Nanostructural Engineering of Vapor-Processed Organic Photovoltaics for Efficient Solar Energy Conversion trom Any Surface MASS CHTSIstIr MASSACHUSETT-S INSiUT OF TECHNOLOGY by Jill Annette (Rowehl) Macko JUN 10 2014 _______________ S.B., Massachusetts Institute of Technology (2008) Submitted to the Department of Materials Science and Engineering in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Materials Science and Engineering at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY June 2014 @ Massachusetts Institute of Technology 2014. All rights reserved. Author Signature redacted Department of Materials Science and Engineering April 16, 2014 Signature redacted Certified by... Vladimir Bulovic Associate Dean, Professor Thesis Supervisor A ccepted by ....................... Signature redacted Gerd Ceder Chair of the Graduate Committee 2 Nanostructural Engineering of Vapor-Processed Organic Photovoltaics for Efficient Solar Energy Conversion from Any Surface by Jill Annette (Rowehli) Macko Submitted to the Department of Materials Science and Engineering on April 16, 2014, in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Materials Science and Engineering Abstract More than two billion people in the world have little or no access to electricity. To be empowered they need robust and lightweightrenewable energy conversion technologies that can be easily transported with high yield from our manufacturing centers to their (often) rural homes. Few conventional photovoltaic technologies are robust enough to fill this need, however organic photovoltaics (OPVs) are ideal candidates due to their potential to be ultra-lightweight and flexible. However, this promising technology is currently limited by its relatively low power conversion efficiencies. This doctoral dissertation seeks to speed the eming of this promising technology. As a proof of concept for the accessibility and ultra-lightweight of OPVs, we integrate vapor-processed carbon-based electrodes and sub-30nm-thin encapsulations in organic photovoltaics, leading to the demonstration of monolithic, robust solar cell arrays as well as the first ever solar cells fabricated directly on paper. Furthermore, we have developed and advanced two unconventional approaches to enhancing power conversion efficiency via conventional methods: (1) optimization of multijunction efficiency via computational optical interference modeling and subcell photocurrent balance quantization and control, and (2) novel implementation of conventional vapor processing methods in the formation of molecular semiconductor crystals. This work has confirmed the potential of carbon-based materials to enable robust, ultra-lightweight, efficient solar arrays, thus advancing their capacity to empower our brothers and sisters even at the ends of the earth. Thesis Supervisor: Vladimir Bulovic Title: Associate Dean. Professor 3 4 Acknowledgments Anything that takes 10 years would surely result in significant indebtedness, as well as (hopefully) significant gratitude. After ten years at MIT, I would need hundreds (or thousands!) of pages to properly thank everyone whon I'n indebted too, but I will do my best to keep it a little shorter than that. First, of course, I thank Vladimir, who is technically my "research" advisor but his advice has expanded to far beyond that. I cannot thank God enough for the past 7.5 years that I have been granted to study and work under your supervision. I have acquired an incomprehensible amount of knowledge on research organic optoelectronics, but more than that. I've learned about communication, teaching, managing, interacting with others, etc. Thank you for your mentorship, and I look forward to seeing how God's plan for you continues to unfold. I believe you can tell a lot about a professor by looking at their group, and I have had the honor to work with excellent and unforgettable group members over the years. John and Alexi, thank you for your mentorship and incredible patience with me when I knew and understood nothing. It was a pleasure to be trained under you. PV sub-group (Johnny, Andrea, Patrick, Joel, Ko, Tim, Ni, Eletha, Melany, Mengfei, Anna): Thanks for enabling my work through our many fruitful discussions as well as commitment to up-keeping and trouble-shooting our lab. And the rest of LOOE/ONE Lab: I can't believe how much I've learned outside of vapor-processed organic photovoltaics. Thank you for expanding my knowledge, and thank you for making ONE Lab such an enjoyable place to work and study. I have also had the special privilege to work with a variety of amazing collaborators. Prof. Peko Hosoi and Tony; Prof. Karen Gleason and Miles, Dave, Rachel, Nan; Prof. Jing Kong and Hyesung; Drs. Andrea Bernardi, Riccardo Po, Petra Scudo. I thank you all, for our work and time together and for expanding imy viewpoints and experiences to other fields and in greater depth. Keep up the great work! Along that lines, I thank my many funding sources. Of course, this PhD wouldn't have been possible without someone else's wallet to pay for it. My first year was gen- erously supported by fellowships from Vasili and Danae Salapatas as well as Jerome and Dorothy Lemelson. The following three years were supported by a NSF Graduate Research Fellowship. And my final year was supported by an Energy Fellowship from the MIT Energy Initiative. Above and far beyond all that was financial support from eni, an energy-producing corporation based in Italy. I have never had to worry about using obsolete equipment or not being able to afford more materials for my experiments due to their unequivocal support of solar research at MIT. My PhD work is also indebted to them. My life at MIT has been more than just research, however. I'd like to thank also Prof. Rajeev Ram and Prof. Craig Carter for their mentorship in my teaching experiences. Thank you for your inspiration, your encouragement, your support, and the practical experience that I will build upon in my career to come. Thank you also to my coworkers in course 6.007: Prof. Marc Baldo and Bill, Lisa, David, Michael, Goran. To my family: thank you for your support and your training of me throughout my life. My grandfather showed me the meaning of hard work and perseverance. Even though he's no longer with us here to see the completion of my PhD, I am thinking of him at this time and spurred on by his memory. My grandmother knew that education would open doors to a better life, and when she pushed her children and even refused to speak her native language to them for the sake of their education in English, I know she was thinking of me, and I am indebted to her vision and passion. My mother and father have pushed me to be the best I can be, both as a student and as a person. They have loved me and sacrificed much for me, and I thank God for them. My sisters, my aunts and uncles, my cousins, and the rest of the family: thank you for your presence in my life. I couldn't be who I am and where I am without you. My husband: thank you for suffering through my PhD and my defense prep with me and for carrying me when I couldn't continue. I hope God-willing that we will continue to point each other (and others!) to Christ for many years to come. And finally I must turn to my spiritual family, at Antioch Baptist Church. My life is truly living because of the work of Jesus Christ in me through you all. P Paul 6 Kim and Becky JDSN, thank you for founding this church, and taking the time and heart to care for and train even me, a completely undeserving sinner who somehow wandered into your flock. P Dave and Angela SMN, my life is forever changed because of your true teaching of the beautiful, wonderful words of God. I can never repay my debt to you. P Thomas and Peggy SMN, words cannot express my gratitude. Who am I that you have invested so much in me and cared for me so much? Thank you for shepherding me in every aspect of life. And what more can I say? Time would fail me to tell of P Heechin and Jean SMN, P James and Donna SMN, P Donald and JY SMN, P Roy and Vania SMN, P Sang and Emily SMN, Amy unni, Tiff, Sue, all of YA, all of Antioch. I am not worthy of their presence in my life. Ultimately, I must thank my lord and savior, Jesus Christ, through whom I have true Life, which is far more important than the temporary things of this world. I confess that the completion of this thesis, of my PhD, and of 10 years at MIT, is only possible through his grace and power, which made me alive and carried me throughout the years. My life and my entirety is wholly devoted to Him and to His coming Kingdom. All that's left of my breath must praise the LORD God: Now to Him who is able to do far more abundantly than all that we ask or think, according to the power at work within us, to Him be glory in the church and in Christ Jesus throughout all generations, forever and ever. Amen. --Ephesians 3:20-21 7 8 Contents 1 Organic Photovoltaics: Motivations, Fundamentals and Objectives 23 The Needs at the Ends of the Earth . . . . . . . . . . . . . . . . . . . 24 The Potential of Organic Photovoltaics . . . . . . . . . . . . . 25 Fundam entals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 . . . . . . . . . . . . . . . . 28 . . . . . . . . . . . . . . . . . . 32 Objectives of this Thesis Work . . . . . . . . . . . . . . . . . . . . . . 38 1.3.1 Robust, Ultra-lightweight Solar Arrays . . . . . . . . . . . . . 38 1.3.2 Efficient Power Conversion . . . . . . . . . . . . . . . . . . . . 38 1.1 1.1.1 1.2 1.3 I 1.2.1 Physics of Organic Photovoltaics 1.2.2 Organic Photovoltaic Devices Electrodes and Encapsulations for Robust, Ultra-lightweight 40 Solar Arrays 2 Robust, Ultra-lightweight Solar Arrays Enabled by Vapor-Processed, 41 Carbon-Based Electrodes 2.1 2.2 Doped Graphene Electrodes for Organic Solar Cells on Glass . . . . . 42 2.1.1 Graphene Electrodes . . . . . . . . . . . . . . . . . . . . . . . 42 2.1.2 Graphene OPVs . . . . . . . . . . . . . . . . . . . . . . . . . . 43 oCVD-Printed Polymer Electrodes Enabling Direct Monolithic Integration of Organic Photovoltaic Circuits on Unmodified Paper . 44 2.2.1 oCVD-printed polymer electrodes . . . . . . . . . . . . . . . . 46 2.2.2 oCVD-printed PVs . . . . . . . . . . . . . . . . . . . . . . . . 48 9 2.3 3 49 2.2.4 Large-area monolithic photovoltaic arrays . . . . . . . . . . . 52 2.2.5 Integrated paper PV demonstrations . . . . . . . . . . . . . . 55 C onclusions 56 Sub-30nm Thin Encapsulation for Enhanced Device Lifetimes 57 3.1 . . . . . . . . . . . . 57 3.1.1 Degradation of OPVs . . . . . . . . . . . . . . . . . . . . . . . 58 3.1.2 Encapsulation . . . . . . . . . . . . . . . . . . . . . . . . . . . 58 Experimental Methods . . . . . . . . . . . . . . . . . . . . . . . . . . 59 3.2.1 Device Fabrication . . . . . . . . . . . . . . . . . . . . . . . . 59 3.2.2 ALD Process and Annealing . . . . . . . . . . . . . . . . . . . 59 3.2.3 Device Characterization . . . . . . . . . . . . . . . . . . . . . 60 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . 60 3.3.1 Initial Performance . . . . . . . . . . . . . . . . . . . . . . . . 60 3.3.2 Degradation and Failure Behavior . . . . . . . . . . . . . . . . 61 3.3.3 Encapsulation with ALD Nanothin Film . . . . . . . . . . . . 63 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65 3.3 3.4 4 oCVD-printed PVs on flexible plastic and paper substrates . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 3.2 II 2.2.3 Introduction........................ Engineering Higher Efficiency Organic Photovoltaics 66 Introduction to Nanostructures and Architectures 67 4.1 Subcell Nanostructures . . . . . . . . . . . . . . . . . . . . . . . . . . 