 80.0 61.64 0.428 ± 0.024 n = 5 7.5CNT 7.5 3.52 252.47 ± 32.65 n = 8 7.5CNT Replicate 7.5 3.52 271.46 ± 48.18 n = 8 10CNT 10.0 4.76 47.27 ± 7.47 n = 6 15CNT 15.0 7.36 8.588 ± 1.039 n = 5 Table 6.3-2 shows the through plane electrical resistivity (US Fuel Cell Council) results for the polymer composites with multiple fillers. Table 6.3-3 shows the through plane electrical resistivity results for samples sent to Dana Corporation for testing [12]. The results that were collected at Michigan Technological University and at Dana Corporation are similar, proving that our test results are accurate. These through plane electrical resistivity results are again higher than the in plane electrical resistivity results in Table 6.2-2, once again likely due to the filler orientation discussed in the paragraph above. Appendix D shows the complete results from the through plane electrical resistivity test. 105 Table 6.3-2: Multiple Filler Through-Plane Electrical Resistivity (US Fuel Cell Council) Results Formulations No filler (PP) Original Replicate 2.5CB*65SG Original Replicate Constituents Electrical Resistivity (ohm-cm) Wt% 100 Vol% 100 Wt% 2.5 65 32.5 2.5CB*6CNT Wt% Original CB 2.5 Replicate CNT 6 PP 91.5 65SG*6CNT Wt% Original SG 65 Replicate CNT 6 PP 29 2.5CB*65SG*6CNT Wt% Original CB 2.5 Replicate SG 65 CNT 6 PP 26.5 Vol% 2.1 43.6 54.3 Vol% 1.3 2.8 95.9 Vol% 45.2 4.7 50.1 Vol% 2.2 46.2 4.8 46.8 PP CB SG PP 1.65 x 1017 ± 5.54 x 1016 n = 8 1.42 x 1017 ± 3.30 x 1016 n = 6 0.708 ± 0.06 n = 5 0.559 ± 0.04 n = 6 58.09 ± 18.17 n = 6 46.85 ± 12.75 n = 6 0.0797 ± 0.0183 n = 3 0.0653 ± 0.0035 n = 3 0.0459 ± 0.0066 n = 5 IM 0.0395 ± 0.0097 n = 7 IM 0.0524 ± 0.0075 n = 3 CM Table 6.3-3: Through-Plane Electrical Resistivity (US Fuel Cell Council) Results from Dana Corporation [12] Formulations Constituents Electrical Resistivity (ohm-cm) 65SG*6CNT Original Wt% SG 65 CNT 6 PP 29 2.5CB*65SG*6CNT Wt% Original CB 2.5 SG 65 CNT 6 PP 26.5 Vol% 45.2 4.7 50.1 Vol% 2.2 46.2 4.8 46.8 106 0.0747 ± 0.0029 n = 3 0.0444 ± 0.0026 n = 3 IM 0.0467 ± 0.0052 n = 3 CM 6.4: Conclusions The object of this research was to determine the effects and interactions of each filler on composite electrical resistivity. For the composites containing single fillers, the percolation threshold was 1.4 vol% for carbon black/PP composites, 2.1 vol% for carbon nanotube/PP composites, and 13 vol% for synthetic graphite/PP composites. Hence, small amounts of carbon black and carbon nanotubes need to be added to dramatically reduce composite electrical resistivity. The lowest electrical resistivity for the composites containing single fillers is 1 ohm-cm for 15 wt% carbon black/PP, 0.4 ohm-cm for 15 wt% carbon nanotubes/PP, and 0.09 ohm-cm for 80 wt% synthetic graphite/PP. Several observations were made from the electrical resistivity factorial design analysis. First, for the composites containing only single fillers, synthetic graphite, followed closely by carbon nanotubes, and then carbon black, cause a statistically significant decrease (negative effect term) in composite electrical resistivity. Thus, adding these single fillers to polypropylene causes a statistically significant decrease in composite electrical resistivity. Second, all composites containing combinations of different fillers, had a statistically significant effect on electrical resistivity. This effect term is positive, which means that the composite electrical resistivity is higher than what would be expected from the additive effect of each single filler. After looking at the results from the through plane electrical resistivity (US Fuel Cell Council) test method, several observations were made. First, the results from the through plane electrical resistivity (US Fuel Cell Council) test method are higher than the results from in plane electrical resistivity test method. This is likely because the filler are 107 oriented more in the in-plane direction compared to the through plane direction. Second the results from Dana Corporation are similar to the results collected at Michigan Technological University, showing that the results are accurate. 6.5: References 1. J. A. King, F. A. Morrison, J. M. Keith, M. G. Miller, R. C. Smith, M. Cruz, A. M. Neuhalfen, and R. L. Barton, Journal of Applied Polymer Science, 101, 2680-2688 (2006). 2. Hyperion Catalysis International Fibril Product Literature, Hyperion Catalysis International, 38 Smith Place, Cambridge, MA, 2008. 3. M. Narkis, G. Lidor, A. Vaxman, and L. Zuri, Journal of Electrostatics, 47, 201214 (1999). 4. M. Weber and M. R. Kamal, Polymer Composites, 18, 711-725 (1997). 5. J. A. King, R. L. Barton, R. A. Hauser, and J. M. Keith, Polymer Composites, 29, 421-428 (2008). 6. J.-B. Donnet, R. C. Bansal, and M.-J. Wang, Carbon Black, 2nd edition, Marcel Dekker, Inc, New York, 1993. 7. Akzo Nobel Electrically Conductive Ketjenblack Product Literature, 300. S. Riverside Plaza, Chicago, IL, 1999. 8. Montgomery, D. C., Design and Analysis of Experiments 5th Edition, John Wiley & Sons, Inc., New York, NY, 2001. 108 9. J. A. Heiser, J. A. King, J. P. Konell, I. Miskioglu, and L. L. Sutter, Advances in Polymer Technology, 23, 135-146 (2004). 10. K. Robberg and V. Trapp, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, W. Vielstick, H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003, 308-314. 11. R. Leaversuch, “Fuel Cells Jolt Plastics Innovation”, Plastics Technology Online, November 2001, www.plasticstechnology.com/articles/200111fa2.html., accessed December 23, 2003. 12. E. Steigerwalt. “Re: Invitation to connect on LinkedIn” Email to Julie King. 18 July 2008. 109 Chapter 7: Thermal Conductivity Results and Design of Experiment Analysis 7.1: Through Plane Thermal Conductivity Results Through-plane thermal conductivity tests were performed on all the formulations created. The through-plane conductivity was tested using the procedure described in Chapter 4.2-4. Each formulation had different concentrations of Ketjenblack EC-600 JD carbon black, Thermocarb TC-300 synthetic graphite, and Hyperion FIBRILSTM Nanotubes in polypropylene semi crystalline homopolymer resin H7012-35RN. For polypropylene formulations it is noted that increasing the filler amount will also increase the composite’s melt viscosity. Because of the large increases in composite melt viscosity for carbon black and FibrilTM carbon nanotubes, these fillers are only used at low loading levels [1, 2]. The maximum single filler amounts that that could be extruded and injection molded were 15 wt% for carbon black, 80 wt% for synthetic graphite, and 15 wt% for FibrilTM carbon nanotubes. Tables 7.1-1, 7.1-2, and 7.1-3 show the through plane thermal conductivities results using the guarded heat flow meter method for the polymer composites with a single filler, as well as the weight and volume percent of the filler in each formulation. Figures 7.1-1 and 7.1-2 show the mean values for the single filler polymer composites as a function of the filler volume fraction as measured using the guarded heat flow method. These figures correspond with the values shown in Tables 7.1-1, 7.1-2, and 7.1-3. The standard deviation for all the single filler formulations was typically less than 5% of the 110 mean. Appendix E shows the complete results for the through-plane thermal conductivities obtained from the guarded heat flow meter. Table 7.1-1: Through Plane Thermal Conductivity at 55º C for Carbon Black in Polypropylene Formulation Filler wt % Filler vol% Through-Plane Thermal Conductivity (W/m. K) Polypropylene H7012-35RN 0.0 0.0 0.206 ± 0.002 n = 4 Polypropylene Replicate 0.0 0.0 0.203 ± 0.002 n = 4 EA2.5P 2.5 1.27 0.221± 0.004 n = 5 EA2.5PR 2.5 1.27 0.225 ± 0.002 n = 5 EA4P 4.0 2.04 0.240 ± 0.006 n = 4 EA5P 5.0 2.56 0.251 ± 0.003 n = 5 EA6P 6.0 3.09 0.261 ± 0.004 n = 4 EA7.5P 7.5 3.90 0.276 ± 0.007 n = 4 EA10P 10.0 5.26 0.298± 0.002 n = 5 EA15P 15.0 8.11 0.337 ± 0.001 n = 5 111 Table 7.1-2: Through Plane Thermal Conductivity at 55º C for FibrilTM carbon nanotubes in Polypropylene Formulation Filler wt % Filler vol% Through-Plane Thermal Conductivity (W/m. K) Polypropylene H7012-35RN 0.0 0.0 0.206 ± 0.002 n = 4 Polypropylene Replicate 0.0 0.0 0.203 ± 0.002 n = 4 EQ1.5P 1.5 0.68 0.215 ± 0.001 n = 5 EQ2.5P 2.5 1.14 0.229 ± 0.002 n = 5 EQ4P 4.0 1.84 0.258 ± 0.002 n = 4 EQ5P 5.0 2.31 0.281 ± 0.002 n = 4 EQ6P 6.0 2.79 0.302 ± 0.003 n = 4 EQ6PR 6.0 2.79 0.297 ± 0.001 n = 4 EQ7.5P 7.5 3.52 0.328 ± 0.002 n = 4 EQ10P 10.0 4.76 0.371 ± 0.004 n = 4 EQ15P 15.0 7.36 0.467 ± 0.004 n = 4 112 Table 7.1-3: Through Plane Thermal Conductivity at 55º C for Synthetic Graphite in Polypropylene Formulation Filler wt % Filler vol% Through-Plane Thermal Conductivity (W/m. K) Polypropylene H7012-35RN 0.0 0.0 0.206 ± 0.002 n = 4 Polypropylene Replicate 0.0 0.0 0.203 ± 0.002 n = 4 EB10P 10.0 4.27 0.234 ± 0.005 n = 5 EB15P 15.0 6.62 0.266 ± 0.003 n = 4 EB20P 20.0 9.13 0.292 ± 0.005 n = 4 EB25P 25.0 11.81 0.352 ± 0.004 n =4 EB30P 30.0 14.69 0.438 ± 0.001 n = 4 EB35P 35.0 17.79 0.503 ± 0.005 n = 4 EB40P 40.0 21.13 0.628 ± 0.008 n = 4 EB45P 45.0 24.74 0.741 ± 0.018 n = 4 EB50P 50.0 28.66 0.896 ± 0.006 n = 4 EB55P 55.0 32.93 1.150 ± 0.005 n = 4 EB60P 60.0 37.60 1.494 ± 0.022 n = 4 EB65P 65.0 42.70 1.971 ± 0.088 n = 4 EB65PR 65.0 42.70 1.987 ± 0.060 n = 4 EB70P 70.0 48.40 2.712 ± 0.049 n = 4 EB75P 75.0 54.66 3.641 ± 0.036 n = 5 EB80P 80.0 61.64 6.042 ± 0.098 n = 5 113 Figure 7.1-1: Single Filler Through-Plane Thermal Conductivity Results for FibrilTM carbon nanotubes and Carbon Black in Polypropylene and Carbon Black in Vectra 114 Figure 7.1-2: Single Filler Through-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene and in Vectra Figure 7.1-1 shows that the carbon black does increase the through-plane thermal conductivity. It causes the thermal conductivity to increase from 0.20 W/m•K for pure polypropylene to 0.34 W/m•K for polypropylene composites containing 15 wt % (8.1 vol %) carbon black. These values are very similar to those previously reported for this same carbon black in Vectra A950RX Liquid Crystal Polymer. Figure 7.1-1 shows the results for composites containing Vectra and carbon black [3]. Figure 7.1-1 also shows the through-plane thermal conductivity for composites containing FibrilTM carbon nanotubes and polypropylene. These composites have a higher thermal conductivity compared to 115 the carbon black at the same volume percent. Composites with 15 wt % (7.4 vol %) FibrilTM carbon nanotubes had a thermal conductivity of 0.47 W/m K. Figure 7.1-2 shows the through plane thermal conductivity results for synthetic graphite in polypropylene and previous results for the same filler in Vectra [3]. Synthetic graphite composites had the highest through plane thermal conductivity values with the composite containing 80 wt % synthetic graphite in polypropylene having the highest value at 6.04 W/m K. Figure 7.1-2 also illustrates the similarity between the through plane thermal conductivity values found for synthetic graphite in polypropylene and Vectra. One possible reason why synthetic graphite had the highest through-plane thermal conductivity compared to carbon black and the FibrilTM carbon nanotubes, is because of the high thermal conductivity of synthetic graphite at 600 W/m K. Another reason for the difference is because not all the filler loadings are the same. When comparing all the fillers at 15 wt %, the data shows that the highest through plane thermal conductivity is FibrilTM carbon nanotubes composite. This implies that the FibrilTM carbon nanotubes form more thermal conductive networks at lower filler levels compared to carbon black and synthetic graphite. However, more fibrils can not be added because of the increase in viscosity at higher filler loadings, making the resin difficult to process. 7.2: Through Plane Thermal Conductivity Factorial Design Results For this project the most efficient type of experiment that can be used to determine what effect an individual filler will have on the thermal conductivity and the possible interactions between the fillers is a factorial design. A factorial design can determine what effect each filler has on the system by calculating a single value to 116 quantify the change in thermal conductivity relative to the increases in the weight percent of the filler in a polymer composite. Once the effects are known they can be ranked to determine what fillers and combinations of fillers produce the greatest change in thermal conductivity [4]. For all three fillers the lowest loading was zero wt% but the high loading level varied depending on the filler. The high loading for carbon black was 2.5% wt, for synthetic graphite 65% wt, and for the FibrilTM carbon nanotubes 6 wt %. Table 7.2-1 shows the different filler loading for the factorial design. The loading levels were chosen so that the composite would be conductive as well as have a low enough viscosity so that it could be extruded and injection molded into samples for testing. Table 7.2-1: Filler Loadings in Factorial Design Formulations Formulations No filler 2.5CB 65SG 6CNT 2.5CB*65SG 2.5CB*6CNT 65SG*6CNT 2.5CB*65SG*6CNT Ketjenblack wt% 0 2.5 0 0 2.5 2.5 0 2.5 Thermocarb wt% 0 0 65 0 65 0 65 65 FIBRILTM wt% 0 0 0 6 0 6 6 6 Table 7.2-2 shows the through-plane thermal conductivity results determined using the guarded heat flow meter (mean, standard deviation, and number of samples tested) for the factorial design formulations (original and replicate). The complete results for the through-plane thermal conductivities values for the combinations obtained from the guarded heat flow meter are in Appendix E. The highest thermal conductivity from the 117 combinations was for the formulation containing three fillers with a result of 5.8 W/m•K when injection molded (IM) and 6.57 W/m•K when compression molded (CM). The compression molded results are slightly higher than the injection molded sample results. An analysis of the factorial design was conducted using the mean thermal conductivity results from Table 7.2-2 in units of W/m•K as the response. Minitab version 13, the statistical software package was used for the factorial design analysis. The two values of interest and that were calculated in this analysis was the effect and P values for the thermal conductivity results. Small P values show that the filler may have a significant effect on the composites thermal conductivity. A confidence level of 95% was used for all of the statistical calculations. Table 7.2-3 the effect and the P-values results for all the filler combinations from the factorial analysis. From the results it can be seen that all of the single fillers cause a statistically significant increase, having a positive effect term and having a P-value of less than 0.05, in the through plane thermal conductivity of the single filler polymer composites. Synthetic graphite had the largest effect term which means it causes the largest increase in a composites thermal conductivity. The carbon nanotubes had the second largest effect on thermal conductivity followed by carbon black having the lowest effect of the three fillers. 118 Table 7.2-2: Filler Loadings in Factorial Design Formulations and Through-Plane Thermal Conductivity Results Formulations No filler (PP) Original Replicate 2.5CB Original Replicate 65SG Original Replicate 6CNT Original Replicate 2.5CB*65SG Original Replicate Constituents PP Wt% 100 Through-Plane Thermal Conductivity (W/m.K) Vol% 100 Wt% Vol% CB 2.5 1.3 PP 97.5 98.7 Wt% Vol% SG 65 42.7 PP 35 57.3 Wt% Vol% CNT 6.0 2.8 PP 94.0 97.2 Wt% Vol% CB 2.5 2.1 SG 65 43.6 PP 32.5 54.3 2.5CB*6CNT Wt% Vol% Original CB 2.5 1.3 Replicate CNT 6 2.8 PP 91.5 95.9 65SG*6CNT Wt% Vol% Original SG 65 45.2 Replicate CNT 6 4.7 PP 29 50.1 2.5CB*65SG*6CNT Wt% Vol% Original CB 2.5 2.2 Replicate SG 65 46.2 CNT 6 4.8 PP 26.5 46.8 119 0.206 ± 0.002 n = 4 0.203 ± 0.002 n = 4 0.221± 0.004 n = 5 0.225 ± 0.002 n = 5 1.971 ± 0.088 n = 4 1.987 ± 0.060 n = 4 0.302 ± 0.003 n = 4 0.297 ± 0.001 n = 4 2.777 ± 0.080 n = 4 2.737 ± 0.084 n = 4 0.333± 0.007 n = 4 0.339 ± 0.003 n = 5 4.752 ± 0.042 n = 4 4.720 ± 0.074 n = 4 5.836 ± 0.095 n = 5 IM 5.818 ± 0.073 n = 4 IM 6.570 ± 0.060 n = 4 CM Table 7.2-3: Factorial Design Analysis for Through-Plane Thermal Conductivity Term Constant CB SG CNT CB*SG CB*CNT SG*CNT CB*SG*CNT Effect 0.481 3.559 1.509 0.454 0.083 1.405 0.074 P 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 The results show that all the combinations cause a statistically significant increase in a composites thermal conductivity, having a P value less than 0.05. The composite that had the greatest increase in thermal conductivity was the synthetic graphite and carbon nanotubes combination. The synthetic graphite and carbon black combination had the next largest effect followed by the combination with the carbon black and carbon nanotubes. The three filler combination had the lowest effect term of the four different combinations. All of the effects for the multiple filler combinations are positive meaning that the thermal conductivity will increase if different fillers are used together in a composite. This means that when two fillers are combined in a composite, that the new composites thermal conductivity will be higher than the combined individual thermal conductivities of the two fillers. For example, when synthetic graphite and carbon nanotubes are combined into a composite, the composite thermal conductivity is higher than what would be expected from the additive effect of each single filler [4]. This result could be because thermally conductive pathways are formed that ‘link’ the carbon fillers 120 and results in a larger composite thermal conductivity. These thermally conductive pathways can be seen in the photos Chapter 5 or in Appendix L. Prior work done with the same carbon black and synthetic graphite in Vectra also showed statically significant effect and positive effect terms for combinations of these fillers [3]. 7.3: In-Plane Thermal Conductivity Results Table 7.3-1 and Table 7.3-2 show the in-plane thermal conductivity results (mean, standard deviation, and number of samples tested) for the most thermally conductive composites. The in-plane thermal conductivity was tested using the Hot Disk Thermal Constants Analyser, the procedure is described in Chapter 4.2-5. The Hot Disk Thermal Constants Analyser also measures through-plane thermal conductivity but because these results were the same as the results found using the guarded heat flow method they are not reported in the tables. Figure 7.3-1 shows the in-plane thermal conductivity for composites containing different amounts of synthetic graphite in polypropylene. Appendix G shows the thermal conductivity results from the Hot Disk Thermal Constants Analyser for all the composites analyzed. The in-plane thermal conductivity for the injection molded composite with 80 wt% (61.6 vol %) synthetic graphite had a result of 28.0 W/m K, which is higher than the minimum desired bipolar plate thermal conductivity of 20.0 W/m K. The 80% wt (61.64 vol %) results are very similar to results found in previous work using the same synthetic graphite in Vectra. The in-plane values for synthetic graphite in Vectra at 59.3 vol% was 21.1 W/m•K and at 65.2 vol% was 28.5 W/m•K [3]. The composite with all three fillers had in-plane thermal conductivity of 17.6 W/m•K when injection molded. 121 Since compression molded samples were made for the three filler composite for electrical resistivity tests, these samples were also tested for thermal conductivities. The in-plane thermal conductivity was 24.0 W/m K, which is above the minimum desired bipolar plate thermal conductivity of 20.0 W/m K. For the one composite the compression molded samples had a slightly higher thermal conductivity compared to the injection molded samples. Table 7.3-1: In-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene Composites Formulation Filler wt % Filler vol% In-Plane Thermal Conductivity (W/m. K) 30SG 30.0 14.69 1.387 ± 0.042 n = 6 35SG 35.0 17.79 1.971 ± 0.060 n = 5 40SG 40.0 21.13 2.573 ± 0.107 n = 6 45SG 45.0 24.74 3.390 ± 0.141 n = 5 50SG 50.0 28.66 4.373 ± 0.028 n = 5 55SG 55.0 32.93 5.306 ± 0.126 n = 5 60SG 60.0 37.60 7.235 ± 0.113 n = 5 65SG 65.0 42.70 9.349 ± 0.040 n = 5 70SG 70.0 48.40 12.316 ± 0.210 n = 5 75SG 75.0 54.66 18.142 ± 0.402 n = 5 80SG 80.0 61.64 28.004 ± 1.518 n = 5 122 Figure 7.3-1: In-Plane Thermal Conductivity Results for Synthetic Graphite in Polypropylene Composites Table 7.3-2: In-Plane Thermal Conductivity Results for Composites Containing Combinations of Different Fillers in Polypropylene Formulations 2.5CB*65SG Constituents Wt% CB 2.5 SG 65 PP 32.5 65SG*6CNT Wt% SG 65 CNT 6 PP 29 2.5CB*65SG*6CNT Wt% CB 2.5 SG 65 CNT 6 PP 26.5 In-Plane Thermal Conductivity (W/m.K) Vol% 2.1 43.6 54.3 Vol% 45.2 4.7 50.1 Vol% 2.2 46.2 4.8 46.8 123 8.754 ± 0.265 n = 5 15.632 ± 0.269 n = 5 17.570 ± 0.394 n = 5 IM 23.960 ± 0.534 n = 6 CM 7.4: Conclusions One objective of this research was to determine the effects and interactions of the three fillers on composite thermal conductivity. For the single filler composites it was shown that synthetic graphite had caused the greatest increase in thermal conductivity. All of the combinations of the three different fillers did cause a statistically significant increase in the through plane thermal conductivity in the composite. The filler combination of synthetic graphite and carbon nanotubes increased the through plane thermal conductivity the most compared to the other filler combinations. The next largest increase in through-plane thermal conductivity was the carbon black and synthetic graphite combination, followed by the carbon black and carbon nanotube combination, and last the three filler combination. When multiple fillers are combined into a composite, the composite thermal conductivity is higher than what would be expected from the additive effect of each single filler. One possible reason for this result is that thermally conductive pathways may be formed to link the different carbon fillers, resulting in a larger composite thermal conductivity. The in-plane thermal conductivity results for two composites were above the minimum desired bipolar plate thermal conductivity of 20.0 W/m•K. The 80 wt% synthetic graphite in polypropylene composite got a result of 28.0 W/m•K and the three filler combination composite that was compression molded got a result of 24.0 W/m• K. Because of these results, future research may be performed to determine if these composites are variable in creating bipolar plates for fuel cells. 124 7.5: References 1. J. A. King, F. A. Morrison, J. M. Keith, M. G. Miller, R. C. Smith, M. Cruz, A. M. Neuhalfen, and R. L. Barton, Journal of Applied Polymer Science, 101, 2680-2688 (2006). 2. Hyperion Catalysis International Fibril Product Literature, Hyperion Catalysis International, 38 Smith Place, Cambridge, MA, 2008. 3. R. A. Hauser, J. A. King, R. M. Pagel, and J. M. Keith, Journal of Applied Polymer Science, 109, 2145-2155 (2008). 4. Montgomery, D. C., Design and Analysis of Experiments 5th Edition, John Wiley & Sons, Inc., New York, NY, 2001. 125 Chapter 8: Summary, Conclusions, and Future Work 8.1: Summary 8.1.1: Effects of Single Conductive Fillers on Electrical Resistivity Electrical resistivity tests were performed on all the formulations each containing different concentrations of Ketjenblack EC-600 JD carbon black, Thermocarb TC-300 synthetic graphite, and Hyperion FIBRILSTM Nanotubes in polypropylene semi crystalline homopolymer resin H7012-35RN. The maximum single filler amounts that that could be extruded and injection molded were 15 wt% for carbon black, 80 wt% for synthetic graphite, and 15 wt% for FibrilTM carbon nanotubes. The electrical resistivity was measured using one of three test methods; the in-plane electrical resistivity test method, the through-plane electrical resistivity test method, or the through-plane electrical resistivity (US Fuel Cell Council) test method; depending on the resistivity of the sample. In summary for the single fillers, the percolation threshold occurs at 1.4 vol% for carbon black, 2.1 vol% for carbon nanotubes, and 13 vol% for synthetic graphite. At the highest filler concentration, the carbon black produced a mean composite resistivity of 1 ohm-cm (15 wt%= 8.1 vol %), the carbon nanotubes produced a mean composite resistivity of 0.4 ohm-cm (15 wt% = 7.4 vol), and the synthetic graphite produced a mean composite resistivity of 0.09 ohm-cm (80 wt% =61.6 vol %). The electrical resistivity results for carbon black and synthetic graphite in Ticona’s Vectra A950 Liquid Crystal Polymer done in a previous study are very similar to the results obtained in this study [1]. For the Vectra composites the percolation threshold is 3.7 vol% for carbon black and 15 126 vol % for synthetic graphite. The lowest electrical resistivity for carbon black in Vectra is 2 ohm-cm (15 wt%= 12.1 vol %) and for the synthetic graphite in Vectra the lowest electrical resistivity for the 80 wt% (71.4 vol %) composite is 0.08 ohm-cm [1]. The full results are discussed in Chapter 6. 8.1.2: Effects of Multiple Conductive Fillers on Electrical Resistivity A factorial design was used to determine which filler had the greatest effect and to determine the interactions between the fillers, in the injection molded samples. For all three fillers the lowest loading was zero wt% but the high loading level varied depending on the filler. The high loading for carbon black was 2.5% wt, for synthetic graphite 65% wt, and for the FibrilTM carbon nanotubes 6 wt %. Table 8.1 -1 shows the different filler loading for the factorial design. The loading levels were chosen so that the composite would be conductive as well as have a low enough viscosity so that it could be extruded and injection molded into samples for testing. Table 8.1-1: Filler Loadings in Factorial Design Formulations Formulations No filler 2.5CB 65SG 6CNT 2.5CB*65SG 2.5CB*6CNT 65SG*6CNT 2.5CB*65SG*6CNT Ketjenblack wt% 0 2.5 0 0 2.5 2.5 0 2.5 Thermocarb wt% 0 0 65 0 65 0 65 65 127 FIBRILTM wt% 0 0 0 6 0 6 6 6 For the composites containing only single fillers, synthetic graphite, followed by carbon nanotubes, and then carbon black, cause a statistically significant decrease (negative effect term) in composite electrical resistivity. Synthetic graphite causes the largest decrease in electrical resistivity, followed closely by the carbon nanotubes. All the combinations of different fillers had a statistically significant effect on electrical resistivity. In every case, the effect is positive, which means that the composite electrical resistivity increases when these two or three different fillers are used together. This statistically significant effect and positive effect term for different carbon fillers has been noted previously in studies [1-2]. The full results are discussed in Chapter 6. The US Department of Energy electrical conductivity target for bipolar plates is 100 S/cm [3]. The composite with a value nearest to the US Department of Energy target is the 2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes formulation compression molded with a mean electrical resistivity of 0.011 ohm-cm, which gives an electrical conductivity result of 91 S/cm. The through-plane electrical resistivity (US Fuel Cell Council) test method was conducted on all of the multi-filler composites. This test simulates actual conditions in a fuel cell. Two observations were made. First the results from the through plane electrical resistivity (US Fuel Cell Council) test method are higher than the results from in plane electrical resistivity test method, likely due to filler are orientation. Second, the results collected at Michigan Technological University are similar to the results collected by Dana Corporation The full results and discussion are in Chapter 6. 128 8.1.3: Effects of Single Conductive Fillers on Thermal Conductivity Thermal conductivity tests were performed on all the formulations each containing different concentrations of Ketjenblack EC-600 JD carbon black, Thermocarb TC-300 synthetic graphite, and Hyperion FIBRILSTM nanotubes in polypropylene semi crystalline homopolymer resin H7012-35RN. The through plane thermal conductivity for all of the formulations was measured using the guarded heat flow meter method at 55ºC. The in-plane thermal conductivity was also measured using the transient plane source method at 23oC for composites that contained more than 30 weight percent synthetic graphite and all the multiple filler combinations (discussed in the next section). For the single filler composites it was shown that synthetic graphite caused the greatest increase in through plane thermal conductivity. Composites containing 80 wt% (61.6 vol%) synthetic graphite increased the through plane thermal conductivity from 0.20 W/m•K to 6.04 W/m•K. Composites containing 15 wt% (7.4 vol %) carbon nanotubes increases the through plane thermal conductivity to 0.47 W/ m•K and composites containing 15 wt% (8.1 vol %) carbon black increases the through plane thermal conductivity to 0.34 W/m•K. These values are very similar to those previously reported for this same carbon black and synthetic graphite in Vectra A950RX Liquid Crystal Polymer [4]. For the in-plane thermal conductivity, the composite containing 80 wt% (61.6 vol %) synthetic graphite had a result of 28.0 W/ m•K. The 80 wt% synthetic graphite composite had in plane thermal conductivity results higher than the desired bipolar plate 129 thermal conductivity target of at least 20.0 W/ m•K. All results are discussed in Chapter 7. 