67 4.1.1 Bilayer/Planar (Tang) Cell . . . . . . . . . . . . . . . . . . . . 67 4.1.2 Bulk Heterojunction and Planar-Mixed Heterojunction . . . . 70 4.1.3 Novel Nanostructures . . . . . . . . . . . . . . . . . . . . . . . 70 4.2 M ultijunction Architecture . . . . . . . . . . . . . . . . . . . . . . . . 71 4.3 Nanostructural Engineering via Processing . . . . . . . . . . . . . . . 72 5 Practical Efficiency Limits of Organic Photovoltaics 5.1 Practical Limits Derived from Literature . . . . . . . . . . . . . . . . 10 75 76 5.2 5.3 5.4 6 Computational Methods . . . . . . . . . . . . . . . . . . . . . . . . . 77 5.2.1 M aterials Choice . . . . . . . . . . . . . . . . . . . . . . . . . 77 5.2.2 Planar Architecture . . . . . . . . . . . . . . . . . . . . . . . . 78 5.2.3 Ideal Nanostructured Architecture . . . . . . . . . . . . . . . . 78 5.2.4 Multijunction Architecture . . . . . . . . . . . . . . . . . . . . 78 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . 79 5.3.1 Single Junction: Planar Architecture 79 5.3.2 Single Junction: Ideal Nanostructured Architecture . . . . . . 80 5.3.3 Tandem Cells (with the Same Subcells) . . . . . . . . . . . . . 81 5.3.4 Multijunction Cells (with Different Subcells) . . . . . . . . . . 82 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82 C onclusions . . . . . . . . . . . . . . Materials and Architecture Design in Sub-100nm Multijunction Pho- 83 tovoltaics 7 6.1 Experimental Methods . . . . . . . . . . . . 84 6.2 Characteristics of Optimized Device . . . . . 89 6.3 Recombination Zone Development . . . . . . 91 6.4 Optical Optimization of Sub-100nin Subcells 93 6.5 Conclusions . . . . . . . . . . . . . . . . . . 96 Subcell Photocurrent Balance in Multijunction Photovoltaics 97 7.1 Introduction . . . . . . . . . . . . . . . . . . . . 97 7.2 Experimental Methods . . . . . . . . . . . . . . 98 7.3 Calculation and Simulation . . . . . . . . . . . 99 7.3.1 Subcell Photocurrent Fitting . . . . . . . 99 7.3.2 Subcell Photocurrent Balance . . . . . . 99 7.3.3 Circuit Simulations . . . . . . . . . . . . 100 R esults . . . . . . . . . . . . . . . . . . . . . . . 101 . . 101 . . . . . . . . . . 103 7.4 7.4.1 Subcells with Dissimilar Fill Factors 7.4.2 Subcell Photocurrents 11 7.4.3 7.5 Dependence of Multijunction Performance on Subcell Photocurrent B alance . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104 D iscussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106 7.5.1 PCE Optimization in Multijunctions 106 7.5.2 Dependence of Subcell Photocurrent Balance on Non-Standard . . . . . . . . . . . . . . C onditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107 7.6 8 C onclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108 Vapor-Processed Crystals and Aggregates of Organic Semiconductors 8.1 8.2 8.3 9 112 Organic Semiconductor Needles Formed via Solvent Annealing' - 111 8.1.1 Experimental Results . . . . . . . . . . . . . . . . . . . . . . 112 8.1.2 Physical Picture . . . . . . . . . . . . . . . . . . . . . . . . . 114 8.1.3 Mathematical Model and Numerical Results . . . . . . . . . 116 8.1.4 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 Low Vacuum Thermal Evaporation of Organic Semiconductors . . . 117 8.2.1 T heory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 8.2.2 Results and Discussion . . . . . . . . . . . . . . . . . . . . . 119 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120 Conclusions ii [21 9.1 Sum m ary 9.2 Looking to the Future . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121 123 A Photovoltaic Primer for U.S. Policy Makers 11 [27 B Fabrication of Vapor-Processed Organic Photovoltaics 133 B.1 Introduction . . . . . . . . . . 133 B.2 Dominance of DBP . . . . . . 133 B.3 Donor Layer . . . . . . . . . . 134 B.3.1 Manufacturer . . . . . 134 B.3.2 Purity . . . . . . . . . 137 12 B.3.3 B.4 . . . . . . . . . . . . . . . . . . . . . . . . . . . 137 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138 Growth Rate Acceptor Layer B.4.1 M aterials Choice . . . . . . . . . . . . . . . . . . . . . . . . . 138 B.4.2 Purity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139 B.5 Anode Interlayer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B.5.1 M aterials Choice B.5.2 Thickness . . . . . . . . . . . . . . . . . . . . . . . . . 139 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139 B.6 Cathode Interlayer . . . . . . . . . . . . . . . . . . . . . . . . . . . . B.7 B.8 139 140 . . . . . . . . . . . . . . . . . . . . . . . . . 140 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141 Substrates and Substrate Treatments . . . . . . . . . . . . . . . . . . 141 B.7.1 Substrate Choice . . . . . . . . . . . . . . . . . . . . . . . . . 141 B.7.2 Substrate Treatments . . . . . . . . . . . . . . . . . . . . . . . 142 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143 B.6.1 M aterials Choice B.6.2 Thickness C Contributions Associated with This Thesis 13 145 14 List of Figures 1-1 Global distribution of population without access to electricity. .... 1-2 Photos comparing use of kerosene-fueled lamp and LED lamp (powered 24 by renewable energy). . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3 Graph chartering the history of record efficiency cells, classified by technology type. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4 25 26 (Top) Cartoon of a pentacene molecule and (Bottom) spatially-resolved measurement of its electronic cloud. . . . . . . . . . . . . . . . . . . . 27 . . . . . . . . . . 28 1-5 Schematic of three steps in photovoltaic operation. 1-6 Absorption spectra of thin filns of the molecules C60, DBP and ClAlPc, each showing multiple peaks of absorption at resonant frequencies. Inset: cartoons of molecular structures. . . . . . . . . . . . . . . . . . . 29 1-7 Schematic of energy states pertinent to organic photovoltaic operation. 30 1-8 Schematic of energy levels at an organic heterojunction. . . . . . . . . 31 1-9 Schematics of vertical and lateral device architectures. . . . . . . . . 32 1-10 Schematic of the interior structure of a vacuum thermal evaporator. . 34 1-11 Cartoon of a current density-voltage characteristic, identifying the Voc, Jsc, and M PP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35 1-12 Cartoons illustrating the Voc, Jsc, and FF and their effects on the maximum power point (and thus PCE) . . . . . . . . . . . . . . . . . 37 2-1 Transmittance of graphene sheets of one to three layers. . . . . . . . . 43 2-2 Current-Voltage characteristics of organic solar cells with different almodes under dark and simulated AM1.5G illumination at 100mW-cn15 2 44 2-3 Relationship between percent transmittance (550 nm) and sheet resistance in ohms per square ( Q/D) for the vapor-printed oCVD PEDOT used in the work. Upper inset: 200-nm thick PEDOT film vapor printed on tissue paper in 15 pt. bold Verdana font. . . . . . . . . . . 2-4 45 Top: Deposition of oCVD PEDOT and solution-processed PEDOT on a variety of surfaces (a-c). Multimeters demonstrate conductivity. Bottom: Patterned, large-area deposition of PEDOT on a variety of surfaces. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5 47 Current density- voltage characteristics under illumination (AM1.5, 100 mW-cm 2 ) for oCVD PEDOT PVs on glass differing only in anode structure (the yellow and red curves are for reference and do not include oCVD PEDOT). . . . . . . . . . . . . . . . . . . . . . . . 2-6 48 (a) Device characteristics and electrode conductivity for oCVD-printed PVs on PET (5-mil thick) after repeated flexes to 5-mm radius. (b) Current density-voltage characteristics for oCVD PVs vapor-printed on as-purchased tracing paper, copy paper, and tissue paper. . . . . . 2-7 Internal and external quantum efficiency comparison for devices on glass/ITO/PEDOT:PSS (black) and tracing paper/oCVD PEDOT. . 2-8 50 51 (a) Printing schematic for 250-cell, series-integrated monolithic arrays. (b) Current-voltage performance curves for series-integrated photovoltaic arrays with vapor-patterned oCVD electrodes. (c) Spatial map of individual cell open-circuit voltages across the arrays. 2-9 . . . . . . . 53 (a) Normalized efficiency of thin-film-packaged and unpackaged arrays as a function of time. The right photograph shows the laminated paper circuit powering an LCD display in air with ambient sunlight. (b) A paper array is progressively folded in air while being tested. (c) The iCVD-coated array (28 series-integrated cells) is submerged in water during operation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 54 3-1 Schematics of the device architectures studied in this work. nesses are listed on right, however the image is not to scale. 3-2 Thick. . . . . Comparison of representative current-voltage characteristics of solar cells of varying architectures, as deposited. . . . . . . . . . . . . . . . 3-3 62 Representative current-voltage characteristics of devices initially and after failure or after 2 weeks (whichever came first). 3-5 61 Comparison of device shelf lives without encapsulation in inert atno- sphere or ambient atmosphere. . . . . . . . . . . . . . . . . . . . . . . 3-4 59 . . . . . . . . . . 63 Impact of ALD encapsulation process on device performance of polymer cells with Al electrode and molecular cells with Ag electrode. Shown are representative current-voltage characteristics of: initial device, after 10 hour annealing, and after ALD process (includes 10 hour annealing) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6 64 Effect of ALD encapsulation on lifetime of polymer cells and molecular cells, both with Al electrodes, stored in ambient environment or in inert environ nent. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1 Historic Advances in Nanlostructural Engineering of OPVs. 4-2 Calculation of the external quantum efficiency (EQE) for donor-acceptor . . . . . 64 68 heterojunction as a function of CiLc (change in line style) and aLJ) (change in color), where LD is exciton diffusion length, a is absorption coefficient, and LC is carrier diffusion length, highlighting the exciton diffusion bottleneck. 4-3 . . . . . . . . . . . . . . . . . . . . . . . . . . . 69 Left: Device structure of a planar heterojunction OPV. Right: Schematic showing the cross-section of the rrP3HT:PCBM BIIJ device. Focused (c) and defocused (e) cross-sectional TEM images; inset: the imagnified image of the rrP3HT:PCBM BHJ layer . 17 . . . . . . . . . . . . . . . . 70 4-4 Effect of annealing on planar-mixed heterojunctions of CuPc-PTCBI. Top (a-d) shows SEM images and bottom (e-h) shows simulations of the morphology. Leftmost images are as deposited, images to right show increased aggregation due to increasing annealing temperatures. 4-5 73 Effect of annealing on bulk heterojunction polymer solar cells. Performance increases with annealing. SEM shows that this is due to increased phase separation of the polymers and fullerene materials. . 73 4-6 Effect of solvent annealing with different solvents on a polymer blend. 73 5-1 Practical Limit PCE for a range of optical bandgaps. Black is for single junction architecture and purple is for multijunction architecture (plotted versus the top subcell bandgap). The bandgaps of DBP and ClAlPc are indicated. . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2 Modeled Jsc for DBP-C60 and ClAlPc-C60 cells with either planar and ideal nanostructure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3 77 79 Calculated PCE of planar and ideal nanostructure single junctions (lines) and planar and ideal nanostructure tandems (squares) for DBPC60 with current demonstrations of FF and Voc. 6-1 . . . . . . . . . . . 80 Absorption spectra of C60 (green), DBP (blue) and ClAlPc (red) thin films, showing broad spectral response. Molecular structures are inset. 