8.1.4: Effects of Multiple Conductive Fillers on Through-Plane Thermal Conductivity A factorial design was used to determine which filler had the greatest effect and to determine the interactions between the fillers, in the injection molded samples. For all three fillers the lowest loading was zero wt% but the high loading level varied depending on the filler. The high loading for carbon black was 2.5% wt, for synthetic graphite 65% wt, and for the FibrilTM carbon nanotubes 6 wt %. Table 8.1 -1 shows the different filler loading for the factorial design. For the composites containing only single fillers, synthetic graphite, followed by carbon nanotubes and then carbon black, cause a statistically significant increase in composite through-plane thermal conductivity. Synthetic graphite causes the largest increase in composite thermal conductivity. All of the combinations of the different fillers did cause a statistically significant increase in the through plane thermal conductivity in the composite. When multiple fillers are combined into a composite, the composite thermal conductivity is higher than what would be expected from the additive effect of each single filler. The composite containing all three fillers; the 2.5 wt% carbon black, 65 wt% synthetic graphite, and 6 wt% carbon nanotubes in polypropylene; had an in-plane thermal conductivity of 17.6 W/m•K when injection molded and a result of 24.0 W/ m•K when compression molded. The three filler compression molded composite had in plane 130 thermal conductivity results higher than the desired bipolar plate thermal conductivity target of at least 20.0 W/ m•K. Complete results are discussed in Chapter 7. 8.1.5: Miscellaneous Results Comparisons between the theoretical and the actual density for all of the formulations and the solvent digestion results showed that the gravimetric feeders used to feed the extruder are accurately putting in the amount of filler specified for each compound. The mean length and the mean aspect ratio results for the synthetic graphite showed that the length and aspect ratio stayed approximately the same even after being extruded and injection molded into samples. The length of the graphite went from 0.067 to on average and the aspect ratio went from 1.757 to on average 1.66. The orientation results on the synthetic graphite showed that when looking at the in-plane surface, the fillers are primarily aligned in the conductivity measurement direction and when looking at the through plane surface, the fillers are primarily aligned perpendicular to the conductivity measurement direction. The FESEM pictures show that the carbon nanotubes are forming networks, and these networks could help to increase the conductivity of the material. The complete results are discussed in Chapter 5. 8.2: Conclusions Below is a listing of some of the significant conclusions and contributions from this work. 131 • The carbon black had the lowest percolation point of the three fillers. Synthetic graphite at 80 wt% has the lowest electrical resistivity of the single fillers composites. The compression molded composite containing all three fillers had the electrical conductivity of 91 S/cm which is nearest to the target of 100 S/cm for fuel cell bipolar plates. • All the combinations of different fillers had a statistically significant effect on electrical resistivity. In each case, the effect term is positive meaning that the composite electrical resistivity increases when two or three different fillers are used together. • Thermocarb TC-300 synthetic graphite had the greatest impact on composite through-plane thermal conductivity, when compared to the carbon black and carbon nanotubes. • The in-plane thermal conductivity for the 80 wt% synthetic graphite injection molded composite (28.0 W/ m•K) and the three filler compression molded composite (24.0 W/ m•K) had results greater than 20 W/m·K, which is the target for fuel cell bipolar plates. • All the combinations of fillers increased the thermal conductivity of the composite. When multiple fillers were combined into a composite, the composite thermal conductivity is higher than what would be expected from the additive effect of each single filler. 132 • The thermal and electrical conductivity values found in this study using the polypropylene were very similar to values that had been previously reported for the same carbon black and synthetic graphite used in Vectra A950RX Liquid Crystal Polymer. 8.3: Recommendations for Future Work This study looked at the effect of three fillers had on electrical and thermal conductivity, as well as the interaction between these fillers in composites containing combinations of fillers. The electrical conductivity target for bipolar plates in fuel cells is 100 S/cm or higher and the thermal conductivity target is 20 W/m·K or higher. In our research, the three filler composite had an electrical conductivity near the target and a thermal conductivity above the target. Further optimization could be achieved by having a higher loading of the carbon nanotubes and synthetic graphite in the polypropylene since they caused largest decrease in electrical resistivity and the largest increase in thermal conductivity. This optimization could be the subject of future work and from this work polymer composites could be created that meet the electrical conductivity goal for bipolar plates and produce thermal conductivity values that are higher than those reported in this study. The process ability of the polymer composite is also a concern when making bipolar plates. If the material cannot be extruded or injection molded easily then the cost for producing bipolar plates will be higher. Increases in the carbon black and the carbon nanotubes in the composites create higher viscosities [5-6], which leads to processing issues. Looking at all these factors, the optimization of the three filler polypropylene 133 composite not only needs to meet the thermal and electrical conductivity targets but it also needs to be easy to work with when injection molding, compression molding, and extruding. Future work regarding the processablitiy of the three filler polypropylene composite should also be considered. Some possible formulations that could be examined are: • 70 wt% Synthetic Graphite, 6 wt% Carbon Nanotubes, 2 wt% Carbon Black • 70 wt% Synthetic Graphite, 7 wt% Carbon Nanotubes, 2 wt% Carbon Black • 65 wt% Synthetic Graphite, 7 wt% Carbon Nanotubes, 2 wt% Carbon Black • 65 wt% Synthetic Graphite, 8 wt% Carbon Nanotubes, 2 wt% Carbon Black Another factor that could be considered is the extruder conditions and screw design. When extruding the RPM and the temperature can make a difference on how well the polymer and carbon fillers mix together. If the screw is not turning fast enough or if the polymer is not melted, then the fillers could not be distributed evenly throughout the polymer matrix. This can lead to lower thermal and electrical conductivity results because the conductive networks will not be uniform. The screw design could also be changed to increase mixing. This could be done by changing the type of elements (kneading disks, kneading blocks, or screw elements) or by changing the position of the elements. Future work could be done to optimize the RPM, the temperature, and the screw design so that mixing with distribute the carbon fillers evenly throughout the polymer matrix and form uniform conductive networks that could achieve the thermal and electrical conductivity goals for bipolar plates. 134 8.4: References 1. J. A. King, R. L. Barton, R. A. Hauser, and J. M. Keith, Polymer Composites, 29, 421-428 (2008). 2. J. A. Heiser, J. A. King, J. P. Konell, I. Miskioglu, and L. L. Sutter, Advances in Polymer Technology, 23, 135-146 (2004). 3. K. Robberg and V. Trapp, Handbook of Fuel Cells- Fundamentals, Technology, and Applications Vol. 3: Fuel Cell Technology and Applications, W. Vielstick, H. A. Gasteiger and A. Lamm (Eds.), John Wiley & Sons, Ltd., West Sussex, England, 2003, 308-314. 4. R. A. Hauser, J. A. King, R. M. Pagel, and J. M. Keith, Journal of Applied Polymer Science, 109, 2145-2155 (2008). 5. J. A. King, F. A. Morrison, J. M. Keith, M. G. Miller, R. C. Smith, M. Cruz, A. M. Neuhalfen, and R. L. Barton, Journal of Applied Polymer Science, 101, 2680-2688 (2006). 6. Hyperion Catalysis International Fibril Product Literature, Hyperion Catalysis International, 38 Smith Place, 135 Cambridge, MA, 2008 Appendix A: Screw Design and Extrusion Run Conditions For Screw Type Elements GFA-d-ee-ff G = co-rotating F = conveying A = Free-Meshing d = number of threads ee = pitch (length in millimeters for one complete rotation) ff = length of screw elements in millimeters Kneading disks KS1-d-hh-i KS1 = Kneading disc d = number of threads h = length of kneading disc in millimeters i = A for initial disc and E for end disc Zones 0D to 4D is Zone 1 (water cooled, not heated) 4D to 8D is Zone 2 and Heating Zone 1 8D to 12D is Zone 3 and Heating Zone 2 12D to 16D is Zone 4 and Heating Zone 3 16D to 20D is Zone 5 and Heating Zone 4 20D to 24D is Zone 6 and Heating Zone 5 24D to 28D is Zone 7 and Heating Zone 6 28D to 32D is Zone 8 and Heating Zone 7 32D to 36D is Zone 9 and Heating Zone 8 36D to 40D is Zone 10 and Heating Zone 9 Nozzle is Heating Kneading disks KBj-d-kk-ll KB = kneading block j = number of kneading segments d = number of threads k = length of kneading block in millimeters l = twisting angle of the individual kneading segments Figure A.1: 5-14-2005 Extruder Screw Design 136 Table A.1: Purge Conditions Using Dow H7012-35RN Polypropylene Homopolymer Only Material Number Extrusion Date Extruder RPM Motor Amperage, % Melt Temperature, °C Melt Pressure, psig #3 Feeder Setting, lb/hr Material in Feeder #3 #4 Feeder Setting, lb/hr Material in Feeder #4 Vacuum Port Zone 5 Side Stuffer Setting, rpm Feeder at Zone 5 Zone 7 Side Stuffer setting, RPM Feeder at Zone 7 Feed Section Temperature Zone 1 Temperature, °C Zone 2 Temperature, °C Zone 3 Temperature, °C Zone 4 Temperature, °C Zone 5 Temperature, °C Zone 6 Temperature, °C Zone 7 Temperature, °C Zone 8 Temperature, °C Zone 9 Temperature, °C Zone 10 Temperature, °C Die Type and Gap Pelletizer Setting Output Rate, lbs/hr purge 5-20-08 250 30 260 0 20 Dow H7012-35RN -----1 atm 300 -300 -H2O cooled 150 180 195 210 220 220 220 215 215 210 3x3 mm H20 bath 20 Feeder 3= As Received Dow H7012-35RN Polypropylene 0.5 inch open helix with end stub, 0.75 inch nozzle side discharge IBM laptop, feeder3_VectraA950RX0.5in open0.75in side discharge jak.par 137 Table A.2: Ketjenblack EC-600 JD Carbon Black Formulations Material Number EA2.5P EA2.5PR EA4P EA5P EA6P EA7.5P EA10P EA15P Extrusion Date 5/20/2008 5/20/2008 5/20/2008 5/20/2008 5/21/2008 5/21/2008 5/21/2008 5/21/2008 Extruder RPM 250 250 275 275 275 275 275 275 Motor Amperage, % 24 23 24 24 25 26 28 34 Melt Temperature, °C 242 240 240 241 241 240 242 242 160 to 340 Melt Pressure, psig 0 0 0 0 0 0 0 to 30 #3 Feeder Setting, lb/hr 9.75 9.75 9.6 9.5 9.4 9.25 9 8.5 Material in Feeder #3 H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN #4 Feeder Setting, lb/hr 0.25 0.25 0.4 0.5 0.6 0.75 1 1.5 Material in Feeder #4 EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD Vacuum Port 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 300 300 300 300 300 300 Feeder at Zone 5 EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD EC600JD Zone 7 Side Stuffer setting, RPM 300 300 300 300 300 300 300 300 Feeder at Zone 7 -- -- -- -- -- -- -- -- Feed Section Temperature H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 150 150 150 150 150 150 Zone 2 Temperature, °C 180 180 180 180 180 180 180 180 Zone 3 Temperature, °C 195 195 195 195 195 195 195 195 Zone 4 Temperature, °C 210 210 210 210 210 210 210 210 Zone 5 Temperature, °C 220 220 220 220 220 220 220 220 Zone 6 Temperature, °C 220 220 220 220 220 220 220 220 Zone 7 Temperature, °C 220 220 220 220 220 220 220 220 Zone 8 Temperature, °C 220 220 220 220 220 220 220 220 Zone 9 Temperature, °C 220 220 220 220 220 220 220 220 Zone 10 Temperature, °C 220 220 220 220 220 220 220 220 Die Type and Gap 3 x 3 mm 3 x 3 mm 3 x 3 mm 3 x 3 mm 3 x 3 mm 3 x 3 mm 3 x 3 mm 3 x 3 mm Pelletizer Setting H2O bath H2O Bath H2O Bath H2O Bath H2O Bath H2O Bath H2O Bath H2O Bath Output Rate, lbs/hr 10 10 10 10 10 10 10 10 Feeder 4= As Received Ketjenblack EC-600 JD, ran on manual, 40:1 gear ratio, 0.5 inch helix with 0.75 inch vinyl nozzle and support Toshiba laptop, feeder4_0.5in open 0.75 in nozzle ketjen ec 600 jd jak.par 138 Table A.3a: Thermocarb TC-300 Synthetic Graphite Formulations Material Number EB10P EB15P EB20P EB25P EB30P EB35P EB40P EB45P Extrusion Date 5/13/2008 5/13/2008 5/13/2008 5/13/2008 5/13/2008 5/13/2008 5/13/2008 5/13/2008 Extruder RPM 250 250 250 300 300 300 300 300 Motor Amperage, % 51 36 32 40 35 35 32 32 Melt Temperature, °C 240 241 241 245 245 245 244 244 Melt Pressure, psig 0 0 0 60-70 70-80 90 50 100-110 #2 Feeder Setting, lb/hr 4.3 4.3 5 10 10 12 12 15 Material in Feeder #2 TC300 TC300 TC300 TC300 TC300 TC300 TC300 TC300 #3 Feeder Setting, lb/hr 38.7 24.4 20 30 23.3 22.3 18 18.3 Material in Feeder #3 H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN Vacuum Port 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 300 300 300 300 300 300 Feeder at Zone 5 TC300 TC300 TC300 TC300 TC300 TC300 TC300 TC300 Zone 7 Side Stuffer setting, RPM 300 300 300 300 300 300 300 300 Feeder at Zone 7 --------Feed Section Temperature H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 150 150 150 150 150 150 Zone 2 Temperature, °C 180 180 180 180 180 180 180 180 Zone 3 Temperature, °C 195 195 195 195 195 195 195 195 Zone 4 Temperature, °C 210 210 210 210 210 210 210 210 Zone 5 Temperature, °C 220 220 220 220 220 220 220 220 Zone 6 Temperature, °C 220 220 220 220 220 220 220 220 Zone 7 Temperature, °C 220 220 220 220 220 220 220 220 Zone 8 Temperature, °C 220 220 220 220 220 220 220 220 Zone 9 Temperature, °C 220 220 220 225 225 225 225 225 Zone 10 Temperature, °C 220 220 220 225 225 225 225 225 Die Type and Gap 3x3 mm 3x3 mm 3x3 mm 3x3 mm 3x3 mm 3x3 mm 3x3 mm 3x3 mm Pelletizer Setting H2O bath H2O bath H2O bath H2O bath H2O bath H2O bath H2O bath H2O bath Output Rate, lbs/hr 43 28.7 25 40 33.3 34.3 30 33.3 Feeder 2, As Received Thermocarb TC-300, 0.75inch open helix with 0.75 inch ID 1.38inch OD polyliner with cross hairs NEC laptop, feeder2_0.75inopen0.75inliner_thermocarb.par 139 Table A.3b: Thermocarb TC-300 Synthetic Graphite Formulations Material Number EB50P EB55P EB60P EB65P EB65PR EB70P EB75P EB80P Extrusion Date 5/13/2008 5/19/2008 5/19/2008 5/19/2008 5/19/2008 5/19/2008 5/19/2008 5/19/2008 Extruder RPM 325 325 350 400 400 400 425 450 Motor Amperage, % 29 30 28 22 22 18 20 18 Melt Temperature, °C 240 241 243 245 240 244 240-250 240 Melt Pressure, psig 120-130 0 0 0 10 0-100 0-230 0-600 #2 Feeder Setting, lb/hr 15 16 18 16 16 11 14 16 Material in Feeder #2 TC300 TC300 TC300 TC300 TC300 TC300 TC300 TC300 #3 Feeder Setting, lb/hr 15 13.1 12 8.6 8.6 4.7 4.7 4 Material in Feeder #3 H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN H7012-35RN Vacuum Port 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 300 300 300 300 300 300 Feeder at Zone 5 TC300 TC300 TC300 TC300 TC300 TC300 TC300 TC300 Zone 7 Side Stuffer setting, RPM 300 300 300 300 300 300 300 300 Feeder at Zone 7 -- -- -- -- -- -- -- -- Feed Section Temperature H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 150 150 150 150 150 150 Zone 2 Temperature, °C 180 180 180 180 180 180 180 180 Zone 3 Temperature, °C 195 195 195 195 195 195 195 195 Zone 4 Temperature, °C 210 210 210 210 210 210 210 210 Zone 5 Temperature, °C 220 220 220 220 220 220 220 220 Zone 6 Temperature, °C 220 220 220 220 220 220 220 220 Zone 7 Temperature, °C 220 220 220 220 220 220 220 220 Zone 8 Temperature, °C 220 220 220 220 220 220 220 220 Zone 9 Temperature, °C 225 225 225 225 225 225 225 225 Zone 10 Temperature, °C 225 225 225 225 225 225 225 225 Die Type and Gap Pelletizer Setting 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath 3x3 mm H2O bath Output Rate, lbs/hr 30 29.1 30 24.6 24.6 15.7 18.7 Feeder 2, As Received Thermocarb TC-300, 0.75inch open helix with 0.75 inch ID 1.38inch OD polyliner with cross hairs NEC laptop, feeder2_0.75inopen0.75inliner_thermocarb.pa 140 20 Table A.4a: Hyperion Fibril Carbon Nanotube Formulations Material Number Extrusion Date Extruder RPM Motor Amperage, % Melt Temperature, °C Melt Pressure, psig #3 Feeder Setting, lb/hr Material in Feeder #3 Vacuum Port Zone 5 Side Stuffer Setting, rpm Feeder at Zone 5 Zone 7 Side Stuffer setting, RPM Feeder at Zone 7 Feed Section Temperature Zone 1 Temperature, °C Zone 2 Temperature, °C Zone 3 Temperature, °C Zone 4 Temperature, °C Zone 5 Temperature, °C Zone 6 Temperature, °C Zone 7 Temperature, °C Zone 8 Temperature, °C Zone 9 Temperature, °C Zone 10 Temperature, °C Die Type and Gap Pelletizer Setting Output Rate, lbs/hr EQ1.5P 5/27/2008 250 43 243 0 30 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 215 215 200 3x3 mm H2O bath 30 EQ2.5P 5/12/2008 250 34 241 0 20 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 215 215 200 3x3 mm H2O bath 20 EQ2.5PR (Went to Dana) 5/27/2008 250 45 240 0 30 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 215 215 200 3x3 mm H2O bath 30 EQ4P EQ5P EQ6P EQ6PR 5/12/2008 5/12/2008 5/12/2008 5/21/2008 250 250 250 250 34 35 35 36 255 256 263 240 50-90 50-80 80-120 70-80 20 20 20 20 H7012-35RN & H7012-35RN & H7012-35RN & H7012-35RN & MB3020-01 MB3020-01 MB3020-01 MB3020-01 1 atm 1 atm 1 atm 1 atm 300 300 300 300 none none none none 300 300 300 300 none none none none H2O Cooled H2O Cooled H2O Cooled H2O Cooled 150 150 150 150 180 180 180 180 195 195 195 195 210 210 210 210 220 220 220 220 220 220 220 220 220 220 220 220 215 215 215 220 215 215 215 215 215 215 215 215 3x3 mm 3x3 mm 3x3 mm 3x3 mm H2O bath H2O bath H2O bath H2O bath 20 20 20 20 Mixed Hyperion MB3020-01 (20% wt fibrils in 80% wt polypropylene with MFI = 30g/10 min) in V Cone blender for 4 min (3lbs/batch) with Dow H7012-35RN prior to adding to Feeder 3 hopper. 141 Table A.4b: Hyperion Fibril Carbon Nanotube Formulations Material Number Extrusion Date Extruder RPM Motor Amperage, % Melt Temperature, °C Melt Pressure, psig #3 Feeder Setting, lb/hr Material in Feeder #3 Vacuum Port Zone 5 Side Stuffer Setting, rpm Feeder at Zone 5 Zone 7 Side Stuffer setting, RPM Feeder at Zone 7 Feed Section Temperature Zone 1 Temperature, °C Zone 2 Temperature, °C Zone 3 Temperature, °C Zone 4 Temperature, °C Zone 5 Temperature, °C Zone 6 Temperature, °C Zone 7 Temperature, °C Zone 8 Temperature, °C Zone 9 Temperature, °C Zone 10 Temperature, °C Die Type and Gap Pelletizer Setting Output Rate, lbs/hr EQ7.5P 5/12/2008 250 37 255 90-150 20 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 215 215 215 3x3 mm H2O bath 20 EQ7.5PR 5/13/2008 250 38 238 0 20 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 220 220 220 3x3 mm H2O bath 20 EQ10P 5/12/2008 250 40 262 100-220 20 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 215 215 220 3x3 mm H2O bath 20 142 EQ15P 5/13/2008 250 49 230 0 20 H7012-35RN & MB3020-01 1 atm 300 none 300 none H2O Cooled 150 180 195 210 220 220 220 220 220 220 3x3 mm H2O bath 20 Table A.5: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite Combinations Material Number Extrusion Date EA2.5B65P 5/22/2008 EA2.5B65PR 5/22/2008 250 Extruder RPM 250 Motor Amperage, % 18 19 Melt Temperature, °C 263 262 200 to 400 Melt Pressure, psig 0 to 200 #2 Feeder Setting, lb/hr 6.5 6.5 Material in Feeder #2 TC300 TC300 #3 Feeder Setting, lb/hr 3.25 3.25 Material in Feeder #3 #4 Feeder Setting, lb/hr H7012-35RN 0.25 H7012-35RN 0.25 Material in Feeder #4 Vacuum Port EC600JD 1 atm EC600JD 1 atm Zone 5 Side Stuffer Setting, rpm Feeder at Zone 5 Zone 7 Side Stuffer setting, RPM Feeder at Zone 7 300 TC300 300 EC600JD 300 TC300 300 EC600JD Feed Section Temperature H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 Zone 2 Temperature, °C 180 180 Zone 3 Temperature, °C 195 195 Zone 4 Temperature, °C 210 210 Zone 5 Temperature, °C 220 220 Zone 6 Temperature, °C 220 220 Zone 7 Temperature, °C 220 220 Zone 8 Temperature, °C 220 220 Zone 9 Temperature, °C Zone 10 Temperature, °C Die Type and Gap 225 225 3x3 mm 225 225 3x3 mm Pelletizer Setting H2O bath H2O bath Output Rate, lbs/hr 10 10 143 Table A.6: Ketjenblack EC-600 JD Carbon Black/Hyperion Fibril Carbon Nanotube Combinations Material Number EA2.5Q6P EA2.5Q6PR Extrusion Date 5/21/2008 5/22/2008 250 Extruder RPM 250 Motor Amperage, % 27 28 Melt Temperature, °C 245 240 Melt Pressure, psig 80-120 0 #3 Feeder Setting, lb/hr Material in Feeder #3 9.75 H7012-35RN & MB3020-01 9.75 H7012-35RN & MB3020-01 #4 Feeder Setting, lb/hr Material in Feeder #4 0.25 EC600JD 0.25 EC600JD Vacuum Port 1 atm 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 Feeder at Zone 5 EC600JD EC600JD Zone 7 Side Stuffer setting, RPM 300 300 Feeder at Zone 7 -- -- Feed Section Temperature H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 Zone 2 Temperature, °C 180 180 Zone 3 Temperature, °C 195 195 Zone 4 Temperature, °C 210 210 Zone 5 Temperature, °C 220 220 Zone 6 Temperature, °C 220 220 Zone 7 Temperature, °C 220 220 Zone 8 Temperature, °C 220 220 Zone 9 Temperature, °C 220 220 Zone 10 Temperature, °C 220 220 Die Type and Gap 3x3 mm 3x3 mm Pelletizer Setting H2O bath H2O bath Output Rate, lbs/hr 10 10 144 Table A.7: Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations Material Number EB65Q6P EB65Q6PR Extrusion Date 5/27/2008 5/27/2008 250 Extruder RPM 250 Motor Amperage, % 29 29 Melt Temperature, °C 260 261 60 to 800 Melt Pressure, psig 0 to 60 #2 Feeder Setting, lb/hr 6.5 6.5 Material in Feeder #2 TC300 TC300 #3 Feeder Setting, lb/hr Material in Feeder #3 3.5 H7012-35RN & MB3020-01 3.5 H7012-35RN & MB3020-01 1 atm Vacuum Port 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 Feeder at Zone 5 TC300 TC300 Zone 7 Side Stuffer setting, RPM Feeder at Zone 7 300 -- 300 -- Feed Section Temperature H2O Cooled H2O Cooled Zone 1 Temperature, °C 150 150 Zone 2 Temperature, °C 180 180 Zone 3 Temperature, °C 195 195 Zone 4 Temperature, °C 210 210 Zone 5 Temperature, °C 220 220 Zone 6 Temperature, °C 220 220 Zone 7 Temperature, °C 220 220 Zone 8 Temperature, °C 220 220 Zone 9 Temperature, °C 225 225 Zone 10 Temperature, °C 225 225 Die Type and Gap 3x3 mm 3x3 mm Pelletizer Setting H2O bath H2O bath Output Rate, lbs/hr 10 10 145 Table A.8: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations Material Number Extrusion Date EA2.5B65Q6P 5/22/2008 EA2.5B65Q6PR 5/22/2008 Extruder RPM 250 250 Motor Amperage, % 33 33 Melt Temperature, °C Melt Pressure, psig 274 0 to 900 270 10 to 1100 #2 Feeder Setting, lb/hr 6.5 6.5 Material in Feeder #2 TC300 TC300 #3 Feeder Setting, lb/hr Material in Feeder #3 3.25 H7012-35RN & MB3020-01 3.25 H7012-35RN & MB3020-01 #4 Feeder Setting, lb/hr Material in Feeder #4 Vacuum Port 0.25 EC600JD 1 atm 0.25 EC600JD 1 atm Zone 5 Side Stuffer Setting, rpm 300 300 TC300 Feeder at Zone 5 TC300 Zone 7 Side Stuffer setting, RPM 300 300 Feeder at Zone 7 Feed Section Temperature EC600JD H2O Cooled EC600JD H2O Cooled Zone 1 Temperature, °C 150 150 Zone 2 Temperature, °C 180 180 Zone 3 Temperature, °C 195 195 Zone 4 Temperature, °C 210 210 Zone 5 Temperature, °C 220 220 Zone 6 Temperature, °C 220 220 Zone 7 Temperature, °C 220 220 Zone 8 Temperature, °C 220 220 Zone 9 Temperature, °C 215 215 Zone 10 Temperature, °C Die Type and Gap 215 3x3 mm 215 3x3 mm Pelletizer Setting H2O bath H2O bath Output Rate, lbs/hr 10 10 146 Appendix B: Injection Mold Run Conditions Table B.1: Ketjenblack EC-600 JD Carbon Black Formulations Notation Tmold Injection Molding Conditions Mold Temperature (F) EA2.5P 6-3-08 100 EA2.5PR 6-3-08 100 EA4P 6-3-08 100 EA5P 6-3-08 100 EA6P 6-3-08 100 EA7.5P 6-3-08 100 EA10P 6-3-08 100 EA15P 6-3-08 100 E1 Zone 1 Temperature (F) (nozzle) 540 540 540 540 540 580 590 600 E2 E3 Zone 2 Temperature (F) Zone 3 Temperature (F) 530 480 530 480 530 480 530 480 530 480 570 560 580 570 590 580 E4 Zone 4 Temperature (F) (feed zone) 300 300 300 300 300 325 325 325 P1 P2 Injection pressure (psi) Hold Pressure (psi) 4522 4522 4522 4522 4522 4522 4522 4522 4522 4522 4522 4522 3391.5 3391.5 9044 9044 P7 Back Pressure (psi) 22.61 22.61 22.61 22.61 22.61 22.61 22.61 22.61 S1 Shot size (mm) 42 42 42 42 42 42 42 42 S2 Pullback before (mm) 0 0 0 0 0 0 0 0 S3 Pullback after (mm) 0 0 0 0 0 0 0 0 S6 Width of mold (mm) 196 196 196 196 196 196 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 15 15 15 15 15 15 T1 Injection Time (s) 10 10 10 10 10 10 10 10 T2 Cool Time (s) 6 6 6 8 8 8 8 8 T3 Interval Time (s) 2 2 2 2 2 2 2 2 T6 Retraction Time (s) 0 0 0 0 0 0 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 0 0 0 0 0 0 T8 Injection Delay Time (s) 0 0 0 0 0 0 0 0 T9 V1 Charge Delay Time (s) Injection Velocity (mm3/s) 0 100907.7 0 100907.7 0 100907.7 0 100907.7 0 100907.7 0 100907.7 0 100907.7 0 100907.7 128 V6 Screw Rotation (rpm) 128 128 128 128 128 128 128 V9 Retraction Velocity (rpm) 288 288 288 288 288 288 288 288 V10 Advance Velocity (rpm) 288 288 288 288 288 288 288 288 V11 Retraction Velocity (rpm) 288 288 288 288 288 288 288 288 CF Clamp Force (US tons) 80 80 80 80 80 80 80 80 147 Table B.2a: Thermocarb TC-300 Synthetic Graphite Formulations Notation Injection Molding Conditions EP 5-29-08 EB10P 5-29-08 EB15P 5-29-08 EB20P 5-29-08 EB25P 5-29-08 EB30P 5-29-08 EB35P 5-29-08 EB40P 5-29-08 EB45P 5-29-08 Tmold Mold Temperature (F) 100 100 100 100 100 100 100 100 100 E1 Zone 1 Temperature (F) (nozzle) 430 440 440 440 440 440 440 440 440 E2 Zone 2 Temperature (F) 400 420 420 420 420 420 420 420 420 E3 Zone 3 Temperature (F) 350 400 400 400 400 400 400 400 400 E4 Zone 4 Temperature (F) (feed zone) 300 300 300 300 300 300 300 300 300 P1 Injection pressure (psi) 9044 9044 9044 9044 9044 9044 9044 9044 9044 P2 Hold Pressure (psi) 9044 9044 9044 9044 9044 9044 9044 9044 9044 P7 Back Pressure (psi) 22.61 22.61 22.61 22.61 22.61 22.61 22.61 22.61 22.61 S1 Shot size (mm) 40 40 40 40 40 40 40 40 40 S2 Pullback before (mm) 2 0 0 0 0 0 0 0 0 S3 Pullback after (mm) 5 0 0 0 0 0 0 0 0 S6 Width of mold (mm) 196 196 196 196 196 196 196 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 15 15 15 15 15 15 15 T1 Injection Time (s) 15 10 10 10 10 10 10 10 10 T2 Cool Time (s) 15 6 6 6 6 6 6 6 6 T3 Interval Time (s) 2 2 2 2 2 2 2 2 2 T6 Retraction Time (s) 2 0 0 0 0 0 0 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 0 0 0 0 0 0 0 T8 Injection Delay Time (s) 0 0 0 0 0 0 0 0 0 0 0 0 0 T9 Charge Delay Time (s) V1 Injection Velocity (mm /s) 40770.8 V6 Screw Rotation (rpm) 128 128 V9 Retraction Velocity (rpm) 128 288 V10 Advance Velocity (rpm) 288 V11 Retraction Velocity (rpm) 288 CF Clamp Force (US tons) 80 3 2 0 0 0 0 100907.7 100907.7 100907.7 100907.7 128 128 128 128 128 128 128 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 288 80 80 80 80 80 80 80 80 100907.7 100907.7 148 100907.7 100907.7 Table B.2b: Thermocarb TC-300 Synthetic Graphite Formulations Notation Injection Molding Conditions EB45P 5-29-08 EB50P 5-29-08 EB55P 5-29-08 EB60P 5-29-08 EB65P 5-29-08 EB65PR 5-29-08 EB70P 5-29-08 EB75P 5-29-08 EB80P 5-29-08 Tmold Mold Temperature (F) 100 100 100 100 100 100 100 100 200 E1 Zone 1 Temperature (F) (nozzle) 440 440 440 440 440 440 440 460 590 E2 Zone 2 Temperature (F) 420 420 420 420 420 420 420 440 570 E3 Zone 3 Temperature (F) 400 400 400 400 400 400 400 420 520 E4 Zone 4 Temperature (F) (feed zone) 300 300 300 300 300 300 300 300 300 P1 P2 Injection pressure (psi) Hold Pressure (psi) 9044 9044 9044 9044 9044 9044 9044 9044 12435.5 12435.5 12435.5 12435.5 14696.5 14696.5 21479.5 21479.5 20349 20349 P7 Back Pressure (psi) 22.61 22.61 22.61 22.61 22.61 22.61 22.61 22.61 22.61 S1 Shot size (mm) 40 40 40 40 42 42 44 44 44 S2 Pullback before (mm) 0 0 0 0 0 0 0 0 0 S3 S6 Pullback after (mm) Width of mold (mm) 0 196 0 196 0 196 0 196 0 196 0 196 0 196 0 196 0 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 15 15 15 15 15 15 15 T1 Injection Time (s) 10 10 10 10 10 10 10 10 10 T2 Cool Time (s) 6 6 6 6 6 6 6 6 6 T3 Interval Time (s) 2 2 2 2 2 2 2 2 2 T6 Retraction Time (s) 0 0 0 0 0 0 0 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 0 0 0 0 0 0 0 T8 Injection Delay Time (s) 0 0 0 0 0 0 0 0 0 T9 Charge Delay Time (s) 0 0 0 0 0 0 0 0 0 3 V1 Injection Velocity (mm /s) 100907.7 100907.7 100907.7 100907.7 100907.7 100907.7 V6 Screw Rotation (rpm) 128 128 128 128 128 128 100907.7 100907.7 100907.7 128 128 128 V9 Retraction Velocity (rpm) 288 288 288 288 288 288 288 288 288 V10 Advance Velocity (rpm) 288 288 288 288 288 288 288 288 288 V11 Retraction Velocity (rpm) 288 288 288 288 288 288 288 288 288 CF Clamp Force (US tons) 80 80 80 80 80 80 80 80 80 149 Table B.3a: Hyperion Fibril Carbon Nanotube Formulations Notation Injection Molding Conditions EQ1.5P 6-4-08 EQ2.5P 6-4-08 EQ4P 6-4-08 EQ5P 6-4-08 EQ6P 6-4-08 EQ6PR 6-4-08 EQ7.5P 6-4-08 Tmold Mold Temperature (F) 100 100 100 100 100 100 100 E1 Zone 1 Temperature (F) (nozzle) 460 470 490 500 500 500 510 E2 Zone 2 Temperature (F) 440 450 470 480 480 480 490 E3 Zone 3 Temperature (F) 420 430 450 450 450 450 470 E4 Zone 4 Temperature (F) (feed zone) 300 300 300 300 300 300 300 P1 P2 P7 Injection pressure (psi) Hold Pressure (psi) Back Pressure (psi) 4522 4522 22.61 4522 4522 22.61 4522 4522 22.61 4522 4522 22.61 4522 4522 22.61 4522 4522 22.61 4522 4522 22.61 S1 Shot size (mm) 40 40 40 40 40 40 40 S2 Pullback before (mm) 0 0 0 0 0 0 0 S3 Pullback after (mm) 0 0 0 0 0 0 0 S6 Width of mold (mm) 196 196 196 196 196 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 15 15 15 15 15 T1 Injection Time (s) 10 10 10 10 10 10 10 T2 T3 Cool Time (s) Interval Time (s) 8 2 8 2 8 2 8 2 8 2 8 2 8 2 T6 Retraction Time (s) 0 0 0 0 0 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 