84 6-2 Energy levels of each component layer of the multijunction cells. . . . 85 6-3 Device cross-section of the multijunction cells. Thicknesses not to scale. 85 6-4 Schematic of the set up for external quantum efficiency measurement. 6-5 Representative current density-voltage characteristics of MJ (green), SJ1 (red) and SJ2 (blue). 6-6 . . . . . . . . . . . . . . . . . . . . . . . . 88 89 Wavelength-resolved external quantum efficiency of SCI (red) and SC2 (blue) selected via optical bias (A=532nm laser, 50mW; and AM 1.5G simulation, 100 mW/cm 2; respectively). . . . . . . . . . . . . . . . . . 6-7 90 Device Characteristics of MJ cels with recombination sonzes of various architectures and thicknesses. . . . . . . . . . . . . . . . . . . . . . . 18 92 6-8 Optical fields for wavelengths absorbed by SCI (A=785nm) and SC2 (A=530in) within the M\J cell modeled via T-matrix formalism. 6-9 93 Architectures of conventional and inverted subeell order. Thicknesses not to scale. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94 6-10 (Left) Modeled external quantum efficiency and (right) experimental current density-voltage characteristics of conventional and inverted sub cell order.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95 6-11 Simulated short-circuit currents for an array of thicknesses of subcell 1 and 2 with fixed donor-acceptor ratios. 7-1 . . . . . . . . . . . . . . . . 95 Theoretical dependence of PCE loss on subeell balance for MJs with similar FF subcells and dissimilar FF subcells. . . . . . . . . . . . . . 7-2 Circuit diagram for the MJ-OPV model. . . . . . . . . . . . . . . . . 7-3 Experimental (solid lines) and simulated (dashed) current density- 98 100 voltage characteristics of single junction devices comprising SCI (red) and SC 2 (blue). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4 Current Density-Voltage Characteristics of single junction cells with the SC I and SC 2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5 101 101 Representative reconstructed current density-voltage characteristics of multijunction devices either balanced (left) or unbalanced (right). The device on right is the maximal-PCE cell. 7-6 . . . . . . . . . . . . . . . . 103 Fitted photocurrent for an array of fabricated cells with the same SCI thickness and varying SC2 thickness. Black lines are fits to the data. Red and Blue lines are modeled subcell photocurrents. 7-7 . . . . . . . . 104 Dependence of FF, Jsc and PCE on SPB for an array of simulated MJ-OPVs. Left and Right show different ranges of SPB. Lines are simulated values and points are experimental values. 19 . . . . . . . . . 105 7-8 (Left) Experimental Current Density-Voltage Characteristics of multijunction devices with increasing SC2 thickness and constant SCI thickness. (Right) Simulated Current Density-Voltage Characteristics of multijunction devices with balanced subeell photocurrents, large negative imbalance, or positive (optimal) imbalance . . . . . . . . . . . . 7-9 107 (Left) Experimental responsivities of max-PCE MJ and corresponding SJ cells versus illumination intensity. (Right) Calculated subcell photocurrent balance and experimental power conversion efficiency for the max-PCE MJ cell versus illumination intensity. . . . . . . . . . . . . 108 7-10 Simulated MJ cell power output versus load resistance. . . . . . . . . 109 8-1 Process flow for growth of Alq3 needles. 112 8-2 (a) Optical micrographs of needles for different thicknesses of Alq3 . . . . . . . . . . . . . . . . films after annealing for 1-5 hours. (b) SEM micrograph of rectangular needles going from a common nucleation site after solvent annealing a film with HAlq3=15nm. . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3 113 (a) Successive snapshots of a cluster of needles growing during solvent annealing. The top-left needle from the cluster is tracked over time in (b). (b) Slice of micrograph pixels along the axis of a needle as a function of tim e. 8-4 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114 (a) Schematic of a needle growing into a fluid film. (b) Optical micrograph of the area surrounding an Alq3 needle after solvent annealing for 3 hours. 8-5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115 (a) Schematic of a needle growing into a fluid film. (b) Optical micrograph of the area surrounding an Alq3 needle after solvent annealing for 3 hours. 8-6 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116 Relation of "air" molecule's monolayer formation time and chamber pressure. The typical length of an active layer deposition is identified w ith the red line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20 118 8-7 Relation of evaporate molecule's mean free path and chamber pressure. . . 119 8-8 SEM image of CuPc "snow" formed by LVTE. . . . . . . . . . . . . . 120 A-1 Solar power per area separated by photon energy . . . . . . . . . . . . 128 A-2 Energy levels of photons and electrons in semiconductors. . . . . . . . 128 A-3 Excitement of electrons by photons in semiconductors . . . . . . . . . 129 B-1 Current Density-Voltage Characteristics of a variety of devices with The throw distance of our chamber is identified with the red line. nominally the same architecture and materials . B-2 . . . . . . . . . . . . 135 Left: Schematic of device architecture highlighting the various layers . . . . . . . . . . . . . 135 . . . . . . . . . . . . . . . . 136 . . . . . 136 . . . . . . . . . . . . . . . . 136 . . . . 137 . . . . . . . . . . . . . . . . 138 for optimization. Right: Device circuit model. B-4 134 Current Density-Voltage Characteristics of a thickness optimization run for two different batches of donor material. B-3 . . . . . . . . . . . . Thickness optimization of various layers. B-5 Thickness optimization of DBP showing various parameters. B-6 JVs with DBP from two manufacturers. B-7 JVs with DBP as purchased or purified once or purified twice. B-8 JVs with DBP grown at variety of rates. B-9 JVs comparing C60 and C70 as acceptor, with the donor material ClAlPc. 138 B-10 JV and EQE for various C60 purities. . . . . . . . . . . . . . . . . . . 139 B-11 JV for various anode interlayers: MoOx and PEDOT. . . . . . . . . . 140 . . . . . . . . . . . . . . . . . . . . 140 B-12 JV for various MoOx thicknesses. B-13 Left: JV comparing various cathode interlayers: BCP and Alq3. Right: JVs of various thicknesses of BCP. . . . . . . . . . . . . . . . . . . . 141 B-14 JVs of various substrates with either purified DBP or as-purchased DBP. 142 B-15 JVs of various substrates with various substrate treatments. 21 . . . . . 143 22 Chapter 1 Organic Photovoltaics: Motivations, Fundamentals and Objectives The International Energy Agency estimates that one billion people worldwide have zero access to electricity, and another one billion people have undependable access to electricity. [1] However, the majority of these 2 billion people are at the ends of the earth, far from the ends of the electric grid, thus filling their need is not as simple as donating money to pay to flip a switch. Micro-generation of electricity is a promising technology for these areas and is already demonstrating progress, however gains are slow. We can speed the coming of omnipresent electricity by developing photovoltaics that are robust and lightweight, thus easing utilization in areas of weak to non-existent infrastructure. Organic semiconductors have generated much interest due to their potential of enabling mechanically-robust, nano-thin photovoltaics, however their implementation is still limited by their utilization of conventional substrate, electrode and encapsulation layers as well as their relatively low power conversion efficiencies. In this thesis, we demonstrate application of nanomaterial-based electrodes and encapsulants fabricated via a variety of novel vapor-deposition processes for robust, lightweight photovoltaics on any surface/substrate. Furthermore, we present guidelines for fabrication 23 BANGLADESH 60 NEPAL $$ AFGHANISTAN N F- 4AITI 2 KE4YA II I WANDA 6 CAMBODIA 71 SOUTH AFRICA 26 Porcentagp of populaion without access to electricity Source Uieid Nations No date 0 25 50 75 .u LI Ouvelopmnenr Prograrn a1 :. IIUS Figure 1-1: Global distribution of population without access to electricity. [2] and optimization of nano-thin multijunction photovoltaics, an architecture with large potential for efficiency enhancement. Finally, we explore two novel approaches to enhance subcell efficiency via enhancement of molecular order via vapor-processes. 1.1 The Needs at the Ends of the Earth The two billion people in need of electricity are at the end of the earth, far from the world's research institutions and industrial centers (Figure 1-1). [2] They are past the end of the electric grid. They are past the end of the paved roads. They are reached by camel and mule and foot. Mostly these people depend on burning carbon for their basic energy needs: heat, light, cooking. However the burning of biofuels leads to health and fire hazards, as well as consumes >30% of household incomes in some areas. Furthermore, as these individuals seek to connect to the rest of the world via radio and cell phones, they must seek out stores that sell electricity by the minute, which are sometimes in neighboring villages tens of miles away. One alternative is clean energy: electricity powered by natural sources. However, 24 Figure 1-2: Photos comparing use of kerosene-fueled lamp and LED lamp (powered by solar energy). [3] the availability of hydroenergy- the most prevalent form of clean energy today- is highly localized and thus not capable of omnipresent micro-generation. The same is true for wind and geothermal energy. The sun, however, is available all over the earth. Indeed. God "makes His sun rise on the evil and on the good." [Matthew 5:45] Everyone has access to it. Therefore, if you want omnipresent clean energy: hydro, wind and geothermal are good, but solar is a must. 1.1.1 The Potential of Organic Photovoltaics Arguably, the best example of omnipresent clean energy today is plants. The LORD God was the first engineer, and when He created the heavens arid the earth[Genesis 1:1] He designed arid implemented in plants a technology for converting solar energy into chenmical energy (i.e. sugar) at efficiencies on the order of 3-6%. [4] This sounds like aii unacceptably low efficiency to those of us in the solar research field, yet it is evidently sufficient to power the earth due to the vastness of its implementation. (Note also that plants are at the bottom of our food chain, so most of our bodily energy is derived from them.) Humankind has also invented and developed a variety of solar technologies. These might be broadly classified under three types: (1) wafer-based technologies, (2) thin-filn technologies, (3) nanomnaterials-based technologies. Wafer-based arid thin filnm solar technologies are already common-place in the developed world, however 25 50 Best Research-Cell Efficiencies MuTijuncftoinCob (ntraiiTTo 4 in.is~~d is~~H 44 4 40 ~0 V T I - w or +now (n-csrah m0r (nsrncntalr -3V ThG" A Twiic-ase A TwoOna ter eoor M Faw-frctnd or mom f a0 Gatraitefnb Sd A~~~ 38 - i MNREL ThinFIlm TochnOagyslo 0 C Cdli -GS 0 Anotmi i i Hi er ) O0 PM" NM icentaw g the *hatiN tecihnoogie) iak hngIrsa Eb Py00(oicehiiaii) pass pFs.iT pamf rgce * Orgaii I" adnM icoosi r et r ra th ie ftioenhn iisesNg r r have ar t us e (CZTS ....... mx)t Sem nt hela arraciHIT) cn28 a gng md C iyitm rni 32 - onistofm 8ti c 4) d s fe, rgr s and (4) an-b-td V T kn-- t-y-h -- -- -- -- -- wt p a re < C --7M r 20 12 4 0r I 1975 1980 1985 1990 1995 2000 2005 2010 I 2015 Aow-ostig-throughuaft acatoroess Figure 1-3: Graph chartering the history of record efficiency cells, classified by tech- nology type. [6,71 porate naoetriae ()hv xioi AAolcrncmtrasta rqatm nanomaterials-lases technologies are "emerging" from research laboratories to industry. Wafer-based technologies are characterized by their high efficiency and energyintensive fabrication processes. Thin film technologies have moderate efficiency and moderate fabrication processes. Nanomaterials-based technologies are still in development but are currently characterized by low efficiency and potential for facile, low-cost, high-throughput fabrication processes. Nanomnaterial-based photovoltaics often possess the following characteristics: (1) they consist of thin films (approx. 