0 0 0 0 0 T8 Injection Delay Time (s) 0 0 0 0 0 0 0 T9 Charge Delay Time (s) 0 0 0 0 0 0 0 V1 Injection Velocity (mm3/s) 100907.7 100907.7 100907.7 100907.7 100907.7 100907.7 100907.7 V6 Screw Rotation (rpm) 128 128 128 128 128 128 128 V9 Retraction Velocity (rpm) 288 288 288 288 288 288 288 V10 Advance Velocity (rpm) 288 288 288 288 288 288 288 V11 Retraction Velocity (rpm) 288 288 288 288 288 288 288 CF Clamp Force (US tons) 80 80 80 80 80 80 80 150 Table B.3b: Hyperion Fibril Carbon Nanotube Formulations Notation Tmold Injection Molding Conditions Mold Temperature (F) EQ7.5PR 6-4-08 100 EQ10P 6-4-08 100 EQ15P 6-4-08 100 EQ20P 6-4-08 100 E1 Zone 1 Temperature (F) (nozzle) 510 520 530 560 E2 Zone 2 Temperature (F) 490 500 510 540 E3 Zone 3 Temperature (F) 470 480 490 520 E4 Zone 4 Temperature (F) (feed zone) 300 300 300 300 P1 Injection pressure (psi) 4522 4522 7913.5 11305 P2 Hold Pressure (psi) 4522 4522 7913.5 11305 P7 Back Pressure (psi) 22.61 22.61 22.61 22.61 S1 Shot size (mm) 40 40 40 42 S2 Pullback before (mm) 0 0 0 0 S3 Pullback after (mm) 0 0 0 0 S6 S8 Width of mold (mm) Screw Position to Switch from P1 to P2 (mm) 196 15 196 15 196 15 196 15 T1 Injection Time (s) 10 10 10 10 T2 Cool Time (s) 8 8 8 8 T3 Interval Time (s) 2 2 2 2 T6 T7 Retraction Time (s) Nozzle Retraction Delay Time (s) 0 0 0 0 0 0 0 0 T8 Injection Delay Time (s) 0 0 0 0 T9 V1 Charge Delay Time (s) Injection Velocity (mm3/s) 0 100907.7 0 100907.7 0 100907.7 0 100907.7 V6 Screw Rotation (rpm) 128 128 128 128 V9 Retraction Velocity (rpm) 288 288 288 288 V10 Advance Velocity (rpm) 288 288 288 288 V11 Retraction Velocity (rpm) 288 288 288 288 CF Clamp Force (US tons) 80 80 80 80 151 Table B.4: Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite Combinations Notation Tmold Injection Molding Conditions Mold Temperature (F) EA2.5B65P 6-4-08 250 EA2.5B65PR 6-4-08 250 E1 Zone 1 Temperature (F) (nozzle) 640 640 E2 Zone 2 Temperature (F) 620 620 E3 Zone 3 Temperature (F) 590 590 E4 Zone 4 Temperature (F) (feed zone) 300 300 P1 Injection pressure (psi) 11305 11305 P2 Hold Pressure (psi) 11305 11305 P7 Back Pressure (psi) 22.61 22.61 S1 Shot size (mm) 20 20 S2 Pullback before (mm) 0 0 S3 Pullback after (mm) 0 0 S6 Width of mold (mm) 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 T1 T2 Injection Time (s) Cool Time (s) 10 10 10 10 T3 Interval Time (s) 2 2 T6 Retraction Time (s) 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 T8 Injection Delay Time (s) 0 0 T9 Charge Delay Time (s) 0 0 100907.73 100907.73 V1 3 Injection Velocity (in /s) V6 Screw Rotation (rpm) 128 128 V9 Retraction Velocity (rpm) 288 288 V10 Advance Velocity (rpm) 288 288 V11 Retraction Velocity (rpm) 288 288 CF Clamp Force (US tons) 80 80 152 Table B.5: Ketjenblack EC-600 JD Carbon Black/Hyperion Fibril Carbon Nanotube Combinations Notation Injection Molding Conditions EA2.5Q6P 6-5-08 EA2.5Q6PR 6-5-08 Tmold Mold Temperature (F) 100 250 E1 Zone 1 Temperature (F) (nozzle) 570 570 E2 Zone 2 Temperature (F) 560 560 E3 Zone 3 Temperature (F) 520 520 E4 Zone 4 Temperature (F) (feed zone) 300 300 P1 Injection pressure (psi) 5652.5 5652.5 P2 P7 Hold Pressure (psi) Back Pressure (psi) 5652.5 22.61 5652.5 22.61 S1 Shot size (mm) 40 40 S2 Pullback before (mm) 0 0 S3 Pullback after (mm) 0 0 S6 Width of mold (mm) 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 T1 Injection Time (s) 10 10 T2 Cool Time (s) 20 20 T3 Interval Time (s) 2 2 T6 Retraction Time (s) 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 T8 Injection Delay Time (s) 0 0 T9 Charge Delay Time (s) 0 0 V1 Injection Velocity (in3/s) 100907.73 100907.73 V6 Screw Rotation (rpm) 128 128 V9 Retraction Velocity (rpm) 288 288 V10 Advance Velocity (rpm) 288 288 V11 Retraction Velocity (rpm) 288 288 CF Clamp Force (US tons) 80 80 153 Table B.6: Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations Notation Injection Molding Conditions EB65Q6P 6-4-08 EB65Q6PR 6-4-08 Tmold Mold Temperature (F) 250 250 E1 Zone 1 Temperature (F) (nozzle) 640 640 E2 Zone 2 Temperature (F) 620 620 E3 Zone 3 Temperature (F) 590 590 E4 Zone 4 Temperature (F) (feed zone) 300 300 P1 Injection pressure (psi) 11305 11305 P2 Hold Pressure (psi) 11305 11305 P7 Back Pressure (psi) 22.61 22.61 S1 Shot size (mm) 20 20 S2 Pullback before (mm) 0 0 S3 Pullback after (mm) 0 0 S6 Width of mold (mm) 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 T1 Injection Time (s) 10 10 T2 Cool Time (s) 10 10 T3 Interval Time (s) 2 2 T6 Retraction Time (s) 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 T8 Injection Delay Time (s) 0 0 T9 Charge Delay Time (s) 0 0 3 V1 Injection Velocity (mm /s) 100907.7 100907.73 V6 Screw Rotation (rpm) 128 128 V9 Retraction Velocity (rpm) 288 288 V10 Advance Velocity (rpm) 288 288 V11 Retraction Velocity (rpm) 288 288 CF Clamp Force (US tons) 80 80 154 Table B.7:Ketjenblack EC-600 JD Carbon Black/Thermocarb TC-300 Synthetic Graphite/ Hyperion Fibril Carbon Nanotube Combinations Notation Injection Molding Conditions EA2.5B65Q6P 6-5-08 EA2.5B65Q6P 6-5-08 Tmold Mold Temperature (F) 250 250 E1 Zone 1 Temperature (F) (nozzle) 680 680 E2 Zone 2 Temperature (F) 680 680 E3 Zone 3 Temperature (F) 670 670 E4 Zone 4 Temperature (F) (feed zone) 300 300 P1 Injection pressure (psi) 22383.9 22383.9 P2 Hold Pressure (psi) 22383.9 22383.9 P7 Back Pressure (psi) 22.61 22.61 S1 Shot size (mm) 30 30 S2 Pullback before (mm) 0 0 S3 Pullback after (mm) 0 0 S6 Width of mold (mm) 196 196 S8 Screw Position to Switch from P1 to P2 (mm) 15 15 T1 Injection Time (s) 10 10 T2 Cool Time (s) 20 20 T3 Interval Time (s) 2 2 T6 Retraction Time (s) 0 0 T7 Nozzle Retraction Delay Time (s) 0 0 T8 Injection Delay Time (s) 0 0 T9 Charge Delay Time (s) 0 0 100907.73 100907.73 V1 3 Injection Velocity (in /s) V6 Screw Rotation (rpm) 128 128 V9 Retraction Velocity (rpm) 288 288 V10 Advance Velocity (rpm) 288 288 V11 Retraction Velocity (rpm) 288 288 CF Clamp Force (US tons) 80 80 155 Appendix C: Electrical Resistivity Through Plane Electrical Resistivity ASTM D257 EP Table C.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/9/2008 6/9/2008 6/9/2008 6/9/2008 6/10/2008 6/10/2008 6/10/2008 6/10/2008 Sample Number EP-TC-34 EP-TC-29 EP-TC-42 EP-TC-31 EP-TC-30 EP-TC-40 EP-TC-38 EP-TC-36 Applied Voltage (V) 100 100 100 100 100 100 100 100 Average Standard Deviation Number of Samples Through-Plane Surface Electrical Resistivity (Ω/square) 3.4485E+17 2.6769E+16 6.6064E+16 2.4065E+17 1.1465E+17 4.0826E+17 7.0552E+16 5.3541E+16 1.6567E+17 1.4639E+17 8 Through-Plane Volume Electrical Resistivity (Ω-cm) 1.2778E+17 9.6452E+16 1.5180E+17 1.6797E+17 1.7246E+17 1.5169E+17 2.8755E+17 1.6753E+17 1.6540E+17 5.5451E+16 8 Table C.2:Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number 6/26/2008 EPR-TC-21 6/26/2008 EPR-TC-14 6/26/2008 EPR-TC-18 6/26/2008 EPR-TC-37 6/26/2008 EPR-TC-19 6/27/2008 EPR-TC-32 Applied Voltage (V) 100 100 100 100 100 100 Average Standard Deviation Number of Samples 156 Through-Plane Volume Electrical Resistivity (Ω-cm) 1.4809E+17 1.0799E+17 1.1145E+17 1.6488E+17 1.9246E+17 1.2581E+17 1.4178E+17 3.3041E+16 6 EAP’s Table C.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number 6/22/2008 EA2.5P-TC-15 6/23/2008 EA2.5P-TC-21 6/24/2008 EA2.5P-TC-27 6/25/2008 EA2.5P-TC-10 6/26/2008 EA2.5P-TC-11 6/27/2008 EA2.5P-TC-16 6/28/2008 EA2.5P-TC-8 6/29/2008 EA2.5P-TC-7 6/30/2008 EA2.5P-TC-6 Applied Voltage (V) 100 100 100 100 100 100 100 100 100 Average Standard Deviation Number of Samples Through-Plane Surface Electrical Resistivity (Ω/square) 8.4963E+16 2.9833E+16 1.6643E+16 6.0122E+15 2.1159E+16 2.0637E+16 3.4423E+15 1.1126E+16 5.9666E+16 2.8165E+16 2.7046E+16 9 Through-Plane Volume Electrical Resistivity (Ω-cm) 7.2907E+15 1.1291E+16 6.1948E+15 1.2104E+16 1.1254E+16 1.0822E+16 2.1485E+16 7.0309E+15 1.1572E+16 1.1005E+16 4.5313E+15 9 Table C.4: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number 6/23/2008 EA2.5PR-TC-23 6/23/2008 EA2.5PR-TC-27 6/23/2008 EA2.5PR-TC-3 6/25/2008 EA2.5PR-TC-28 6/25/2008 EA2.5PR-TC-17 6/25/2008 EA2.5PR-TC-13 Applied Voltage (V) 100 100 100 100 100 100 Average Standard Deviation Number of Samples 157 Through-Plane Through-Plane Surface Electrical Volume Electrical Resistivity Resistivity (Ω/square) (Ω-cm) 3.6056E+15 9.9202E+15 2.8088E+15 1.1018E+16 1.3384E+15 1.6600E+16 2.8593E+15 1.9300E+16 5.5352E+15 1.2312E+16 5.0930E+15 9.7245E+15 3.5401E+15 1.3146E+16 1.5647E+15 3.9278E+15 6 6 EBP’s Table C.5: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/9/2008 6/9/2008 6/9/2008 6/9/2008 6/10/2008 6/10/2008 6/10/2008 6/10/2008 Through-Plane Through-Plane Surface Electrical Volume Electrical Resistivity Resistivity Sample Number Applied Voltage (V) (Ω/square) (Ω-cm) EB10P-TC-14 100 2.1659E+17 1.1045E+17 EB10P-TC-21 100 4.0659E+17 1.2347E+17 EB10P-TC-15 100 1.9818E+17 1.1974E+17 EB10P-TC-22 100 4.9996E+16 1.8176E+17 EB10P-TC-20 100 2.2019E+17 1.8084E+17 EB10P-TC-37 100 4.1565E+17 1.2439E+17 EB10P-TC-30 100 1.5417E+17 1.5417E+17 EB10P-TC-31 100 1.1639E+17 1.1639E+17 Average 2.2222E+17 1.3890E+17 Standard Deviation 1.2957E+17 2.9182E+16 Number of Samples 8 8 Table C.6: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/9/2008 6/9/2008 6/9/2008 6/9/2008 6/11/2008 6/11/2008 Sample Number EB15P-TC-32 EB15P-TC-26 EB15P-TC-29 EB15P-TC-24 EB15P-TC-31 EB15P-TC-25 Applied Voltage (V) 100 100 100 100 100 100 Average Standard Deviation Number of Samples 158 Through-Plane Surface Through-Plane Electrical Volume Electrical Resistivity Resistivity (Ω/square) (Ω-cm) 5.2021E+17 8.7512E+16 7.8426E+16 8.8833E+16 1.6663E+17 9.5645E+16 1.9415E+14 9.5948E+16 8.0739E+16 1.1524E+17 5.6607E+15 8.2221E+16 1.4198E+17 9.4233E+16 1.9501E+17 1.1531E+16 6 6 Table C.7: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/10/2008 6/10/2008 6/13/2008 6/13/2008 6/13/2008 6/13/2008 Sample Number EB20P-TC-28 EB20P-TC-25 EB20P-TC-32 EB20P-TC-33 EB20P-TC-21 EB20P-TC-22 Through-Plane Surface Electrical Resistivity (Ω/square) Applied Voltage (V) 100 3.5911E+17 100 5.6122E+17 100 4.6663E+17 100 1.4002E+17 100 1.2464E+17 100 1.9275E+17 Average 3.0740E+17 Standard Deviation 1.8276E+17 Number of Samples 6 Through-Plane Volume Electrical Resistivity (Ω-cm) 6.5416E+16 6.9713E+16 3.9997E+16 6.9254E+16 7.4065E+16 5.2983E+16 6.1905E+16 1.2921E+16 6 Table C.8: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/10/2008 6/10/2008 6/13/2008 6/13/2008 6/13/2008 6/13/2008 Sample Number EB25P-TC-22 EB25P-TC-30 EB25P-TC-27 EB25P-TC-21 EB25P-TC-24 EB25P-TC-25 Through-Plane Surface Through-Plane Electrical Volume Electrical Resistivity Resistivity (Ω-cm) Applied Voltage (V) (Ω/square) 100 3.7318E+16 2.7989E+16 100 1.8916E+16 3.8646E+16 100 6.2911E+16 3.8805E+16 100 3.0026E+16 3.0026E+16 100 2.9757E+16 2.9757E+16 100 2.2309E+16 3.4860E+16 Average 3.3540E+16 3.3347E+16 Standard Deviation 1.5771E+16 4.7494E+15 Number of Samples 6 6 159 Table C.9: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/25/2008 6/13/2008 6/13/2008 6/13/2008 6/16/2008 6/16/2008 Sample Number EB30P-TC-15 EB30P-TC-23 EB30P-TC-29 EB30P-TC-24 EB30P-TC-26 EB30P-TC-28 Through-Plane Through-Plane Surface Volume Electrical Electrical Resistivity Resistivity Applied Voltage (V) (Ω/square) (Ω-cm) 10 1.9360E+08 1.4528E+08 10 3.7185E+07 8.8690E+07 10 3.2852E+08 1.0053E+08 10 9.0414E+08 1.3546E+08 10 1.6717E+08 7.5678E+07 10 1.2344E+08 9.7935E+07 Average 2.9234E+08 1.0726E+08 Standard Deviation 3.1453E+08 2.7259E+07 Number of Samples 6 6 160 EQP’s Table C.10: 1.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/18/2008 6/18/2008 6/18/2008 6/18/2008 6/18/2008 6/18/2008 Sample Number EQ1.5P-TC-22 EQ1.5P-TC-25 EQ1.5P-TC-28 EQ1.5P-TC-12 EQ1.5P-TC-34 EQ1.5P-TC-20 Through-Plane Surface Electrical Resistivity Applied Voltage (V) (Ω/square) 100 3.9428E+17 100 6.3633E+16 100 2.5774E+17 100 4.2213E+17 100 3.2529E+17 100 3.8497E+17 Average 3.0801E+17 Standard Deviation 1.3337E+17 Number of Samples 6 Through-Plane Volume Electrical Resistivity (Ω-cm) 9.9821E+16 1.0361E+17 1.0210E+17 9.3794E+16 9.6150E+16 9.8689E+16 9.9027E+16 3.6566E+15 6 Table C.11: 2.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/19/2008 Sample Number EQ2.5P-TC-25 EQ2.5P-TC-30 EQ2.5P-TC-19 EQ2.5P-TC-12 EQ2.5P-TC-22 EQ2.5P-TC-17 EQ2.5P-TC-31 EQ2.5P-TC-27 EQ2.5P-TC-16 Through-Plane Through-Plane Surface Volume Electrical Electrical Resistivity Resistivity (Ω/square) (Ω-cm) Applied Voltage (V) 100 8.8323E+15 2.4614E+16 100 2.3801E+15 1.4223E+16 100 1.2076E+16 1.6333E+16 100 3.8142E+16 1.1546E+16 100 4.7513E+15 1.4296E+16 100 2.9664E+16 7.8107E+15 100 1.1756E+16 1.4512E+16 100 1.3312E+16 1.0702E+16 100 4.1869E+16 8.6357E+15 Average 1.8087E+16 1.3630E+16 Standard Deviation 1.4625E+16 5.0156E+15 Number of Samples 9 9 161 Table C.12: 4 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 6/17/2008 6/17/2008 6/17/2008 6/17/2008 6/17/2008 Sample Number EQ4P-TC-16 EQ4P-TC-28 EQ4P-TC-21 EQ4P-TC-26 EQ4P-TC-10 EQ4P-TC-31 Through-Plane Through-Plane Surface Volume Electrical Electrical Resistivity Resistivity Applied Voltage (V) (Ω/square) (Ω-cm) 100 2.7264E+16 2.3197E+15 1 3.3201E+15 3.1579E+15 10 3.4009E+15 2.8855E+15 10 4.1535E+16 2.8807E+15 10 2.4869E+16 2.4076E+15 100 4.0697E+17 2.5928E+15 Average 8.4560E+16 2.7074E+15 Standard Deviation 1.5864E+17 3.2188E+14 Number of Samples 6 6 Table C.13: 5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/19/2008 6/19/2008 6/19/2008 6/19/2008 6/20/2008 6/20/2008 Sample Number EQ5P-TC-24 EQ5P-TC-14 EQ5P-TC-23 EQ5P-TC-13 EQ5P-TC-9 EQ5P-TC-15 Through- Through-Plane Volume Plane Surface Electrical Electrical Resistivity Resistivity Applied Voltage (V) (Ω/square) (Ω-cm) 10 1.2527E+07 9.0142E+06 10 5.0093E+10 5.6735E+07 10 1.0334E+10 1.7431E+08 10 2.1893E+11 3.7837E+06 10 8.4092E+08 5.5229E+07 10 1.3138E+09 1.4064E+07 Average 4.6921E+10 5.2189E+07 Standard Deviation 8.6417E+10 6.4194E+07 Number of Samples 6 6 162 In Plane Electrical Conductivity EAP’s 163 Table C.14: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/18/2008 Test Date 6/18/2008 Test Date 6/18/2008 Test Date 6/18/2008 Test Date 6/18/2008 Sample Number EA10P-T-26 Sample Number EA10P-T-20 Sample Number EA10P-T-28 Sample Number EA10P-T-22 Sample Number EA10P-T-25 Dot 1 2 4 5 Dot 1 2 3 4 5 6 Dot 1 2 3 4 5 6 Dot 1 2 3 4 5 6 Dot 1 2 3 4 Thickness(mm) 1.63 1.63 1.63 1.64 Thickness(mm) 1.62 1.63 1.62 1.6 1.62 1.62 Thickness(mm) 1.64 1.63 1.62 1.65 1.64 1.64 Thickness(mm) 1.65 1.65 1.62 1.61 1.62 1.63 Thickness(mm) 1.66 1.6 1.09 1.6 Width (mm) 2.01 2.02 2.05 2.1 Width (mm) 2.07 2.09 2.13 2.08 2.09 2.2 Width (mm) 2.01 1.99 2.01 2.19 2.25 2.26 Width (mm) 1.98 2.01 2.01 2.04 2.1 2.24 Width (mm) 2.33 2.14 1.51 2.28 Amps (A) Volts(mV) 4.00E-05 2.150 4.00E-05 2.060 4.00E-05 1.770 4.00E-05 1.840 Average Standard Deviation Number of Samples ER (ohm-cm) 3.036 2.924 2.549 2.731 Amps (A) Volts(mV) 4.00E-05 1.990 4.00E-05 1.990 4.00E-05 2.000 4.00E-05 2.040 4.00E-05 2.000 4.00E-05 1.900 Average Standard Deviation Number of Samples ER (ohm-cm) 2.876 2.922 2.975 2.926 2.919 2.919 Amps (A) Volts(mV) 4.00E-05 1.900 1.00E-05 0.530 1.00E-05 0.520 1.00E-05 0.462 1.00E-05 0.468 1.00E-05 0.472 Average Standard Deviation Number of Samples ER (ohm-cm) 2.700 2.964 2.919 2.878 2.977 3.016 Amps (A) Volts(mV) 1.00E-05 0.499 1.00E-05 0.514 1.00E-05 0.519 1.00E-05 0.530 1.00E-05 0.510 1.00E-05 0.481 Average Standard Deviation Number of Samples ER (ohm-cm) 2.811 2.939 2.914 3.001 2.991 3.028 Amps (A) Volts(mV) 1.00E-05 0.440 2.00E-05 0.990 2.00E-05 2.490 4.00E-05 1.870 Average Standard Deviation Number of Samples ER (ohm-cm) 2.934 2.922 3.533 2.940 Overall Average Overall Std Deviation Number of Samples 164 2.810 0.215 4 2.923 0.031 6 2.909 0.113 6 2.947 0.079 6 3.082 0.300 4 2.933 0.163 26 Table C.15: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/18/2008 EA15P-T-27 1 1.58 2.2 1.00E-03 19.21 1.151 2 1.59 2.05 1.00E-03 21.01 1.181 3 1.59 2.03 1.00E-03 20.65 1.149 4 1.57 2.2 1.00E-03 19.19 1.143 5 1.58 2.18 1.00E-03 19.49 1.157 Average Standard Deviation Number of Samples 1.156 0.015 5 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/18/2008 EA15P-T-21 1 1.61 2.22 1.00E-03 19.10 1.177 3 1.61 2.15 1.00E-03 18.58 1.109 6 1.61 2.11 1.00E-03 18.51 Average Standard Deviation Number of Samples 1.084 1.123 0.048 3 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/18/2008 EA15P-T-29 1 1.59 2.02 1.00E-03 20.44 1.132 2 1.55 1.99 1.00E-03 21.64 1.151 3 1.55 1.88 1.00E-03 22.76 1.143 4 1.58 2.04 1.00E-03 20.08 1.116 5 1.57 2.15 1.00E-03 19.90 1.158 6 1.57 2.2 1.00E-03 19.50 1.161 Average 1.144 Standard Deviation 0.017 Number of Samples Width (mm) Amps (A) Volts(mV) 6 Test Date Sample Number Dot Thickness(mm) ER (ohm-cm) 6/17/2008 EA15P-T-25 1 1.57 2.1 1.00E-03 20.54 1.168 2 1.59 1.97 1.00E-03 22.26 1.202 3 1.56 2.01 1.00E-03 22.14 1.197 4 1.53 2.43 1.00E-03 17.60 1.128 5 1.57 2.06 1.00E-03 20.02 1.116 Average 1.162 Standard Deviation Number of Samples 0.039 5 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/17/2008 EA15P-T-23 1 1.55 2.04 1.00E-03 20.63 1.125 2 1.59 2.1 1.00E-03 20.73 1.193 3 1.6 2.05 1.00E-03 20.05 1.134 4 1.62 2.07 1.00E-03 19.39 1.121 6 1.63 2.21 1.00E-03 18.31 Average Standard Deviation Number of Samples 1.137 1.142 0.029 5 Overall Average 1.147 Overall Standard Deviation 0.029 Number of Samples 165 24 EBP’s Table C.16: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) 6/14/2008 EB35P-T-23 2 1.63 2.2 5.00E-07 49.0 6059.103 4 5 1.63 1.62 2.17 2.17 5.00E-07 5.00E-07 49.0 39.0 5976.479 4727.607 6 1.61 2.12 5.00E-07 34.2 4025.222 Test Date Sample Number Average 5197.103 Standard Deviation Number of Samples 990.657 Sample Number 6/14/2008 EB35P-T-28 Thickness(mm) Width (mm) Amps (A) Volts(mV) 4 1.65 1.91 5.00E-07 36.5 3966.543 5 1.64 1.9 5.00E-07 32.5 Average 3492.069 3729.306 Standard Deviation 335.504 Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) Sample Number 6/14/2008 EB35P-T-21 ER (ohm-cm) 2 ER (ohm-cm) 1 1.61 2.14 5.00E-07 56.0 6653.186 2 1.58 2.14 5.00E-07 37.0 4313.945 3 1.58 2.12 5.00E-07 47.5 5486.414 6 1.62 2.13 5.00E-07 66.0 Average 7853.090 6076.659 Standard Deviation 1521.363 Number of Samples Test Date 4 Dot Number of Samples Test Date ER (ohm-cm) Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) 4 ER (ohm-cm) 1 1.59 2.11 5.00E-07 35.7 4124.213 2 1.61 2.17 5.00E-07 44.0 5300.786 3 1.59 2.13 5.00E-07 46.0 5372.007 5 1.64 2.1 5.00E-07 59.5 Average 7066.138 5465.786 Standard Deviation 1210.642 Number of Samples Test Date Sample Number Dot Thickness(mm) Width (mm) 6/14/2008 EB35P-T-22 4 1.59 2.09 Amps (A) Volts(mV) 5.00E-07 68.5 Average Number of Samples 166 4 ER (ohm-cm) 7849.391 7849.391 1 Overall Average 5484.413 Overall Standard Deviation Number of Samples 1411.329 15 Table C.17: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/14/2008 EB40P-T-22 1 2 1.57 1.61 2.08 2.1 5.00E-06 5.00E-06 27.1 35.1 305.165 409.218 4 1.66 2.12 5.00E-06 29.0 351.920 6 1.69 2.12 5.00E-06 39.0 481.825 Average Standard Deviation Number of Samples 387.032 76.186 4 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/14/2008 EB40P-T-24 1 2 1.6 1.6 2.15 2.13 5.00E-06 5.00E-06 36.9 32.9 437.710 386.632 4 1.6 2.16 5.00E-06 37.0 440.938 5 1.67 2.13 5.00E-06 40.9 501.674 Average Standard Deviation Number of Samples 441.738 47.067 4 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/14/2000 EB40P-T-25 2 3 1.72 1.71 2.16 2.15 5.00E-06 5.00E-06 29.4 34.9 376.644 442.448 5 1.66 2.18 5.00E-06 30.5 380.598 Test Date Sample Number 6/14/2008 EB40P-T-27 Dot Average 399.897 Standard Deviation Number of Samples 36.903 Amps (A) Volts(mV) Width (mm) 2 1.65 2.08 5.00E-06 23.6 278.702 3 4 1.65 1.74 2.1 2.12 5.00E-06 5.00E-06 35.7 40.0 426.553 508.800 Sample Number 6/14/2008 EB40P-T-29 Dot Thickness(mm) Width (mm) ER (ohm-cm) Average 404.685 Standard Deviation 116.597 Number of Samples Test Date 3 Thickness(mm) Amps (A) Volts(mV) 3 ER (ohm-cm) 1 2.08 1.67 5.00E-06 27.6 330.591 2 1.66 2.05 5.00E-06 23.8 279.281 3 4 2.01 2.02 1.67 1.64 5.00E-06 5.00E-06 32.0 37.4 370.742 427.237 5 1.61 2.03 5.00E-06 31.2 351.624 Average 351.895 Standard Deviation 54.218 Number of Samples 167 5 Overall Average 394.121 Overall Standard Deviation Number of Samples 68.456 19 Table C.18: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/16/2008 EB45P-T-20 1 2 1.68 1.68 2.21 2.18 1.00E-05 1.00E-05 14.35 15.76 91.860 99.516 3 1.68 2.17 1.00E-05 18.91 118.859 4 1.63 2.15 1.00E-05 18.12 109.485 5 1.64 2.15 1.00E-05 15.53 94.412 6 1.64 2.15 1.00E-05 15.29 Average Standard Deviation Number of Samples 92.953 101.181 10.814 6 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/16/2008 EB45P-T-24 1 1.63 2.12 1.00E-05 17.58 104.740 2 1.62 2.13 1.00E-05 14.90 88.645 3 1.67 2.1 1.00E-05 18.75 113.373 4 5 1.68 1.69 2.09 2.11 1.00E-05 1.00E-05 15.75 17.14 95.347 105.378 Average Standard Deviation Number of Samples 101.497 9.613 5 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/16/2008 EB45P-T-23 1 2 1.68 1.7 2.11 2.09 1.00E-05 1.00E-05 14.28 17.32 87.275 106.100 3 1.68 2.27 1.00E-05 16.08 105.729 4 1.64 2.09 1.00E-05 17.39 102.769 5 1.64 2.08 1.00E-05 19.36 Average Standard Deviation Number of Samples 113.864 103.147 9.776 5 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) 6/16/2008 EB45P-T-27 1 1.68 2.1 1.00E-05 14.00 85.159 2 1.58 2.14 1.00E-05 19.88 115.894 3 1.53 2.08 1.00E-05 20.70 113.579 4 5 1.62 1.59 2.04 1.98 1.00E-05 1.00E-05 14.05 16.67 80.056 90.484 6 1.56 2.02 1.00E-05 17.53 Average Standard Deviation 95.242 96.735 14.861 Number of Samples ER (ohm-cm) 6 Test Date Sample Number Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 6/16/2008 EB45P-T-29 2 3 1.64 1.65 2.06 2.13 1.00E-05 1.00E-05 14.90 13.93 86.790 84.409 4 1.63 2.04 1.00E-05 15.58 89.322 5 1.61 2.03 1.00E-05 19.10 107.629 6 1.65 2.07 168 1.00E-05 15.50 Average Standard Deviation Number of Samples Overall Average Overall Standard Deviation Number of Samples 91.276 91.885 9.174 5 98.894 11.106 27 Table C.19: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) Amps (A) EB50P-T-23 2 1.67 2.14 3.00E-05 3 1.68 2.16 3.00E-05 4 1.63 2.11 3.00E-05 5 1.63 2.11 3.00E-05 6 1.66 2.14 3.00E-05 Volts(mV) 22.07 17.00 17.69 17.98 19.01 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) Amps (A) EB50P-T-25 1 1.65 2.13 3.00E-05 2 1.63 2.13 3.00E-05 3 1.53 2.12 3.00E-05 4 1.73 2.18 3.00E-05 5 1.74 2.17 3.00E-05 6 1.74 2.18 3.00E-05 Volts(mV) 20.97 21.65 18.92 15.54 18.11 17.02 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) Amps (A) EB50P-T-28 1 1.61 2.15 3.00E-05 2 1.6 2.14 3.00E-05 3 1.6 2.12 3.00E-05 4 1.52 2.14 3.00E-05 5 1.53 2.15 3.00E-05 6 1.58 2.13 3.00E-05 Volts(mV) 20.71 20.41 17.97 22.21 17.27 18.56 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) Amps (A) EB50P-T-29 1 1.72 2.1 3.00E-05 2 1.72 2.1 3.00E-05 4 2.1 1.68 3.00E-05 5 1.69 2.09 3.00E-05 6 1.69 2.11 3.00E-05 169 Volts(mV) 20.85 22.26 21.54 23.71 16.23 ER (ohm-cm) 45.330 35.454 34.966 35.539 38.811 38.020 4.362 5 ER (ohm-cm) 42.356 43.199 35.269 33.683 39.299 37.104 38.485 3.826 6 ER (ohm-cm) 41.200 40.163 35.031 41.520 32.649 35.898 37.743 3.709 6 ER (ohm-cm) 43.282 46.209 43.674 48.130 33.261 Average Standard Deviation Number of Samples 42.911 5.743 5 Overall Average Overall Standard Deviation Number of Samples 39.183 4.586 22 Table C.20: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB55P-T-21 1 1.66 2.18 2 1.64 2.15 3 1.65 2.19 4 1.59 2.16 6 1.59 2.13 Amps (A) 6.00E-05 6.00E-05 6.00E-05 6.00E-05 6.00E-05 Volts(mV) 12.68 18.82 16.62 19.30 18.50 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB55P-T-24 1 1.63 2.19 3 1.61 2.16 4 1.59 2.13 5 1.58 2.14 6 1.6 2.13 Amps (A) 6.00E-05 6.00E-05 6.00E-05 6.00E-05 6.00E-05 Volts(mV) 13.49 20.35 14.84 19.33 20.64 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB55P-T-25 1 1.68 2.09 3 1.62 2.09 4 1.61 2.05 5 1.61 2.06 6 1.6 2.08 Amps (A) 6.00E-05 6.00E-05 6.00E-05 6.00E-05 6.00E-05 Volts(mV) 14.25 21.50 14.49 22.70 18.49 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB55P-T-27 1 1.63 2.11 2 1.62 2.1 3 1.62 2.13 4 1.56 2.05 Amps (A) 6.00E-05 6.00E-05 6.00E-05 6.00E-05 Volts(mV) 15.78 19.18 20.01 17.89 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB55P-T-29 1 1.59 2.13 2 1.57 2.1 3 1.56 2.13 4 1.57 2.08 6 1.55 2.16 170 Amps (A) 6.00E-05 6.00E-05 6.00E-05 6.00E-05 6.00E-05 Volts(mV) 18.62 23.61 18.19 21.58 18.82 ER (ohm-cm) 13.186 19.069 17.258 19.047 18.004 17.313 2.429 5 ER (ohm-cm) 13.838 20.336 14.442 18.781 20.213 17.522 3.155 5 ER (ohm-cm) 14.378 20.918 13.743 21.634 17.682 17.671 3.624 5 ER (ohm-cm) 15.595 18.750 19.841 16.440 17.657 1.974 4 ER (ohm-cm) 18.121 22.368 17.368 20.250 18.106 Average Standard Deviation Number of Samples 19.243 2.052 5 Overall Average Overall Standard Deviation Number of Samples 17.890 2.608 24 Table C.21: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB60P-T-20 1 1.66 3 1.65 4 1.68 5 1.68 6 1.72 Width (mm) 2.13 2.11 2.16 2.15 2.14 Amps (A) 1.00E-04 1.00E-04 1.00E-04 1.00E-04 1.00E-04 Volts(mV) 12.67 15.94 12.35 15.55 13.04 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB60P-T-22 1 1.8 2 1.7 5 1.7 6 1.7 Width (mm) 2.15 2.15 2.15 2.15 Amps (A) 1.00E-04 1.00E-04 1.00E-04 1.00E-04 Volts(mV) 11.71 12.23 14.19 11.99 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB60P-T-25 3 1.5 4 1.6 6 1.55 Width (mm) 2.15 2.1 2.15 Amps (A) 1.00E-04 1.00E-04 1.00E-04 Volts(mV) 15.28 13.92 13.45 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB60P-T-29 1 1.45 3 1.44 4 1.48 5 1.48 6 1.47 Width (mm) 2.15 2.1 2.07 2.1 2.08 Amps (A) 1.00E-04 1.00E-04 1.00E-04 1.00E-04 1.00E-04 Volts(mV) 14.63 18.00 14.18 15.74 17.93 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB60P-T-27 1 1.47 3 1.42 5 1.51 6 1.54 Width (mm) 2.09 2.12 2.09 2.1 171 Amps (A) 1.00E-04 1.00E-04 1.00E-04 1.00E-04 Volts(mV) 16.41 15.02 17.52 15.32 ER (ohm-cm) 7.724 9.568 7.727 9.684 8.275 8.596 0.968 5 ER (ohm-cm) 7.813 7.707 8.942 7.556 8.005 0.634 4 ER (ohm-cm) 8.496 8.064 7.728 8.096 0.385 3 ER (ohm-cm) 7.864 9.385 7.490 8.434 9.452 8.525 0.883 5 ER (ohm-cm) 8.692 7.796 9.533 8.542 Average Standard Deviation Number of Samples 8.641 0.712 4 Overall Average Overall Standard Deviation Number of Samples 8.403 0.751 21 Table C.22: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB65P-T-21 1 1.4 3 1.4 4 1.41 5 1.41 6 1.4 Width (mm) 2.08 2.1 2.1 2.12 2.11 Amps (A) Volts(mV) 2.50E-04 15.59 2.50E-04 16.07 2.50E-04 16.07 2.50E-04 22.29 2.50E-04 16.17 Average Standard Deviation Number of Samples ER (ohm-cm) 3.131 3.258 3.282 4.595 3.294 3.512 0.609 5 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB65P-T-23 1 1.36 3 1.34 4 1.36 5 1.37 6 1.36 Width (mm) 2.09 2.06 2.08 2.05 2.02 Amps (A) 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 ER (ohm-cm) 2.750 3.175 2.796 4.556 3.607 Volts(mV) 14.03 16.68 14.33 23.52 19.04 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB65P-T-24 1 1.54 2 1.55 3 1.54 4 1.52 5 1.52 6 1.53 Width (mm) 2.24 2.19 2.15 2.22 2.15 2.11 Amps (A) 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 Volts(mV) 15.53 19.25 10.85 11.36 19.45 14.21 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB65P-T-27 1 1.55 2 1.55 3 1.53 4 1.56 6 1.55 Width (mm) 2.1 2.06 2.07 2.12 2.08 Amps (A) 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 Volts(mV) 12.55 20.41 16.30 13.27 17.05 Average Standard Deviation Number of Samples Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB65P-T-29 1 1.55 2 1.55 3 1.55 4 1.55 5 1.55 6 1.55 Width (mm) 2.25 2.2 2.25 2.2 2.15 2.15 172 Amps (A) 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 2.50E-04 Volts(mV) 9.88 16.74 13.79 10.46 17.50 15.72 3.377 0.744 5 ER (ohm-cm) 3.695 4.506 2.478 2.644 4.384 3.164 3.478 0.863 6 ER (ohm-cm) 2.817 4.494 3.560 3.027 3.791 3.538 0.663 5 ER (ohm-cm) 2.376 3.937 3.317 2.460 4.022 3.613 Average Standard Deviation Number of Samples 3.287 0.719 6 Overall Average Overall Standard Deviation Number of Samples 3.434 0.679 27 Table C.23: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/16/2008 Sample Number EB65PR-T-24 Dot 1 2 3 4 5 6 Thickness(mm) 1.55 1.55 1.55 1.6 1.6 1.6 Width (mm) 2.15 2.15 2.15 2.15 2.15 2.2 Test Date 6/16/2008 Sample Number EB65PR-T-25 Dot 1 2 3 4 5 6 Thickness(mm) 1.55 1.55 1.55 1.5 1.5 1.6 Width (mm) 2.15 2.15 2.2 2.15 2.1 2.15 Test Date 6/16/2008 Sample Number EB65PR-T-20 Dot 1 2 3 4 5 6 Thickness(mm) 1.55 1.55 1.55 1.55 1.55 1.55 Width (mm) 2.2 2.15 2.15 2.15 2.15 2.15 Test Date 6/16/2008 Sample Number EB65PR-23 Dot 1 2 3 4 5 6 Thickness(mm) 1.55 1.55 1.55 1.6 1.5 1.55 Width (mm) 2.1 2.05 2.15 2.1 2.1 2.1 Test Date 6/16/2008 Sample Number EB65PR-29 Dot 1 2 3 4 5 6 Thickness(mm) 1.55 1.55 1.55 1.55 1.55 1.55 Width (mm) 2.2 2.1 2.15 2.1 2.05 2.05 173 Amps (A) Volts(mV) 2.50E-04 13.04 2.50E-04 16.54 2.50E-04 9.68 2.50E-04 15.82 2.50E-04 16.98 2.50E-04 9.81 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.50E-04 11.80 2.50E-04 20.78 2.50E-04 12.64 2.50E-04 11.11 2.50E-04 18.88 2.50E-04 15.17 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.50E-04 12.46 2.50E-04 18.76 2.50E-04 11.57 2.50E-04 11.44 2.50E-04 17.13 2.50E-04 11.55 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.50E-04 12.64 2.50E-04 19.29 2.50E-04 13.99 2.50E-04 14.68 2.50E-04 19.20 2.50E-04 12.03 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.50E-04 13.72 2.50E-04 20.60 2.50E-04 12.34 2.50E-04 11.78 2.50E-04 14.44 2.50E-04 19.45 Average Standard Deviation Number of Samples Overall Average Overall Standard Deviation Number of Samples ER (ohm-cm) 2.997 3.801 2.225 3.753 4.028 2.381 3.198 0.777 6 ER (ohm-cm) 2.712 4.776 2.973 2.471 4.102 3.599 3.439 0.887 6 ER (ohm-cm) 2.930 4.312 2.659 2.629 3.937 2.655 3.187 0.744 6 ER (ohm-cm) 2.837 4.227 3.215 3.402 4.171 2.701 3.426 0.650 6 ER (ohm-cm) 3.227 4.624 2.836 2.644 3.164 4.262 3.460 0.799 6 3.342 0.731 30 Table C.24: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number EB70P-T-21 Dot 1 2 3 4 5 6 Thickness(mm) 1.6 1.65 1.6 1.6 1.65 1.65 Width (mm) 2.2 2.1 2.1 2.1 2.1 2.1 Amps (A) Volts(mV) 1.00E-03 18.42 1.00E-03 25.90 1.00E-03 22.53 1.00E-03 17.44 1.00E-03 25.10 1.00E-03 20.52 Average Standard Deviation Number of Samples ER (ohm-cm) 1.118 1.547 1.305 1.010 1.500 1.226 1.284 0.211 6 Test Date 6/16/2008 Sample Number EB70P-T-20 Dot 1 2 3 4 5 6 Thickness(mm) 1.6 1.6 1.6 1.55 1.55 1.55 Width (mm) 2.15 2.1 2.1 2.1 2.1 2.1 Amps (A) Volts(mV) 1.00E-03 24.01 1.00E-03 26.13 1.00E-03 17.17 1.00E-03 23.25 1.00E-03 26.59 1.00E-03 18.90 Average Standard Deviation Number of Samples ER (ohm-cm) 1.424 1.514 0.995 1.305 1.492 1.061 1.298 0.223 6 Test Date 6/16/2008 Sample Number EB70P-T-25 Dot 1 2 3 4 5 6 Thickness(mm) 1.7 1.7 1.7 1.65 1.65 1.6 Width (mm) 2.1 2.1 2.15 2.1 2.15 2.1 Amps (A) Volts(mV) 1.00E-03 17.90 1.00E-03 23.37 1.00E-03 22.61 1.00E-03 16.99 1.00E-03 24.80 1.00E-03 22.05 Average Standard Deviation Number of Samples ER (ohm-cm) 1.102 1.438 1.425 1.015 1.517 1.277 1.296 0.201 6 Test Date 6/16/2008 Sample Number EB70P-T-28 Dot 1 2 3 4 5 6 Thickness(mm) 1.7 1.7 1.7 1.7 1.7 1.7 Width (mm) 2.05 2 2.05 2.1 2.1 2.1 Amps (A) Volts(mV) 1.00E-03 20.30 1.00E-03 29.76 1.00E-03 20.92 1.00E-03 18.87 1.00E-03 27.64 1.00E-03 17.16 Average Standard Deviation Number of Samples ER (ohm-cm) 1.220 1.745 1.257 1.161 1.701 1.056 1.357 0.292 6 Test Date 6/16/2008 Sample Number EB70P-T-26 Dot 1 3 4 5 6 Thickness(mm) 1.7 1.7 1.7 1.7 1.7 Width (mm) 2.1 2.1 2 2 2.1 Amps (A) Volts(mV) 1.00E-03 18.95 1.00E-03 22.30 1.00E-03 18.20 1.00E-03 28.84 1.00E-03 22.71 Average Standard Deviation Number of Samples ER (ohm-cm) 1.166 1.373 1.067 1.691 1.398 1.339 0.241 5 Overall Average Overall Standard Deviation Number of Samples 1.314 0.220 29 174 Table C.25: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB75P-T-20 1 1.57 2.07 2 1.55 2.04 3 1.56 2.05 4 1.55 2.05 5 1.55 2.06 6 1.54 2.07 Amps (A) ER (ohm-cm) 3.00E-03 0.32854 3.00E-03 0.48193 3.00E-03 0.35803 3.00E-03 0.33400 3.00E-03 0.44041 3.00E-03 0.36641 Average Standard Deviation Number of Samples ER (ohm-cm) 0.32854 0.48193 0.35803 0.33400 0.44041 0.36641 0.38489 0.06217 6 Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB75P-T-24 1 1.56 2.04 2 1.54 2.05 3 1.53 2.06 4 1.53 2.12 6 1.53 2.11 Amps (A) ER (ohm-cm) 3.00E-03 0.35098 3.00E-03 0.46012 3.00E-03 0.30467 3.00E-03 0.35736 3.00E-03 0.32561 Average Standard Deviation Number of Samples ER (ohm-cm) 0.35098 0.46012 0.30467 0.35736 0.32561 Amps (A) ER (ohm-cm) 3.00E-03 0.33028 3.00E-03 0.43751 3.00E-03 0.34649 3.00E-03 0.33539 3.00E-03 0.43670 3.00E-03 0.35094 Average Standard Deviation Number of Samples ER (ohm-cm) 0.33028 0.43751 0.34649 0.33539 0.43670 0.35094 Amps (A) ER (ohm-cm) 3.00E-03 0.38225 3.00E-03 0.37881 3.00E-03 0.35647 3.00E-03 0.50296 3.00E-03 0.34037 Average Standard Deviation Number of Samples ER (ohm-cm) 0.38225 0.37881 0.35647 0.50296 0.34037 Test Date 6/16/2008 Test Date 6/16/2008 Sample Number Dot Thickness(mm) Width (mm) EB75P-T-26 1 1.54 2.1 2 1.53 2.12 3 1.53 2.13 4 1.52 2.12 5 1.52 2.14 6 1.5 2.17 Sample Number Dot Thickness(mm) Width (mm) EB75P-T-29 1 1.52 2.04 3 1.5 2.04 4 1.49 2.07 5 1.5 2.05 6 1.48 2.05 Overall Average Overall Standard Deviation Number of Samples 175 0.35975 0.05991 5 0.37289 0.05030 6 0.39217 0.06424 5 0.37756 0.05604 22 Table C.26: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Test Date 6/16/2008 Test Date 6/16/2008 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EB80P-T-25 1 1.43 2 1.42 3 1.42 4 1.47 6 1.46 Sample Number Dot Thickness(mm) EB80P-T-26 1 1.39 2 1.4 3 1.41 4 1.41 5 1.43 6 1.43 Sample Number Dot Thickness(mm) EB60P-T-28 1 1.38 2 1.38 3 1.4 4 1.26 6 1.27 Sample Number Dot Thickness(mm) EB80P-29 1 1.29 3 1.32 4 1.32 6 1.35 Width (mm) 2.11 2.1 2.12 2.09 2.09 Width (mm) 2.11 2.09 2.11 2.08 2.06 2.07 Width (mm) 2 1.99 1.97 2.01 1.99 Width (mm) 2.03 2.06 1.98 2 176 Amps (A) Volts(mV) 1.00E-02 15.25 1.00E-02 22.00 1.00E-02 16.96 1.00E-02 15.01 1.00E-02 15.79 Average Standard Deviation Number of Samples ER (ohm-cm) 0.07933 0.11311 0.08803 0.07951 0.08307 Amps (A) Volts(mV) 1.00E-02 16.05 1.00E-02 22.29 1.00E-02 15.44 1.00E-02 16.62 1.00E-02 23.60 1.00E-02 18.03 Average Standard Deviation Number of Samples ER (ohm-cm) 0.08116 0.11245 0.07920 0.08404 0.11986 0.09202 Amps (A) Volts(mV) 1.00E-02 17.59 1.00E-02 25.09 1.00E-02 18.30 1.00E-02 19.22 1.00E-02 22.03 Average Standard Deviation Number of Samples ER (ohm-cm) 0.08370 0.11880 0.08702 0.08393 0.09599 Amps (A) 1.00E-02 1.00E-02 1.00E-02 1.00E-02 ER (ohm-cm) 0.08958 0.07679 0.08454 0.08002 Volts(mV) 19.84 16.38 18.76 17.19 0.08861 0.01414 5 0.09479 0.01728 6 0.09389 0.01479 5 Average Standard Deviation Number of Samples 0.08273 0.00556 4 Overall Average Overall Std Deviation Number of Samples 0.09061 0.01393 20 EQP’s 177 Table C.27: 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6P-T-25 1 1.53 2 1.59 3 1.61 4 1.68 5 1.68 6 1.68 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6P-T-20 1 1.68 3 1.67 4 1.59 5 1.56 6 1.57 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-23 1 1.61 2 1.54 3 1.55 4 1.68 5 1.68 6 1.69 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6P-T-29 1 1.62 2 1.51 3 1.61 4 1.65 5 1.66 6 1.66 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6P-T-27 1 1.52 2 1.54 3 1.51 4 1.68 5 1.68 6 1.67 Width (mm) 1.98 2 2.03 1.96 1.98 2 Amps (A) Volts(mV) 1.00E-04 29.59 1.00E-04 31.55 1.00E-04 27.06 1.00E-04 32.39 1.00E-04 31.98 1.00E-04 27.99 Average Standard Deviation Number of Samples Width (mm) Amps (A) Volts(mV) 2.22 1.00E-04 27.82 2.04 1.00E-04 27.63 2.07 1.00E-04 30.73 2.03 1.00E-04 31.73 2.01 1.00E-04 32.15 Average Standard Deviation Number of Samples Width (mm) Amps (A) Volts(mV) 2.04 4.00E-05 11.91 2 4.00E-05 11.44 2 4.00E-05 11.59 2.37 1.00E-04 26.83 2.06 1.00E-04 29.24 2.04 1.00E-04 28.47 Average Standard Deviation Number of Samples Width (mm) Amps (A) Volts(mV) 1.95 1.00E-04 27.71 1.9 1.00E-04 25.45 1.95 1.00E-04 24.04 1.97 1.00E-04 27.30 1.95 1.00E-04 25.25 1.96 1.00E-04 24.37 Average Standard Deviation Number of Samples ER (ohm-cm) 15.455 17.298 15.248 18.389 18.341 16.215 16.824 1.393 6 ER (ohm-cm) 17.889 16.229 17.438 17.325 17.492 17.275 0.622 5 ER (ohm-cm) 16.861 15.188 15.487 18.418 17.447 16.923 16.721 1.212 6 ER (ohm-cm) 15.092 12.589 13.013 15.300 14.092 13.671 13.959 1.091 6 Width (mm) 1.95 1.88 1.88 2 2 1.93 ER (ohm-cm) 14.467 14.656 14.586 15.682 16.730 18.155 15.713 1.479 6 Amps (A) Volts(mV) 1.00E-04 28.31 1.00E-04 29.36 1.00E-06 0.298 1.00E-04 27.07 1.00E-04 28.88 1.00E-04 32.67 Average Standard Deviation Number of Samples Overall Average Overall Standard Deviation Number of Samples 178 15.858 1.650 29 Table C.28: 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-25 1 1.49 2 1.53 3 1.5 4 1.59 5 1.6 6 1.58 Width (mm) 2.09 2.05 2.1 2.08 2.1 2.08 Amps (A) Volts(mV) 1.00E-04 33.47 1.00E-04 35.04 1.00E-04 36.62 1.00E-04 30.97 1.00E-04 31.79 1.00E-04 33.05 Average Standard Deviation Number of Samples ER (ohm-cm) 17.971 18.949 19.888 17.659 18.416 18.727 18.602 0.789 6 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-20 1 1.63 2 1.66 3 1.64 4 1.63 5 1.56 6 1.52 Width (mm) 2.13 2.05 2.07 2.11 2.09 2.09 Amps (A) Volts(mV) 1.00E-04 29.53 1.00E-04 29.71 1.00E-04 29.19 1.00E-04 33.12 1.00E-04 31.62 1.00E-04 30.09 Average Standard Deviation Number of Samples ER (ohm-cm) 17.677 17.432 17.085 19.640 17.775 16.481 17.681 1.068 6 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-28 1 1.55 2 1.54 3 1.56 4 1.48 5 1.49 6 1.45 Width (mm) 2.1 2.04 2.08 2.19 2.07 2.16 Amps (A) Volts(mV) 1.00E-05 3.51 1.00E-05 3.40 1.00E-05 3.16 1.00E-05 3.13 1.00E-05 3.13 1.00E-05 3.09 Average Standard Deviation Number of Samples ER (ohm-cm) 19.698 18.416 17.679 17.491 16.645 16.686 17.769 1.154 6 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-21 1 1.66 2 1.66 3 1.98 5 1.55 6 1.56 Width (mm) 2.06 2.04 2.12 2.06 2.16 Amps (A) Volts(mV) 1.00E-05 2.88 1.00E-05 3.37 1.00E-05 3.09 1.00E-05 3.41 1.00E-05 3.47 Average Standard Deviation Number of Samples ER (ohm-cm) 16.980 19.676 22.363 18.773 20.160 19.590 1.969 5 Test Date 6/16/2008 Sample Number Dot Thickness(mm) EQ6PR-T-24 1 1.59 2 1.58 3 1.58 4 1.49 5 1.49 6 1.5 Width (mm) 2.08 2.08 2.05 2.04 2.06 2.03 Amps (A) Volts(mV) 5.00E-05 16.32 5.00E-05 16.26 1.00E-05 3.19 1.00E-05 3.56 1.00E-05 3.41 1.00E-05 3.12 Average Standard Deviation Number of Samples ER (ohm-cm) 18.612 18.427 17.815 18.657 18.046 16.380 17.989 0.854 6 Overall Average Overall Std Deviation Number of Samples 179 18.283 1.310 29 Table C.29: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Test Date 6/17/2008 Test Date 6/17/2008 Sample Number EQ7.5P-T-29 Sample Number EQ7.5-T-20 Sample Number EQ7.5-T-21 Dot Thickness(mm) Width (mm) 1 1.3 1.94 2 1.31 1.99 3 1.3 2.01 4 1.39 1.99 6 1.39 1.95 Dot Thickness(mm) Width (mm) 1 1.51 2.06 2 1.53 2.04 3 1.57 2.03 4 1.46 2.1 5 1.48 2.04 6 1.48 2.03 Dot Thickness(mm) Width (mm) 1 1.3 2.02 2 1.29 1.98 4 1.41 2.04 5 1.39 2.04 6 1.39 2.1 Amps (A) Volts(mV) 1.00E-04 10.51 1.00E-04 10.77 1.00E-04 9.62 1.00E-04 12.50 1.00E-04 12.81 Average Standard Deviation Number of Samples ER (ohm-cm) 4.570 4.841 4.334 5.961 5.986 1.00E-04 Volts(mV) 1.00E-04 9.16 1.00E-04 8.96 1.00E-04 9.39 1.00E-04 8.96 1.00E-04 9.21 1.00E-04 8.92 Average Standard Deviation Number of Samples ER (ohm-cm) 4.913 4.822 5.160 4.736 4.794 4.621 1.00E-04 Volts(mV) 1.00E-04 11.08 1.00E-04 11.74 1.00E-04 10.64 1.00E-04 10.66 1.00E-04 9.70 Average Standard Deviation Number of Samples ER (ohm-cm) 5.017 5.170 5.277 5.212 4.882 5.139 0.783 5 4.841 0.184 6 5.111 0.160 5 Test Date 6/17/2008 Sample Number EQ7.5P-T-23 Dot Thickness(mm) Width (mm) 1 1.41 2.06 2 1.39 2.03 3 1.4 2.08 4 1.31 2.02 5 1.3 2.02 6 1.3 1.99 Amps (A) Volts(mV) 1.00E-04 10.30 1.00E-04 10.50 1.00E-04 9.92 1.00E-04 11.84 1.00E-04 11.77 1.00E-04 11.37 Average Standard Deviation Number of Samples ER (ohm-cm) 5.158 5.108 4.981 5.402 5.329 5.071 5.175 0.160 6 Test Date 6/17/2008 Sample Number EQ7.5P-T-26 Dot Thickness(mm) Width (mm) 1 1.42 1.99 2 1.43 1.97 4 1.32 2.05 5 1.3 1.98 6 1.28 2.1 1.00E-04 Volts(mV) 1.00E-04 10.40 1.00E-04 11.49 1.00E-04 11.12 1.00E-04 11.73 1.00E-04 10.93 Average Standard Deviation Number of Samples ER (ohm-cm) 5.067 5.581 5.188 5.206 5.065 5.221 0.211 5 Overall Average Overall Standard Deviation Number of Samples 180 5.091 0.369 27 Table C.30: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ7.5PR-T-29 1 1.27 2 1.25 3 1.25 4 1.36 5 1.35 6 1.39 Width (mm) 2.01 1.88 1.96 2.02 1.96 1.95 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ7.5PR-T-21 1 1.34 2 1.38 3 1.39 4 1.28 5 1.29 6 1.27 Width (mm) 2.06 1.96 2.04 2.02 2.02 2.07 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ7.5PR-T-25 1 1.3 2 1.26 3 1.27 4 1.36 5 1.36 6 1.35 Width (mm) 1.97 1.96 1.96 1.96 1.93 1.95 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ7.5PR-T-24 1 1.32 2 1.32 3 1.34 4 1.48 5 1.32 6 1.44 Width (mm) 2.08 2.08 2.05 2.08 2.06 2.08 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ7.5PR-T-27 1 1.38 2 1.42 3 1.39 4 1.28 5 1.29 6 1.27 Width (mm) 2 1.95 1.96 2 1.98 2.08 181 Amps (A) Volts(mV) 2.00E-04 22.25 1.00E-04 11.61 1.00E-04 11.89 1.00E-04 10.04 1.00E-04 11.08 1.00E-04 10.71 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 1.00E-04 10.06 1.00E-04 10.53 1.00E-04 10.11 1.00E-04 10.04 1.00E-04 10.71 1.00E-04 10.78 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 1.00E-04 11.80 1.00E-04 12.19 1.00E-04 11.96 1.00E-04 11.07 1.00E-04 11.51 1.00E-04 11.34 Average Standard Deviation Number of Samples ER (ohm-cm) 4.896 4.704 5.023 4.755 5.055 5.005 4.906 0.148 6 ER (ohm-cm) 4.788 4.911 4.943 4.476 4.812 4.886 4.802 0.171 6 ER (ohm-cm) 5.210 5.190 5.133 5.088 5.209 5.147 5.163 0.049 6 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-04 10.90 5.160 1.00E-04 11.40 5.397 1.00E-04 11.30 5.352 1.00E-04 9.96 5.286 1.00E-04 10.03 4.702 1.00E-04 10.32 5.329 Average 5.204 Standard Deviation 0.259 Number of Samples 6 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-04 10.71 5.096 1.00E-04 10.40 4.965 1.00E-04 11.04 5.186 1.00E-04 11.32 4.996 1.00E-04 12.37 5.447 1.00E-04 11.85 5.397 Average 5.181 Standard Deviation 0.203 Number of Samples 6 Overall Average 5.051 Overall Standard Deviation 0.236 Number of Samples 30 Table C.31: 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Sample Number Dot EQ10P-T-20 1 2 3 4 5 6 Thickness(mm) 1.91 1.91 1.99 1.9 1.9 1.95 Width (mm) 1.38 1.42 1.38 1.28 1.42 1.31 Test Date 6/17/2008 Sample Number Dot EQ10P-T-28 1 2 3 4 5 6 Thickness(mm) 1.23 1.25 1.26 1.33 1.39 1.35 Width (mm) 1.92 1.99 1.98 1.97 1.98 2.03 Test Date 6/17/2008 Sample Number Dot EQ10P-T-25 1 2 3 4 5 6 Thickness(mm) 1.29 1.25 1.25 1.35 1.34 1.32 Width (mm) 2.06 2.06 2.03 2.02 2.02 2.04 Test Date 6/17/2008 Sample Number Dot EQ10P-T-23 1 2 3 4 5 6 Thickness(mm) 1.33 1.27 1.3 1.39 1.39 1.42 Width (mm) 1.99 2.03 2.03 2.02 2.01 2 Test Date 6/17/2008 Sample Number Dot EQ10P-T-26 1 2 3 4 5 6 Thickness(mm) 1.34 1.32 1.35 1.44 1.41 1.46 Width (mm) 1.93 1.88 2.07 2.2 1.9 2.07 182 Amps (A) Volts(mV) 5.00E-04 15.92 5.00E-04 15.88 5.00E-04 14.91 5.00E-04 18.49 5.00E-04 17.41 5.00E-04 16.67 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 5.00E-04 18.39 5.00E-04 15.93 5.00E-04 18.70 5.00E-04 15.95 5.00E-04 15.87 5.00E-04 17.06 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 5.00E-04 17.51 5.00E-04 17.60 5.00E-04 17.39 5.00E-04 16.55 5.00E-04 16.11 5.00E-04 17.96 Average Standard Deviation Number of Samples 2.00E-03 Volts(mV) 5.00E-04 18.07 5.00E-04 16.28 5.00E-04 17.60 5.00E-04 17.51 5.00E-04 15.95 5.00E-04 15.95 Average Standard Deviation Number of Samples 2.00E-03 Volts(mV) 5.00E-04 18.82 5.00E-04 19.10 5.00E-04 16.69 5.00E-04 15.10 5.00E-04 17.34 5.00E-04 15.13 Average Standard Deviation Number of Samples Overall Average Overall Standard Deviation Number of Samples ER (ohm-cm) 1.447 1.485 1.412 1.551 1.620 1.468 1.497 0.076 6 ER (ohm-cm) 1.498 1.366 1.609 1.441 1.506 1.612 1.505 0.095 6 ER (ohm-cm) 1.605 1.563 1.522 1.556 1.504 1.668 1.569 0.060 6 ER (ohm-cm) 1.649 1.447 1.602 1.695 1.537 1.562 1.582 0.088 6 ER (ohm-cm) 1.678 1.634 1.608 1.650 1.602 1.577 1.625 0.037 6 1.556 0.084 30 Table C.32: 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ15P-T-29 1 1.68 2 1.64 3 1.62 4 1.57 5 1.54 6 1.53 Width (mm) 2.06 2.08 2.02 2.05 2.02 2.03 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ15P-T-23 1 1.18 2 1.21 3 1.24 4 1.29 5 1.27 6 1.33 Width (mm) 2 2 2.05 2.06 2.04 2.31 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ15P-T-21 1 1.25 2 1.24 3 1.23 4 1.31 5 1.34 6 1.3 Width (mm) 2.08 2.08 2.01 2.09 2.1 2.12 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ15P-T-25 1 1.18 2 1.18 3 1.2 4 1.28 5 1.26 6 1.28 Width (mm) 1.94 2.04 2.1 1.77 2.25 2.02 Test Date 6/17/2008 Sample Number Dot Thickness(mm) EQ15P-T-27 1 1.62 2 1.67 3 1.62 4 1.71 5 1.74 6 1.81 Width (mm) 2.01 2.02 2.02 2 2 2.05 Amps (A) Volts(mV) 2.00E-03 12.64 2.00E-03 14.49 2.00E-03 13.39 2.00E-03 14.07 2.00E-03 15.68 2.00E-03 14.21 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.00E-03 18.46 2.00E-03 21.41 2.00E-03 19.34 2.00E-03 16.04 2.00E-03 18.47 2.00E-03 15.11 Average Standard Deviation Number of Samples 183 ER (ohm-cm) 0.37711 0.42611 0.37774 0.39038 0.42049 0.38047 0.39538 0.02221 6 ER (ohm-cm) 0.37557 0.44666 0.42381 0.36745 0.41252 0.40019 0.40437 0.02981 6 Amps (A) Volts(mV) ER (ohm-cm) 2.00E-03 17.73 0.39740 2.00E-03 18.96 0.42157 2.00E-03 19.73 0.42050 2.00E-03 16.71 0.39440 2.00E-03 17.06 0.41385 2.00E-03 15.15 0.35994 Average 0.40128 Standard Deviation 0.02328 Number of Samples 6 Amps (A) Volts(mV) ER (ohm-cm) 2.00E-03 19.48 0.38443 2.00E-03 20.79 0.43143 2.00E-03 18.27 0.39690 2.00E-03 20.53 0.40097 2.00E-03 16.07 0.39275 2.00E-03 17.40 0.38784 Average 0.39905 Standard Deviation 0.01695 Number of Samples 6 Amps (A) Volts(mV) ER (ohm-cm) 2.00E-03 13.61 0.38204 2.00E-03 14.66 0.42633 2.00E-03 12.88 0.36335 2.00E-03 12.86 0.37915 2.00E-03 13.72 0.41160 2.00E-03 12.64 0.40432 Average 0.39446 Standard Deviation 0.02351 Number of Samples 6 Overall Average 0.39891 Overall Standard Deviation 0.02215 Number of Samples 30 Combinations Table C.33: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Sample Number EA2.5Q6P-T-27 Dot Thickness(mm) 1 1.3 2 1.31 3 1.35 4 1.42 5 1.41 6 1.43 Width (mm) 1.98 1.95 1.96 2.04 1.95 2 Amps (A) Volts(mV) 5.00E-04 22.44 5.00E-04 23.11 2.00E-04 8.39 2.00E-04 8.38 2.00E-04 8.53 2.00E-04 8.20 Average Standard Deviation Number of Samples ER (ohm-cm) 1.992 2.036 1.914 2.093 2.022 2.022 2.013 0.059 6 Test Date 6/17/2008 Sample Number EA2.5Q6P-T-28 Dot Thickness(mm) 1 1.48 2 1.44 3 1.44 4 1.18 5 1.49 6 1.5 Width (mm) 2.02 2 2.06 2.02 2.03 2.19 Amps (A) Volts(mV) 2.00E-04 9.00 2.00E-04 9.87 5.00E-05 2.45 5.00E-04 21.26 2.00E-04 8.91 2.00E-04 8.42 Average Standard Deviation Number of Samples ER (ohm-cm) 2.320 2.450 2.506 1.747 2.323 2.384 2.289 0.275 6 Test Date 6/17/2008 Sample Number EA2.5Q6P-T-26 Dot Thickness(mm) 1 1.46 2 1.45 3 1.49 4 1.47 5 1.42 6 1.4 Width (mm) 2.05 2.02 2.08 2.08 2.03 2.07 Amps (A) Volts(mV) 2.00E-04 7.97 2.00E-04 9.09 2.00E-04 9.00 2.00E-04 8.31 2.00E-04 8.59 2.00E-04 9.04 Average Standard Deviation Number of Samples ER (ohm-cm) 2.056 2.295 2.405 2.190 2.135 2.258 2.223 0.123 6 Test Date 6/17/2008 Sample Number EA2.5Q6P-T-20 Dot Thickness(mm) 2 1.4 4 1.43 Width (mm) 2.06 2.06 Amps (A) Volts(mV) 2.00E-04 9.19 2.00E-04 8.56 Average Standard Deviation Number of Samples ER (ohm-cm) 2.285 2.174 2.229 0.079 2 Test Date 6/17/2008 Sample Number EA2.5Q6P-T-24 Dot Thickness(mm) 1 1.41 2 1.39 3 1.4 4 1.44 5 1.45 6 1.44 Width (mm) 2.06 2.08 2.05 2.18 2.06 2.06 Amps (A) Volts(mV) 2.00E-04 8.59 2.00E-04 8.62 1.00E-05 0.48 2.00E-04 7.86 2.00E-05 0.90 2.00E-04 9.20 Average Standard Deviation Number of Samples ER (ohm-cm) 2.151 2.148 2.375 2.127 2.318 2.353 2.245 0.115 6 Overall Average Overall Standard Deviation Number of Samples 184 2.195 0.181 26 Table C.34: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/17/2008 Sample Number EA2.5Q6PR-T-20 Dot 1 2 3 4 5 6 Thickness(mm) 1.57 2.17 1.55 1.56 1.51 1.51 Width (mm) 2.19 1.56 2.1 2.24 2.14 2.13 Amps (A) Volts(mV) 2.00E-04 7.13 2.00E-04 7.42 2.00E-06 0.0748 2.00E-04 7.217 2.00E-04 8.00 1.00E-04 3.92 Average Standard Deviation Number of Samples ER (ohm-cm) 2.113 2.165 2.099 2.174 2.229 2.174 2.159 0.047 6 Test Date 6/17/2008 Sample Number EA2.5Q6PR-T-24 Dot 1 2 4 5 6 Thickness(mm) 1.59 1.59 1.61 1.62 1.68 Width (mm) Amps (A) Volts(mV) 2.11 2.00E-04 8.34 2.17 2.00E-04 7.76 2.1 2.00E-04 7.80 2.14 2.00E-04 7.47 2.3 2.00E-04 6.29 Average . Standard Deviation Number of Samples ER (ohm-cm) 2.412 2.308 2.273 2.232 2.095 2.264 0.116 5 Test Date 6/17/2008 Sample Number EA2.5Q6PR-T-23 Dot 1 2 3 4 5 Thickness(mm) 1.63 1.66 1.67 1.6 1.62 Width (mm) 2.13 2.09 2.33 2.21 2.15 Amps (A) Volts(mV) 2.00E-04 7.19 2.00E-04 7.38 2.00E-04 7.09 2.00E-04 6.89 2.00E-04 7.45 Average Standard Deviation Number of Samples ER (ohm-cm) 2.152 2.207 2.378 2.100 2.237 2.215 0.105 5 Test Date 6/17/2008 Sample Number EA2.5Q6PR-T-26 Dot 1 2 3 4 5 6 Thickness(mm) 1.48 1.48 1.45 1.51 1.5 1.51 Width (mm) 2.08 2.1 2.11 2.12 2.14 2.32 Amps (A) Volts(mV) 2.00E-04 7.42 2.00E-04 7.51 2.00E-04 7.57 2.00E-04 7.23 2.00E-04 7.13 2.00E-04 6.64 Average Standard Deviation Number of Samples ER (ohm-cm) 1.969 2.012 1.997 1.995 1.973 2.005 1.992 0.017 6 Test Date 6/17/2008 Sample Number EA2.5Q6PR-T-29 Dot 1 2 3 5 6 Thickness(mm) 1.71 1.67 1.65 1.74 1.76 Width (mm) 2.17 2.18 2.21 2.26 2.3 Amps (A) Volts(mV) 2.00E-04 6.82 2.00E-04 7.00 2.00E-04 6.89 2.00E-04 6.56 2.00E-04 6.33 Average Standard Deviation Number of Samples ER (ohm-cm) 2.182 2.197 2.166 2.146 2.209 2.180 0.025 5 Overall Average Overall Standard Deviation Number of Samples 185 2.156 0.117 27 Table C.35: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number 6/17/2008 EA2.5B65P-TC-22 Test Date Sample Number 6/17/2008 EA2.5B65P-TC-24 Test Date Sample Number 6/17/2008 EA2.5B65P-TC-27 Dot Thickness(mm) 1 2 3 4 5 6 1.86 1.79 1.76 1.74 1.69 1.71 Dot Thickness(mm) 1 2 3 4 5 6 1.72 1.68 1.65 1.62 1.57 1.56 Dot Thickness(mm) 1 2 3 4 5 6 1.41 1.4 1.43 1.47 1.5 1.52 Width (mm) 2.15 2.17 2.2 2.4 2.32 2.24 Width (mm) 2.21 2.25 2.14 2.38 2.61 2.22 Width (mm) 2.05 2.05 2.09 2.14 2.16 2.26 Amps (A) Volts(mV) 2.00E-03 9.66 2.00E-03 10.07 2.00E-03 10.78 2.00E-03 9.33 2.00E-03 9.67 2.00E-03 10.25 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 2.00E-03 10.9 2.00E-03 11.21 2.00E-03 12.64 2.00E-03 9.24 2.00E-03 10.04 2.00E-03 11.24 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 0.33302 0.33720 0.35983 0.33588 0.32685 0.33846 0.33854 0.01122 6 ER (ohm-cm) 0.35718 0.36529 0.38476 0.30712 0.35466 0.33557 0.35076 0.02668 6 ER (ohm-cm) 2.00E-03 15.12 2.00E-03 14.27 2.00E-03 14.82 2.00E-03 15.29 2.00E-03 13.65 2.00E-03 12.46 Average Standard Deviation Number of Samples 0.37676 0.35306 0.38183 0.41465 0.38126 0.36899 0.37942 0.02030 6 Overall Average 0.35624 Overall Standard Deviation 0.02605 Number of Samples 186 ER (ohm-cm) 18 Table C.36: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/17/2008 Sample Number EA2.5B65PR-TC-26 Dot Thickness(mm) Width (mm) 4 1.32 2.07 5 1.32 2.06 6 1.32 2.07 Amps (A) Volts(mV) 2.00E-03 15.10 2.00E-03 14.01 2.00E-03 14.75 Average Standard Deviation Number of Samples ER (ohm-cm) 0.35568 0.32841 0.34744 0.34385 0.01399 3 Test Date 6/17/2008 Sample Number EA2.5B65PR-TC-23 Dot Thickness(mm) Width (mm) 1 1.36 2.21 4 1.33 2.12 6 1.36 2.37 Amps (A) Volts(mV) 2.00E-03 15.56 2.00E-03 16.37 2.00E-03 13.16 Average Standard Deviation Number of Samples ER (ohm-cm) 0.40316 0.39790 0.36567 0.38891 0.02030 3 Test Date 6/17/2008 Sample Number EA2.5B65PR-T-22 Dot Thickness(mm) Width (mm) 5 1.42 2.25 Amps (A) Volts(mV) 2.00E-03 13.98 Average Number of Samples ER (ohm-cm) 0.38505 0.38505 1 Test Date 6/17/2008 Sample Number EA2.5B65PR-T-29 Dot Thickness(mm) Width (mm) 3 1.33 1.99 Amps (A) 2.00E-03 16.69 Average Number of Samples ER (ohm-cm) 0.38081 0.38081 1 Test Date 7/8/2008 Sample Number EA2.5B65PR-T-17 Dot Thickness(mm) Width (mm) 1 1.42 1.85 2 1.41 1.84 3 1.44 1.9 Amps (A) 0.005 38.03 0.005 36.14 0.005 39.22 Average Standard Deviation Number of Samples ER (ohm-cm) 0.34450 0.32332 0.37002 0.34595 0.02339 3 Test Date 7/8/2008 Sample Number EA2.5B65PR-T-30 Dot Thickness(mm) Width (mm) 1 1.36 1.9 2 1.36 1.85 Amps (A) Volts(mV) 0.005 43.98 0.005 40.12 Average Standard Deviation Number of Samples ER (ohm-cm) 0.39188 0.34808 0.36998 0.03097 2 Test Date 7/8/2008 Sample Number EA2.5B65PR-T-7 Dot Thickness(mm) Width (mm) 4 1.48 1.87 5 1.52 1.88 Amps (A) Volts(mV) 0.005 30.86 0.005 33.69 Average Standard Deviation Number of Samples ER (ohm-cm) 0.29451 0.33197 0.31324 0.02649 2 Overall Average Overall Standard Deviation Number of Samples 187 0.35789 0.03096 15 Table C.37: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Sample Number Dot EB6Q6P-T-28 Thickness(mm) Width (mm) Amps (A) Volts(mV) 1 1.46 2.05 1.00E-02 10.23 0.05279 2 1.46 2.02 1.00E-02 11.57 0.05883 3 1.45 2.08 1.00E-02 11.93 0.06204 4 1.5 2.09 1.00E-02 11.89 0.06427 5 1.47 2.1 1.00E-02 11.40 0.06068 6 1.48 2.14 1.00E-02 Average 11.41 0.06231 0.06015 Standard Deviation 0.00403 Number of Samples Test Date 7/8/2008 Sample Number Dot EB65Q6P-T-36 6 Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 1 1.69 1.86 0.01 8.16 0.04422 2 1.66 1.84 0.01 7.76 0.04087 3 1.68 1.86 0.01 8.85 0.04768 4 1.63 1.85 0.01 7.68 0.03993 6 1.63 1.81 0.01 Average 9.59 0.04878 0.04430 Standard Deviation 0.00395 Number of Samples Test Date 7/8/2008 Sample Number Dot EB65Q6P-T-14 Thickness(mm) Width (mm) 5 Amps (A) Volts(mV) 4 1.89 1.67 0.01 11.20 0.06095 1.75 1.93 0.01 9.33 0.05433 6 1.72 2.09 0.01 Average 8.65 0.05361 0.05630 0.00404 Number of Samples 7/8/2008 Sample Number Dot EB65Q6P-T-9 ER (ohm-cm) 5 Standard Deviation Test Date ER (ohm-cm) Amps (A) 3 Thickness(mm) Width (mm) Volts(mV) 1 1.75 1.85 0.01 12.96 0.07234 3 1.63 1.9 0.01 Average 13.13 0.07011 0.07123 Standard Deviation Number of Samples 0.00158 Overall Average 0.05586 Overall Standard Deviation 0.00977 Number of Samples 188 ER (ohm-cm) 2 16 Table C.38a: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/17/2008 Sample Number EB65Q6PR-T-29 Dot 1 2 3 Thickness(mm) 1.73 1.75 1.69 Width (mm) 2.14 2 1.42 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-02 7.91 0.05049 1.00E-02 11.69 0.07054 1.00E-02 17.09 0.07071 Average 0.06391 Standard Deviation 0.01163 Number of Samples 3 Test Date 6/17/2008 Sample Number EB65Q6PR-T-27 Dot 1 2 Thickness(mm) 1.72 1.72 Width (mm) 2.1 2.18 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-02 7.64 0.04758 1.00E-02 6.71 0.04338 Average 0.04548 Standard Deviation 0.00297 Number of Samples 2 Test Date 6/17/2008 Sample Number EB65Q6PR-T-25 Dot 1 2 3 4 5 6 Thickness(mm) 1.72 1.74 1.74 1.7 1.72 1.73 Width (mm) 2.15 2.13 2.11 2.14 2.14 2.12 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-02 8.43 0.05375 1.00E-02 8.94 0.05713 1.00E-02 9.93 0.06286 1.00E-02 7.90 0.04955 1.00E-02 7.85 0.04982 1.00E-02 8.07 0.05103 Average 0.05402 Standard Deviation 0.00518 Number of Samples 6 Test Date 6/17/2008 Sample Number EA2.5B65PR-T-23 Dot 1 2 3 4 5 6 Thickness(mm) 1.6 1.58 1.57 1.66 1.63 1.61 Width (mm) 2.17 2.17 2.17 2.35 2.17 2.21 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-02 11.39 0.06818 1.00E-02 10.87 0.06426 1.00E-02 11.19 0.06573 1.00E-02 7.51 0.05051 1.00E-02 8.47 0.05165 1.00E-02 7.93 0.04865 Average 0.05816 Standard Deviation 0.00879 Number of Samples 6 Test Date 6/17/2008 Sample Number EA2.5B65PR-T-21 Dot 1 2 3 4 Thickness(mm) 1.58 1.54 1.56 1.53 Width (mm) 2.05 1.8 1.81 2.05 Amps (A) Volts(mV) ER (ohm-cm) 1.00E-02 10.34 0.05774 1.00E-02 10.26 0.04904 1.00E-02 10.36 0.05044 1.00E-02 12.32 0.06662 Average 0.05596 Standard Deviation 0.00807 Number of Samples 4 Test Date 7/8/2008 Sample Number EA2.5B65PR-T-35 Dot 1 2 3 4 Thickness(mm) 1.68 1.61 1.61 1.63 Width (mm) 1.82 1.87 1.96 1.85 Amps (A) Volts(mV) ER (ohm-cm) 0.01 8.03 0.04233 0.01 13.10 0.06800 0.01 10.87 0.05914 0.01 10.60 0.05511 Average 0.05615 Standard Deviation 0.01067 Number of Samples 4 189 Table C.38b: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 7/8/2008 Sample Number EA2.5B65PR-T-24 Dot 2 4 6 Thickness(mm) 1.83 1.85 1.66 Width (mm) 1.63 1.66 1.87 Amps (A) 0.01 0.01 0.01 Average Volts(mV) 12.04 10.44 10.70 Standard Deviation Number of Samples Test Date Sample Number 7/8/2008 EA2.5B65PR-T-28 Dot Thickness(mm) Width (mm) Amps (A) Volts(mV) ER (ohm-cm) 0.06192 0.05528 0.05727 0.05816 0.00341 3 ER (ohm-cm) 1 1.61 1.85 0.01 7.51 0.03857 2 1.61 1.89 0.01 7.65 0.04013 4 1.66 1.86 0.01 10.47 0.05574 5 1.66 1.9 0.01 11.33 0.06161 6 1.28 1.66 0.01 18.55 0.06796 Average 0.05280 Standard Deviation 0.01303 Number of Samples 5 Overall Average 0.05584 Overall Standard Deviation 0.00895 Number of Samples 190 33 Table C.39: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 Sample Number EA2.5B65Q6P-35 Dot Thickness(mm) Width (mm) 1 1.69 2.1 2 1.69 2.1 3 1.69 2.17 4 1.7 2.08 5 1.69 2.08 6 1.69 2.27 Amps (A) Volts(mV) 2.00E-02 10.31 2.00E-02 9.51 2.00E-02 9.40 2.00E-02 8.22 2.00E-02 7.82 2.00E-02 7.55 Average Standard Deviation Number of Samples ER (ohm-cm) 0.03154 0.02910 0.02972 0.02506 0.02370 0.02497 0.02735 0.00318 6 Test Date 6/17/2008 Sample Number EA2.5B65Q6P-34 Dot Thickness(mm) Width (mm) 1 1.71 2.04 2 1.7 2.17 4 1.71 2.24 5 1.71 2.1 6 1.71 2.12 Amps (A) Volts(mV) 2.00E-02 10.63 2.00E-02 9.49 2.00E-02 7.48 2.00E-02 8.61 2.00E-02 8.68 Average Standard Deviation Number of Samples ER (ohm-cm) 0.03197 0.03018 0.02470 0.02665 0.02713 0.02813 0.00291 5 Test Date 6/17/2008 Sample Number EA2.5B65Q6P-22 Dot Thickness(mm) Width (mm) 1 1.09 1.74 2 1.74 2.11 Amps (A) Volts(mV) 2.00E-02 13.25 2.00E-02 6.77 Average Standard Deviation Number of Samples ER (ohm-cm) 0.02166 0.02143 0.02155 0.00017 2 Test Date 6/17/2008 Sample Number EA2.5B65Q6P-T-23 Dot Thickness(mm) Width (mm) 2 1.73 2.1 4 1.74 2.11 5 1.74 2.21 Amps (A) Volts(mV) 2.00E-02 7.24 2.00E-02 6.67 2.00E-02 7.09 Average Standard Deviation Number of Samples ER (ohm-cm) 0.02267 0.021111 0.02350 0.02243 0.00122 3 Test Date 6/17/2008 Sample Number EA2.5B65Q6P-27 Dot Thickness(mm) Width (mm) 1 1.72 2.04 2 1.71 2.1 3 1.71 2.07 5 1.72 2.1 6 1.72 2.09 Amps (A) Volts(mV) 2.00E-02 8.37 2.00E-02 7.16 2.00E-02 6.51 2.00E-02 10.69 2.00E-02 10.25 Average Standard Deviation Number of Samples ER (ohm-cm) 0.02532 0.02217 0.01987 0.03329 0.03176 0.02648 0.00587 5 Overall Average Overall Standard Deviation Number of Samples 0.02607 0.00411 21 191 Table C.40: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/17/2008 Test Date 6/17/2008 Test Date 6/17/2008 Test Date 7/8/2008 Test Date 6/17/2008 Sample Number EA2.5B65Q6PR-T-27 Sample Number EA2.5B65Q6PR-T-35 Sample Number EA2.5B65Q6PR-T-33 Sample Number EA2.5B65QPR-T-39 Sample Number EA2.5B65Q6PR-40 Dot 1 2 4 5 6 Dot 1 2 3 Dot 4 5 6 Dot 2 3 Dot 1 2 3 4 5 6 Thickness(mm) 1.66 1.65 1.43 1.65 1.65 Thickness(mm) 1.59 1.59 1.6 Thickness(mm) 1.62 1.62 1.61 Thickness(mm) 1.86 1.8 Thickness(mm) 1.56 1.56 1.56 1.57 1.56 1.56 Width (mm) 1.78 1.98 1.66 2.29 2 Width (mm) 1.96 2.15 2.29 Width (mm) 2.18 2.45 2.48 Width (mm) 1.57 1.52 Width (mm) 2.13 2.12 2.12 2.12 2.09 2.09 Amps (A) Volts(mV) 2.00E-02 12.88 2.00E-02 11.12 2.00E-02 15.59 2.00E-02 7.84 2.00E-02 9.37 Average Standard Deviation Number of Samples ER (ohm-cm) 0.03281 0.03132 0.03190 0.02554 0.02666 Amps (A) Volts(mV) 2.00E-02 8.76 2.00E-02 7.89 2.00E-02 7.67 Average Standard Deviation Number of Samples ER (ohm-cm) 0.02353 0.02325 0.02423 Amps (A) Volts(mV) 2.00E-02 6.49 2.00E-02 6.02 2.00E-02 6.43 Average Standard Deviation Number of Samples ER (ohm-cm) 0.01976 0.02060 0.02213 Amps (A) Volts(mV) 1.00E-02 6.82 1.00E-02 7.15 Average Standard Deviation Number of Samples ER (ohm-cm) 0.03434 0.03373 Amps (A) Volts(mV) 2.00E-02 8.95 2.00E-02 9.11 2.00E-02 9.28 2.00E-02 9.42 2.00E-02 9.14 2.00E-02 