2 microns) of semiconductor material, (2) incorporate nanometer-scale optoelectronic materials that (3) have excitonic or quantumconfinement character and (4) can be fabricated entirely with low-temperature (<300C) processing steps. [5] We limit the scope of this thesis to vapor-processed molecules. This is not to suggest that other nanomaterials are not worth investigating, but rather it indicates the expertise of this researcher as well as her limited time and cap~acities. Note a fourth type labeled in Figure 1-3: "MJ-PV". This type has the highest 26 Figure 1-4: (Top) Cartoon of a pentacene molecule and (Bottom) spatially-resolved measurement of its electronic cloud. [8] efficiencies yet reported, up to 44.4%. [7] However the "MJ-PV" category is not a specific materials set but rather a very special device architecture. The majority of the MJ-PVs shown on this graph are comprised of wafer-based technologies aid are thus difficult to process and commonly cost-prohibitive. In Part II of this thesis we discuss the implementation of this architecture with nanoriaterials. Conventional photovoltaics are already being significantly utilized in developing nations (see figure 1-2). But due to their weight and fragility, they are limited to small units with careful packaging. Can we instead fabricate a solar cell as lightweight arid robust as a leaf, creation's original solar cell?' In this thesis we demonstrate a robust and ultra-lightweight organic solar array as well as propose and explore multiple approaches to enhancing its power conversion efficiency. But first, we describe the fundamentals of organic photovoltaics: the physics and the device. 1.2 Fundamentals Here we describe the key physical processes occurring within and the materials arid device architectures of organic photovoltaics (OPVs). Note that Appendix A is a primer that introduces physics anid devices of photovoltaics in elementary terms, arid a newcomer to the field may find it beneficial to start there. 'Leaves may not seem very robust, but neither does glass and yet glass is used to stabilize and protect conventional photovoltaics. It just goes to show that robustness is relative. 27 13 3 Figure 1-5: Schematic of three steps in photovoltaic operation. 1.2.1 Physics of Organic Photovoltaics Fundamentally, the conversion of optical energy to electrical energy via a photovoltaic device requires 3 steps: 1. Interaction of photon and electron to form an exciton 2. Dissociation of exciton into charge carriers 3. Collection of charge carriers by an electrical circuit Exciton Formation Electrons on molecules 2 are like balls on springs, with an equilibrium position but with some freedom to wiggle back and forth over the length of the molecule. The spring constant of that wiggling (i.e. the attraction between positive nuclei and electronic cloud) determines its resonant frequency. If you hit the electron with an electric field wiggling at that resonant frequency (or close to it), the electron itself will begin to wiggle back and forth at the same frequency and thence absorb the energy of that electric field. [9] We know that the energy of a photon, EoPT, is proportional to the frequency of its oscillating electro-magnetic field, v. Thus the electronic cloud's 2 Note that on the molecular scale (length scale of 1 nm=10- 9 m) electrons should not be considered to exist at a single point, but rather to have a certain probability distribution, which looks like a cloud such as that shown in figure 1-4. However on the device scale (length scale of 1 micron=10- 6 m) they are effectively point charges. 28 2.0 d . 0 DBP 1.5 CIAIPc a2) 0 o 1.0 C 0 0.5 0.0 C60 400 500 600 700 800 Wavelength ( nm ) 900 Figure 1-6: Absorption spectra of thin films of the molecules C60, DBP and CIAlPc, each showing multiple peaks of absorption at resonant frequencies. Inset: cartoons of molecular structures. resonant frequency will determine which Eop 0 it will absorb. The minimum value of this is EGOPT, the molecule's optical bandgap energy. If a ground-state electron absorbs a photon with an energy equal to the molecule's optical bandgap, then it will be excited and form an exciton. An exciton is the 3 bound pair of a positive polaron and negative polaron. The exciton diffuses freely from molecule to molecule. However, note that it is neutrally-charged so it is neither attracted nor repelled by electric fields. Molecules have distributions of ground and/or excited state energy levels, and so they will not have a sharp peak at resonance but rather a distribution. Furthermore, molecules may have multiple resonant frequencies and therefore have multiple absorption peaks. An representative absorption spectrum is shown in figure 1-6. The convolution of a device's absorption spectrum with the spectrum of the incident light gives the number of excitons formed within a device. This is often identified as the absorption efficiency, 'rA. [10] 3 Polarons are the charge carriers in organics. They are simply slightly positive or slightly negative electrical dipoles in the electrical cloud on each molecule. Positive polarons occupy the HOMO energy band and negative polarons occupy the LUMO energy band. They move through an organic film by hopping from one molecule to the next. They behave similarly to free electrons and holes, and thus you will find many places in this thesis (as well as many, many publications elsewhere) where polarons are mis-identified as electrons and holes. I apologize in advance but will continue to do so for the sake of convenience and consistency. 29 EnergBd EG,OPT HOMO-LUMC Photons Ground Exciton Free Carriers AEDA Free at HJ Figure 1-7: Schematic of energy states pertinent to organic photovoltaic operation. Exciton Dissociation Excitons are all well and good, but they do not give us electricity. We must also convert the excitons into free charge carriers (which are typically polarons in organics, as noted above), the flow of which is identified as current. The energy needed to dissociate an exciton into a polaron pair is called the exciton binding energy, EBinding. In conventional semiconductors, EBinding is significantly lower than kT at room temperature (=0.026 eV). [11] Such excitons can dissociate into free charge carriers simply due to thermal variation. But in organic semiconductors, EBinding is >0-3eV. [12-14] An energy step of this scale sometimes occurs at crystal defects but such a low percentage of excitons were generated within a diffusion length of these defects that the earliest organic photovoltaic efficiencies were unacceptably low. [15,16] In 1985 Tang introduced a radical new approach to exciton dissociation: the heterojunction. [17] By combining two organic semiconductors with different energy levels, Tang introduced a photoactive interface where the molecular energy level difference was sufficient such that excitons dissociated with high probability. The next step forward was the development of processing methods that distributed this photoactive interface throughout the active layer of the photovoltaic. This work was initially led by Heeger et al with the formation of the bulk heterojunction [18] and has been pushed forward by a number of groups over the past two decades. A more indepth review of nanostructural engineering and its effect on photocharge generation is presented in Chapter 4. 30 Donor Energ Acceptor LUMO AEDA -HOMO Position Figure 1-8: Schematic of energy levels at an organic heterojunction. The percentage of excitons converted to charge carriers is equal to the product of the exciton diffusion efficiency, 'rEr and the charge transfer efficiency, 'roT. Exciton diffusion efficiency depends on materials properties and nanostructure. Charge transfer efficiency depends on voltage, light intensity, and temperature, [10] but is often assumed to equal unity. Charge Carrier Collection Polarons will accumulate at the heterojunction interface as they are generated. At this interface they are free to move in one direction (towards an electrode) but not the other (towards the heterojunction) due to the energetic barrier. Thus, we find that the distribution of polarons effectively spreads out towards the neighboring electrode and is thus collected by the electrode. Whether this spread towards to the electrode is due to diffusion (simply the non-uniform concentration) and/or drift (due to polaron repulsion or from an applied electric field) depends on the device architecture and materials as well as operating voltage. The percentage of charge carriers collected compared to charge carriers generated is often identified as the carrier collection efficiency, 71cc. Note that the electrical power collected is equal to current multiplied by voltage. Care must be taken to maximize the number of charges collected (which leads to current) as well as the potential energy of those charges (which leads to voltage). This will be discussed in more detail below. 31 BCP ACCEPTOR DONOR ITO Glass Figure 1-9: Left: Schematic of device architecture of a organic photovoltaic with planar subcell, electrodes and interfacial layers. Note that the vertical length scale is in the 100s of nanometers. Right: Schematic of lateral device architecture of a organic photovoltaic with subcell (green), bottom electrode (pink) and top electrode (blue). Note that the square is 0.5 inches long on each side. 1.2.2 Organic Photovoltaic Devices Device Architecture The central component of the OPV device is the photoactive layer (the subcell), on which we have focused above. However, there are multiple other components. On the most fundamental level, an electrode is required on either side of the device to collect positive and negative charge carriers and channel them to a circuit for utilization. One of the electrodes should be transparent to allow for the transmittance of photons to the photoactive layer. Initial OPV demonstrations were simply thin films of molecules deposited between thin films of two metals. [19] This is the simplest possible device architecture. However, significant enhancements in performance can be gained by adding interfacial layers (e.g. [20]), which assist in charge collection and minimize resistance between the electrodes and the active layer. Furthermore, the device is usually prepared upon a substrate to provide stability. (Vapor-processed organic photovoltaics have thicknesses <1 micron, thus they need additional support to prevent fracture.) The sum of the above layers comprise our standard device architecture, which is shown in figure 1-9a. Additionally, devices benefit greatly from encapsulation to minimize exposure to 32 the environment. Most semiconducting materials have been shown to be significantly affected by normal chemicals in the air such as water and oxygen. Thus solar panels are almost always encapsulated to slow degradation. In chapter 3 of this thesis, we introduce potential encapsulations for ultra-lightweight solar panels. Please note, however, that most of the devices reported in this thesis do not have encapsulation and instead are fully fabricated and characterized in vacuum and/or inert atmosphere. Note that this merely describes the vertical architecture of the device. It is also necessary to design and control the lateral architecture of the device, including the designation of positions where either of the electrodes can be electrically contacted while ensuring that the electrodes are continually separated by the subcell to limit shorting. The lateral architecture that we have primarily utilized in this thesis is shown in figure 1-9b. [21] Device Fabrication Firstly, one must start out with the best possible materials, especially the organic semiconductors. The impurity chemistry and concentration significantly impact the optoelectronic behavior of semiconductors, [22] thus the source of materials matters and post-purchasing treatment must be considered. Organic molecules may be purified via a three-zone furnace, which separates bulk materials by sublimation temperature. This process is described elsewhere. [21] The considerations of materials manufacturers and purity for devices in this thesis are described in Appendix B. The foundation of any thin film solar cell is a clean substrate, usually pre-coated with commercially-deposited ITO (which is significantly higher quality than that which is manufactured in house, see again Appendix B). Prior to any device fabrication, the ITO-coated glass substrates are solvent cleaned (dilute Micro-90, DI water, Acetone and boiling Isopropanol), dried with a N2-gun, and stored in fluoroware in inert atmosphere. In ONE Lab, our 'dry' glovebox is connected to a vacuum thermal evaporation chamber (amongst others) via a ultra-high vacuum transfer line. This minimizes exposure of the substrates and sequential layers to ambient atmosphere. All materials discussed in this thesis are deposited via vacuum thermal evapora- 33 substrate holder thickness monitor gate shutter to pump stack source material source *boat* power supply Figure 1-10: Schematic of the interior structure of a vacuum thermal evaporator. [23] tion. A schematic of this chamber is shown in figure 1-10. Inside the chamber, a crucible filled with the selected material is resistive-heated above sublimation temperature, thus vaporizing the material as individual molecules. Due to the ultra-high vacuum pressure, the molecules travel line of sight out of the crucible and deposit onto the substrate placed directly above. The deposition is non-conformal and may lead to shadowing and non-uniform deposition, thus the substrate is rotated during deposition. Thin film thickness is measured via a quartz crystal thickness monitor. The thickness monitor is calibrated separately with a profiler. The thermal evaporation process is repeated for each of the layers within the device. Our chamber holds up to 6 crucibles of materials and thus usually does not need to be reloaded at any point during the full device fabrication process. Electrode thin films are patterned in situ via shadow masking to generate a controlled device area. Further details and tips for fabrication are included in Appendix B. Device Characterization The most fundamental method for characterizing the operation of a photovoltaic is by measuring its electrical power output relative to the optical power input. This mea34 J Power Conversion Efficiency, PCE = max. power point input optical power dark Open Circuit Voltage, Voc Vnt- light KV Short Circuit Current, Jsc Maximum power rectangle Fill Factor, FF = max. power point Voc - Jsc Figure 1-11: Cartoon of a current density-voltage characteristic, identifying the Voc, Jsc, and MPP . surement gives us the power conversion efficiency, PCE. The conventional method for doing so is to illuminate the PV with a lamp with known optical power (preferably a solar simulator" with a color spectrum close to that of the sun) and measure current output as you vary an applied voltage. ' Electrical power is calculated by multi- plying current and voltage, and the maximum power point (MPP)is determined by investigating the full sweep of voltages in the fourth quadrant of the current-voltage characteristic. A cartoon of a current density-voltage characteristic is illustrated in figure 1-11. 5 There are 4 key parameters that can be derived from a current-voltage characteristic: 1. Open Circuit Voltage. V 00 Open circuit voltage, Voc; is the voltage that must be applied to the photovoltaic such that zero current is flowing (i.e. the photovoltaic is in an open circuit). This doesn't necessarily mean that there is zero motion of charges but rather that the number of charges flowing out is equal to the number of charges flowing in. Voc is related to the electronic energy levels, as shown in figure 1-7. Theoretically and 4 A terrific description of ONE Lab's opto-electrical characterization procedures is published in the PhD thesis of Alexi Arango [21]. 'Caution!: I usually intend to discuss current density, J, which is current per unit area. However imany times I say simply "current" (which would be I). practically the Voc is proportional to the optical band gap, [5, 241 however there is much speculation within the OPV field that it is instead dependent on the donoracceptor interfacial energy difference. [25] In either case, there are multiple energy losses within the device which leads to Voc significantly lower than both the donoracceptor interfacial energy (except in situations with recombination dominated by the bulk rather than the interface [26]) and the optical band gap. 2. Short Circuit Current, Jsc Short circuit current density, Jsc, is the current that is flowing out of the photovoltaic when there is zero voltage applied (i.e. the photovoltaic is shorted). Current density is proportional to the number of positive charge carriers moving through the device area over a given time, t. Thus Jsc is approximately equal to the flux of photo-generated charges in the device due to the incident optical power. However there are losses due to resistances and recombination within the device. 3. Fill Factor, FF Fill factor simply describes the shape of the J-V characteristic. As illustrated in figure 1-12, the shape of the curve significantly affects the maximum power output. The effect of shape is quantified as the fill factor, FF = VOC * Jsc (1.1) 4. Power Conversion Efficiency, PCE Power Conversion Efficiency, PCE is the ratio of electrical power out to optical power in: o=*Jsc*FF PCE = PIN (1.2) PIN where MPP is maximal electrical power outputted and PIN is optical power. Power conversion efficiency is the most commonly cited parameter of a photovoltaic and arguably the most important, however the other parameters listed above allow us to identify limitations and potentials of photovoltaics and guide us in the enhancement of power conversion efficiency. 36 J dark Voc light V dark J V light dark V light Jsc Figure 1-12: Cartoons illustrating the Voc, Jsc, and FF and their effects on the maximum power point (and thus PCE). Spectral Response There is another perspective of characterizing a photovoltaic: spectral response. The spectral response is necessary for understanding how the device responds to sunlight as well as identifying which layer is behaving how. This is quantified by measuring the external quantum efficiency, EQE. External quantum efficiency is equal to the number of positive charge carriers moving through the device area during time t divided by the number of photons incident on that device area during that same time t, i.e.: Holes Collected Photons Incident This parameter is also sometimes called Incident Photon to Current Efficiency, IPCE. Internal quantum efficiency, IQE is a measure of the device performance regardless of optical effects. It is equal to the number of positive charge carriers moving through a device area during time t divided by the number of photons absorbed by that device area during that same time t, i.e.: Holes Collected Photons Absorbed 37 (1.4) 1.3 1.3.1 Objectives of this Thesis Work Robust, Ultra-lightweight Solar Arrays Organic photovoltaics (OPVs) have generated much excitement in part due to their potential as ultra-lightweight, flexible solar modules [27-30]. This potential is primarily due to the favorable mechanical properties of the photoactive layer (namely, their minimally ordered nanostructure), however a complete solar module is limited by the electrodes, substrates, and encapsulates. Herein, we report on development of carbon-based electrodes enabled by novel vapor-processes, which can be deposited on any surface/substrate (Chapter 2). Furthermore, we discuss development of a nanothin, conformally deposited encapsulant, for encapsulation of ultra-lightweight solar cells (Chapter 3). 1.3.2 Efficient Power Conversion Every percentage increase in power conversion efficiency equates to a decrease in area (and weight) required of solar cells for generation of a specified amount of electrical power. Photovoltaics generally available in the US have PCE in the range of 15-25%. However, current record organic photovoltaics are only 11.1%. [7] Can organic photovoltaics match the efficiency levels of conventional solar technology? This is where I have directed the remainder of this thesis. Firstly, we survey the current OPV nano-structures and architectures in literature (Chapter 4). Then we explore the trends of best OPVs in literature and apply it to two standard OPV structures to understand the practical efficiency limits of these standard sets if we were to increase the cells to previously demonstrated bests in every aspect. Chapters 6-8 reports our work advancing OPV power efficiency via multijunction architectures and novel vapor processes for organic semiconductors. 38 Multijunction Photovoltaics The theriodynamic limit for converting solar power to electricity on Earth is 89%, but the limit for a single-junction photovoltaic at 33%. [24] The tried method for simultaneously reducing thermalization and absorption losses is to stack multiple cells with varying bandgaps. Indeed, this approach has led to record PV efficiencies of 44.4% with triple junction cells. [7,31] While stacking of high efficiency inorganic cells is limited by epitaxial growth considerations (i.e., lattice matching) and can add substantial cost to PV fabrication, nanostructured materials do not have such restrictions. This makes stacked growth of nano-PVs feasible on arbitrary substrates and with arbitrary combinations of subcells, as already demonstrated for molecular PV structures. [32] Optimization of multijunction cells, however, requires cognizant choice of complementary subcells as well as balancing of the photocurrents (for series connection) or photovoltages (for parallel connection) of the subcells. Chapters 6 and 7 of this thesis discusses the design and optimization of nano-thin mnultijunction organic photovoltaics. Nano-Structural Engineering Ultimately, however, multijunction OPVs are still limited by the subcells within. One common approach towards enhanced subcell efficiency is generating greater mixing of the donor and acceptor materials, however this can impede photocharge collection and detrimentally increase series resistance. An alternative approach is to enhance molecular ordering to extend the exciton and charge carrier diffusion lengths, thus potentially increasing Jsc concurrently with VOC and FF. In Chapter 8, we present two novel approaches to nano-structural engineering of vapor-processed organic semiconductors for enhancement of power conversion efficiency. 