10.34 Average Standard Deviation Number of Samples ER (ohm-cm) 0.02564 0.02597 0.02646 0.02703 0.02569 0.02906 0.02664 0.00130 6 Overall Average Overall Std Deviation Number of Samples 192 0.02964 0.00331 5 0.02367 0.00050 3 0.02083 0.00120 3 0.03403 0.00043 2 0.02682 0.00433 19 Table C.41a: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Test Date 7/10/2008 Sample Number EA2.5B65Q6P-1C Dot 1 2 3 4 5 7 Thickness(mm) 1.77 1.63 1.63 1.77 1.32 1.78 Test Date Sample Number 7/10/2008 EA2.5B65Q6P-2C Dot Thickness(mm) 1 1.7 2 1.71 3 1.67 4 1.35 5 1.44 6 1.54 Test Date 7/10/2008 Dot 1 4 5 6 Test Date 7/10/2008 Test Date 7/10/2008 Sample Number EA2.5B65Q6P-3C Sample Number EA2.5B65Q6P-4C Sample Number EA2.5B65Q6P-5C Dot 1 2 3 4 5 6 Dot 1 6 Thickness(mm) 1.61 1.74 1.68 1.74 Thickness(mm) 1.76 1.75 1.76 1.69 1.8 1.69 Thickness(mm) 1.79 1.75 Width (mm) 1.6 1.81 1.87 1.56 1.74 1.67 Width (mm) 1.8 1.8 1.79 1.76 1.79 1.79 Width (mm) 1.81 1.66 1.73 1.68 Width (mm) 1.75 1.75 1.73 1.79 1.71 1.79 Width (mm) 1.61 1.36 193 Amps (A) Volts(mV) 1.00E-01 22.53 1.00E-01 21.18 1.00E-01 19.18 1.00E-01 25.40 1.00E-01 22.00 1.00E-01 19.86 Average Standard Deviation Number of Samples Amps (A) Volts(mV) 1.00E-01 18.85 1.00E-01 20.70 1.00E-01 21.71 1.00E-01 28.68 1.00E-01 26.92 1.00E-01 24.35 Average Standard Deviation Number of Samples ER (ohm-cm) 0.01100 0.01077 0.01008 0.01209 0.00871 0.01018 0.01047 0.00113 6 ER (ohm-cm) 0.00995 0.01099 0.01119 0.01175 0.01196 0.01157 0.01123 0.00073 6 Amps (A) Volts(mV) 1.00E-01 24.65 1.00E-01 19.87 1.00E-01 21.91 1.00E-01 18.52 Average Standard Deviation Number of Samples ER (ohm-cm) 0.01238 0.00990 0.01098 0.00933 Amps (A) Volts(mV) 1.00E-01 21.39 1.00E-01 22.99 1.00E-01 20.99 1.00E-01 18.65 1.00E-01 20.03 1.00E-01 20.59 Average Standard Deviation Number of Samples ER (ohm-cm) 0.01136 0.01214 0.01102 0.00973 0.01063 0.01074 Amps (A) Volts(mV) 1.00E-01 22.15 1.00E-01 30.89 Average Standard Deviation Number of Samples ER (ohm-cm) 0.01101 0.01268 0.01065 0.00134 4 0.01094 0.00080 6 0.01184 0.00118 2 Table C.41b: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Test Date 7/10/2008 Sample Number EA2.5B65Q6P-6C Dot 1 2 3 4 5 6 Thickness(mm) 1.68 1.68 1.68 1.76 1.76 1.74 Width (mm) 1.78 1.76 1.77 1.6 1.49 1.45 Amps (A) 1.00E-01 1.00E-01 1.00E-01 0.1 0.1 0.1 Volts(mV) 20.47 20.77 19.76 23.42 26.02 27.92 Average 0.01109 Standard Deviation 0.00079 Number of Samples Test Date 7/10/2008 Sample Number EA2.5B65Q6P-7C Dot 1 2 4 5 Thickness(mm) 1.77 1.78 1.77 1.77 Width (mm) 1.68 1.7 1.68 1.68 Amps (A) 0.1 0.1 0.1 0.1 Volts(mV) 19.58 21.33 19.28 20.08 6 ER (ohm-cm) 0.01004 0.01113 0.00988 0.01029 Average 0.01034 Standard Deviation 0.00055 Number of Samples 4 Overall Average 0.01088 Overall Standard Deviation 0.00093 Number of Samples 194 ER (ohm-cm) 0.01055 0.01059 0.01013 0.01137 0.01176 0.01214 34 Appendix D: US Fuel Cell Council Through Plane Electrical Resistivity Results EAP’s Table D.1: Poco Reference June 23, 2008 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/23/2008 0.325 31.669 1.5 R (mohm) 11.8 11.9 12.03 12.26 12.12 12.14 12.13 12.25 12.17 12.29 Average 12.109 Stand. Dev. 0.158 R Poco = p t / A 0.015 Rpoco + lead resistance = 12.109 lead resistance (mohm) 12.094 Table D.2: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results tested Sample Number sanded by hand Thickness 0.33 cm cm2 mohm cm mohm mohm mohm 195 inj mold 6/23/2008 tested cm 2 Area Diameter 29.94 6.174 cm cm Test # 1 2 3 4 5 6 R (mohm) 82400 83100 82100 79100 76000 84000 Average Std. Dev. n R corrected (mohm) 82387.91 83087.91 82087.91 79087.91 75987.91 83987.91 81104.57 3003.61 6 Test # 1 2 3 4 5 6 7 8 9 10 EA4P-TC-18 Resistivity Conductivity (ohm cm) (S/cm) 7474.34 1.34E-04 7537.84 1.33E-04 7447.12 1.34E-04 7174.96 1.39E-04 6893.72 1.45E-04 7619.49 1.31E-04 7357.91 1.36E-04 272.49 5.20E-06 6 6 Table D.4: EA4P Disk 5 Results Table D.3: EA4P Disk 10 Results Sample Data sanded by hand Thickness 0.33 EA4P-TC-10 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.336 tested cm 2 Area Diameter 29.94 6.174 cm cm Test # 1 2 3 4 5 R (mohm) 70000 71600 71400 67800 69000 Average Std. Dev. n R corrected (mohm) 69987.91 71587.91 71387.91 67787.91 68987.91 69947.91 1608.73 5 Resistivity Conductivity (ohm cm) (S/cm) 6349.39 1.57E-04 6494.55 1.54E-04 6476.40 1.54E-04 6149.81 1.63E-04 6258.67 1.60E-04 6345.76 1.58E-04 145.95 3.65E-06 5 5 196 EA4P-TC-5 inj mold 6/23/2008 tested cm 2 Area Diameter 29.86 6.166 cm cm Test # 1 2 3 4 5 R (mohm) 69000 71000 68000 67000 66000 Average Std. Dev. n R corrected (mohm) 68987.91 70987.91 67987.91 66987.91 65987.91 68187.91 1923.54 5 Resistivity Conductivity (ohm cm) (S/cm) 6258.67 1.60E-04 6440.11 1.55E-04 6167.95 1.62E-04 6077.23 1.65E-04 5986.51 1.67E-04 6186.09 1.62E-04 174.51 4.52E-06 5 5 Table D.6: EA4P Disk 6 Results Table D.5: EA4P Disk 25 Results Sample Data sanded by hand Thickness 0.336 EA4P-TC-25 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.336 tested cm 2 Area Diameter 29.89 6.169 cm cm Test # 1 2 3 4 5 R (mohm) 91000 82000 89000 89000 88000 Average Std. Dev. n R corrected (mohm) 90987.91 81987.91 88987.91 88987.91 87987.91 87787.91 3420.53 5 Resistivity Conductivity (ohm cm) (S/cm) 8254.54 1.21E-04 7438.05 1.34E-04 8073.10 1.24E-04 8073.10 1.24E-04 7982.38 1.25E-04 7964.23 1.26E-04 310.31 5.10E-06 5 5 197 Area Diameter 29.89 6.169 Test # 1 2 3 4 5 R (mohm) 67000 70000 67000 64000 68000 Average Std. Dev. n EA4P-TC-6 inj mold 6/23/2008 tested cm 2 cm cm R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 66987.91 6077.23 1.65E-04 69987.91 6349.39 1.57E-04 66987.91 6077.23 1.65E-04 63987.91 5805.07 1.72E-04 67987.91 6167.95 1.62E-04 67187.91 6095.37 1.64E-04 2167.95 196.68 5.35E-06 5 5 5 Table D.7: Overall Results for 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 6/23/2008 EA4P-TC-18 6/23/2008 EA4P-TC-10 6/23/2008 EA4P-TC-5 6/23/2008 EA4P-TC-25 6/23/2008 EA4P-TC-6 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 7357.911 6345.764 6186.094 7964.232 6095.373 6811.722 828.537 5 198 Table D.8: Poco Reference June 23, 2008 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/23/2008 tested 0.325 cm 31.669 1.5 cm mohm cm R (mohm) 11.8 11.9 12.03 12.26 12.12 12.14 12.13 12.25 12.17 12.29 Average 12.109 Stand. Dev. 0.158 R Poco = p t / A 0.015 Rpoco + lead resistance = 12.109 lead resistance (mohm) 12.094 Table D.9: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 2 EA5P-TC-18 inj mold 6/23/2008 cm 2 cm cm tested Test # 1 2 3 4 5 6 7 8 9 10 Test # 1 2 3 4 5 mohm mohm mohm 199 R (mohm) 7700 7510 7100 6800 6700 Average Std. Dev. n R corrected Resistivity Conductivity (S/cm) (mohm) (ohm cm) 7687.91 697.46 1.43E-03 7497.91 680.22 1.47E-03 7087.91 643.02 1.56E-03 6787.91 615.81 1.62E-03 6687.91 606.74 1.65E-03 7149.91 648.65 1.55E-03 435.57 39.52 9.35E-05 5 5 5 Table D.11: EA5P Disk 5 Results Table D.10: EA5P Disk 23 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 8050 7220 7450 7920 7610 Average Std. Dev. n EA5P-TC-23 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 tested cm 2 cm cm R corrected (mohm) 8037.91 7207.91 7437.91 7907.91 7597.91 7637.91 338.90 5 Resistivity (ohm cm) 729.21 653.91 674.78 717.42 689.29 692.92 30.75 5 Conductivity (S/cm) 1.37E-03 1.53E-03 1.48E-03 1.39E-03 1.45E-03 1.45E-03 6.43E-05 5 Test # 1 2 3 4 5 200 R (mohm) 7650 7460 7700 7310 7760 Average Std. Dev. n EA5P-TC-5 inj mold 6/23/2008 tested cm 2 cm cm R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 7637.91 692.92 1.44E-03 7447.91 675.68 1.48E-03 7687.91 697.46 1.43E-03 7297.91 662.08 1.51E-03 7747.91 702.90 1.42E-03 7563.91 686.21 1.46E-03 186.36 16.91 3.63E-05 5 5 5 Table D.13: EA5P Disk 13 Results Table D.12: EA5P Disk 6 Results Sample Data sanded by hand Thickness 0.336 Area 29.86 Diameter 6.166 Test # 1 2 3 4 5 R (mohm) 6440 6400 6400 6400 6250 Average Std. Dev. n EA5P-TC-6 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.336 Area 29.89 Diameter 6.169 tested cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 6427.91 583.15 6387.91 579.52 6387.91 579.52 6387.91 579.52 6237.91 565.91 6365.91 577.52 73.62 6.68 5 5 Conductivity (S/cm) 1.71E-03 1.73E-03 1.73E-03 1.73E-03 1.77E-03 1.73E-03 2.03E-05 5 Test # 1 2 3 4 5 201 R (mohm) 7210 6740 6800 6250 6210 Average Std. Dev. n EA5P-TC-13 inj mold 6/23/2008 tested cm 2 cm cm R corrected (mohm) 7197.91 6727.91 6787.91 6237.91 6197.91 6629.91 417.58 5 Resistivity Conductivity (S/cm) (ohm cm) 653.00 1.53E-03 610.36 1.64E-03 615.81 1.62E-03 565.91 1.77E-03 562.28 1.78E-03 601.47 1.67E-03 37.88 1.04E-04 5 5 Table D.14: Overall Results for 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Average Sample Resistivity Date Number (ohm cm) 6/23/2008 EA5P-TC-18 648.65 6/23/2008 EA5P-TC-23 692.92 6/23/2008 EA5P-TC-5 686.21 6/23/2008 EA5P-TC-6 577.52 6/23/2008 EA5P-TC-13 601.47 Overall Average 641.35 Overall Standard Deviation 50.96 Number of Samples 5 202 Table D.15: Poco Reference 6-23-08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/23/2008 Table D.16: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 22 Results tested 0.325 cm 31.669 1.5 cm mohm cm R (mohm) 11.80 11.90 12.03 12.26 12.12 12.14 12.13 12.25 12.17 12.29 Average 12.11 Stand. Dev. 0.158 R Poco = p t / A 0.015 Rpoco + lead resistance = 12.109 lead resistance (mohm) 12.094 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 2 EA6P-TC-22 inj mold 6/23/2008 tested Resistivity (ohm cm) 218.45 201.66 190.32 201.21 187.60 199.85 12.16 5 Conductivity (S/cm) 4.58E-03 4.96E-03 5.25E-03 4.97E-03 5.33E-03 5.02E-03 2.97E-04 5 cm 2 cm cm Test # 1 2 3 4 5 6 7 8 9 10 Test # 1 2 3 4 5 mohm mohm mohm 203 R (mohm) 2420 2235 2110 2230 2080 Average Std. Dev. n R corrected (mohm) 2407.91 2222.91 2097.91 2217.91 2067.91 2202.91 134.07 5 Table D.18: EA6P Disk 33 Results Table D.17: EA6P Disk 8 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 1860 1760 1700 1830 1650 Average Std. Dev. n EA6P-TC-8 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.336 Area 29.86 Diameter 6.166 tested cm 2 cm cm R corrected (mohm) 1847.91 1747.91 1687.91 1817.91 1637.91 1747.91 87.46 5 Resistivity (ohm cm) 167.64 158.57 153.13 164.92 148.59 158.57 7.93 5 Conductivity (S/cm) 5.97E-03 6.31E-03 6.53E-03 6.06E-03 6.73E-03 6.32E-03 3.18E-04 5 Test # 1 2 3 4 5 204 R (mohm) 2600 2550 2530 2470 2380 Average Std. Dev. n EA6P-TC-33 inj mold 6/23/2008 tested Resistivity (ohm cm) 234.78 230.24 228.43 222.98 214.82 226.25 7.66 5 Conductivity (S/cm) 4.26E-03 4.34E-03 4.38E-03 4.48E-03 4.66E-03 4.42E-03 1.52E-04 5 cm 2 cm cm R corrected (mohm) 2587.91 2537.91 2517.91 2457.91 2367.91 2493.91 84.44 5 Table D.20: EA6P Disk 12 Results Table D.19: EA6P Disk 23 Results Sample Data sanded by hand Thickness 0.336 Area 29.89 Diameter 6.169 Test # 1 2 3 4 5 R (mohm) 1860 1830 1750 1700 1770 Average Std. Dev. n EA6P-TC-23 inj mold 6/23/2008 Sample Data sanded by hand Thickness 0.336 Area 29.89 Diameter 6.169 tested cm 2 cm cm R corrected (mohm) 1847.91 1817.91 1737.91 1687.91 1757.91 1769.91 63.80 5 Resistivity Conductivity (ohm cm) (S/cm) 167.64 5.97E-03 164.92 6.06E-03 157.67 6.34E-03 153.13 6.53E-03 159.48 6.27E-03 160.57 6.23E-03 5.79 2.25E-04 5 5 Test # 1 2 3 4 5 205 R (mohm) 2550 2460 2460 2200 2310 Average Std. Dev. n EA6P-TC-12 inj mold 6/23/2008 tested cm 2 cm cm R corrected (mohm) 2537.91 2447.91 2447.91 2187.91 2297.91 2383.91 139.39 5 Resistivity Conductivity (ohm cm) (S/cm) 230.24 4.34E-03 222.08 4.50E-03 222.08 4.50E-03 198.49 5.04E-03 208.47 4.80E-03 216.27 4.64E-03 12.65 2.78E-04 5 5 Table D.21: Overall Results for 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample Date Number 6/23/2008 EA6P-TC-22 6/23/2008 EA6P-TC-8 6/23/2008 EA6P-TC-33 6/23/2008 EA6P-TC-23 6/23/2008 EA6P-TC-12 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 199.85 158.57 226.25 160.57 216.27 192.30 31.34 5 206 Table D.23: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 8 Results Table D.22: Poco Reference 6-25-08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/25/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13.20 2 13.30 3 13.30 4 13.20 5 13.20 6 13.00 7 13.10 8 13.30 9 13.20 10 13.30 Average 13.21 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.210 lead resistance (mohm) 13.195 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 207 R (mohm) 141 142 141 141 141 Average Std. Dev. n EA7.5P-TC-8 inj mold 6/25/2008 tested Resistivity (ohm cm) 11.595 11.685 11.595 11.595 11.595 11.613 0.041 5 Conductivity (S/cm) 0.0862 0.0856 0.0862 0.0862 0.0862 0.0861 2.99E-04 5 cm 2 cm cm R corrected (mohm) 127.81 128.81 127.81 127.81 127.81 128.01 0.45 5 Table D.25: EA7.5P Disk 26 Results Table D.24: EA7.5P Disk 27 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 EA7.5P-TC-27 inj mold 6/25/2008 tested cm 2 cm cm R corrected Resistivity Conductivity R (mohm) (mohm) (ohm cm) (S/cm) 146 132.81 12.048 0.0830 144 130.81 11.867 0.0843 142 128.81 11.685 0.0856 143 129.81 11.776 0.0849 140 126.81 11.504 0.0869 Average 129.81 11.776 0.0849 Std. Dev. 2.24 0.203 1.46E-03 n 5 5 5 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 208 R (mohm) 142 143 146 143 143 Average Std. Dev. n EA7.5P-TC-26 cm 2 cm cm R corrected (mohm) 128.81 129.81 132.81 129.81 129.81 130.21 1.52 5 inj mold 6/25/2008 tested Resistivity Conductivity (ohm cm) (S/cm) 11.685 0.0856 11.776 0.0849 12.048 0.0830 11.776 0.0849 11.776 0.0849 11.812 0.0847 0.138 9.74E-04 5 5 Table D.27: EA7.5P Disk 5 Results Table D.26: EA7.5P Disk 6 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 130 134 133 135 139 Average Std. Dev. n EA7.5P-TC-6 inj mold 6/25/2008 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 tested cm 2 cm cm R corrected (mohm) 116.81 120.81 119.81 121.81 125.81 121.01 3.27 5 Resistivity Conductivity (ohm cm) (S/cm) 10.597 0.0944 10.960 0.0912 10.869 0.0920 11.050 0.0905 11.413 0.0876 10.978 0.0911 0.297 2.45E-03 5 5 Test # 1 2 3 4 5 209 R (mohm) 143 150 149 148 145 Average Std. Dev. n EA7.5P-TC-5 inj mold 6/25/2008 cm 2 cm cm R corrected (mohm) 129.81 136.81 135.81 134.81 131.81 133.81 2.92 5 tested Resistivity Conductivity (ohm cm) (S/cm) 11.776 0.0849 12.411 0.0806 12.320 0.0812 12.230 0.0818 11.958 0.0836 12.139 0.0824 0.264 1.81E-03 5 5 Table D.28: Overall Results for 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Average Resistivity Date Sample Number (ohm cm) 6/25/2008 EA7.5P-TC-8 11.613 6/25/2008 EA7.5P-TC-27 11.776 6/25/2008 EA7.5P-TC-26 11.812 6/25/2008 EA7.5P-TC-6 10.978 6/25/2008 EA7.5P-TC-5 12.139 Overall Average 11.664 Overall Standard Deviation 0.428 Number of Samples 5 210 EBP’s Table D.30: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 20 Results Table D.29: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 211 R (mohm) 373 370 363 362 357 Average Std. Dev. n EB65P-TC-20 6/26/2008 cm 2 cm cm R corrected (mohm) 360.005 357.005 350.005 349.005 344.005 352.005 6.442 5 Resistivity (ohm cm) 31.700 31.435 30.819 30.731 30.291 30.995 0.567 5 inj mold tested Conductivity (S/cm) 0.0315 0.0318 0.0324 0.0325 0.0330 0.0323 0.0006 5 Table D.32: EB65P Disk 6 Results Table D.31: EB65P Disk 30 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 356 350 346 348 339 Average Std. Dev. n EB65P-TC-30 6/26/2008 cm 2 cm cm R corrected (mohm) 343.005 337.005 333.005 335.005 326.005 334.805 6.181 5 Resistivity (ohm cm) 31.118 30.574 30.211 30.392 29.576 30.374 0.561 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0321 0.0327 0.0331 0.0329 0.0338 0.0329 0.0006 5 Test # 1 2 3 4 5 212 R (mohm) 391 396 396 391 398 Average Std. Dev. n EB65P-TC-6 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 378.005 34.293 383.005 34.747 383.005 34.747 378.005 34.293 385.005 34.928 381.405 34.602 3.209 0.291 5 5 inj mold tested Conductivity (S/cm) 0.0292 0.0288 0.0288 0.0292 0.0286 0.0289 0.0002 5 Table D.34: EB65P Disk 21 Results Table D.33: EB65P Disk 19 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 350 342 351 352 351 Average Std. Dev. n EB65P-TC-19 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 337.005 30.574 329.005 29.848 338.005 30.664 339.005 30.755 338.005 30.664 336.205 30.501 4.087 0.371 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0327 0.0335 0.0326 0.0325 0.0326 0.0328 0.0004 5 Test # 1 2 3 4 5 213 R (mohm) 242 239 239 234 231 Average Std. Dev. n EB65P-TC-21 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 229.005 20.776 226.005 20.503 226.005 20.503 221.005 20.050 218.005 19.778 224.005 20.322 4.416 0.401 5 5 inj mold tested Conductivity (S/cm) 0.0481 0.0488 0.0488 0.0499 0.0506 0.0492 0.0010 5 Table D.36: EB65P Disk 7 Results Table D.35: Poco Reference 6/27/08 POCO Reference Data 6/27/2008 tested Carbon Paper Thickness 0.325 cm Area 31.669 cm2 Resistivity 1.5 mohm cm Test # R (mohm) 1 12.77 2 12.57 3 12.46 4 12.6 5 12.44 6 12.51 7 12.46 8 12.87 9 12.39 10 12.49 Average 12.556 Stand. Dev. 0.154 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 12.556 mohm lead resistance (mohm) 12.541 mohm Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 214 R (mohm) 270 269 266 264 264 Average Std. Dev. n EB65P-TC-7 6/27/2008 cm 2 cm cm R corrected (mohm) 257.459 256.459 253.459 251.459 251.459 254.059 2.793 5 Resistivity (ohm cm) 22.670 22.582 22.318 22.142 22.142 22.371 0.246 5 inj mold tested Conductivity (S/cm) 0.0441 0.0443 0.0448 0.0452 0.0452 0.0447 0.0005 5 Table D.37: Overall Results for 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 6/26/2008 EB65P-TC-20 6/26/2008 EB65P-TC-30 6/26/2008 EB65P-TC-6 6/26/2008 EB65P-TC-19 6/26/2008 EB65P-TC-21 6/27/2008 EB65P-TC-7 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 30.995 30.374 34.602 30.501 20.322 22.371 28.194 5.565 6 215 Table D.39: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 24 Results Table D.38: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 216 R (mohm) 236 238 234 230 225 Average Std. Dev. n EB65PR-TC-24 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 223.005 19.636 225.005 19.812 221.005 19.460 217.005 19.108 212.005 18.668 219.605 19.337 5.177 0.456 5 5 inj mold tested Conductivity (S/cm) 0.0509 0.0505 0.0514 0.0523 0.0536 0.0517 0.0012 5 Table D.41: EB65PR Disk 23 Results Table D.40: EB65PR Disk 30 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 276 273 268 276 270 Average Std. Dev. n EB65PR-TC-30 6/26/2008 cm 2 cm cm R corrected (mohm) 263.005 260.005 255.005 263.005 257.005 259.605 3.578 5 Resistivity (ohm cm) 23.860 23.588 23.134 23.860 23.316 23.552 0.325 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0419 0.0424 0.0432 0.0419 0.0429 0.0425 0.0006 5 Test # 1 2 3 4 5 217 R (mohm) 279 273 272 268 265 Average Std. Dev. n EB65PR-TC-23 6/26/2008 cm 2 cm cm R corrected (mohm) 266.005 260.005 259.005 255.005 252.005 258.405 5.320 5 Resistivity (ohm cm) 24.132 23.588 23.497 23.134 22.862 23.443 0.483 5 inj mold tested Conductivity (S/cm) 0.0414 0.0424 0.0426 0.0432 0.0437 0.0427 0.0009 5 Table D.43: EB65PR Disk 19 Results Table D.42: EB65PR Disk 13 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 293 287 279 279 277 Average Std. Dev. n EB65PR-TC-13 6/26/2008 cm 2 cm cm R corrected (mohm) 280.005 274.005 266.005 266.005 264.005 270.005 6.782 5 Resistivity (ohm cm) 25.402 24.858 24.132 24.132 23.951 24.495 0.615 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0394 0.0402 0.0414 0.0414 0.0418 0.0408 0.0010 5 Test # 1 2 3 4 5 218 R (mohm) 296 295 294 291 304 Average Std. Dev. n EB65PR-TC-19 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 283.005 25.675 282.005 25.584 281.005 25.493 278.005 25.221 291.005 26.400 283.005 25.675 4.848 0.440 5 5 inj mold tested Conductivity (S/cm) 0.0389 0.0391 0.0392 0.0396 0.0379 0.0390 0.0007 5 Table D.44: Overall Results for 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Date Sample Number 6/26/2008 EB65PR-TC-24 6/26/2008 EB65PR-TC-30 6/26/2008 EB65PR-TC-23 6/26/2008 EB65PR-TC-13 6/26/2008 EB65PR-TC-19 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 19.337 23.552 23.443 24.495 25.675 23.300 2.390 5 219 Table D.46: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 7 Results Table D.45: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 220 R (mohm) 161 157 156 159 160 Average Std. Dev. n EB70P-TC-7 6/26/2008 cm 2 cm cm R corrected (mohm) 148.005 144.005 143.005 146.005 147.005 145.605 2.074 5 Resistivity (ohm cm) 13.032 12.680 12.592 12.856 12.944 12.821 0.183 5 inj mold tested Conductivity (S/cm) 0.0767 0.0789 0.0794 0.0778 0.0773 0.0780 0.0011 5 Table D.48: EB70P Disk 18 Results Table D.47: EB70P Disk 6 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 172 168 173 164 163 Average Std. Dev. n EB70P-TC-6 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 159.005 14.425 155.005 14.062 160.005 14.516 151.005 13.699 150.005 13.609 155.005 14.062 4.528 0.411 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0693 0.0711 0.0689 0.0730 0.0735 0.0712 0.0021 5 Test # 1 2 3 4 5 221 R (mohm) 156 154 151 147 144 Average Std. Dev. n EB70P-TC-18 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 143.005 12.974 141.005 12.792 138.005 12.520 134.005 12.157 131.005 11.885 137.405 12.466 4.930 0.447 5 5 inj mold tested Conductivity (S/cm) 0.0771 0.0782 0.0799 0.0823 0.0841 0.0803 0.0029 5 Table D.50: EB70P Disk 30 Results Table D.49: EB70P Disk 15 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 178 179 179 175 168 Average Std. Dev. n EB70P-TC-15 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 165.005 14.970 166.005 15.060 166.005 15.060 162.005 14.697 155.005 14.062 162.805 14.770 4.658 0.423 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.0668 0.0664 0.0664 0.0680 0.0711 0.0678 0.0020 5 Test # 1 2 3 4 5 222 R (mohm) 160 159 158 156 153 Average Std. Dev. n EB70P-TC-30 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 147.005 13.337 146.005 13.246 145.005 13.155 143.005 12.974 140.005 12.701 144.205 13.082 2.775 0.252 5 5 inj mold tested Conductivity (S/cm) 0.0750 0.0755 0.0760 0.0771 0.0787 0.0765 0.0015 5 Table D.51: Overall Results for 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 6/26/2008 EB70P-TC-7 6/26/2008 EB70P-TC-6 6/26/2008 EB70P-TC-18 6/26/2008 EB70P-TC-15 6/26/2008 EB70P-TC-30 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 12.821 14.062 12.466 14.770 13.082 13.440 0.951 5 223 Table D.53: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 19 Results Table D.52: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 224 R (mohm) 83.1 86.5 85.5 83.6 81.8 Average Std. Dev. n EB75P-TC-19 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 70.105 6.173 73.505 6.472 72.505 6.384 70.605 6.217 68.805 6.059 71.105 6.261 1.888 0.166 5 5 inj mold tested Conductivity (S/cm) 0.1620 0.1545 0.1566 0.1608 0.1651 0.1598 0.0042 5 Table D.55: EB75P Disk 14 Results Table D.54: EB75P Disk 8 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 81 80.5 80.2 80.2 80.2 Average Std. Dev. n EB75P-TC-8 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 68.005 6.170 67.505 6.124 67.205 6.097 67.205 6.097 67.205 6.097 67.425 6.117 0.349 0.032 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.1621 0.1633 0.1640 0.1640 0.1640 0.1635 0.0008 5 Test # 1 2 3 4 5 225 R (mohm) 75.7 76.9 79.1 77.3 77 Average Std. Dev. n EB75P-TC-14 6/26/2008 cm 2 cm cm R corrected (mohm) 62.705 63.905 66.105 64.305 64.005 64.205 1.225 5 Resistivity (ohm cm) 5.689 5.798 5.997 5.834 5.807 5.825 0.111 5 inj mold tested Conductivity (S/cm) 0.1758 0.1725 0.1667 0.1714 0.1722 0.1717 0.0032 5 Table D.57: EB75P Disk 18 Results Table D.56: EB75P Disk 15 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 70.3 69.7 72.8 73.1 72.3 Average Std. Dev. n EB75P-TC-15 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 57.305 5.199 56.705 5.144 59.805 5.426 60.105 5.453 59.305 5.380 58.645 5.320 1.539 0.140 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 0.1924 0.1944 0.1843 0.1834 0.1859 0.1881 0.0050 5 Test # 1 2 3 4 5 226 R (mohm) 70.5 71.3 71.9 69.9 71.2 Average Std. Dev. n EB75P-TC-18 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 57.505 5.217 58.305 5.290 58.905 5.344 56.905 5.163 58.205 5.280 57.965 5.259 0.773 0.070 5 5 inj mold tested Conductivity (S/cm) 0.1917 0.1891 0.1871 0.1937 0.1894 0.1902 0.0025 5 Table D.58: Poco Reference 7/1/08 Table D.59: EB75P Disk 7 Results POCO Reference Data 7/1/2008 tested Carbon Paper Thickness 0.325 cm Area 31.669 cm2 Resistivity 1.5 mohm cm Test # R (mohm) 1 14.1 2 14.2 3 14.1 4 14.1 5 14.1 6 13.9 7 14.1 8 13.8 9 13.6 10 13.6 Average 13.960 Stand. Dev. 0.222 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 13.960 mohm lead resistance (mohm) 13.945 mohm Sample Data sanded by hand Thickness 0.36 Area 31.47 Diameter 6.33 Test # 1 2 3 4 5 227 R (mohm) 69.7 70.3 69.6 69.2 69.1 Average Std. Dev. n EB75P-TC-7 7/1/2008 cm 2 cm cm R corrected (mohm) 55.755 56.355 55.655 55.255 55.155 55.635 0.476 5 Resistivity (ohm cm) 4.874 4.926 4.865 4.830 4.822 4.863 0.042 5 inj mold tested Conductivity (S/cm) 0.2052 0.2030 0.2055 0.2070 0.2074 0.2056 0.0018 5 Table D.61: EB75P Disk 14 Results Table D.60: EB75P Disk 25 Results Sample Data sanded by hand Thickness 0.359 Area 31.47 Diameter 6.33 Test # 1 2 3 4 5 EB75P-TC-25 7/1/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 67.7 53.755 4.712 67.6 53.655 4.703 67.1 53.155 4.660 67.2 53.255 4.668 67.4 53.455 4.686 Average 53.455 4.686 Std. Dev. 0.255 0.022 n 5 5 inj mold tested Sample Data sanded by hand Thickness 0.357 Area 31.50 Diameter 6.333 Conductivity (S/cm) 0.2122 0.2126 0.2146 0.2142 0.2134 0.2134 0.0010 5 Test # 1 2 3 4 5 228 EB75P-TC-14 7/1/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 67.75 53.805 4.748 67.4 53.455 4.717 66.9 52.955 4.673 66.8 52.855 4.664 66.4 52.455 4.628 Average 53.105 4.686 Std. Dev. 0.529 0.047 n 5 5 inj mold tested Conductivity (S/cm) 0.2106 0.2120 0.2140 0.2144 0.2161 0.2134 0.0021 5 Table D.62: Overall Results for 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample Date Number 6/26/2008 EB75P-TC-19 6/26/2008 EB75P-TC-8 6/26/2008 EB75P-TC-14 6/26/2008 EB75P-TC-15 6/26/2008 EB75P-TC-18 7/1/2008 EB75P-TC-7 7/1/2008 EB75P-TC-25 7/1/2008 EB75P-TC-14 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 6.261 6.117 5.825 5.320 5.259 4.863 4.686 4.686 5.377 0.629 8 229 Table D.64: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 15 Results Table D.63: Poco Reference 7/2/08 POCO Reference Data 7/2/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 14.1 2 14.1 3 14.1 4 13.8 5 14.1 6 14 7 14 8 13.8 9 14 10 14 Average 14.000 Stand. Dev. 0.115 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 14.000 mohm lead resistance (mohm) 13.985 mohm Sample Data sanded by hand Thickness 0.354 Area 30.04 Diameter 6.184 Test # 1 2 3 4 5 230 R (mohm) 18.7 18.6 18.8 18.8 19 Average Std. Dev. n EB80P-TC-15 7/2/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 4.715 0.4001 4.615 0.3916 4.815 0.4086 4.815 0.4086 5.015 0.4255 4.795 0.4069 0.148 0.0126 5 5 inj mold tested Conductivity (S/cm) 2.500 2.554 2.448 2.448 2.350 2.460 0.075 5 Table D.66: EB80P Disk 24 Results Table D.65: EB80P Disk 18 Results Sample Data sanded by hand Thickness 0.35 Area 31.40 Diameter 6.323 Test # 1 2 3 4 5 EB80P-TC-18 7/2/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 18.99 5.005 0.4491 18.97 4.985 0.4473 18.93 4.945 0.4437 18.93 4.945 0.4437 19.42 5.435 0.4876 Average 5.063 0.4543 Std. Dev. 0.210 0.0188 n 5 5 inj mold tested Sample Data sanded by hand Thickness 0.351 Area 31.42 Diameter 6.325 Conductivity (S/cm) 2.227 2.236 2.254 2.254 2.051 2.204 0.087 5 Test # 1 2 3 4 5 231 EB80P-TC-24 7/2/2008 . cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 18.9 4.915 0.4400 18.8 4.815 0.4311 18.7 4.715 0.4221 18.9 4.915 0.4400 19 5.015 0.4490 Average 4.875 0.4364 Std. Dev. 0.114 0.0102 n 5 5 inj mold tested Conductivity (S/cm) 2.273 2.320 2.369 2.273 2.227 2.292 0.054 5 Table D.68: EB80P Disk 30 Results Table D.67: EB80P Disk 12 Results Sample Data sanded by hand Thickness 0.353 Area 31.44 Diameter 6.327 Test # 1 2 3 4 5 EB80P-TC-12 7/2/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 19 5.015 0.4467 19.1 5.115 0.4556 18.9 4.915 0.4378 18.8 4.815 0.4289 19 5.015 0.4467 Average 4.975 0.4431 Std. Dev. 0.114 0.0102 n 5 5 inj mold tested Sample Data sanded by hand Thickness 0.353 Area 31.47 Diameter 6.33 Conductivity (S/cm) 2.239 2.195 2.284 2.332 2.239 2.258 0.052 5 Test # 1 2 3 4 5 232 EB80P-TC-30 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 18.5 4.515 0.4025 18.6 4.615 0.4115 18.4 4.415 0.3936 18.3 4.315 0.3847 18.4 4.415 0.3936 Average 4.455 0.3972 Std. Dev. 0.114 0.0102 n 5 5 inj mold 39631 Conductivity (S/cm) 2.484 2.430 2.540 2.599 2.540 2.519 0.064 5 Table D.69: Overall Results for 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number Average Resistivity (ohm cm) 7/2/2008 EB80P-TC-15 0.4069 7/2/2008 EB80P-TC-18 0.4543 7/2/2008 EB80P-TC-24 0.4364 7/2/2008 EB80P-TC-12 0.4431 7/2/2008 EB80P-TC-30 0.3972 Overall Average 0.4276 Overall Standard Deviation 0.0244 Number of Samples 5 233 EQP’s Table D.71: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Disk 19 Results Table D.70: Poco Reference 6/30/08 POCO Reference Data 6/30/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 12.11 2 12.02 3 11.97 4 12.16 5 12 6 12.09 7 12.01 8 12.13 9 12.1 10 11.98 Average 12.057 Stand. Dev. 0.068 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 12.057 mohm lead resistance (mohm) 12.042 mohm Sample Data sanded by hand Thickness 0.335 Area 30.09 Diameter 6.19 Test # 1 2 3 4 5 234 R (mohm) 2490 2430 2450 2360 2550 Average Std. Dev. n EQ7.5P-TC-19 6/30/2008 cm 2 cm cm R corrected (mohm) 2477.96 2417.96 2437.96 2347.96 2537.96 2443.96 70.57 5 Resistivity (ohm cm) 222.60 217.21 219.00 210.92 227.99 219.54 6.34 5 inj mold tested Conductivity (S/cm) 4.49E-03 4.60E-03 4.57E-03 4.74E-03 4.39E-03 4.56E-03 1.32E-04 5 Table D.73: Poco Reference 7/11/08 Table D.72: EQ7.5P Disk 32 Results POCO Reference Data Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 3010 2960 2860 2860 3020 Average Std. Dev. n EQ7.5P-TC-32 6/30/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 2997.96 271.98 2947.96 267.44 2847.96 258.37 2847.96 258.37 3007.96 272.89 2929.96 265.81 78.23 7.10 5 5 inj mold tested 7/11/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 10.46 2 10.39 3 10.35 4 10.33 5 10.28 6 10.46 7 10.39 8 10.32 9 10.41 10 10.36 Average 10.375 Stand. Dev. 0.059 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 10.375 mohm lead resistance (mohm) 10.360 mohm Conductivity (S/cm) 3.68E-03 3.74E-03 3.87E-03 3.87E-03 3.66E-03 3.76E-03 1.01E-04 5 235 Table D.75: EQ7.5P Disk 24 Results Table D.74: EQ7.5P Disk 20 Results Sample Data as molded Thickness 0.333 Area 30.14 Diameter 6.195 Test # 1 2 3 4 5 R (mohm) 3120 3120 3070 3060 3080 Average Std. Dev. n EQ7.5P-TC-20 7/11/2008 cm 2 cm cm R corrected (mohm) 3109.64 3109.64 3059.64 3049.64 3069.64 3079.64 28.28 5 Resistivity (ohm cm) 281.47 281.47 276.95 276.04 277.85 278.76 2.56 5 inj mold tested Sample Data as molded Thickness 0.335 Area 30.09 Diameter 6.19 Conductivity (S/cm) 3.55E-03 3.55E-03 3.61E-03 3.62E-03 3.60E-03 3.59E-03 3.29E-05 5 Test # 1 2 3 4 5 236 R (mohm) 2550 2520 2550 2500 2450 Average Std. Dev. n EQ7.5P-TC-24 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 2539.64 228.14 2509.64 225.44 2539.64 228.14 2489.64 223.65 2439.64 219.16 2503.64 224.90 41.59 3.74 5 5 inj mold tested Conductivity (S/cm) 4.38E-03 4.44E-03 4.38E-03 4.47E-03 4.56E-03 4.45E-03 7.46E-05 5 Table D.77: EQ7.5P Disk 17 Results Table D.76: EQ7.5P Disk 13 Results Sample Data as molded Thickness 0.34 Area 30.12 Diameter 6.193 Test # 1 2 3 4 5 R (mohm) 2520 2460 2480 2400 2400 Average Std. Dev. n EQ7.5P-TC-13 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 2509.64 222.34 2449.64 217.03 2469.64 218.80 2389.64 211.71 2389.64 211.71 2441.64 216.32 52.15 4.62 5 5 inj mold tested Sample Data as molded Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 4.50E-03 4.61E-03 4.57E-03 4.72E-03 4.72E-03 4.62E-03 9.86E-05 5 Test # 1 2 3 4 5 237 R (mohm) 3320 3350 3300 3280 3240 Average Std. Dev. n EQ7.5P-TC-17 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 3309.64 300.25 3339.64 302.98 3289.64 298.44 3269.64 296.63 3229.64 293.00 3287.64 298.26 41.47 3.76 5 5 inj mold tested Conductivity (S/cm) 3.33E-03 3.30E-03 3.35E-03 3.37E-03 3.41E-03 3.35E-03 4.24E-05 5 Table D.79: EQ7.5P Disk 12 Results Table D.78: EQ7.5P Disk 15 Results Sample Data as molded Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 3080 3110 3120 3170 3190 Average Std. Dev. n EQ7.5P-TC-15 7/11/2008 cm 2 cm cm inj mold tested Sample Data as molded Thickness 0.33 Area 29.94 Diameter 6.174 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 3069.64 278.48 3.59E-03 3099.64 281.20 3.56E-03 3109.64 282.11 3.54E-03 3159.64 286.65 3.49E-03 3179.64 288.46 3.47E-03 3123.64 283.38 3.53E-03 45.06 4.09 5.08E-05 5 5 5 Test # 1 2 3 4 5 238 R (mohm) 2590 2530 2550 2570 2640 Average Std. Dev. n EQ7.5P-TC-12 7/11/2008 cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 2579.64 234.03 4.27E-03 2519.64 228.59 4.37E-03 2539.64 230.40 4.34E-03 2559.64 232.21 4.31E-03 2629.64 238.56 4.19E-03 2565.64 232.76 4.30E-03 42.19 3.83 7.01E-05 5 5 5 Table D.80: Overall Results for 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 6/30/2008 EQ7.5P-TC-19 6/30/2008 EQ7.5P-TC-32 7/11/2008 EQ7.5P-TC-20 7/11/2008 EQ7.5P-TC-24 7/11/2008 EQ7.5P-TC-13 7/11/2008 EQ7.5P-TC-17 7/11/2008 EQ7.5P-TC-15 7/11/2008 EQ7.5P-TC-12 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 219.54 265.81 278.76 224.90 216.32 298.26 283.38 232.76 252.47 32.65 8 239 Table D.82: 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Replicate Disk 29 Results Table D.81: Poco Reference 6/30/08 POCO Reference Data 6/30/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 12.11 2 12.02 3 11.97 4 12.16 5 12 6 12.09 7 12.01 8 12.13 9 12.1 10 11.98 Average 12.057 Stand. Dev. 0.068 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 12.057 mohm lead resistance (mohm) 12.042 mohm Sample Data sanded by hand Thickness 0.336 Area 30.11 Diameter 6.192 Test # 1 2 3 4 5 240 R (mohm) 2570 2690 2550 2660 2550 Average Std. Dev. n EQ7.5PR-TC-29 6/30/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 2557.96 229.25 2677.96 240.00 2537.96 227.46 2647.96 237.31 2537.96 227.46 2591.96 232.30 66.18 5.93 5 5 tested Conductivity (S/cm) 4.36E-03 4.17E-03 4.40E-03 4.21E-03 4.40E-03 4.31E-03 1.09E-04 5 Table D.84: EQ7.5PR Disk 17 Results Table D.83: EQ7.5PR Disk 6 Results Sample Data sanded by hand Thickness 0.338 Area 30.17 Diameter 6.198 Test # 1 2 3 4 5 EQ7.5PR-TC-6 6/30/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 2480 2467.96 220.30 2390 2377.96 212.27 2450 2437.96 217.62 2470 2457.96 219.41 2540 2527.96 225.66 Average 2453.96 219.05 Std. Dev. 54.13 4.83 n 5 5 inj mold tested Sample Data sanded by hand Thickness 0.338 Area 30.11 Diameter 6.192 Conductivity (S/cm) 4.54E-03 4.71E-03 4.60E-03 4.56E-03 4.43E-03 4.57E-03 1.01E-04 5 Test # 1 2 3 4 5 241 EQ7.5PR-TC-17 6/30/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 2400 2387.96 212.75 2280 2267.96 202.06 2380 2367.96 210.96 2250 2237.96 199.38 2290 2277.96 202.95 Average 2307.96 205.62 Std. Dev. 65.95 5.88 n 5 5 inj mold tested Conductivity (S/cm) 4.70E-03 4.95E-03 4.74E-03 5.02E-03 4.93E-03 4.87E-03 1.38E-04 5 Table D.86: EQ7.5PR Disk 22 Results Table D.85: Poco Reference 7/11/08 POCO Reference Data 7/11/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 10.46 2 10.39 3 10.35 4 10.33 5 10.28 6 10.46 7 10.39 8 10.32 9 10.41 10 10.36 Average 10.375 Stand. Dev. 0.059 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 10.375 mohm lead resistance (mohm) 10.360 mohm Sample Data as molded Thickness 0.34 Area 30.13 Diameter 6.194 Test # 1 2 3 4 5 242 R (mohm) 3730 3710 3790 3710 3670 Average Std. Dev. n EQ7.5PR-TC-22 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 3719.64 329.65 3699.64 327.88 3779.64 334.97 3699.64 327.88 3659.64 324.33 3711.64 328.94 43.82 3.88 5 5 inj mold tested Conductivity (S/cm) 3.03E-03 3.05E-03 2.99E-03 3.05E-03 3.08E-03 3.04E-03 3.57E-05 5 Table D.88: EQ7.5PR Disk 32 Results Table D.87: EQ7.5PR Disk 17 Results Sample Data as molded Thickness 0.335 Area 30.17 Diameter 6.198 Test # 1 2 3 4 5 R (mohm) 3680 3600 3590 3640 3690 Average Std. Dev. n EQ7.5PR-TC-17 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 3669.64 330.50 3589.64 323.30 3579.64 322.39 3629.64 326.90 3679.64 331.40 3629.64 326.90 45.28 4.08 5 5 inj mold tested Sample Data as molded Thickness 0.338 Area 30.11 Diameter 6.192 Conductivity (S/cm) 3.03E-03 3.09E-03 3.10E-03 3.06E-03 3.02E-03 3.06E-03 3.82E-05 5 Test # 1 2 3 4 5 243 R (mohm) 3470 3420 3350 3400 3370 Average Std. Dev. n EQ7.5PR-TC-32 7/11/2008 . cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 3459.64 308.22 3409.64 303.77 3339.64 297.53 3389.64 301.99 3359.64 299.31 3391.64 302.17 46.58 4.15 5 5 inj mold tested Conductivity (S/cm) 3.24E-03 3.29E-03 3.36E-03 3.31E-03 3.34E-03 3.31E-03 4.52E-05 5 Table D.90: EQ7.5PR Disk 24 Results Table D.89: EQ7.5PR Disk 27 Results Sample Data as molded Thickness 0.34 Area 30.12 Diameter 6.193 Test # 1 2 3 4 5 R (mohm) 3290 3020 2980 2960 2920 Average Std. Dev. n EQ7.5PR-TC-27 7/11/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 3279.64 290.56 3009.64 266.64 2969.64 263.10 2949.64 261.33 2909.64 257.78 3023.64 267.88 147.58 13.08 5 5 inj mold tested Sample Data as molded Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 3.44E-03 3.75E-03 3.80E-03 3.83E-03 3.88E-03 3.74E-03 1.73E-04 5 Test # 1 2 3 4 5 244 R (mohm) 3230 3210 3210 3190 3130 Average Std. Dev. n EQ7.5PR-TC-24 7/11/2008 cm 2 cm cm R corrected (mohm) 3219.64 3199.64 3199.64 3179.64 3119.64 3183.64 38.47 5 Resistivity (ohm cm) 292.09 290.28 290.28 288.46 283.02 288.82 3.49 5 inj mold tested Conductivity (S/cm) 3.42E-03 3.45E-03 3.45E-03 3.47E-03 3.53E-03 3.46E-03 4.23E-05 5 Table D.91: Overall Results for 7.5 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Average Sample Resistivity Date Number (ohm cm) 6/30/2008 EQ7.5PR-TC-29 232.30 6/30/2008 EQ7.5PR-TC-6 219.05 6/30/2008 EQ7.5PR-TC-17 205.62 7/11/2008 EQ7.5PR-TC-22 328.94 7/11/2008 EQ7.5PR-TC-17 326.90 7/11/2008 EQ7.5PR-TC-32 302.17 7/11/2008 EQ7.5PR-TC-27 267.88 7/11/2008 EQ7.5PR-TC-24 288.82 Overall Average 271.46 Overall Standard Deviation 48.18 Number of Samples 8 245 Table D.93: 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Disk 11 Results Table D.92: Poco Reference 7/1/08 POCO Reference Data 7/1/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 14.1 2 14.2 3 14.1 4 14.1 5 14.1 6 13.9 7 14.1 8 13.8 9 13.6 10 13.6 Average 13.960 Stand. Dev. 0.222 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 13.960 mohm lead resistance (mohm) 13.945 mohm Sample Data sanded by hand Thickness 0.336 Area 30.13 Diameter 6.194 Test # 1 2 3 4 5 246 R (mohm) 510 500 470 480 470 Average Std. Dev. n EQ10P-TC-11 7/1/2008 cm 2 cm cm R corrected (mohm) 496.06 486.06 456.06 466.06 456.06 472.06 18.17 5 Resistivity (ohm cm) 44.486 43.589 40.899 41.796 40.899 42.334 1.629 5 inj mold tested Conductivity (S/cm) 0.0225 0.0229 0.0245 0.0239 0.0245 0.0236 0.0009 5 Table D.95: EQ10P Disk 18 Results Table D.94: EQ10P Disk 12 Results Sample Data sanded by hand Thickness 0.335 Area 30.17 Diameter 6.198 Test # 1 2 3 4 5 R (mohm) 530 530 510 510 490 Average Std. Dev. n EQ10P-TC-12 7/1/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 516.06 46.478 516.06 46.478 496.06 44.676 496.06 44.676 476.06 42.875 500.06 45.037 16.73 1.507 5 5 inj mold tested Sample Data sanded by hand Thickness 0.335 Area 30.21 Diameter 6.202 Conductivity (S/cm) 0.0215 0.0215 0.0224 0.0224 0.0233 0.0222 0.0008 5 Test # 1 2 3 4 5 247 R (mohm) 560 560 540 540 520 Average Std. Dev. n EQ10P-TC-18 7/1/2008 cm 2 cm cm R corrected (mohm) 546.06 546.06 526.06 526.06 506.06 530.06 16.73 5 Resistivity (ohm cm) 49.243 49.243 47.439 47.439 45.636 47.800 1.509 5 inj mold tested Conductivity (S/cm) 0.0203 0.0203 0.0211 0.0211 0.0219 0.0209 0.0007 5 Table D.97: EQ10P Disk 16 Results Table D.96: EQ10P Disk 24 Results Sample Data sanded by hand Thickness 0.335 Area 30.16 Diameter 6.197 Test # 1 2 3 4 5 R (mohm) 700 700 660 660 650 Average Std. Dev. n EQ10P-TC-24 7/1/2008 cm 2 cm cm R corrected (mohm) 686.06 686.06 646.06 646.06 636.06 660.06 24.08 5 Resistivity (ohm cm) 61.769 61.769 58.167 58.167 57.267 59.428 2.168 5 inj mold tested Sample Data sanded by hand Thickness 0.333 Area 30.19 Diameter 6.2 Conductivity (S/cm) 0.0162 0.0162 0.0172 0.0172 0.0175 0.0168 0.0006 5 Test # 1 2 3 4 5 248 R (mohm) 460 440 430 420 410 Average Std. Dev. n EQ10P-TC-16 7/1/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 446.06 40.441 426.06 38.627 416.06 37.721 406.06 36.814 396.06 35.907 418.06 37.902 19.24 1.744 5 5 tested Conductivity (S/cm) 0.0247 0.0259 0.0265 0.0272 0.0278 0.0264 0.0012 5 Table D.99: Overall Results for 10 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Table D.98: EQ10P Disk 23 Results Sample Data sanded by hand Thickness 0.334 Area 30.13 Diameter 6.194 Test # 1 2 3 4 5 R (mohm) 580 580 580 560 580 Average Std. Dev. n EQ10P-TC-23 7/1/2008 cm 2 cm cm inj mold tested Average Sample Resistivity Date Number (ohm cm) 7/1/2008 EQ10P-TC-11 42.33 7/1/2008 EQ10P-TC-12 45.04 7/1/2008 EQ10P-TC-18 47.80 7/1/2008 EQ10P-TC-24 59.43 7/1/2008 EQ10P-TC-16 37.90 7/1/2008 EQ10P-TC-23 50.96 Overall Average 47.24 Overall Standard Deviation 7.47 Number of Samples 6 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 566.06 51.320 0.0195 566.06 51.320 0.0195 566.06 51.320 0.0195 546.06 49.507 0.0202 566.06 51.320 0.0195 562.06 50.958 0.0196 8.94 0.811 0.0003 5 5 5 249 Table D.101: 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Disk 32 Results Table D.100: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 Sample Data sanded by hand Thickness 0.34 Area 29.93802 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 250 R (mohm) 113 124 122 117 116 Average Std. Dev. n EQ15P-TC-32 6/26/2008 cm 2 cm cm R corrected (mohm) 100.005 111.005 109.005 104.005 103.005 105.405 4.506 5 Resistivity (ohm cm) 8.806 9.774 9.598 9.158 9.070 9.281 0.397 5 inj mold tested Conductivity (S/cm) 0.1136 0.1023 0.1042 0.1092 0.1103 0.1079 0.0046 5 Table D.103: EQ15P Disk 23 Results Table D.102: EQ15P Disk 34 Results Sample Data sanded by hand Thickness 0.33 Area 29.93802 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 110 105 102 96 95 Average Std. Dev. n EQ15P-TC-34 6/26/2008 cm 2 cm cm R corrected (mohm) 97.005 92.005 89.005 83.005 82.005 88.605 6.269 5 Resistivity (ohm cm) 8.800 8.347 8.075 7.530 7.440 8.038 0.569 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.93802 Diameter 6.174 Conductivity (S/cm) 0.1136 0.1198 0.1238 0.1328 0.1344 0.1249 0.0088 5 Test # 1 2 3 4 5 251 R (mohm) 103 98 98 94 95 Average Std. Dev. n EQ15P-TC-23 6/26/2008 cm 2 cm cm R corrected (mohm) 90.005 85.005 85.005 81.005 82.005 84.605 3.507 5 Resistivity (ohm cm) 8.165 7.712 7.712 7.349 7.440 7.676 0.318 5 inj mold tested Conductivity (S/cm) 0.1225 0.1297 0.1297 0.1361 0.1344 0.1305 0.0053 5 Table D.105: EQ15P Disk 19 Results Table D.104: EQ15P Disk 29 Results Sample Data sanded by hand Thickness 0.33 Area 29.93802 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 132 126 123 121 118 Average Std. Dev. n EQ15P-TC-29 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 119.005 10.796 113.005 10.252 110.005 9.980 108.005 9.798 105.005 9.526 111.005 10.071 5.339 0.484 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.93802 Diameter 6.174 Conductivity (S/cm) 0.0926 0.0975 0.1002 0.1021 0.1050 0.0995 0.0047 5 Test # 1 2 3 4 5 252 R (mohm) 107 102 102 94 94 Average Std. Dev. n EQ15P-TC-19 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 94.005 8.528 89.005 8.075 89.005 8.075 81.005 7.349 81.005 7.349 86.805 7.875 5.675 0.515 5 5 inj mold tested Conductivity (S/cm) 0.1173 0.1238 0.1238 0.1361 0.1361 0.1274 0.0083 5 Table D.106: Overall Results for 15 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number Average Resistivity (ohm cm) 6/26/2008 EQ15P-TC-32 9.281 6/26/2008 EQ15P-TC-34 8.038 6/26/2008 EQ15P-TC-23 7.676 6/26/2008 EQ15P-TC-29 10.071 6/26/2008 EQ15P-TC-19 7.875 Overall Average 8.588 Overall Standard Deviation 1.039 Number of Samples 5 253 Combinations Table D.107: Poco Reference 6/27/08 Table D.108: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 15 Results POCO Reference Data 6/27/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 12.77 2 12.57 3 12.46 4 12.30 5 12.44 6 12.51 7 12.46 8 12.87 9 12.39 10 12.49 Average 12.53 Stand. Dev. 0.172 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 12.526 mohm lead resistance (mohm) 12.511 mohm Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 254 R (mohm) 19.9 19.81 19.72 19.79 19.77 Average Std. Dev. n EA2.5B65P-TC-15 6/27/2008 cm 2 cm cm R corrected (mohm) 7.389 7.299 7.209 7.279 7.259 7.287 0.066 5 Resistivity (ohm cm) 0.6507 0.6427 0.6348 0.6410 0.6392 0.6417 0.0058 5 inj mold tested Conductivity (S/cm) 1.5369 1.5559 1.5753 1.5601 1.5644 1.5585 0.0141 5 Table D.110: EA2.5B65P Disk 36 Results Table D.109: EA2.5B65P Disk 31 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 20.8 20.7 20.6 20.8 20.8 Average Std. Dev. n EA2.5B65P-TC-31 6/27/2008 . cm 2 cm cm R corrected (mohm) 8.289 8.189 8.089 8.289 8.289 8.229 0.089 5 Resistivity (ohm cm) 0.7520 0.7430 0.7339 0.7520 0.7520 0.7466 0.0081 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 1.3297 1.3460 1.3626 1.3297 1.3297 1.3396 0.0147 5 Test # 1 2 3 4 5 255 R (mohm) 21.6 21.2 21.3 21.3 21.2 Average Std. Dev. n EA2.5B65P-TC-36 6/26/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 9.089 0.8246 8.689 0.7883 8.789 0.7974 8.789 0.7974 8.689 0.7883 8.809 0.7992 0.164 0.0149 5 5 inj mold tested Conductivity (S/cm) 1.2127 1.2685 1.2541 1.2541 1.2685 1.2516 0.0229 5 Table D.112: EA2.5B65P Disk 17 Results Table D.111: EA2.5B65P Disk 30 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 19.8 19.82 19.91 19.88 19.78 Average Std. Dev. n EA2.5B65P-TC-30 6/27/2008 cm 2 cm cm inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 7.289 0.6613 1.5122 7.309 0.6631 1.5080 7.399 0.6713 1.4897 7.369 0.6686 1.4958 7.269 0.6595 1.5163 7.327 0.6648 1.5044 0.055 0.0050 0.0113 5 5 5 Test # 1 2 3 4 5 256 R (mohm) 20.1 20.02 20.08 20.18 20.11 Average Std. Dev. n EA2.5B65P-TC-17 6/27/2008 cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 7.589 0.6885 1.4524 7.509 0.6813 1.4679 7.569 0.6867 1.4562 7.669 0.6958 1.4372 7.599 0.6894 1.4505 7.587 0.6883 1.4528 0.058 0.0052 0.0110 5 5 5 Table D.113: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 6/27/2008 EA2.5B65P-TC-15 6/27/2008 EA2.5B65P-TC-31 6/27/2008 EA2.5B65P-TC-36 6/27/2008 EA2.5B65P-TC-30 6/27/2008 EA2.5B65P-TC-17 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.6417 0.7466 0.7992 0.6648 0.6883 0.7081 0.0642 5 257 Table D.115: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 10 Results Table D.114: Poco Reference 6/27/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/27/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 12.77 2 12.57 3 12.46 4 12.30 5 12.44 6 12.51 7 12.46 8 12.87 9 12.39 10 12.49 Average 12.53 Stand. Dev. 0.172 R Poco = p t / A 0.015 Rpoco + lead resistance = 12.526 lead resistance (mohm) 12.511 Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 mohm mohm mohm 258 EA2.5B65PR-TC-10 inj mold 6/27/2008 tested cm 2 cm cm R corrected Resistivity Conductivity R (mohm) (mohm) (ohm cm) (S/cm) 18.89 6.379 0.5787 1.7279 18.75 6.239 0.5660 1.7666 18.83 6.319 0.5733 1.7443 18.68 6.169 0.5597 1.7867 18.72 6.209 0.5633 1.7752 Average 6.263 0.5682 1.7601 Std. Dev. 0.085 0.0077 0.0238 n 5 5 5 Table D.117: EA2.5B65PR Disk 7 Results Table D.116: Poco Reference 6/26/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 6/26/2008 0.325 31.669 1.5 Test # R (mohm) 1 13 2 13.2 3 13 4 12.9 5 12.9 6 12.9 7 13 8 13 9 13.1 10 13.1 Average 13.010 Stand. Dev. 0.099 R Poco = p t / A 0.015 Rpoco + lead resistance = 13.010 lead resistance (mohm) 12.995 tested Sample Data sanded by hand Thickness 0.34 Area 29.94 Diameter 6.174 cm 2 cm mohm cm Test # 1 2 3 4 5 mohm mohm mohm 259 R (mohm) 19.02 18.86 18.89 18.68 18.76 Average Std. Dev. n EA2.5B65PR-TC-7 6/26/2008 cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 6.025 0.5306 1.8848 5.865 0.5165 1.9362 5.895 0.5191 1.9264 5.685 0.5006 1.9975 5.765 0.5077 1.9698 5.847 0.5149 1.9430 0.130 0.0114 0.0430 5 5 5 Table D.119: EA2.5B65PR Disk 30 Results Table D.118: EA2.5B65PR Disk 17 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 R (mohm) 18.99 18.89 18.9 18.84 18.97 Average Std. Dev. n EA2.5B65PR-TC-17 6/26/2008 cm 2 cm cm R corrected (mohm) 5.995 5.895 5.905 5.845 5.975 5.923 0.061 5 Resistivity (ohm cm) 0.5439 0.5348 0.5357 0.5303 0.5421 0.5374 0.0056 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 1.8385 1.8697 1.8666 1.8857 1.8447 1.8610 0.0193 5 Test # 1 2 3 4 5 260 EA2.5B65PR-TC-30 6/26/2008 cm 2 cm cm inj mold tested R R corrected Resistivity Conductivity (mohm) (mohm) (ohm cm) (S/cm) 19.01 6.015 0.5457 1.8324 18.91 5.915 0.5367 1.8634 18.92 5.925 0.5376 1.8603 18.98 5.985 0.5430 1.8416 18.98 5.985 0.5430 1.8416 Average 5.965 0.5412 1.8479 Std. Dev. 0.043 0.0039 0.0133 n 5 5 5 Table D.121: EA2.5B65PR Disk 16 Results Table D.120: EA2.5B65PR Disk 19 Results Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Test # 1 2 3 4 5 EA2.5B65PR-TC-19 6/26/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 19.26 6.265 0.5684 19.21 6.215 0.5639 19.13 6.135 0.5566 19.16 6.165 0.5593 19.23 6.235 0.5657 Average 6.203 0.5628 Std. Dev. 0.053 0.0048 n 5 5 inj mold tested Sample Data sanded by hand Thickness 0.33 Area 29.94 Diameter 6.174 Conductivity (S/cm) 1.7593 1.7735 1.7966 1.7878 1.7678 1.7770 0.0151 5 Test # 1 2 3 4 5 261 EA2.5B65PR-TC-16 6/26/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 19.94 6.945 0.6301 19.93 6.935 0.6292 19.92 6.925 0.6283 20.04 7.045 0.6392 19.85 6.855 0.6219 Average 6.941 0.6297 Std. Dev. 0.068 0.0062 n 5 5 inj mold tested Conductivity (S/cm) 1.5871 1.5894 1.5916 1.5645 1.6079 1.5881 0.0155 5 Table D.122: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Date Sample Number Average Resistivity (ohm cm) 6/26/2008 EA2.5B65PR-TC-7 0.5149 6/26/2008 EA2.5B65PR-TC-17 0.5374 6/26/2008 EA2.5B65PR-TC-30 0.5412 6/26/2008 EA2.5B65PR-TC-19 0.5628 6/26/2008 EA2.5B65PR-TC-16 0.6297 6/27/2008 EA2.5B65PR-TC-10 0.5682 Overall Average 0.5590 Overall Standard Deviation Number of Samples 0.0396 6 262 Table D.124: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 29 Results Table D.123: Poco Reference 7/3/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/3/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 14.5 2 14.2 3 14.2 4 14.1 5 14 6 13.9 7 13.9 8 13.8 9 13.8 10 13.6 Average 14.000 Stand. Dev. 0.258 R Poco = p t / A 0.015 Rpoco + lead resistance = 14.000 lead resistance (mohm) 13.985 Sample Data sanded by hand Thickness 0.335 Area 30.09339 Diameter 6.19 Test # 1 2 3 4 5 mohm mohm mohm 263 R (mohm) 528 514 506 475 481 Average Std. Dev. n EA2.5Q6P-TC-29 7/3/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 514.02 46.17 500.02 44.92 492.02 44.20 461.02 41.41 467.02 41.95 486.82 43.73 22.35 2.01 5 5 inj mold tested Conductivity (S/cm) 0.0217 0.0223 0.0226 0.0241 0.0238 0.0229 0.0011 5 Table D.126: EA2.5Q6P Disk 32 Results Table D.125: EA2.5Q6P Disk 17 Results Sample Data sanded by hand Thickness 0.3334 Area 30.00595 Diameter 6.181 Test # 1 2 3 4 5 R (mohm) 407 412 394 389 387 Average Std. Dev. n EA2.5Q6P-TC-17 7/3/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 393.02 35.37 398.02 35.82 380.02 34.20 375.02 33.75 373.02 33.57 383.82 34.54 11.12 1.00 5 5 inj mold tested Sample Data sanded by hand Thickness 0.334 Area 30.09339 Diameter 6.19 Conductivity (S/cm) 0.0283 0.0279 0.0292 0.0296 0.0298 0.0290 0.0008 5 Test # 1 2 3 4 5 264 R (mohm) 1020 970 970 940 890 Average Std. Dev. n EA2.5Q6P-TC-32 7/3/2008 . cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 1006.02 90.64 0.0110 956.02 86.14 0.0116 956.02 86.14 0.0116 926.02 83.43 0.0120 876.02 78.93 0.0127 944.02 85.06 0.0118 47.64 4.29 0.0006 5 5 5 Table D.128: EA2.5Q6P Disk 34 Results Table D.127: EA2.5Q6P Disk 39 Results Sample Data sanded by hand Thickness 0.335 Area 30.00595 Diameter 6.181 Test # 1 2 3 4 5 R (mohm) 720 700 670 650 630 Average Std. Dev. n EA2.5Q6P-TC-39 7/3/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 706.02 63.24 686.02 61.45 656.02 58.76 636.02 56.97 616.02 55.18 660.02 59.12 36.47 3.27 5 5 inj mold tested Sample Data sanded by hand Thickness 0.338 Area 29.96713 Diameter 6.177 Conductivity (S/cm) 0.0158 0.0163 0.0170 0.0176 0.0181 0.0170 0.0009 5 Test # 1 2 3 4 5 265 R (mohm) 890 840 800 780 740 Average Std. Dev. n EA2.5Q6P-TC-34 7/3/2008 cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 876.02 77.67 0.0129 826.02 73.23 0.0137 786.02 69.69 0.0143 766.02 67.92 0.0147 726.02 64.37 0.0155 796.02 70.57 0.0142 57.45 5.09 0.0010 5 5 5 Table D.130: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Table D.129: EA2.5Q6P Disk 26 Results Sample Data sanded by hand Thickness 0.335 Area 30.08367 Diameter 6.189 Test # 1 2 3 4 5 R (mohm) 670 660 640 630 600 Average Std. Dev. n EA2.5Q6P-TC-26 7/3/2008 cm 2 cm cm R corrected (mohm) 656.02 646.02 626.02 616.02 586.02 626.02 27.39 5 inj mold tested Date Sample Number 7/3/2008 EA2.5Q6P-TC-29 7/3/2008 EA2.5Q6P-TC-17 7/3/2008 EA2.5Q6P-TC-32 7/3/2008 EA2.5Q6P-TC-39 7/3/2008 EA2.5Q6P-TC-34 7/3/2008 EA2.5Q6P-TC-26 Overall Average Overall Standard Deviation Number of Samples Resistivity Conductivity (S/cm) (ohm cm) 58.16 0.0172 57.28 0.0175 55.50 0.0180 54.62 0.0183 51.96 0.0192 55.50 0.0180 2.43 0.0008 5 5 266 Average Resistivity (ohm cm) 43.731 34.543 85.056 59.118 70.575 55.503 58.088 18.174 6 Table D.132: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 20 Results Table D.131: Poco Reference 7/7/08 POCO Reference Data 7/7/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 14.3 2 14.3 3 14.2 4 13.8 5 13.9 6 13.8 7 13.8 8 13.8 9 13.9 10 13.7 Average 13.950 Stand. Dev. 0.227 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 13.950 mohm lead resistance (mohm) 13.935 mohm Sample Data sanded by hand Thickness 0.333 Area 29.95 Diameter 6.175 Test # 1 2 3 4 5 267 R (mohm) 303 328 316 318 304 Average Std. Dev. n EA2.5Q6PR-TC-20 7/7/2008 cm 2 cm cm R corrected (mohm) 289.07 314.07 302.07 304.07 290.07 299.87 10.45 5 inj mold tested Resistivity Conductivity (ohm cm) (S/cm) 26.00 0.0385 28.24 0.0354 27.17 0.0368 27.35 0.0366 26.09 0.0383 26.97 0.0371 0.94 0.0013 5 5 Table D.134: EA2.5Q6PR Disk 31 Results Table D.133: EA2.5Q6PR Disk 27 Results Sample Data sanded by hand Thickness 0.33 Area 30.02 Diameter 6.182 Test # 1 2 3 4 5 R (mohm) 608 622 618 608 566 Average Std. Dev. n EA2.5Q6PR-TC-27 7/7/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 594.07 54.03 608.07 55.31 604.07 54.94 594.07 54.03 552.07 50.21 590.47 53.71 22.33 2.03 5 5 inj mold tested Sample Data sanded by hand Thickness 0.334 Area 30.02 Diameter 6.182 Conductivity (S/cm) 0.0185 0.0181 0.0182 0.0185 0.0199 0.0186 0.0007 5 Test # 1 2 3 4 5 268 R (mohm) 461 454 443 442 435 Average Std. Dev. n EA2.5Q6PR-TC-31 7/7/2008 . cm 2 cm cm R corrected (mohm) 447.07 440.07 429.07 428.07 421.07 433.07 10.37 5 Resistivity (ohm cm) 40.18 39.55 38.56 38.47 37.84 38.92 0.93 5 inj mold tested Conductivity (S/cm) 0.0249 0.0253 0.0259 0.0260 0.0264 0.0257 0.0006 5 Table D.136: EA2.5Q6PR Disk 18 Results Table D.135: EA2.5Q6PR Disk 22 Results Sample Data sanded by hand Thickness 0.331 Area 30.00 Diameter 6.18 Test # 1 2 3 4 5 R (mohm) 730 732 707 681 667 Average Std. Dev. n EA2.5Q6PR-TC-22 7/7/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 716.07 64.89 718.07 65.07 693.07 62.81 667.07 60.45 653.07 59.18 689.47 62.48 29.01 2.63 5 5 inj mold tested Sample Data sanded by hand Thickness 0.332 Area 30.01 Diameter 6.181 Conductivity (S/cm) 0.0154 0.0154 0.0159 0.0165 0.0169 0.0160 0.0007 5 Test # 1 2 3 4 5 269 EA2.5Q6PR-TC-18 7/7/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 525 511.07 46.19 519 505.07 45.65 503 489.07 44.20 503 489.07 44.20 485 471.07 42.57 Average 493.07 44.56 Std. Dev. 15.68 1.42 n 5 5 inj mold tested Conductivity (S/cm) 0.0216 0.0219 0.0226 0.0226 0.0235 0.0225 0.0007 5 Table D.138: Overall Results for 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM Nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H701235RN Replicate Table D.137: EA2.5Q6PR Disk 26 Results Sample Data sanded by hand Thickness 0.337 Area 30.00 Diameter 6.18 Test # 1 2 3 4 5 R (mohm) 637 628 614 601 601 Average Std. Dev. n EA2.5Q6PR-TC-26 7/7/2008 cm 2 cm cm inj mold tested Date Sample Number 7/7/2008 EA2.5Q6PR-TC-20 7/7/2008 EA2.5Q6PR-TC-27 7/7/2008 EA2.5Q6PR-TC-31 7/7/2008 EA2.5Q6PR-TC-22 7/7/2008 EA2.5Q6PR-TC-18 7/7/2008 EA2.5Q6PR-TC-26 Overall Average Overall Standard Deviation Number of Samples R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 623.07 56.31 0.0178 614.07 55.50 0.0180 600.07 54.23 0.0184 587.07 53.06 0.0188 587.07 53.06 0.0188 602.27 54.43 0.0184 16.12 1.46 0.0005 5 5 5 270 Average Resistivity (ohm cm) 26.968 53.707 38.918 62.481 44.563 54.432 46.845 12.746 6 Table D.140: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 18 Results Table D.139: Poco Reference 7/7/08 POCO Reference Data 7/7/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 14.3 2 14.3 3 14.2 4 13.8 5 13.9 6 13.8 7 13.8 8 13.8 9 13.9 10 13.7 Average 13.950 Stand. Dev. 0.227 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 13.950 mohm lead resistance (mohm) 13.935 mohm Sample Data sanded by hand Thickness 0.335 Area 30.97 Diameter 6.28 Test # 1 2 3 4 5 271 R (mohm) 10.88 10.9 10.85 10.9 10.87 Average Std. Dev. n EB65Q6P-TC-18 7/7/2008 cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 0.6914 0.0639 15.643 0.7114 0.0658 15.203 0.6614 0.0612 16.352 0.7114 0.0658 15.203 0.6814 0.0630 15.872 0.6914 0.0639 15.655 0.0212 0.0020 0.485 5 5 5 Table D.142: EB65Q6P Disk 17 Results Table D.141: EB65Q6P Disk 16 Results Sample Data sanded by hand Thickness 0.335 Area 30.97 Diameter 6.28 Test # 1 2 3 4 5 R (mohm) 10.96 10.99 11.06 11 11.01 Average Std. Dev. n EB65Q6P-TC-16 7/7/2008 cm 2 cm cm inj mold tested Sample Data sanded by hand Thickness 0.335 Area 30.97 Diameter 6.28 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 0.7714 0.0713 14.020 0.8014 0.0741 13.496 0.8714 0.0806 12.411 0.8114 0.0750 13.329 0.8214 0.0759 13.167 0.8154 0.0754 13.285 0.0365 0.0034 0.584 5 5 5 Test # 1 2 3 4 5 272 R (mohm) 11.24 11.34 11.21 11.35 11.2 Average Std. Dev. n EB65Q6P-TC-17 7/7/2008 cm 2 cm cm R corrected (mohm) 1.0514 1.1514 1.0214 1.1614 1.0114 1.0794 0.0719 5 Resistivity (ohm cm) 0.0972 0.1065 0.0944 0.1074 0.0935 0.0998 0.0066 5 inj mold tested Conductivity (S/cm) 10.287 9.393 10.589 9.312 10.693 10.055 0.659 5 Table D.143: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Date Sample Number 7/7/2008 EB65Q6P-TC-18 7/7/2008 EB65Q6P-TC-16 7/7/2008 EB65Q6P-TC-17 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0639 0.0754 0.0998 0.0797 0.0183 3 273 Table D.145: Dana Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disk 16 Table D.144: Dana Corporation Poco Reference 7/18/08 POCO Reference Data 7/18/2008 Thickness 0.3047 cm Area 12 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 2 3 4 5 6 7 8 9 10 Average R Poco = p t / A Rpoco + lead resistance = lead resistance (mohm) 0.3763 0.3741 0.3787 0.3765 0.3735 0.3746 0.3753 0.3697 0.3658 0.3623 0.3727 0.0381 0.3727 0.3346 tested Sample Data Sanded Thickness Area 2 Test # 1 2 3 4 5 mohm mohm 274 EB65Q6P-TC-16 inj mold 0.3666 cm 2 12.00 cm R (mohm) 2.511 2.494 2.492 2.478 2.476 Average Std. Dev. n R corrected (mohm) 2.176 2.159 2.157 2.143 2.141 2.156 0.0141 5 7/18/2008 tested Thickness (mm) 3.666 3.52 