39 Part I Electrodes and Encapsulations for Robust, Ultra-lightweight Solar Arrays 40 Chapter 2 Robust, Ultra-lightweight Solar Arrays Enabled by Vapor-Processed, Carbon-Based Electrodes Electrodes connect the photoactive materials with the real world; they collect photo charges from the active layer for utilization as electricity. The most commonly used electrode materials in OPVs are tin-doped indium oxide (ITO) and aluminum. ITO utilized in a full 95% of published devices [33]. However ITO is an intrinsically critical material due to the scarcity of indium. [34-37] Furthermore, the inechanical properties of ITO thin films are incompatible with lightweight and/or flexible substrates. [38 -42] Therefore the OPV field has been collectively seeking a substitute for ITO which is transparent, conductive, flexible, easily processed, and earth abundant. [34, 4345] Current materials under research are: conductive polymers, graphene/carbon nanotubes, thin metal films or grids, and metal oxides. In spite of demonstrations and progress, the opto-electrical properties need much further improvement before reaching the "gold standard" of ITO. 41 Here I describe two approaches that we have taken in collaboration with other groups here at MIT. Both are vapor-deposited, carbon-based electrodes. One is graphene (planar, crystalline carbon), [46] and the other is PEDOT (amorphous polymerized carbon). [38] 2.1 Doped Graphene Electrodes for Organic Solar Cells on Glass 2.1.1 Graphene Electrodes Graphene is a hexagonal arrangement of carbon atoms forming a one-atom thick planar sheet. This layer is the building block of graphite and carbon nanotubes and it has been studied widely by theorists since the middle of the last century [47, 48]. The successful isolation of single- and few-layer graphene by the mechanical cleaving of highly ordered pyrolytic graphite (HOPG) [49] has led to an explosion of research activities, and significant attention has been focused on their high electron and hole mobility (up to 200,000 cm 2 y-is') [50, 51], high current carrying capability (up to 3x108 A-cm- 2 ) [52], and high mechanical robustness [53]. Graphene has also been shown to have a uniformly high transparency in the visible and near infrared region and thus can be utilized to form ultra-thin transparent electrodes [54]. Recently, the Kong group at MIT has developed a procedure to produce large, area, continuous graphene sheets on copper foil via low pressure chemical vapor deposition (LPCVD). These sheets may then be transferred via a PMMA stamp to an arbitrary substrate. Since the as-grown graphene is mostly single layered, in principle, one can control the number of graphene layers through multiple transfers which results in overall improvements in the conductivity of the graphene electrode: for the OPVs in this report, three-layered graphene sheets were used. The sheet resistance (Rsh) of graphene on quartz substrates can be varied from 500 to 300 Q/sq and transmittance from 97.1% to 91.2% for 13-layered graphene sheets (figure 2-1). As shown in figure 1(b), the optical transparency of our graphene sheet agrees quite 42 100 95 iF 90 C 96 so 70 4 Soo0 600 700 800 Wavolength (nm) Figure 2-1: Transmittance of graphene sheets of onethree layers. As-grown LPCVDsynthesized graphene films are mostly single layered and each additional layer contributes approximately 2.3%O opacity over the range of wavelength. The inset indicates the transmittance at 550 nm as a function of the number of graphene layers. well with the rnasuremient performed by Nair et al [55] where each graphene layer was reported to have approximately 2.3% opacity. This result confirms that our Cu grown graphene layers are monolayer and the multiple transfer steps are successful to maintain the integrity of the graphene layers. Furthermore, Kim [56] reported that AuCl 3 (loping on graphene films resulted in up to 77% decrease in Rah with only 2%X decrease in transmittance. 2.1.2 Graphene OPVs Here we report the implementation of this large area, continuous, highly conductive and transparent graphene sheet, with controllable number of layers, as an anode material in organic photovoltaic cells. The rest of the device architecture followed our typical structure (electrode/PEDOT: PSS/active layer/BCP/Ag). The active layer of the photovoltaics was comprised of copper phthalocyanine (CuPc) and fullerene (C 60 ). Optimization of the device included adjustment of electrode surface energy via fabrication and cleaning procedures as well as enhancement of graphene electrical (i.e., withproperties. Typical power conversion efficiency (PCE) of pristine graphene out doping) based solar cells using copper plithalocyanine (CuPc) and fullerene (Co) is 1.37%, which is about 77.3% of the PCE of the equivalent indium tin oxide (ITO) 43 (d) M~A ITO (0, 0lama)-daft 0 IIA. ITO (0,P"naLMurm0Wd1 * tC. Grapheme (DopdWdark 7t1C. Graphieme (DOped)Uumrnne 0 I-Jo. E2 0 *-2 vs. Graphene STO -0.4 -0,2 0.0 0.2 0.4 0.6 0.A Voltage (V) Figure 2-2: Current Density-Voltage characteristics of organic solar cells with different anodes under dark and simulated AM1.5G illumination at 100mW-cm- 2 .Shown here is the comparison of performances of ITO with modified PEDOT:PSS by 02 plasma (IIIA) and graphene doped with AuCl3 (10 mM) (1IC). based cells (1.77%). By chemically doping (p-type) the graphene with AuCl3 , we found the PCE of graphene solar cells to be further improved (PCE: 1.63%), which is comparable to (92.1% of) the device performance of ITO based solar cells. Continuing work from the Kong group has further improved power conversion efficiency strates 2.2 [57] as well as demonstrated graphene electrodes deposited on flexible sub- [58]. oCVD-Printed Polymer Electrodes Enabling Direct Monolithic Integration of Organic Photovoltaic Circuits on Unmodified Paper Here we examine the use of a substrate-independent vapor printing process to deposit the conducting polymer poly(3,4-ethylenedioxythiophene) in place of the conventional transparent conductive electrode (e.g., indium-tin oxide (ITO)) in organic solar cells on glass, plastic, and paper substrates. This process combines oxidative chemical vapor deposition (oCVD) [59, 60] with in situ shadow masking to create 44 a 100 800 so 0-00 13100'"0 0 op 'Thickness 50 100 150 20 (n) Sheet Resitance (fl/o) Figure 2-3: Relationship between percent transmittance (550 nm) and sheet resistance in ohms per square ( Q/D) for the vapor-printed oCVD PEDOT used in thre work. The red line is a fit to Equation (1) giving udc/u 0 p=9 (the dashedl black line is for reference and corresponds to udc/ug),= 3 5, representative for traditional metal oxidle electrodes). Lower inset: sheet resistance plottedl versus film thickness. Upper inset: 200-nm thick PEDOT film vapor printed on tissue paper in 15 pt. bold Verdana font. well-defined polymer patterns on the surface of choice (Fig. 2-3, inset). For oCVD, the polymnerized thin films form by simultaneous exposure to vap~or-p~hase monomer (EDOT) and oxidant (FeCl3 ) reactants at low slubstrate temperatures (20-100~ C), moderate vacuum (~-0. 1 Torr). The printed polymer patterns (down to 20 ipm resolution) result from the presence of a shadow mask by maintaining the partial pressure of the vapor-dlelivered oxidanit species sufficiently (lose to its saturation pressure at the substrate, which prevents significant mask undercutting. The vapor delivery of the oxidant species makes this process unique from other techniques that rely on solvent casting of oxidants prior to vapor delivery steps. [61, 621 Because the process is all dry, there arc no wettability or surface tension effects on rough substrates like paper, and exactly the same process steps are used to fabricate devices oni glass, plastics, andl papers. 45 2.2.1 oCVD-printed polymer electrodes For use as a transparent electrode, the conducting polymer layer must provide both low sheet resistance (Reh) and high optical transmittance (T) which are related by the following equation: [63,64] T= 1+ (2.1 ZOop 2Rsh (2.1 where ZO is the impedance of free space (377 Q), and Ordc and oo optical conductivities, respectively. PEDOT deposited on glass at 80 are the dc and Figure 2-3 shows this relationship for oCVD and 0.1 Torr. The data fits well to equation 1 across the full data range, giving fcfd/JOO =9. This value is comparable to the best commercially available conducting polymer solutions and is slightly lower than that reported for carbon nanotube conductors rdc/aOP=15 and traditional metal oxide electrodes adc/cop=35. [63,64] The ability to integrate these other electrode materials with paper has also not yet been demonstrated. As shown in Figure 2-4, conductive, 150-nm thick, oCVD PEDOT polymer electrodes (100-1000 S-cm- 1 ) are uniformly deposited on ultra-delicate substrates with no pre- or post-treatment and at identical conditions: ~10-pni thick SaranTM wrap (A, upper left), water-soluble rice paper (B, upper middle), and a single ply of bathroom tissue that is porous and absorbent (C, upper right). In contrast, the conventional drop-cast conducting polymer solution (CleviosTM PH 750) does not wet the hydrophobic surface (A, lower left), easily dissolves the soluble substrate (B, lower middle), and soaks through and easily damages the delicate fiber matrix (C, lower right). Measurement in the lower half of the figure indicates the 2-point film resistances of 130Q, 1200Q, and 5.9 kQ respectively. (D) 200-nm thick, oCVD PEDOT polymer electrodes are vapor-patterned in situ directly on the substrate of choice. The figure shows examples of PEDOT printed in 15 pt. bold Verdana font on 10-mil thick PET, SaranTM wrap, Tracing Paper, and Tissue Paper. With the chemistry and conditions used here, the low vapor pressure of the FeCl3 oxidant at the substrate allows for pseudo-directional flow of this species through the mask to substrate. This, in com- 46 A Saran"m wrap (hydrophobic) B Rice wraper (solub) C 1-ply bathroom tissue (porous, absorbent) 5.9kl pDchusetts Fu2: v ts E Institute of Technolo achusetts Institute of Technoto m lgaring daper Meassachusetts Institute of Tech TissuP per W assachus Figure 2-4: Top: Deposition of oCVD PEDOT and solution-processed PEDOT oil a variety of surfaces (a-c). Multimieters demionstrate conductivity. Bottomn: Patterned, large-area deposition of PEDOT on a variety of surfaces. 47 b10 a f iv. ITO/PEDOT:PSS 0 0.3 0.6 Vo1tage MV Figure 2-5: Current density- voltage characteristics under illumination (AM1.5, 100 mW-cm-2 ) for oCVD PEDOT PVs on glass differing only in anode structure (the yellow and red curves are for reference and do not include oCVD PEDOT). bination with its fast reaction rate with the more-volatile EDOT monomer, creates well-defined oCVD PEDOT anodes in the masked pattern and prevents significant mask undercutting. 2.2.2 oCVD-printed PVs We first established the integration of oCVD PEDOT anodes into thin-film or- ganic PV devices on smooth glass surfaces using the well-documented CuPc/C6 0 (or PTCBI)/BCP/Ag molecular organic heterojunction architecture (Fig. 2-5, inset). [20,65-68] Fig. 2-5 compares representative current density-voltage characteris- tics for individual devices on glass and differing only in anode structure: (i) oCVD PEDOT (50 nm), (ii) indium tin oxide (ITO), (iii) ITO/oCVD PEDOT (10 nm), (iv) ITO/PEDOT:poly(styrenesulfonate (PSS). The series resistance (R) allel (shunt) resistance (R) were determined by fitting the dark current data shown) across the voltage range to the generalized Shockley diode equation: Jdark -- and par- Ruas (gnp (--VojRn ) where n is the diode ideality factor and J is the reverse saturation current. 