3.783 3.88 3.537 Resistivity (ohm cm) 0.0769 0.0763 0.0762 0.0757 0.0756 0.0761 5.00E-04 5 Conductivity (S/cm) 13.007 13.109 13.121 13.207 13.219 13.133 0.0860 5 Table D.147: Dana Results for EB65Q6P Disk 18 Table D.146: Dana Results for EB65Q6P Disk 17 Sample Data Sanded Thickness Area Test # 1 2 3 4 5 EB65Q6P-TC-17 inj mold 0.3426 cm 2 12.00 cm R (mohm) 2.527 2.508 2.485 2.48 2.47 Average Std. Dev. n R corrected (mohm) 2.192 2.173 2.150 2.145 2.135 2.159 0.0231 5 Sample Data Sanded Thickness Area 7/18/08 tested Thickness (mm) 3.424 3.443 3.418 3.451 3.426 Resistivity (ohm cm) 0.0777 0.0770 0.0762 0.0760 0.0757 0.0765 8.19E-04 5 Conductivity (S/cm) 12.870 12.983 13.122 13.152 13.214 13.068 0.1393 5 Test # 1 2 3 4 5 275 EB65Q6P-TC-18 inj mold 0.3403 cm 2 12.00 cm R (mohm) 2.421 2.37 2.352 2.328 2.32 Average Std. Dev. n 7/18/2008 tested Thickness (mm) 3.4 3.374 3.483 3.403 3.404 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 2.086 0.0736 13.592 2.035 0.0718 13.933 2.017 0.0711 14.057 1.993 0.0703 14.226 1.985 0.0700 14.283 2.024 0.0714 14.018 0.0403 1.42E-03 0.2757 5 5 5 Table D.148: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN from Dana Corporation Date Sample Number 7/18/2008 EB65Q6P-TC-16 7/18/2008 EB65Q6P-TC-17 7/18/2008 EB65Q6P-TC-18 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0761 0.0765 0.0714 0.0747 0.0029 3 276 Table D.150: 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Disk 25 Results Table D.149: Poco Reference 7/8/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/8/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 10.27 2 10.24 3 10.26 4 10.29 5 10.23 6 10.22 7 10.26 8 10.29 9 10.27 10 10.22 Average 10.255 Stand. Dev. 0.026 R Poco = p t / A 0.015 Rpoco + lead resistance = 10.255 lead resistance (mohm) 10.240 Sample Data sanded by hand Thickness 0.333 Area 30.63 Diameter 6.245 Test # 1 2 3 4 5 mohm mohm mohm 277 R (mohm) 10.87 10.95 10.92 10.89 10.92 Average Std. Dev. n EB65Q6PR-TC-25 7/8/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 0.6304 0.0580 0.7104 0.0653 0.6804 0.0626 0.6504 0.0598 0.6804 0.0626 0.6704 0.0617 0.0308 0.0028 5 5 inj mold tested Conductivity (S/cm) 17.246 15.303 15.978 16.715 15.978 16.244 0.750 5 Table D.152: EB65Q6PR Disk 38 Results Table D.151: EB65Q6PR Disk 15 Results Sample Data sanded by hand Thickness 0.334 Area 30.78 Diameter 6.26 Test # 1 2 3 4 5 R (mohm) 10.93 10.98 10.93 10.98 10.93 Average Std. Dev. n EB65Q6PR-TC-15 7/8/2008 cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 0.6904 0.0636 0.7404 0.0682 0.6904 0.0636 0.7404 0.0682 0.6904 0.0636 0.7104 0.0655 0.0274 0.0025 5 5 inj mold tested Sample Data sanded by hand Thickness 0.335 Area 30.78 Diameter 6.26 Conductivity (S/cm) 15.719 14.657 15.719 14.657 15.719 15.294 0.581 5 Test # 1 2 3 4 5 278 R (mohm) 11.04 11.01 10.98 10.94 10.97 Average Std. Dev. n EB65Q6PR-TC-38 7/8/2008 cm 2 cm cm R corrected (mohm) 0.8004 0.7704 0.7404 0.7004 0.7304 0.7484 0.0383 5 Resistivity (ohm cm) 0.0735 0.0708 0.0680 0.0643 0.0671 0.0688 0.0035 5 inj mold tested Conductivity (S/cm) 13.599 14.128 14.701 15.540 14.902 14.574 0.743 5 Table D.153: Overall Results for 6 wt% Hyperion FIBRILTM Nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Date Sample Number 7/8/2008 EB65Q6PR-TC-25 7/8/2008 EB65Q6PR-TC-15 7/8/2008 EB65Q6PR-TC-38 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0617 0.0655 0.0688 0.0653 0.0035 3 279 Table D.155: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Disk 40 Results Table D.154: Poco Reference 7/7/08 POCO Reference Data 7/7/2008 tested Carbon Paper Thickness 0.325 cm 2 Area 31.669 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 14.3 2 14.3 3 14.2 4 13.8 5 13.9 6 13.8 7 13.8 8 13.8 9 13.9 10 13.7 Average 13.950 Stand. Dev. 0.227 R Poco = p t / A 0.015 mohm Rpoco + lead resistance = 13.950 mohm lead resistance (mohm) 13.935 mohm Sample Data sanded by hand Thickness 0.335 Area 31.00445 Diameter 6.283 Test # 1 2 3 4 5 280 R (mohm) 10.64 10.59 10.61 10.61 10.63 Average Std. Dev. n EA2.5B65Q6P-TC-40 7/7/2008 . cm 2 cm cm R corrected Resistivity (mohm) (ohm cm) 0.4514 0.0418 0.4014 0.0371 0.4214 0.0390 0.4214 0.0390 0.4414 0.0409 0.4274 0.0396 0.0195 0.0018 5 5 inj mold tested Conductivity (S/cm) 23.937 26.918 25.641 25.641 24.479 25.323 1.160 5 Table D.157: EA2.5B65Q6P Disk 25 Results Table D.156: Poco Reference 7/21/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/21/2008 0.325 31.669 1.5 Test # R (mohm) 1 11.01 2 10.91 3 10.9 4 10.88 5 10.84 6 10.84 7 10.99 8 10.85 9 11.02 10 10.85 Average 10.909 Stand. Dev. 0.072 R Poco = p t / A 0.015 Rpoco + lead resistance = 10.909 lead resistance (mohm) 10.894 tested Sample Data sanded by hand Thickness 0.336 Area 30.97485 Diameter 6.28 cm 2 cm mohm cm Test # 1 2 3 4 5 mohm mohm mohm 281 R (mohm) 11.48 11.5 11.51 11.43 11.45 Average Std. Dev. n EA2.5B65Q6P-TC-25 7/21/2008 cm 2 cm cm R corrected (mohm) 0.5864 0.6064 0.6164 0.5364 0.5564 0.5804 0.0336 5 inj mold tested Resistivity Conductivity (ohm cm) (S/cm) 0.0541 18.499 0.0559 17.889 0.0568 17.598 0.0494 20.223 0.0513 19.496 0.0535 18.741 0.0031 1.102 5 5 Table D.159: EA2.5B65Q6P Disk 43 Results Table D.158: EA2.5B65Q6P Disk 46 Results Sample Data sanded by hand Thickness 0.337 Area 30.87628 Diameter 6.27 Test # 1 2 3 4 5 R (mohm) 11.38 11.4 11.4 11.4 11.39 Average Std. Dev. n EA2.5B65Q6P-TC-46 7/21/2008 cm 2 cm cm R corrected (mohm) 0.4864 0.5064 0.5064 0.5064 0.4964 0.5004 0.0089 5 inj mold tested Sample Data sanded by hand Thickness 0.336 Area 30.97485 Diameter 6.28 Resistivity Conductivity (ohm cm) (S/cm) 0.0446 22.440 0.0464 21.553 0.0464 21.553 0.0464 21.553 0.0455 21.988 0.0458 21.818 0.0008 0.395 5 5 Test # 1 2 3 4 5 282 R (mohm) 11.47 11.46 11.46 11.45 11.42 Average Std. Dev. n EA2.5B65Q6P-TC-43 7/21/2008 cm 2 cm cm R corrected (mohm) 0.5764 0.5664 0.5664 0.5564 0.5264 0.5584 0.0192 5 inj mold tested Resistivity Conductivity (ohm cm) (S/cm) 0.0531 18.820 0.0522 19.152 0.0522 19.152 0.0513 19.496 0.0485 20.607 0.0515 19.445 0.0018 0.692 5 5 Table D.161: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Table D.160: EA2.5B65Q6P Disk 16 Results Sample Data sanded by hand Thickness 0.336 Area 30.97485 Diameter 6.28 Test # 1 2 3 4 5 R (mohm) 11.31 11.32 11.31 11.34 11.31 Average Std. Dev. n EA2.5B65Q6P-TC-16 7/21/2008 cm 2 cm cm inj mold tested R corrected Resistivity (mohm) (ohm cm) 0.4164 0.0384 0.4264 0.0393 0.4164 0.0384 0.4464 0.0412 0.4164 0.0384 0.4244 0.0391 0.0130 0.0012 5 5 Conductivity (S/cm) 26.051 25.440 26.051 24.300 26.051 25.579 0.762 5 283 Date Sample Number 7/7/2008 EA2.5B65Q6P-TC-40 7/21/2008 EA2.5B65Q6P-TC-25 7/21/2008 EA2.5B65Q6P-TC-46 7/21/2008 EA2.5B65Q6P-TC-43 7/21/2008 EA2.5B65Q6P-TC-16 Overall Average Overall Standard Deviation Average Resistivity (ohm cm) 0.0396 0.0535 0.0458 0.0515 0.0391 0.0459 0.0066 Number of Samples 5 Table D.163: Dana Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Disk 14 Table D.162: Dana Corporation Poco Reference 7/18/08 POCO Reference Data 7/18/2008 Thickness 0.3047 cm Area 12 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 2 3 4 5 6 7 8 9 10 Average R Poco = p t / A Rpoco + lead resistance = lead resistance (mohm) 0.3763 0.3741 0.3787 0.3765 0.3735 0.3746 0.3753 0.3697 0.3658 0.3623 0.3727 0.0381 0.3727 0.3346 tested 2 Sample Data EA2.5B65Q6P- TC-14 inj mold Sanded Thickness 0.3397 cm 2 Area 12.00 cm Test # 1 2 3 4 5 mohm mohm 284 R (mohm) 1.5466 1.5148 1.5016 1.4956 1.4895 Average Std. Dev. n R corrected (mohm) 1.212 1.180 1.167 1.161 1.155 1.175 0.0227 5 7/18/2008 tested Thickness (mm) 3.388 3.4 3.413 3.384 3.397 Resistivity Conductivity (ohm cm) (S/cm) 0.0428 23.357 0.0417 23.986 0.0412 24.257 0.0410 24.383 0.0408 24.511 0.0415 24.099 8.02E-04 0.4581 5 5 Table D.165: Dana Results for EA2.5B65Q6P Injection Molded Disk 57 Table D.164: Dana Results for EA2.5B65Q6P Injection Molded Disk 36 Sample Data Sanded Thickness Area Test # 1 2 3 4 5 EA2.5B65Q6P- TC-36 inj mold 0.3386 cm 2 12.00 cm R (mohm) 1.6383 1.619 1.5994 1.5954 1.5918 Average Std. Dev. n R corrected (mohm) 1.304 1.284 1.265 1.261 1.257 1.274 0.0196 5 Sample Data Sanded Thickness Area 7/18/2008 tested Thickness (mm) 3.346 3.389 3.415 3.38 3.386 Resistivity Conductivity (S/cm) (ohm cm) 0.0462 21.643 0.0455 21.969 0.0448 22.309 0.0447 22.380 0.0446 22.444 0.0452 22.149 6.93E-04 0.3369 5 5 Test # 1 2 3 4 5 285 EA2.5B65Q6P- TC-57 inj mold 0.3403 cm 2 12.00 cm R (mohm) 1.6765 1.6589 1.6654 1.6451 1.6389 Average Std. Dev. n R corrected (mohm) 1.342 1.324 1.331 1.311 1.304 1.322 0.0152 5 7/18/2008 tested Thickness (mm) 3.387 3.434 3.403 3.429 3.391 Resistivity Conductivity (S/cm) (ohm cm) 0.0473 21.133 0.0467 21.414 0.0469 21.309 0.0462 21.639 0.0460 21.742 0.0466 21.447 5.36E-04 0.2464 5 5 Table D.166: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded from Dana Corporation Date Sample Number 7/18/2008 EA2.5B65Q6P-TC-14 7/18/2008 EA2.5B65Q6P-TC-36 7/18/2008 EA2.5B65Q6P-TC-57 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0415 0.0452 0.0466 0.0444 0.0026 3 286 Table D.168: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded Disk 47 Results Table D.167: Poco Reference 7/8/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/8/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 10.27 2 10.24 3 10.26 4 10.29 5 10.23 6 10.22 7 10.26 8 10.29 9 10.27 10 10.22 Average 10.255 Stand. Dev. 0.026 R Poco = p t / A 0.015 Rpoco + lead resistance = 10.255 lead resistance (mohm) 10.240 Sample Data sanded by hand Thickness 0.331 Area 30.87 Diameter 6.269 Test # 1 2 3 4 5 mohm mohm mohm 287 R (mohm) 10.66 10.59 10.59 10.59 10.64 Average Std. Dev. n EA2.5B65Q6PR-TC-47 7/8/2008 cm 2 cm cm R corrected (mohm) 0.4204 0.3504 0.3504 0.3504 0.4004 0.3744 0.0336 5 Resistivity (ohm cm) 0.0392 0.0327 0.0327 0.0327 0.0373 0.0349 0.0031 5 inj mold tested Conductivity (S/cm) 25.509 30.605 30.605 30.605 26.783 28.821 2.483 5 Table D.170: EA2.5B65Q6PR Disk 41 Results Table D.169: EA2.5B65Q6PR Disk 16 Results Sample Data sanded by hand Thickness 0.34 Area 30.19 Diameter 6.2 Test # 1 2 3 4 5 R (mohm) 10.72 10.7 10.72 10.7 10.74 Average Std. Dev. n EA2.5B65Q6PR-TC-16 7/8/2008 cm 2 cm cm R corrected (mohm) 0.4804 0.4604 0.4804 0.4604 0.5004 0.4764 0.0167 5 Resistivity (ohm cm) 0.0427 0.0409 0.0427 0.0409 0.0444 0.0423 0.0015 5 inj mold tested Sample Data sanded by hand Thickness 0.34 Area 30.19 Diameter 6.2 Conductivity (S/cm) 23.443 24.461 23.443 24.461 22.506 23.663 0.823 5 Test # 1 2 3 4 5 288 R (mohm) 10.85 10.86 10.83 10.81 10.81 Average Std. Dev. n EA2.5B65Q6PR-TC-41 7/8/2008 . cm 2 cm cm inj mold tested R corrected Resistivity (mohm) (ohm cm) 0.6104 0.0542 0.6204 0.0551 0.5904 0.0524 0.5704 0.0506 0.5704 0.0506 0.5924 0.0526 0.0228 0.0020 5 5 Conductivity (S/cm) 18.450 18.153 19.075 19.744 19.744 19.033 0.729 5 Table D.172: EA2.5B65Q6PR Disk 19 Results Table D.171: EA2.5B65Q6PR Disk 12 Results Sample Data sanded by hand Thickness 0.339 Area 30.89 Diameter 6.271 Test # 1 2 3 4 5 R (mohm) 11.46 11.32 11.31 11.42 11.22 Average Std. Dev. n EA2.5B65Q6PR-TC-12 7/8/2008 cm 2 cm cm R corrected (mohm) 0.4834 0.3434 0.3334 0.4434 0.2434 0.3694 0.0953 5 inj mold tested Sample Data sanded by hand Thickness 0.335 Area 31.00 Diameter 6.283 Resistivity Conductivity (ohm cm) (S/cm) 0.0440 22.706 0.0313 31.963 0.0304 32.921 0.0404 24.754 0.0222 45.095 0.0337 31.488 0.0087 8.802 5 5 Test # 1 2 3 4 5 289 R (mohm) 11.36 11.36 11.36 11.33 11.28 Average Std. Dev. n EA2.5B65Q6PR-TC-19 7/8/2008 . cm 2 cm cm inj mold tested R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 0.3834 0.0355 28.182 0.3834 0.0355 28.182 0.3834 0.0355 28.182 0.3534 0.0327 30.575 0.3034 0.0281 35.613 0.3614 0.0334 30.147 0.0349 0.0032 3.227 5 5 5 Table D.174: EA2.5B65Q6PR Disk 41 Results Table D.173: EA2.5B65Q6PR Disk 22 Results Sample Data sanded by hand Thickness 0.337 Area 30.88 Diameter 6.27 Test # 1 2 3 4 5 R (mohm) 11.31 11.27 11.31 11.27 11.24 Average Std. Dev. n EA2.5B65Q6PR-TC-22 7/8/2008 cm 2 cm cm inj mold tested Sample Data sanded by hand Thickness 0.331 Area 30.87 Diameter 6.269 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 0.3334 0.0305 32.738 0.2934 0.0269 37.201 0.3334 0.0305 32.738 0.2934 0.0269 37.201 0.2634 0.0241 41.438 0.3034 0.0278 36.263 0.0300 0.0027 3.654 5 5 5 Test # 1 2 3 4 5 290 R (mohm) 11.67 11.57 11.56 11.45 11.42 Average Std. Dev. n EA2.5B65Q6PR-TC-41 7/8/2008 cm 2 cm cm R corrected (mohm) 0.6934 0.5934 0.5834 0.4734 0.4434 0.5574 0.1006 5 Resistivity (ohm cm) 0.0647 0.0553 0.0544 0.0441 0.0413 0.0520 0.0094 5 inj mold tested Conductivity (S/cm) 15.465 18.072 18.381 22.653 24.185 19.751 3.576 5 Table D.175: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded Date 7/8/2008 7/8/2008 7/8/2008 7/8/2008 7/8/2008 7/8/2008 7/8/2008 Sample Number EA2.5B65Q6PR-TC-47 EA2.5B65Q6PR-TC-16 EA2.5B65Q6PR-TC-41 EA2.5B65Q6PR-TC-12 EA2.5B65Q6PR-TC-19 EA2.5B65Q6PR-TC-22 EA2.5B65Q6PR-TC-41 Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0349 0.0423 0.0526 0.0337 0.0334 0.0278 0.0520 0.0395 0.0097 7 291 Table D.177: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Disk 8C Results Table D.176: Poco Reference 7/21/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/21/2008 tested 0.325 31.669 1.5 cm 2 cm mohm cm Test # R (mohm) 1 11.01 2 10.91 3 10.9 4 10.88 5 10.84 6 10.84 7 10.99 8 10.85 9 11.02 10 10.85 Average 10.909 Stand. Dev. 0.072 R Poco = p t / A 0.015 Rpoco + lead resistance = 10.909 lead resistance (mohm) 10.894 Sample Data sanded by hand Thickness 0.336 Area 30.97 Diameter 6.28 Test # 1 2 3 4 5 mohm mohm mohm 292 R (mohm) 11.6 11.57 11.59 11.56 11.53 Average Std. Dev. n EA2.5B65Q6PR-8C comp mold 7/21/2008 tested cm 2 cm cm R corrected (mohm) 0.6521 0.6221 0.6421 0.6121 0.5821 0.6221 0.0274 5 Resistivity Conductivity (ohm cm) (S/cm) 0.0601 16.634 0.0574 17.436 0.0592 16.893 0.0564 17.721 0.0537 18.634 0.0574 17.464 0.0025 0.783 5 5 Table D.179: EA2.5B65Q6P Disk 1C Results Table D.178: Poco Reference 7/9/08 POCO Reference Data Carbon Paper Thickness Area Resistivity 7/9/2008 0.326 20.2683 1.5 Test # R (mohm) 1 10.87 2 10.91 3 10.88 4 10.83 5 10.71 6 10.85 7 10.72 8 10.76 9 10.69 10 10.73 Average 10.795 Stand. Dev. 0.081 R Poco = p t / A 0.024 Rpoco + lead resistance = 10.795 lead resistance (mohm) 10.771 tested Sample Data sanded by hand Thickness 0.336 Area 19.62 Diameter 4.998 cm 2 cm mohm cm Test # 1 2 3 4 5 mohm mohm mohm 293 R (mohm) 11.69 11.69 11.88 11.66 11.73 Average Std. Dev. n EA2.5B65Q6PR-1C 7/9/2008 cm 2 cm cm R corrected (mohm) 0.9191 0.9191 1.1091 0.8891 0.9591 0.9591 0.0875 5 comp mold tested Resistivity Conductivity (ohm cm) (S/cm) 0.0537 18.633 0.0537 18.633 0.0648 15.441 0.0519 19.262 0.0560 17.856 0.0560 17.965 0.0051 1.496 5 5 Table D.181: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Table D.180: EA2.5B65Q6P Disk 3C Results Sample Data sanded by hand Thickness 0.328 Area 19.59 Diameter 4.994 Test # 1 2 3 4 5 EA2.5B65Q6PR-3C 7/9/2008 cm 2 cm cm R corrected Resistivity R (mohm) (mohm) (ohm cm) 11.55 0.7791 0.0465 11.55 0.7791 0.0465 11.44 0.6691 0.0400 11.45 0.6791 0.0406 11.53 0.7591 0.0453 Average 0.7331 0.0438 Std. Dev. 0.0546 0.0033 n 5 5 comp mold tested Conductivity (S/cm) 21.492 21.492 25.025 24.657 22.058 22.945 1.751 5 294 Date Sample Number Average Resistivity (ohm cm) 7/21/2008 EA2.5B65Q6P-TC-8C 0.0574 7/9/2008 EA2.5B65Q6P-TC-1C 0.0560 7/9/2008 EA2.5B65Q6P-TC-3C 0.0438 Overall Average 0.0524 Overall Standard Deviation 0.0075 Number of Samples 5 Table D.183: Dana Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Disk 1C Table D.182: Dana Corporation Poco Reference 7/18/08 POCO Reference Data 7/18/2008 Thickness 0.3047 cm Area 12 cm Resistivity 1.5 mohm cm Test # R (mohm) 1 2 3 4 5 6 7 8 9 10 Average R Poco = p t / A Rpoco + lead resistance = lead resistance (mohm) 0.3763 0.3741 0.3787 0.3765 0.3735 0.3746 0.3753 0.3697 0.3658 0.3623 0.3727 0.0381 0.3727 0.3346 tested 2 Sample Data EA2.5B65Q6P- 1C comp mold Sanded Thickness Area 0.3393 12.00 cm cm 2 7/18/2008 tested Thickness (mm) 3.402 3.393 3.388 3.38 3.394 Test # 1 2 3 4 5 mohm mohm 295 R (mohm) 1.8063 1.7957 1.7913 1.7875 1.7791 Average Std. Dev. n R corrected (mohm) 1.472 1.461 1.457 1.453 1.445 1.457 0.0101 5 Resistivity Conductivity (ohm cm) (S/cm) 0.0520 19.212 0.0517 19.352 0.0515 19.410 0.0514 19.461 0.0511 19.574 0.0515 19.402 3.56E-04 0.1338 5 5 Table D.185: Dana Results for EA2.5B65Q6P Disk 3C Table D.184: Dana Results for EA2.5B65Q6P Disk 2C Sample Data EA2.5B65Q6P- 2C comp mold Sanded Thickness 0.3383 cm Area 12.00 cm 2 7/18/2008 Sample Data tested Thickness (mm) EA2.5B65Q6P- 3C comp mold Sanded 3.395 3.383 Thickness 0.3304 cm 3.387 3.344 Area 12.00 cm 2 3.372 Test # 1 2 3 4 5 R (mohm) 1.5111 1.5038 1.4933 1.4877 1.4848 Average Std. Dev. n 7/18/2008 tested Thickness (mm) 3.312 3.28 3.273 3.336 3.304 R corrected Resistivity Conductivity (mohm) (ohm cm) (S/cm) 1.177 0.0417 23.962 1.169 0.0415 24.112 1.159 0.0411 24.330 1.153 0.0409 24.448 1.150 0.0408 24.510 1.162 0.0412 24.273 0.0111 3.93E-04 0.2307 5 5 5 Test # 1 2 3 4 5 296 R (mohm) 1.6561 1.6365 1.6444 1.6237 1.6158 Average Std. Dev. n R corrected (mohm) 1.322 1.302 1.310 1.289 1.281 1.301 0.0161 5 Resistivity (ohm cm) 0.0480 0.0473 0.0476 0.0468 0.0465 0.0472 5.83E-04 5 Conductivity (S/cm) 20.835 21.148 21.021 21.358 21.490 21.171 0.2613 5 Table D.186: Overall Results for 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM Nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded from Dana Corporation Date Sample Number 7/18/2008 EA2.5B65Q6P-1C 7/18/2008 EA2.5B65Q6P-2C 7/18/2008 EA2.5B65Q6P-3C Overall Average Overall Standard Deviation Number of Samples Average Resistivity (ohm cm) 0.0515 0.0412 0.0472 0.0467 0.0052 3 297 Appendix E: TCA 300 Through-Plane Thermal Conductivity Results at 55°C EP Table E.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/9/2008 6/9/2008 6/9/2008 6/9/2008 Sample Number EP-TC-13 EP-TC-17 EP-TC-22 EP-TC-20 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2049 0.2045 0.2077 0.2083 0.2063 0.0019 4 Table E.2: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 8/25/2008 8/25/2008 8/25/2008 8/25/2008 Sample Number EPR-TC-21 EPR-TC-29 EPR-TC-33 EPR-TC-37 Average Standard Deviation Number of Samples 298 Through Plane Thermal Conductivity (W/m•K) 0.2019 0.2051 0.2029 0.2054 0.2038 0.0017 4 EAP’s Table E.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/9/2008 6/9/2008 6/9/2008 6/10/2008 6/10/2008 Sample Number EA2.5P-TC-14 EA2.5P-TC-25 EA2.5P-TC-19 EA2.5P-TC-28 EA2.5P-TC-30 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2176 0.2235 0.2166 0.2212 0.2252 0.2208 0.0037 5 Table E.4: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/10/2008 6/10/2008 6/10/2008 6/10/2008 6/10/2008 Sample Number EA2.5PR-TC-14 EA2.5PR-TC-19 EA2.5PR-TC-22 EA2.5PR-TC-24 EA2.5PR-TC-30 Average Standard Deviation Number of Samples 299 Through Plane Thermal Conductivity (W/m•K) 0.2210 0.2270 0.2266 0.2244 0.2249 0.2248 0.0024 5 Table E.5: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/11/2008 6/12/2008 6/11/2008 6/11/2008 Sample Number EA4P-TC-17 EA4P-TC-24 EA4P-TC-34 EA4P-TC-30 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2464 0.2381 0.2325 0.2441 0.2403 0.0062 4 Table E.6: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/13/2008 6/13/2008 6/13/2008 6/13/2008 6/13/2008 Sample Number EA5P-TC-21 EA5P-TC-22 EA5P-TC-24 EA5P-TC-25 EA5P-TC-26 Average Standard Deviation Number of Samples 300 Through Plane Thermal Conductivity (W/m•K) 0.2536 0.2525 0.2530 0.2486 0.2470 0.2509 0.0029 5 Table E.7: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/11/2008 7/15/2008 7/15/2008 7/11/2008 Sample Number EA6P-TC-24 EA6P-TC-27 EA6P-TC-28 EA6P-TC-29 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2665 0.2569 0.2612 0.2589 0.2608 0.0041 4 Table E.8: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/21/2008 7/21/2008 7/21/2008 7/21/2008 Sample Number EA7.5P-TC-20 EA7.5P-TC-23 EA7.5P-TC-24 EA7.5P-TC-25 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2846 0.2667 0.2780 0.2780 0.2768 0.0074 4 Table E.9: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/21/2008 7/22/2008 7/22/2008 7/22/2008 7/22/2008 Through Plane Thermal Conductivity Sample Number (W/m•K) EA10P-TC-24 0.3000 EA10P-TC-34 0.3003 EA10P-TC-23 0.2960 EA10P-TC-25 0.2960 EA10P-TC-32 0.2990 Average 0.2983 Standard Deviation 0.0021 Number of Samples 5 301 Table E.10: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/15/2008 7/15/2008 7/15/2008 7/15/2008 7/15/2008 Through Plane Thermal Conductivity Sample Number (W/m•K) EA15P-TC-21 0.3363 EA15P-TC-22 0.3369 EA15P-TC-30 0.3380 EA15P-TC-31 0.3380 EA15P-TC-35 0.3380 Average 0.3374 Standard Deviation 0.0008 Number of Samples 5 302 EBP’s Table E.11: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/23/2008 6/23/2008 6/23/2008 6/23/2008 6/23/2008 Sample Number EB10P-TC-12 EB10P-TC-19 EB10P-TC-35 EB10P-TC-27 EB10P-TC-23 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2325 0.2269 0.2373 0.2326 0.2385 0.2335 0.0046 5 Table E.12: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/23/2008 6/23/2008 6/24/2008 6/24/2008 Sample Number EB15P-TC-17 EB15P-TC-20 EB15P-TC-22 EB15P-TC-23 Average Standard Deviation Number of Samples 303 Through Plane Thermal Conductivity (W/m•K) 0.2645 0.2692 0.2683 0.2628 0.2662 0.0030 4 Table E.13: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/24/2008 6/24/2008 6/24/2008 6/24/2008 Sample Number EB20P-TC-13 EB20P-TC-15 EB20P-TC-20 EB20P-TC-31 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2993 0.2879 0.2929 0.2885 0.2922 0.0053 4 Table E.14: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/24/2008 6/24/2008 6/24/2008 6/24/2008 Sample Number EB25P-TC-8 EB25P-TC-9 EB25P-TC-11 EB25P-TC-33 Average Standard Deviation Number of Samples 304 Through Plane Thermal Conductivity (W/m•K) 0.3529 0.3520 0.3573 0.3485 0.3527 0.0036 4 Table E.15: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/25/2008 6/25/2008 6/25/2008 6/25/2008 Sample Number EB30P-TC-17 EB30P-TC-20 EB30P-TC-25 EB30P-TC-30 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.4391 0.4384 0.4381 0.4392 0.4387 0.0005 4 Table E.16: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/26/2008 6/26/2008 6/26/2008 6/26/2008 Sample Number EB35P-TC-22 EB35P-TC-26 EB35P-TC-31 EB35P-TC-32 Average Standard Deviation Number of Samples 305 Through Plane Thermal Conductivity (W/m•K) 0.5033 0.4958 0.5066 0.5082 0.5034 0.0055 4 Table E.17: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/27/2008 6/26/2008 6/26/2008 6/26/2008 Sample Number EB40P-TC-10 EB40P-TC-16 EB40P-TC-32 EB40P-TC-34 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.6200 0.6361 0.6348 0.6218 0.6282 0.0084 4 Table E.18: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/27/2008 6/27/2008 6/27/2008 6/27/2008 Sample Number EB45P-TC-8 EB45P-TC-17 EB45P-TC-26 EB45P-TC-31 Average Standard Deviation Number of Samples 306 Through Plane Thermal Conductivity (W/m•K) 0.7557 0.7553 0.7350 0.7183 0.7411 0.0180 4 Table E.19: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/30/2008 6/30/2008 6/30/2008 6/30/2008 Sample Number EB50P-TC-29 EB50P-TC-26 EB50P-TC-25 EB50P-TC-24 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.8958 0.8966 0.8896 0.9038 0.8964 0.0058 4 Table E.20: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/22/2008 7/1/2008 7/1/2008 7/2/2008 Sample Number EB55P-TC-28 EB55P-TC-28 EB55P-TC-26 EB55P-TC-27 Average Standard Deviation Number of Samples 307 Through Plane Thermal Conductivity (W/m•K) 1.154 1.149 1.156 1.144 1.151 0.005 4 Table E.21: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/2/2008 7/2/2008 7/2/2008 8/18/2008 Sample Number EB60P-TC-22 EB60P-TC-24 EB60P-TC-27 EB60P-TC-21 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 1.487 1.474 1.526 1.490 1.494 0.022 4 Table E.22: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/3/2008 7/3/2008 7/3/2008 7/3/2008 Sample Number EB65P-TC-22 EB65P-TC-25 EB65P-TC-27 EB65P-TC-29 Average Standard Deviation Number of Samples 308 Through Plane Thermal Conductivity (W/m•K) 1.889 1.903 2.035 2.060 1.972 0.088 4 Table E.23: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 7/3/2008 7/3/2008 7/7/2008 7/7/2008 Sample Number EB65PR-TC-22 EB65PR-TC-20 EB65PR-TC-21 EB65PR-TC-29 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 2.028 2.049 1.926 1.946 1.987 0.060 4 Table E.24: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/8/2008 7/9/2008 7/9/2008 8/18/2008 Sample Number EB70P-TC-29/21 EB70P-TC-25/27 EB70P-TC-28/29 EB70P-TC-21/25 Average Standard Deviation Number of Samples 309 Through Plane Thermal Conductivity (W/m•K) 2.733 2.766 2.701 2.650 2.713 0.049 4 Table E.25: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/18/2008 7/8/2008 7/18/2008 7/8/2008 7/23/2008 Sample Number EB75P-TC-24/28 EB75P-TC-24/23 EB75P-TC-29/28 EB75P-TC-27/28 EB75P-TC-21/17 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 3.603 3.655 3.614 3.693 3.640 3.641 0.036 5 Table E.26: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/9/2008 7/9/2008 7/10/2008 7/10/2008 7/10/2008 Sample Number EB80P-TC-23,20 EB80P-TC-23/25 EB80P-TC-20/27 EB80P-TC-20/27/23 EB80P-TC-29/23 Average Standard Deviation Number of Samples 310 Through Plane Thermal Conductivity (W/m•K) 6.118 6.101 5.911 6.119 5.962 6.042 0.098 5 EQP’s Table E.27: 1.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/15/2008 7/15/2008 7/15/2008 7/15/2008 7/15/2008 Sample Number EQ1.5P-TC-21 EQ1.5P-TC-24 EQ1.5P-TC-30 EQ1.5P-TC-27 EQ1.5P-TC-33 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2156 0.2144 0.2155 0.2138 0.2162 0.2151 0.0010 5 Table E.28: 2.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/16/2008 7/16/2008 7/16/2008 7/16/2008 7/16/2008 Sample Number EQ2.5P-TC-23 EQ2.5P-TC-26 EQ2.5P-TC-20 EQ2.5P-TC-29 EQ2.5P-TC-21 Average Standard Deviation Number of Samples 311 Through Plane Thermal Conductivity (W/m•K) 0.2295 0.2250 0.2287 0.2310 0.2308 0.2290 0.0024 5 Table E.29: 4 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/17/2008 6/17/2008 6/18/2008 6/18/2008 Sample Number EQ4P-TC-20 EQ4P-TC-22 EQ4P-TC-24 EQ4P-TC-30 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.2581 0.2561 0.2611 0.2583 0.2584 0.0021 4 Table E.30: 5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/18/2008 6/18/2008 6/18/2008 6/19/2008 Sample Number EQ5P-TC-20 EQ5P-TC-31 EQ5P-TC-22 EQ5P-TC-26 Average Standard Deviation Number of Samples 312 Through Plane Thermal Conductivity (W/m•K) 0.2833 0.2803 0.2791 0.2837 0.2816 0.0023 4 Table E.31: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/16/2008 7/16/2008 7/16/2008 7/16/2008 Sample Number EQ6P-TC-22 EQ6P-TC-24 EQ6P-TC-29 EQ6P-TC-30 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.3000 0.3060 0.3030 0.2997 0.3022 0.0030 4 Table E.32: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/19/2008 6/19/2008 6/19/2008 6/19/2008 Sample Number EQ6PR-TC-22 EQ6PR-TC-24 EQ6PR-TC-27 EQ6PR-TC-28 Average Standard Deviation Number of Samples 313 Through Plane Thermal Conductivity (W/m•K) 0.2983 0.2965 0.2992 0.2965 0.2976 0.0014 4 Table E.33: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 6/19/2008 6/19/2008 6/19/2008 8/15/2008 Sample Number EQ7.5P-TC-23 EQ7.5P-TC-25 EQ7.5P-TC-34 EQ7.5P-TC-28 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.3268 0.3317 0.3283 0.3287 0.3288 0.0021 4 Table E.34: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 6/20/2008 6/20/2008 6/20/2008 8/15/2008 Sample Number EQ7.5PR-TC-23 EQ7.5PR-TC-25 EQ7.5PR-TC-33 EQ7.5PR-TC-30 Average Standard Deviation Number of Samples 314 Through Plane Thermal Conductivity (W/m•K) 0.3277 0.3225 0.3229 0.3190 0.3230 0.0036 4 Table E.35: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/21/2008 7/21/2008 7/21/2008 7/21/2008 Sample Number EQ10P-TC-22 EQ10P-TC-26 EQ10P-TC-29 EQ10P-TC-31 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.3670 0.3703 0.3745 0.3761 0.3720 0.0041 4 Table E.36: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/17/2008 7/17/2008 7/17/2008 7/17/2008 Sample Number EQ15P-TC-24 EQ15P-TC-26 EQ15P-TC-30 EQ15P-TC-33 Average Standard Deviation Number of Samples 315 Through Plane Thermal Conductivity (W/m•K) 0.4624 0.4716 0.4651 0.4677 0.4667 0.0039 4 Combinations Table E.37: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/25/2008 7/25/2008 7/31/2008 8/18/2008 Sample Number EA2.5B65P-TC-26 EA2.5B65P-TC-21 EA2.5B65P-TC-29 EA2.5B65P-TC-14 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 2.880 2.730 2.799 2.700 2.777 0.080 4 Table E.38: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 7/31/2008 7/25/2008 7/28/2008 7/31/2008 Sample Number EA2.5B65PR-TC-35 EA2.5B65PR-TC-19 EA2.5B65PR-TC-13 EA2.5B65PR-TC-29 Average Standard Deviation Number of Samples 316 Through Plane Thermal Conductivity (W/m•K) 2.700 2.640 2.780 2.830 2.738 0.084 4 Table E.39: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 7/11/2008 7/11/2008 7/11/2008 8/15/2008 Sample Number EA2.5Q6P-TC-22 EA2.5Q6P-TC-30 EA2.5Q6P-TC-37 EA2.5Q6P-TC-21 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 0.3426 0.3277 0.3350 0.3280 0.3333 0.0070 4 Table E.40: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 7/24/2008 7/24/2008 7/24/2008 7/24/2008 7/24/2008 Sample Number EA2.5Q6PR-TC-24 EA2.5Q6PR-TC-19 EA2.5Q6PR-TC-26 EA2.5Q6PR-TC-30 EA2.5Q6PR-TC-32 Average Standard Deviation Number of Samples 317 Through Plane Thermal Conductivity (W/m•K) 0.3368 0.3416 0.3384 0.3361 0.3437 0.3393 0.0032 5 Table E.41: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 8/7/2008 8/7/2008 7/29/2008 8/7/2008 Sample Number EB65Q6P-TC-31,34,19 EB65Q6P-TC-24,31,19 EB65Q6P-TC-31,34 EB65Q6P-TC-34,31,28 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 4.780 4.770 4.770 4.690 4.753 0.042 4 Table E.42: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date 7/30/2008 7/30/2008 7/30/2008 8/6/2008 Sample Number EB65Q6PR-TC-11,20 EB65Q6PR-TC-37,26 EB65Q6PR-TC-11,30 EB65Q6PR-TC-37,20,26 Average Standard Deviation Number of Samples 318 Through Plane Thermal Conductivity (W/m•K) 4.632 4.690 4.800 4.760 4.721 0.074 4 Table E.43: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Test Date 8/5/2008 8/5/2008 8/5/2008 8/5/2008 8/5/2008 Sample Number EA2.5B65Q6P-TC-29,37 EA2.5B65Q6P-TC-54,50 EA2.5B65Q6P-TC-37,17 EA2.5B65Q6P-TC-29,54 EA2.5B65Q6P-TC-54,37 Average Standard Deviation Number of Samples Through Plane Thermal Conductivity (W/m•K) 5.812 5.810 5.980 5.860 5.720 5.836 0.095 5 Table E.44: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Injection Molded Test Date 8/8/2008 8/14/2008 8/13/2008 8/13/2008 Sample Number EA2.5B65Q6PR-TC-7,31 EA2.5B65Q6PR-TC-35,24 EA2.5B65Q6PR-TC-46,7 EA2.5B65Q6PR-TC-7,26 Average Standard Deviation Number of Samples 319 Through Plane Thermal Conductivity (W/m•K) 5.844 5.750 5.770 5.910 5.819 0.073 4 Table E.45: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Test Date 9/4/2008 9/4/2008 9/4/2008 9/5/2008 Sample Number EA2.5B65Q6P-1,2,3C EA2.5B65Q6P-5,3,1C EA2.5B65Q6P-7,6,2C EA2.5B65Q6P-6,7,1C Average Standard Deviation Number of Samples 320 Through Plane Thermal Conductivity (W/m•K) 6.610 6.620 6.489 6.560 6.570 0.060 6.610 Appendix F: Heat Capacity Table F.1: Density and Specific Heat Values for Each Component Used [1] Component Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Specific Heat (J/kg•K) Density (Kg/m3) 1390 900 Thermocarb TC-300 (B) 720 2240 Ketjenblack EC-600 JD (A) 900 1800 Hyperion FIBRILTM Nanotubes (Q) 650 2000 The theoretical specific heat for each formulation of polypropylene and components A, B, and Q was calculated using Equation 1 below. Equation 1 uses individual components weight fraction is Фi and the specific heat of the individual component Cpi (J/kg·K) to calculate the specific heat, Cpc (J/kg·K), for each individual formulation. To calculate the theoretical density for each individual formulation Equation 2, shown below, was used where ρtheo is the density (g/cm3) of the formulation, 3 Фi is the weight fraction of component and ρi is the density (g/cm ) of the individual component. From the theoretical density and specific heat we could use Equation 3 shown on the next page to calculate the theoretical volumetric specific heat c (MJ/m3·K) for all the formulations. This value is necessary when using the HotDisk to determine the through-plane and in-plane thermal conductivity of a formulation n C pc = ∑ Φi ⋅ C pi i =1 321 (1) 1 ρTheo = c= (C (2) φ ∑i ρi i pc ⋅ ρtheo ) 3 10 322 (3) Table F.2: Theoretical Specific Heat, Density, and Volumetric Specific Heat for Thermocarb TC-300 Synthetic Graphite, Ketjenblack EC-600 JD Carbon Black, and Hyperion FIBRILTM Nanotubes Formulations Formulation EP EB10P EB15P EB20P EB25P EB30P EB35P EB40P EB45P EB50P EB55P EB60P EB65P EB70P EB75P EB80P EA2.5P EA4P EA5P EA6P EA7.5P EA10P EA15P EQ1.5P EQ2.5P EQ4P EQ5P EQ6P EQ7.5P EQ10P EQ15P EQ20P EA2.5Q6P EA2.5B65P EB65Q6P EA2.5B65Q6P Weight Fraction of Filler 0.000 0.100 0.150 0.200 0.250 0.300 0.350 0.400 0.450 0.500 0.550 0.600 0.650 0.700 0.750 0.800 0.025 0.040 0.050 0.060 0.075 0.100 0.150 0.015 0.025 0.040 0.050 0.060 0.075 0.100 0.150 0.200 Weight Fraction of Polymer 1.000 0.900 0.850 0.800 0.750 0.700 0.650 0.600 0.550 0.500 0.450 0.400 0.350 0.300 0.250 0.200 0.975 0.960 0.950 0.940 0.925 0.900 0.850 0.985 0.975 0.960 0.950 0.940 0.925 0.900 0.850 0.800 Theoretical Volumetric Theoretical Specific Heat Specific 3 Heat (J/kg•K) (MJ/m K) 1390 1.2510 1323 1.2665 1290 1.2750 1256 1.2840 1223 1.2937 1189 1.3041 1156 1.3154 1122 1.3274 1089 1.3405 1055 1.3547 1022 1.3702 988 1.3871 955 1.4056 921 1.4261 888 1.4487 854 1.4740 1378 1.2557 1370 1.2585 1366 1.2605 1361 1.2624 1353 1.2654 1341 1.2704 1317 1.2809 1379 1.2513 1372 1.2516 1360 1.2519 1353 1.2521 1346 1.2524 1335 1.2527 1316 1.2533 1279 1.2546 1242 1.2560 1333 1.2572 942 1.4165 910 1.4167 898 1.4285 323 Theoretical Density 3 (g/cm ) 0.9000 0.9573 0.9887 1.0223 1.0583 1.0968 1.1383 1.1831 1.2315 1.2841 1.3413 1.4039 1.4726 1.5484 1.6324 1.7260 0.9114 0.9184 0.9231 0.9278 0.9351 0.9474 0.9730 0.9075 0.9125 0.9202 0.9254 0.9307 0.9387 0.9524 0.9809 1.0112 0.9429 1.5034 1.5567 1.5911 EP Table F.3: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample EP-2 EP-3 EP-4 EP-5 EP-6 EP-7 Disks Used Average Stdev Specific Heat (J/kgK) 1409.4 1396.7 1391.6 1379.2 1386.9 1377.1 1390.15 11.97 324 Volumetric Specific Heat 3 (MJ/m K) 1.26 1.257 1.252 1.241 1.248 1.239 1.25 0.01 Points 160-200 160-200 160-200 170-200 160-200 160-200 EAP’s Table F.4: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Disks Specific Heat Used (J/kgK) Sample EA10P-1 25,22,28 1386 EA10P-2 25,22,28 1314 EA10P-3 25,22,28 1303 Average 1335 Stdev 45 325 Volumetric Specific Heat 3 (MJ/m K) 1.313 1.244 1.234 1.264 0.043 Points 80-200 100-200 120-200 EBP’s Table F.5: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample EB20P-1 EB20P-2 EB20P-3 Specific Disks Used Heat (J/kgK) 18,16,23 1257 18,16,23 1265 18,16,23 1265 Average 1262 Stdev 5 Volumetric Specific Heat 3 (MJ/m K) 1.131 1.293 1.293 1.239 0.094 Points 100-200 100-200 100-200 Table F.6: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample EB80P-1 EB80P-2 EB80P-3 Specific Disks Used Heat (J/kgK) 14,26,27 825 14,26,27 845 14,26,27 868 Average 846 Stdev 22 326 Volumetric Specific Heat 3 (MJ/m K) 1.424 1.458 1.498 1.460 0.037 Points 160-200 100-200 150-200 EQP’s Table F.7: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample Disks Used EQ7.5P-1 27,29,32 EQ7.5P-2 27,29,32 EQ7.5P-3 27,29,32 Average Stdev Specific Heat (J/kgK) 1320 1357 1294 1324 32 Volumetric Specific Heat 3 (MJ/m K) 1.239 1.274 1.215 1.243 0.030 Points 160-200 160-200 70-200 Table F.8: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample Disks Used EQ10P-1 21,10,14 EQ10P-2 21,10,14 EQ10P-3 21,10,14 Average Stdev Specific Heat (J/kgK) 1320 1297 1297 1304 13 Volumetric Specific Heat 3 (MJ/m K) 1.256 1.234 1.234 1.241 0.013 Points 150-200 160-200 160-200 Table F.9: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Sample Disks Used EQ15P-2 20,27,36 EQ15P-3 20,27,36 Average Stdev Specific Heat (J/kgK) 1250 1280 1265 21 327 Volumetric Specific Heat 3 (MJ/m K) 1.226 1.256 1.241 0.021 Points 150-200 140-200 Appendix F References: 1. J. Hone, M.C. Llaguno, M.J. Biercuk, A.T. Johnson, B. Batlogg, Z. Benes, J.E. Fischer, Applied Physics 74, 339-343, (2002). 328 Appendix G: Hot Disk Thermal Conductivity at 23°C EBP’s Table G.1: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 8/4/2008 Disks Used 26,28 22,31 27,29 32,21 18,23 16,12 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 0.4426 1.377 0.4458 1.430 0.4430 0.4371 0.4450 0.4421 0.4426 0.0031 6 1.375 1.320 1.432 1.388 1.387 0.041 6 Power (W) 0.08 0.08 Time (sec) 10 10 Points 17-200 12-200 0.08 0.08 0.08 0.08 10 10 10 10 12-200 5-175 5-140 10-200 Sensor C5465 r = 3.189 mm Table G.2: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Through Plane In Plane Thermal Thermal Disks Conductivity Conductivity (W/m•K) Test Date Used (W/m•K) 8/5/2008 21,19 0.5018 1.973 28,33 0.4947 1.993 23,18 0.4922 2.057 27,29 0.5040 1.931 24,30 0.5043 1.902 Average 0.4994 1.971 Standard Deviation 0.0056 0.060 Number of Samples 5 5 329 Power (W) 0.1 0.1 0.1 0.1 0.1 Time (sec) 5 5 5 5 5 Points 5-150 5-150 6-186 15-150 10-200 Sensor C5465 r = 3.189 mm Table G.3: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Through Plane In Plane Thermal Thermal Disks Conductivity Conductivity (W/m•K) Test Date Used (W/m•K) 8/5/2008 31,33 0.6271 2.566 22,25 0.6273 2.376 20,26 0.6220 2.576 17,21 0.6301 2.666 24,19 0.6249 2.583 27,29 0.6345 2.670 Average 0.6277 2.572 Standard Deviation 0.0043 0.107 Number of Samples 6 6 Power (W) 0.25 0.25 0.25 0.25 0.25 0.25 Time (sec) 5 5 5 5 5 5 Points 12-200 10-150 7-120 8-140 10-180 7-150 Sensor C5465 r = 3.189 mm Table G.4: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Through Plane In Plane Thermal Thermal Disks Conductivity Conductivity Test Date Used (W/m•K) (W/m•K) 8/6/2008 21,24 0.7265 3.491 29,27 0.7279 3.221 28,23 0.7276 3.419 16,19 0.7262 3.270 11,15 0.7231 3.548 Average 0.7263 3.390 Standard Deviation 0.0019 0.141 Number of Samples 5 5 330 Power (W) 0.25 0.25 0.25 0.25 0.25 Time (sec) 5 5 5 5 5 Points 5-175 8-115 6-165 6-150 6-175 Sensor C5465 r = 3.189 mm Table G.5: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN In Plane Through Plane Thermal Thermal Disks Conductivity Conductivity Test Date Used (W/m•K) (W/m•K) 8/6/2008 21,23 0.9020 4.371 16,14 0.8861 4.414 28,30 0.8959 4.383 17,20 0.8922 4.352 31,32 0.8953 4.344 Average 0.8943 4.373 Standard Deviation 0.0058 0.028 Number of Samples 5 5 Power (W) 0.25 0.25 0.25 0.25 0.25 Time (sec) 5 5 5 5 5 Points 9-120 9-111 9-120 12-115 9-135 Sensor C5465 r = 3.189 mm Table G.6: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Through Plane In Plane Thermal Thermal Disks Conductivity Conductivity Test Date Used (W/m•K) (W/m•K) 8/6/2008 21,20 1.168 5.132 23,19 1.105 5.478 8/7/2008 29,30 1.157 5.281 15,16 1.133 5.280 18,24 1.290 5.358 Average 1.171 5.306 Standard Deviation 0.071 0.126 Number of Samples 5 5 331 Power (W) 0.3 0.3 0.3 0.3 0.3 Time (sec) 5 5 5 5 5 Points 9-60 10-115 10-100 10-100 10-100 Sensor C5465 r = 3.189 mm Table G.7: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Disks Used 8/12/2008 28,30,19,15 8/13/2008 18,31,32,23 13,10,17,16 9,11,12,29 16,28,13,32 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 1.507 7.373 1.501 7.086 1.495 7.184 1.501 7.316 1.508 7.218 1.502 7.235 0.005 0.113 5 5 Power (W) 0.3 0.3 0.3 0.3 0.3 Time (sec) 5 5 5 5 5 Points 8-100 7-115 8-104 7-125 8-115 Sensor C5501 r=6.403 Table G.8: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN In Plane Through Plane Thermal Thermal Conductivity Conductivity Test Date Disks Used (W/m•K) (W/m•K) 8/13/2008 10,11,26,14 2.021 9.354 5,6,10,11 2.013 9.365 26,14,5,6 1.973 9.282 6,11,14,4 1.999 9.390 6,10,26,4 2.021 9.354 Average 2.005 9.349 Standard Deviation 0.020 0.040 Number of Samples 5 5 332 Power (W) 0.45 0.45 0.45 0.45 0.45 Time (sec) 5 5 5 5 5 Points 7-109 7-102 6-129 7-98 7-109 Sensor C5501 r=6.403 Table G.9: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Disks Used 8/13/2008 15,20,27,31 17,25,16,12 14,9,11,15 8/14/2008 16,12,8,20 9,14,11,10 Average Standard Deviation Number of Samples In Plane Through Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 1.977 9.090 1.987 9.285 2.022 9.370 2.102 9.466 2.030 9.417 2.024 9.326 0.049 0.148 5 5 Power (W) 0.45 0.45 0.45 0.45 0.45 Time (sec) 5 5 5 5 5 Points 5-138 6-129 6-115 7-90 6-129 Sensor C5501 r=6.403 Table G.10: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Disks Used 8/14/2008 17,29,28,24 12,13,14,16 19,20,10,11 14,16,24,28 12,20,13,29 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 2.739 12.450 2.737 12.200 2.733 12.000 2.725 12.470 2.736 12.460 2.734 12.316 0.005 0.210 5 5 333 Power (W) 0.45 0.45 0.45 0.45 0.45 Time (sec) 5 5 5 5 5 Points 7-88 7-93 7-87 7-96 7-85 Sensor C5501 r=6.403 Table G.11: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Disks Used 8/14/2008 6,26,16,22 10,22,26,12 16,6,11,9 8/15/2008 9,22,26,111 10,6,16,12 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 3.608 18.020 3.611 18.850 3.632 18.050 3.652 17.880 3.659 17.910 3.632 18.142 0.023 0.402 5 5 Power (W) 0.5 0.5 0.5 0.5 0.5 Time (sec) 5 5 5 5 5 Points 10-47 10-47 9-54 9-57 10-50 Sensor C5501 r=6.403 Table G.12: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Through Plane In Plane Thermal Thermal Conductivity Conductivity Test Date Disks Used (W/m•K) (W/m•K) 8/15/2008 8,9,18,6 6.021 30.680 9,18,8,16 6.056 27.620 8/18/2008 8,28,9,18 6.128 27.560 8,17,6,10 6.072 27.040 28,16,8,9 6.040 27.120 Average 6.063 28.004 Standard Deviation 0.041 1.518 Number of Samples 5 5 334 Power (W) 0.9 0.5 1 1 1 Time (sec) 1.5 2.5 2.5 2.5 2.5 Points 12-137 20-74 30-86 33-79 11-122 Sensor C5501 r=6.403 Combinations Table G.13: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Disks Used 8/25/2008 23,9,16,13 18,11,19,33 12,7,16,23 13,18,19,33 33,23,19,12 Average Standard Deviation Number of Samples In Plane Through Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 2.750 8.490 2.791 8.965 2.787 8.871 2.727 8.998 2.774 8.448 2.766 8.754 0.027 0.265 5 5 Power (W) 0.45 0.65 0.5 0.65 0.045 Time (sec) 5 5 4 5 5 Points 8-87 8-84 8-110 8-87 8-91 Sensor C5501 r=6.403 Table G.14: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Disks Used 8/26/2008 14,34,17,18 9,32,28,19 12,18,39,32 7,12,13,10 7,31,28,10 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 4.622 15.160 4.681 15.670 4.685 15.740 4.666 15.810 4.791 15.780 4.689 15.632 0.062 0.269 5 5 335 Power (W) 0.45 0.45 0.45 0.45 0.45 Time (sec) 5 5 5 5 5 Points 6-79 6-73 7-67 7-70 7-72 Sensor C5501 r=6.403 Table G.15: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Injection Molded Test Date Disks Used 8/28/2008 20,32,18,17 R 37,34,29,32 R 8/26/2008 21,41,47,32 8/27/2008 49,32,18,21 55,56,41,48 Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 5.757 16.910 5.832 17.560 5.810 17.680 5.790 17.940 5.822 17.760 5.802 17.570 0.030 0.394 5 5 Power (W) 1 1 1 1 1 Time (sec) 2.5 2.5 2.5 2.5 2.5 Points 11-49 10-88 24-79 18-91 17-71 Sensor C5501 r=6.403 Table G.16: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Compression Molded Test Date Disks Used 9/4/2008 10,11,12,13 C 9/5/2008 19,12,20,15 C 14,19,20,18 C 13,11,19,15 C 18,17,12,13 C Average Standard Deviation Number of Samples Through Plane In Plane Thermal Thermal Conductivity Conductivity (W/m•K) (W/m•K) 6.5930 23.910 6.5520 24.190 6.521 24.54 6.5360 24.060 6.5500 23.100 6.550 23.960 0.027 0.534 5 5 336 Power (W) 1 1 1 1 1 Time (sec) 2.5 2.5 2.5 2.5 2.5 Points 9-51 9-49 14-47 9-49 15-43 Sensor C5501 r=6.403 Appendix H: Density EP Table H.1: Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/2/2008 EP-TC-12 0.9000 0.9079 EP-TC-16 0.9000 0.9092 EP-TC-23 0.9000 0.9100 EP-TC-27 0.9000 0.9096 EP-TC-37 0.9000 0.9087 Average 0.9091 Standard Deviation 0.0008 Number of Samples 5 337 EAP’s Table H.2: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA2.5P-TC-9 0.9114 0.9208 EA2.5P-TC-15 0.9114 0.9211 EA2.5P-TC-21 0.9114 0.9218 EA2.5P-TC-26 0.9114 0.9216 EA2.5P-TC-30 0.9114 0.9215 Average 0.9214 Standard Deviation 0.0004 Number of Samples 5 Table H.3: 2.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA2.5PR-TC-10 0.9114 0.9218 EA2.5PR-TC-17 0.9114 0.9217 EA2.5PR-TC-20 0.9114 0.9221 EA2.5PR-TC-24 0.9114 0.9221 EA2.5PR-TC-30 0.9114 0.9221 Average 0.9220 Standard Deviation 0.0002 Number of Samples 338 5 Table H.4: 4 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA4P-TC-9 0.9184 0.9316 EA4P-TC-13 0.9184 0.9316 EA4P-TC-17 0.9184 0.9314 EA4P-TC-32 0.9184 0.9316 Average 0.9316 Standard Deviation 0.0001 Number of Samples 4 Table H.5: 5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA5P-TC-9 0.9231 0.9357 EA5P-TC-12 0.9231 0.9359 EA5P-TC-19 0.9231 0.9361 EA5P-TC-25 0.9231 0.9361 EA5P-TC-31 0.9231 0.9346 Average 0.9357 Standard Deviation 0.0006 Number of Samples 5 339 Table H.6: 6 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA6P-TC-7 0.9278 0.9387 EA6P-TC-11 0.9278 0.9388 EA6P-TC-16 0.9278 0.9386 EA6P-TC-20 0.9278 0.9391 EA6P-TC-31 0.9278 0.9388 Average 0.9388 Standard Deviation 0.0002 Number of Samples 5 Table H.7: 7.5 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA7.5P-TC-7 0.9351 0.9454 EA7.5P-TC-10 0.9351 0.9452 EA7.5P-TC-14 0.9351 0.9435 EA7.5P-TC-18 0.9351 0.9455 EA7.5P-TC-28 0.9351 0.9458 Average 0.9451 Standard Deviation 0.0009 Number of Samples 5 340 Table H.8: 10 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA10P-TC-6 0.9474 0.9600 EA10P-TC-10 0.9474 0.9603 EA10P-TC-16 0.9474 0.9595 EA10P-TC-19 0.9474 0.9601 EA10P-TC-33 0.9474 0.9602 Average 0.9600 Standard Deviation 0.0003 Number of Samples 5 Table H.9: 15 wt% Ketjenblack EC-600 JD in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/3/2008 EA15P-TC-9 0.9730 0.9833 EA15P-TC-12 0.9730 0.9836 EA15P-TC-18 0.9730 0.9833 EA15P-TC-20 0.9730 0.9840 EA15P-TC-32 0.9730 0.9834 Average 0.9835 Standard Deviation 0.0003 Number of Samples 5 341 EBP’s Table H.10: 10 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/2/2008 EB10P-TC-8 0.9573 0.9666 EB10P-TC-14 0.9573 0.9679 EB10P-TC-30 0.9573 0.9667 Average 0.9671 Standard Deviation 0.0007 Number of Samples 3 Table H.11: 15 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/2/2008 EB15P-TC-7 0.9887 0.9971 EB15P-TC-14 0.9887 0.9961 EB15P-TC-19 0.9887 0.9985 EB15P-TC-27 0.9887 0.9979 Average 0.9974 Standard Deviation 0.0010 Number of Samples 4 Table H.12: 20 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB20P-TC-19 1.0223 1.0268 EB20P-TC-30 1.0223 1.0252 EB20P-TC-25 1.0223 1.0257 EB20P-TC-32 1.0223 1.0240 EB20P-TC-17 1.0223 1.0246 Average 1.0252 Standard Deviation 0.0011 Number of Samples 5 342 Table H.13: 25 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date 5/30/2008 Sample Number Theoretical Density (g/ml) Actual Density (g/ml) EB25P-TC-7 1.0583 1.0597 EB25P-TC-23 1.0583 1.0593 EB25P-TC-28 1.0583 1.0620 Average 1.0603 Standard Deviation 0.0014 Number of Samples 3 Table H.14: 30 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB30P-TC-7 1.0968 1.0958 EB30P-TC-11 1.0968 1.0960 EB30P-TC-15 1.0968 1.0960 EB30P-TC-20 1.0968 1.0956 EB30P-TC-23 1.0968 1.0966 Average 1.0960 Standard Deviation 0.0004 Number of Samples 5 Table H.15: 35 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB35P-TC-8 1.1383 1.1375 EB35P-TC-22 1.1383 1.1377 EB35P-TC-25 1.1383 1.1389 EB35P-TC-34 1.1383 1.1367 Average 1.1377 Standard Deviation 0.0009 Number of Samples 4 343 Table H.16: 40 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB40P-TC-9 1.1831 1.1816 EB40P-TC-10 1.1831 1.1807 EB40P-TC-13 1.1831 1.1809 EB40P-TC-16 1.1831 1.1811 EB40P-TC-34 1.1831 1.1807 Average 1.1810 Standard Deviation 0.0004 Number of Samples 5 Table H.17: 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB45P-TC-11 1.2315 1.2279 EB45P-TC-18 1.2315 1.2282 EB45P-TC-19 1.2315 1.2296 EB45P-TC-21 1.2315 1.2288 EB45P-TC-32 1.2315 1.2283 Average 1.2286 Standard Deviation 0.0006 Number of Samples 5 344 Table H.18: 50 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB50P-TC-6 1.2841 1.2792 EB50P-TC-14 1.2841 1.2792 EB50P-TC-19 1.2841 1.2787 EB50P-TC-30 1.2841 1.2795 EB50P-TC-33 1.2841 1.2800 Average 1.2793 Standard Deviation 0.0005 Number of Samples 5 Table H.19: 55 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB55P-TC-12 1.3413 1.3336 EB55P-TC-13 1.3413 1.3342 EB55P-TC-22 1.3413 1.3335 EB55P-TC-32 1.3413 1.3354 Average 1.3342 Standard Deviation 0.0009 Number of Samples 4 Table H.20: 60 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB60P-TC-11 1.4039 1.3920 EB60P-TC-19 1.4039 1.3926 EB60P-TC-21 1.4039 1.3920 EB60P-TC-28 1.4039 1.3927 EB60P-TC-30 1.4039 1.3926 Average 1.3924 Standard Deviation 0.0003 Number of Samples 5 345 Table H.21: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB65P-TC-8 1.4726 1.4662 EB65P-TC-12 1.4726 1.4644 EB65P-TC-13 1.4726 1.4646 EB65P-TC-22 1.4726 1.4660 Average 1.4653 Standard Deviation 0.0009 Number of Samples 4 Table H.221: 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB65PR-TC-8 1.4726 1.4649 EB65PR-TC-12 1.4726 1.4649 EB65PR-TC-22 1.4726 1.4642 EB65PR-TC-25 1.4726 1.4651 EB65PR-TC-31 1.4726 1.4660 Average 1.4650 Standard Deviation 0.0006 Number of Samples 5 346 Table H.23: 70 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB70P-TC-6 1.5484 1.5430 EB70P-TC-13 1.5484 1.5428 EB70P-TC-14 1.5484 1.5438 EB70P-TC-16 1.5484 1.5432 EB70P-TC-26 1.5484 1.5440 Average 1.5433 Standard Deviation 0.0005 Number of Samples 5 Table H.24: 75 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB75P-TC-8 1.6324 1.6274 EB75P-TC-14 1.6324 1.6267 EB75P-TC-17 1.6324 1.6274 EB75P-TC-24 1.6324 1.6263 EB75P-TC-29 1.6324 1.6273 Average 1.6270 Standard Deviation 0.0005 Number of Samples 5 Table H.25: 80 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 5/30/2008 EB80P-TC-13 1.7260 1.7207 EB80P-TC-17 1.7260 1.7202 EB80P-TC-23 1.7260 1.7193 EB80P-TC-30 1.7260 1.7199 Average 1.7200 Standard Deviation 0.0006 Number of Samples 4 347 EQP’s Table H.26: 1.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ1.5P-TC-7 0.9075 0.9172 EQ1.5P-TC-11 0.9075 0.9170 EQ1.5P-TC-16 0.9075 0.9172 EQ1.5P-TC-19 0.9075 0.9169 EQ1.5P-TC-31 0.9075 0.9172 Average 0.9171 Standard Deviation 0.0001 Number of Samples 5 Table H.27: 2.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ2.5P-TC-8 0.9125 0.9212 EQ2.5P-TC-12 0.9125 0.9225 EQ2.5P-TC-18 0.9125 0.9213 EQ2.5P-TC-25 0.9125 0.9219 EQ2.5P-TC-31 0.9125 0.9221 Average 0.9218 Standard Deviation 0.0006 Number of Samples 5 348 Table H.28: 4 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ4P-TC-9 0.9202 0.9302 EQ4P-TC-16 0.9202 0.9295 EQ4P-TC-19 0.9202 0.9295 EQ4P-TC-28 0.9202 0.9298 EQ4P-TC-31 0.9202 0.9285 Average 0.9295 Standard Deviation 0.0006 Number of Samples 5 Table H.29: 5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ5P-TC-9 0.9254 0.9354 EQ5P-TC-19 0.9254 0.9352 EQ5P-TC-23 0.9254 0.9346 EQ5P-TC-33 0.9254 0.9345 Average 0.9349 Standard Deviation 0.0005 Number of Samples 4 Table H.30: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ6P-TC-6 0.9307 0.9387 EQ6P-TC-9 0.9307 0.9397 EQ6P-TC-14 0.9307 0.9400 EQ6P-TC-18 0.9307 0.9399 EQ6P-TC-23 0.9307 0.9401 Average 0.9397 Standard Deviation 0.0006 Number of Samples 5 349 Table H.31: 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ6PR-TC-8 0.9307 0.9400 EQ6PR-TC-11 0.9307 0.9402 EQ6PR-TC-13 0.9307 0.9404 EQ6PR-TC-18 0.9307 0.9402 EQ6PR-TC-29 0.9307 0.9398 Average 0.9401 Standard Deviation 0.0002 Number of Samples 5 Table H.32: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ7.5P-TC-9 0.9387 0.9475 EQ7.5P-TC-14 0.9387 0.9474 EQ7.5P-TC-18 0.9387 0.9475 EQ7.5P-TC-26 0.9387 0.9471 Average 0.9474 Standard Deviation 0.0002 Number of Samples 4 Table H.33: 7.5 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ7.5PR-TC-6 0.9387 0.9481 EQ7.5PR-TC-10 0.9387 0.9480 EQ7.5PR-TC-19 0.9387 0.9481 EQ7.5PR-TC-22 0.9387 0.9482 EQ7.5PR-TC-31 0.9387 0.9478 Average 0.9481 Standard Deviation 0.0002 Number of Samples 5 350 Table H.34: 10 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ10P-TC-9 0.9524 0.9607 EQ10P-TC-13 0.9524 0.9611 EQ10P-TC-19 0.9524 0.9606 EQ10P-TC-27 0.9524 0.9603 EQ10P-TC-30 0.9524 0.9608 Average 0.9607 Standard Deviation 0.0003 Number of Samples 5 Table H.35: 15 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EQ15P-TC-17 0.9809 0.9887 EQ15P-TC-21 0.9809 0.9908 EQ15P-TC-31 0.9809 0.9890 Average 0.9895 Standard Deviation 0.0011 Number of Samples 3 Table H.36: 20 wt% Hyperion FIBRILTM nanotubes in Polypropylene Masterbatch MB3020-01 Test Date 6/5/2008 Sample Number Theoretical Density (g/ml) Actual Density (g/ml) EQ20P-TC-6 ≈1.0112 1.0035 EQ20P-TC-19 1.0112 1.0064 EQ20P-TC-25 1.0112 1.0043 EQ20P-TC-30 1.0112 1.0030 Average 1.0043 Standard Deviation 0.0015 Number of Samples 4 351 Combinations Table H.37: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/8/2008 EA2.5B65P-7 1.5034 1.4822 EA2.5B65P-13 1.5034 1.4796 EA2.5B65P-33 1.5034 1.4809 Average 1.4809 Standard Deviation 0.0013 Number of Samples 3 Table H.38: 2.5 wt% Ketjenblack EC-600 JD and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/6/2008 EA2.5B65PR-7 1.5034 1.4780 EA2.5B65PR-15 1.5034 1.4799 EA2.5B65PR-16 1.5034 1.4805 Average 1.4795 Standard Deviation 0.0013 Number of Samples 3 Table H.39: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/5/2008 EA2.5Q6P-TC-16 0.9429 0.9541 EA2.5Q6P-TC-24 0.9429 0.9530 EA2.5Q6P-TC-28 0.9429 0.9527 EA2.5Q6P-TC-34 0.9429 0.9529 EA2.5Q6P-TC-39 0.9429 0.9537 Average 0.9533 Standard Deviation 0.0006 Number of Samples 5 352 Table H.40: 2.5 wt% Ketjenblack EC-600 JD and 6 wt% Hyperion FIBRILTM nanotubes in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Theoretical Density Actual Density (g/ml) (g/ml) Test Date Sample Number 6/5/2008 EA2.5Q6PR-TC-7 0.9429 0.9511 EA2.5Q6PR-TC-12 0.9429 0.9520 EA2.5Q6PR-TC-15 0.9429 0.9524 EA2.5Q6PR-TC-23 0.9429 0.9525 EA2.5Q6PR-TC-30 0.9429 0.9523 Average 0.9521 Standard Deviation 0.0006 Number of Samples 5 Table H.41: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/6/2008 EB65Q6P-TC-11 1.5567 1.5370 EB65Q6P-TC-14 1.5567 1.5385 EB65Q6P-TC-36 1.5567 1.5360 Average 1.5371 Standard Deviation 0.0012 Number of Samples 3 Table H.42: 6 wt% Hyperion FIBRILTM nanotubes and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/8/2008 EB65Q6PR-TC-18 1.5567 1.5396 EB65Q6PR-TC-31 1.5567 1.5383 EB65Q6PR-TC-39 1.5567 1.5410 Average 1.5397 Standard Deviation 0.0014 Number of Samples 3 353 Table H.43: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/8/2008 EA2.5B65Q6P-TC-14 1.5911 1.5750 EA2.5B65Q6P-TC-25 1.5911 1.5757 EA2.5B65Q6P-TC-36 1.5911 1.5768 EA2.5B65Q6P-TC-46 1.5911 1.5747 EA2.5B65Q6P-TC-52 1.5911 1.5744 Average 1.5753 Standard Deviation 0.0009 Number of Samples 5 Table H.44: 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN Replicate Test Date Sample Number Theoretical Density (g/ml) Actual Density (g/ml) 6/8/2008 EA2.5B65Q6PR-TC-11 1.5911 1.5750 EA2.5B65Q6PR-TC-28 1.5911 1.5780 EA2.5B65Q6PR-TC-39 1.5911 1.5784 EA2.5B65Q6PR-TC-45 1.5911 1.5775 EA2.5B65Q6PR-TC-50 1.5911 1.5766 Average 1.5771 Standard Deviation 0.0014 Number of Samples 5 354 Appendix I: Solvent Digestion Results Table I.1: Solvent Digestion Results for 25 wt% and 45 wt% Thermocarb TC-300 in Polypropylene Semi Crystalline Homopolymer Resin H7012-35RN DATE FORMULATION 6/3/2008 6/3/2008 6/3/2008 6/5/2008 6/3/2008 6/3/2008 6/3/2008 6/3/2008 6/3/2008 EP-1 EP-2 EP-3 EP-5 EB25P-1 EB25P-2 EB25P-3 EB45P-1 EB45P-3 FILTER + FILLER + FILTER + COMPOSITE PETRI DISH PETRI DISH WEIGHT (g) BOTTOM (g) BOTTOM (g) 0.1916 0.1744 0.1810 0.2058 0.1973 0.2350 0.1963 0.2094 0.1786 4.1320 4.1294 4.1958 4.1584 4.1942 4.1990 4.1570 4.1208 4.1112 4.2531 4.2659 4.2141 4.2185 4.1992 355 ACTUAL WEIGHT FRACTION TARGET WEIGHT FRACTION 0.30 0.28 0.29 0.47 0.49 0 0 0 0 0.25 0.25 0.25 0.45 0.45 Appendix J: Filler Length and Aspect Ratio Results Table J.1: Filler Length and Aspect Ratio Results for Single Filler Thermocarb TC-300 Formulations Fabrication Mean Length Standard Mean Aspect Formulation Filler Method (mm) Deviation (mm) Ratio As Received Thermocarb Injection Molded 0.0670 0.0590 1.757 EB25P Thermocarb Injection Molded 0.0411 0.0302 1.671 EB45P Thermocarb Injection Molded 0.0379 0.0520 1.660 EB65P Thermocarb Injection Molded 0.0379 0.0560 356 1.652 Standard Deviation 0.412 0.372 0.355 n 3533 855 412 0.037 830 Appendix K: Orientation Results and Photomicrographs Table K.1: Orientation Results – Single Filler Thermocarb TC-300 Formulations and Three Filler Formulation Formulation Fabrication Method Surface Studied EB30P Injection Molded In Plane EB20P Injection Molded Through Plane EB45P Injection Molded In Plane EB45P Injection Molded XY Plane EB45P Injection Molded Through Plane EB65P Injection Molded In Plane EB65P Injection Molded XY Plane EB65P Injection Molded Through Plane EA2.5B65Q6P Injection Molded In Plane EA2.5B65Q6P Injection Molded XY Plane EA2.5B65Q6P Injection Molded Through Plane EA2.5B65Q6P Compression Molded In Plane EA2.5B65Q6P Compression Molded XY Plane EA2.5B65Q6P Compression Molded Through Plane 357 Angle Mean ± Stdev (Degrees) 33.71± 25.4 58.35± 24.25 26.05± 22.58 30.82± 25.3 51.27± 27.59 27.49± 25.7 29.17± 23.36 60.70± 27.1 26.03± 23.87 26.3± 23.11 67.85± 21.45 23.92± 24.25 24.13± 23.63 65.3± 23.65 n 175 489 1249 1466 1608 609 1438 1438 841 362 805 331 808 789 Figure K.1: In-Plane Photomicrograph for Injection Molded 30 wt% Thermocarb TC300 in Polypropylene at 200X Magnification Figure K.2: Through-Plane Photomicrograph for Injection Molded 20 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 358 Figure K.3: In-Plane Photomicrograph for Injection Molded 45 wt% Thermocarb TC300 in Polypropylene at 200X Magnification Figure K.4: Through-Plane Photomicrograph for Injection Molded 45 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 359 Figure K.5: In-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC300 in Polypropylene at 200X Magnification Figure K.6: Through-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 360 Figure K.7: XY-Plane Photomicrograph for Injection Molded 65 wt% Thermocarb TC300 in Polypropylene at 200X Magnification 361 Figure K.8: In-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification Figure K.9: Through-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 362 Figure K.10: XY-Plane Photomicrograph for Injection Molded 2.5 wt% Ketjenblack EC600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 363 Figure K.11: In-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification Figure K.12: Through-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 364 Figure K.13: XY-Plane Photomicrograph for Compression Molded 2.5 wt% Ketjenblack EC-600 JD, 6 wt% Hyperion FIBRILTM nanotubes, and 65 wt% Thermocarb TC-300 in Polypropylene at 200X Magnification 365 Appendix L: Field Emission Scanning Electron Microscope Photomicrographs Carbon Black Figure L.1: Field Emission Scanning Electron Microscope Photomicrograph of 15% wt Carbon Black in Polypropylene Composite 366 Nanotube Figure L.2: Field Emission Scanning Electron Microscope Photomicrograph of 15% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite Figure L.3: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite 367 Thermocarb Figure L.4: Field Emission Scanning Electron Microscope Photomicrograph of 2.5% wt Carbon Black, 65% wt Synthetic Graphite, and 6% wt Hyperion Fibrils Carbon Nanotubes in Polypropylene Composite 368 Appendix M: Permission Letters Figure M.1: Email from Matt Clingerman for Figures 4.2-1 and 4.2-2 Figure M.2: Email from Rebecca Hauser for Figures 2.1-1 369 Figure M.3: Email from Rebecca Hauser for Figures 4.2-4 and 4.2-11 Figure M.4: Email from Asbury Carbon for Figures 3.3-2 370