48 (not [10] (2 .2) The devices incorporating oCVD anodes (i and iii) perform comparably to the devices with conventional ITO anode structures (ii and iv), and both oCVD PEDOT and PEDOT:PSS devices exhibit improved open-circuit voltage (0.48V) relative to those on bare ITO (0.41V). [20,69,70] Both oCVD PEDOT and PEDOT:PSS have comparable work functions (~5.2 eV); [59] however, the conductance of oCVD PEDOT thin films is several orders of magnitude more conductive than the PEDOT:PSS (CLEVIOST P VP Al 4083) buffer layer (<10 S-cm-1) [60], which contributes to the higher observed fill factor (>0.6) in the devices with ITO/oCVD PEDOT electrodes (iii) due to the lower device series resistance (1.2 Q-cm 2 vs. 4.2 Q-cm 2 ). For the ITO-free oCVD electrodes (i), the trade-off between sheet resistance and transparency with thickness accounts for the decrease in the fill factor (0.54) due to series resistance (4.4 Q-ci 2 )and the short-circuit current (3.8 mA/cm 2 ) relative to (ii). Moreover, we note that the power lost due to the electrode sheet resistance for a cell of width a) and length 1, where current is collected along I can be estimated by the following equation: [71] PIOSS = sI 3sc)3 (2.3) For the PEDOT electrodes used here, this corresponds to less than 1% fraction of power lost (Pi0 s./generated total power) for these 0.5x2.0 mm 2 cells, and to prevent a power loss of over 10% the cells should each be kept below 5 mmni wide. 2.2.3 oCVD-printed PVs on flexible plastic and paper substrates Next, we demonstrate the processing versatility of oCVD printed electrodes, by fabricating these organic photovoltaics-device structure (i)-directly on various flexible substrates, including common fiber-based papers (Fig. 2-6). We observed the oCVD PEDOT electrodes and the full device to be electrically robust to mechanical deformations, which is highly desirable for low-cost roll-to-roll processing and potential applications (Fig. 2-6a). After 1000 compressive flexing cycles at <5 mm radius, the electrical conductivity of oCVD PEDOT on PET is minimally affected. In contrast, 49 a b niwe. PMust (PET) Substrate 10Tssue 0.6.cg V.t Paper 8 0Jsc Cp Paer 10 1 - - Paper %R 10S 10' PEW 101 1061 0 .7s000mwea 25 50 75 0 100 Flexing Cycles (R=S mm) 0.1 0.2 0.3 Voltage (V) Figure 2-6: (a) Device characteristics under illumination (AM1.5, 100 mW -cm- 2 ) and electrode conductivity for oCVD-printed PVs on PET (5-mil thick) after repeated flexes to 5-mm radius. The dashed black line shows the conductivity of ITO/PET for reference. (b) Current density-voltage characteristics under illumination (AM1.5, 500 mW - cm- 2 ) for oCVD PVs vapor-printed on as-purchased tracing paper (~40- pm thick), copy paper ( ~120-pm thick), and tissue paper ( ~40- pm thick). flexing of commercially fabricated ITO-coated PET substrates decreases the film conductance over 400-fold due to formation of cracks visible under optical microscope. Moreover, after over 100 compressive flexing cycles, devices with oCVD PEDOT electrodes on PET, display no significant change in performance. In contrast, we observed the equivalent ITO-based cells to become electrically shorted immediately upon flexing. Further examination shows that upon flexing the cracking features observed for the underlying ITO electrode become visible on top of the full device (cathode surface) with feature heights on the order of the device thickness. This suggests that the electrode cracks compromise the integrity of the subsequent device layers as has been reported elsewhere, [72] in contrast to the flexible oCVD PEDOT devices, which maintain function and are visibly unchanged after repeated flexing. Paper substrates have a range of light transmission properties, typically characterized by high light scattering (transmissive and reflective) due to surface roughness but low absorptive losses. The surface reflectivity is evident in the performance curves for devices on various papers (Fig 2-6b), in which the short-circuit currents scale inversely with losses due to reflection. This is also evident by comparing the quantum efficiency and absorption spectra for oCVD PEDOT devices on tracing paper with conventional 50 C 30 c6 PTCBI PAcceptor Acceptor a, 10 4W0 Figure 2-7: 60W NO 4W0 IWAWFIGmOR Wh (n) 6W0 SW Internal and external quantum efficiency comparison for devices on glass/ITO/PEDOT:PSS (black) and tracing paper/oCVD PEDOT. glass/ITO/PEDOT:PSS devices (Fig. 2-7). While the external quantum efficiencies (charges collected per incident photons) are lower on the paper substrates due to substrate/electrode losses, the estimated internal quantum efficiencies (charges collected per absorbed photons) are comparable across the visible spectrum, indicating similar upper bounds on efficiency for both the paper and conventional ITO/glass structures if effective light trapping schemes are incorporated. We note that such schemes may be uniquely designable for paper substrates because of their good reflectance and scattering (non-specular) properties, where >90% of the light absorbed by the active layer in the paper-based devices stems from diffuse transmission (scattering) compared to <10% on smooth ITO/glass. We emphasize that these solar cells are integrated directly onto as-purchased papers: no pretreatment is used to fill in the spaces between the fibers. Thus, we retain the breathability, deformability, and low weight of the underlying paper, making the devices truly wearable and portable. Because the surface of paper is quite rough, a key to this breakthrough is the adherent formation of the first layer of the device conformal around the individual fibers of the paper. This is evident under scanning electron microscope in which the bare paper looks nearly identical to that coated with the PEDOT electrode. Because our methods do not expose the substrates to high temperature or solvents, even delicate substrates like paper are not damaged. 51 2.2.4 Large-area monolithic photovoltaic arrays The ability to print patterned device layers on any substrate enables facile monolithic integration of arrays of individual PV cells. We demonstrate this here by fabricating 250-cell (0.1xO.3 cm 2 each) series-integrated monolithic arrays on both paper and glass substrates. Figure 2-8 shows the pattern for each device layer (achieved by in situ shadow masking), which ultimately create anode-to-cathode interconnections between the individual cells. Ultimately, the specific circuit design should be explicitly optimized to minimize efficiency losses due to parasitic resistances, absorption, and fractional device coverage. [73] For this demonstration, we have chosen a relatively small device area both to minimize the losses due to resistance through each device and improve device yield at the expense of low fractional area coverage (~25%). The current-voltage characteristics show high open-circuit voltages of 50V and 67V, respectively (Fig. 2-8b), representing a near summation of voltages from all working cells in each series (minus losses from shorted devices). Spatial distribution maps of individual solar cell performance in the series-integrated arrays were recorded to gain insight about overall cell statistics. The cell voltage distributions on both glass and paper substrates (Fig. 2-8c) show that devices on each substrate achieve similar maxima (~0.4 V), with higher variance across the rougher paper. Moreover, high (low) cell voltages are grouped spatially across the paper substrate. More work is required to understand the exact failure mechanisms but we believe that the higher density of low open-circuit voltages on the paper substrate is likely a result of small shunt resistances in local areas of high roughness across the less-conformal, evaporated photoactive layers. However, as was discussed recently for paper-based organic transistors, [74] a specific correlation was not immediately apparent by examining optical and SEM surface images of functional and non-functional cells. 52 now y Anod AnofAc~ CuPf/PTC8l/BCP oCVD PEDOT Ag - c b.. Series-lntegrated oCVDOIPV 250 PV cells In serles C66010 7 cm i. - (MV) 3501 0 Paper 110. Glass rCIUft Voc-SOV 0 50 rCIult j400 Voc-67V 10 0 0 MM O Figure 2-8: (a) Printing schematic for 250-cell, series-integrated monolithic arrays. The photographs show the printed PEDOT (~50-nm thick) pattern (left) and a completed array (right) on tracing paper. (b) Current-voltage performance curves for series- integrated photovoltaic arrays with vapor-patterned oCVD electrodes on 2 paper (red) and glass (black) under illumination (AM1.5, 80 mW - cm- ) (bold) and in the dark (thin). (c) Spatial map of individual cell open-circuit voltages across the respective 50 cm 2 arrays. The lower insets show the cumulative fraction of devices producing at or below a given voltage. 53 a IAL 4 somWem .IddevWca 0.6 0.4 -N 7"n s L"o Nomr Innwtd 0 b 0.2 1.0 p 640* 90 -uww ~ LO KEWM@nsftpqpwdftA y\ 0.4 0.2 0.0 . 0.2 0 2 0 4 3 6 Nunber of Fokds 10 20 TWO (s) A Figure 2-9: (a) Normalized efficiency of thin-film-packaged and unpackaged arrays 2 (250 series-integrated cells) subjected to constant illumination (80 mW - cm- , halogen lamp) in air at 42 C (108 0 F) as a function of time. The right photograph shows the laminated paper circuit powering an LCD display in air with ambient sunlight. (b) A paper array is progressively folded in air while being tested at AM 1.5, 80 mW cm 2 . The final folded structure can be dynamically unfolded and refolded without loss of performance in each three-dimensional configuration. (c) The iCVD-coated array (28 series-integrated cells) is submerged in water during operation. The right inset shows a nearly spherical droplet of water on the surface of the paper photovoltaic array. The same device also withstood tortuous roll-to-roll processing by an office laser-jet printer. 54 2.2.5 Integrated paper PV demonstrations As noted earlier, the light weight and foldability of these devices could provide an advantage in reducing the cost of their installations and opening new venues for application. However, for final deployment these lightweight structures will require flexible thin film encapsulation to achieve sufficiently long lifetimes and provide other environmental protections. [75] Thus, here we briefly show that simple, passive, flexible thin-film encapsulation techniques can significantly improve cell lifetimes and can provide other unique protective benefits while maintaining the foldability and papery qualities of the unpackaged circuits (Fig. 2-9). 250-cell series-integrated ar- rays on tracing paper were encapsulated on both sides with three encapsulants 1) 5-mil thick plastic laminate applied with an office laminating machine, 2) 750-un thick poly (monochloro- p-xylylene) ("parylene-C") deposited by self-initiated CVD polymerization, and 3) 750-urn thick hydrophobic and crosslinked poly (1H,1H,2H,2Hperfluorodecyl acrylate) ("PPFDA") film deposited by initiated CVD (iCVD) polymierization [59]. The packaged and unpackaged series-integrated arrays were then aged in air,, accelerated by exposure to constant illumination (80 mW-cim-2, halogen lamp) and elevated temperature (42' C/108' F) at open-circuit (Fig. 2-9a). The power-efficiency/time trajectory shows that each thin-film encapsulant significantly improves lifetime over the unpackaged counterparts. The influence of ultrathin films on circuit lifetime is also evident in the unpackaged cells in which removing the 10-nm thick exciton blocking layer (BCP) [20] more than doubles the rate of power decay. We emphasize that this lifetime test was performed on the full monolithic series-integrated arrays and thus approaches a lower limit on power lifetime, since the photocurrent of the full array is limited by that of the worst cell in the series. The longest lifetime (half-life) observed here, >500 hrs, compares favorably with other reports of shorter illumninated lifetime, [76, 77] similar " shelf' lifetime of hybrid-encapsulated cells, [78] and similar illuminated lifetime for an encapsulated single tandem cell. [79] The right hand inset, shows a laminated paper PV array powering an LCD display and related circuitry in air using sunlight from the window, 55 which has remained operational after over 6000 hours of ambient-light shelf life in air. With specific engineering and more sophisticated encapsulation techniques (active desiccants, multilayers, etc.) the lifetime dynamics should be readily extendable. The foldability of the paper photovoltaic arrays is shown in Fig. 2-9b, in which high voltages are produced in each folded three-dimensional configuration and are maintained during dynamic folding and unfolding. The decrease in voltage with additional folds is partially a result of individual cell damage, which we observed to manifest as localized short circuits to the next device in the series. The voltage and current also decrease as a result of the geometry of illumination, as is evident by the increase in voltage when the accordion structure (- 450 incidence) is flattened out (normal incidence). Finally, we note that the various encapsulating films can also add specific functionalities to the integrated arrays of paper photovoltaics. The submicron iCVD- coated array is foldable and also hydrophobic, withstanding extended exposure to water droplets and even complete water submersion without shorting or exhibiting significant changes in performance (Fig. 2-9c). This paper photovoltaic array was also resilient to subsequent laser-jet printing, where the whole cell was fed through a roll-to-roll printer, while still maintaining efficiencies sufficient to power the LCD clock. 2.3 Conclusions Herein we report our investigations of novel carbon-based electrode materials from the Kong and Gleason groups and demonstrated their capacity for use as transparent electrodes. Further, we develop and optimized surface treatments and fabrication methods for integrating these electrodes with organic semiconductors. Finally, we demonstrated the first ever solar cell fabricated directly on paper, and further demonstrated a monolithic solar cell array on paper. This advances the development of robust nano-thin electrodes for use with ultra-lightweight, low cost substrates. 56 Chapter 3 Sub-30nm Thin Encapsulation for Enhanced Device Lifetimes 3.1 Introduction Organic photovoltaics (OPVs) have generated much excitement in part due to their potential as ultra-lightweight, flexible solar modules [28 30], however the current range of device lifetimes in literature (0-5 years) [80-82] do not yet achieve the lifetimes necessary for commercialization (5-10 years). [5] Device lifetime is a key figure of merit for solar cells because it impacts the levelized energy cost ( $/(kW-hr) ) of a photovoltaic module as well as its carbon release factor. [5] Its importance necessitates the solar cell encapsulation, however the prevalent commercial encapsulation (polymer thin film plus glass sheet [81,83,84]) is inflexible and significantly increases the weight of the module, thereby increasing the installation and balance-of-systems costs. In this work we characterize the device behavior of OPVs of various archi- tectures over time, and further we implement a 27nm-thin film of alternating layers of HfOx and AlOx deposited by atomic layer deposition (ALD) as an encapsulation layer [85] and characterize its impact on shelflife. 57 3.1.1 Degradation of OPVs Literature contains many investigations of degradation in OPVs, most pointing to oxygen, water, and light exposure as dominant sources of performance decay. [86-89] However, device degradation behavior depends greatly on the architecture of the OPV: on its active layer, interlayers, electrodes, substrate, and encapsulation. [75,80,84,87,90-96] In this letter, we compare the impact of degradation on device characteristics for two different active materials: the archetypal polymer system P3HT:PCBM (solution-deposited) [97, 98] and the common small molecular system ClAlPc:C60 (vapor-deposited) [99, 100], as well as electrodes of either Al or Ag composition (both vapor-deposited). 3.1.2 Encapsulation A variety of thin film encapsulations have been proposed and explored, including many that are based on organic and/or inorganic thin films that are potentially flexible and light-weight [80,101-108]. Atomic Layer Deposition (ALD) is promising for controllably depositing nanothin inorganic films, however this process is often done at relatively high temperatures and with exposure of the device to reactive reagents (e.g. water). [109, 110] In this letter we implement an ALD nano-thin composite proposed by Chang et al. [85, 111] Even with thickness <30nm, the WVTR of the nano-multilayer film is <5 x 10- 4 g-m 2 -day- 1 , [111] at or below the proposed thresh- old necessary foreffective encapsulation of organic electronics [75]. Furthermore, it is highly transparent, potentially flexible, and can be conformally deposited over 3-D large areas on any surface (beneficial for PVs deposited on highly structured substrates such as fibrous paper or for nanostructured PVs for enhanced optical behavior). 58 Molecular PMHJ Polymer BHJ 25 nm Encapsulant 100 nm Al or Ag 25 nm 110nm BCP ACCEPTOR 125 nm MIXED - 40 nm DONOR 110 nm | ITO S | ITO i 90 nm Glass Glass Figure 3-1: Schematics of the device architectures studied in this work. Thicknesses are listed on right, however the image is not to scale. 3.2 3.2.1 Experimental Methods Device Fabrication The device architectures studied in this work are shown in Figure 3-1. The photovoltaic devices are fabricated on solvent-cleaned, pre-patterned ITO-coated glass (Thin Film Devices, 20 Q/D). The polymer solar cells consisted of an anodic buffer layer of PEDOT:PSS and an active layer of a blend of P3HT and PCBM (Plexcore PV1000). The molecular solar cells consisted of 20nm of MoOx as the anodic interlayer, 10nm of ClAlPc, 20nm of a 1:1 blend of ClAlPc:C60, 20 nm of C60, and 7.5nm of BCP as cathodic interlayer. Stripes of either 100nm of aluminum or 100nm silver were deposited via vacuum thermal evaporation orthogonal to the ITO layer, generating a 0.0121 cm 2 device area. 3.2.2 ALD Process and Annealing An ALD barrier multilayer film comprised of AlOx and HfOx was deposited on top of completed devices using a Savannah 200 system by Cambridge NanoTech. Trimethylaluminium (TMA) and water were used as the precursors for the aluminum 59 oxide layers. Tetrakis(dimethylami-do)hafnium (TDMAH) and water were used as precursors for hafnium oxide layers. The growth rates for the two oxides were respectively 1.2 A/cycle for AlOx and 0.9A/cycle for HfOx. In this study we used four cycles of deposition of AlOx and 4 cycles of HfOx, and we repeated the deposition of the two materials 30 times for a final thickness of 27nm. The ALD process took approximately 10 hours, and the substrates were held at a substrate temperature of 100'C during the entire deposition time. In order to make more comparable the fabrication processes for the cells with and without the barrier film, all completed devices that were not encapsulated were annealed at 100'C for 10 hours in inert atmosphere. 3.2.3 Device Characterization OPV shelf life was tested according to the recommended protocol ISOS-D-1 Shelf [112]. To describe briefly, the devices were stored in dark at open circuit, at ambient temperature and humidity (approx. 25'C, 55% RH). All opto-electrical characterization was completed in a glovebox with inert atmosphere. Current density-voltage characteristics are measured under dark conditions and under 1 sun illumination (100 mW/cm 2 , AM 1.5G), using a 150 W solar simulator (Newport, 6255) illuminated through a AM1.5G filter (Newport, 81094) calibrated with an NREL-certified monocrystalline-Si photodiode (Newport, 91150V). Results are not corrected for spectral mismatch. Electrical characteristics are measured using a picoammeter (Keithley, 6487) employing a switch mainframe (Keithley, 7001) for switching between cells. 3.3 3.3.1 Results and Discussion Initial Performance The performance of the cells as fabricated are shown in Figure 3-2. The polymer system P3HT:PCBM gives a higher power conversion efficiency (3.1%) than the molecular system ClAlPc:C60 (2.0%). This is primarily due to the higher Jsc (8.84 vs 5.45 mA/cm 2 ), which is due to higher absorption efficiency of the polymer cell under 60 4- 0~ -2- - Polymer, Al Polymer, Ag - Molecular, Al Molecular, Ag 1.0 - -0.5 0.5 0.0 Voltage [V ] Figure 3-2: Comparison of representative current-voltage characteristics of solar cells of varying architectures, as deposited. solar illumination. The polymer cells have highest initial performance with aluimnun electrodes, and the molecular cells have highest initial performance with silver electrodes. However, we fabricated both active layers with both electrodes to study the electrode effects on lifetime. Utilizing an Ag electrode with the polyier cell decreases the overall efficiency (3.1% to 0.5%), primarily by decreasing the shunt resistance, likely due to shorting of the Ag atons through the polymer blend layer. The molecular cell, oii the other hand, has a BCP thin film between the active layer and cathode, that significantly decreases the issues with Ag shorting through the device. [20] Anm alunminun electrode decreases the short circuit current of the molecular cell in comparison with a silver electrode (5.45 mnA/cmn2 to 3.45 mA/cm'). This gives a significant but smaller decrease in efficiency (2.0% to 1.2%). 3.3.2 Degradation and Failure Behavior Figure 3-3 shows the lifetime of each of the solar cell architectures after storage in inert atmosphere or in ambient atmosphere without encapsulation. The polymer solar cells "died" within 20 hours of storage in ambient atmnosphere. However the molecular cells continued to generate power after 450 hours in ambient atmosphere, regardless of electrode composition. The significant difference in shelflife between polymeric and 61 Inert Atmosphere I 3.0 - - 40 II . I II . I e h Ambient Atmos Atmnounhuru 13.5 Inert AtosphereAmbient . 3.0 - - Polymer, A] 2.5 2.5 2.0M 2.0- U 1.5- 1.5- 1.0. 0.5 - S Molecular, Ag 1.0t y? r 0.0 0 200 400 600 800 1000 0.5 a Molecular Ar 0. P lymer. Ag 1200 0 Time (hours) 100 - 200 - 300 400 500 Time (hours) Figure 3-3: Comparison of device shelf lives without encapsulation in inert atmosphere or ambient atmosphere. molecular cells with either electrode rules out electrode oxidation as the dominating factor in polymeric cell degradation. Therefore the dominate degradation mechanism can be atributed to the effect of moisture on either P3HT or PEDOT:PSS. [88,89] For cells with an Ag electrode, the fraction of devices shorted increased over time, far faster in comparison with the Al electrode cells. This suggests that the silver atoms continue to migrate even after fabrication to cause shorts, and the BCP isn't completely protective. [20] All solar cells show substantial decreases in performance over 500 hours in ambient atmosphere (75-100% of initial PCE), however they have significantly lower PCE decay when stored in inert atmosphere over the same length of time (8-11% of PCE) (Figure 3-3), thus they have the potential for substantial enhancement in lifetime due to encapsulation from atmosphere. Figure 3-4 shows the J-Vs of devices initially and after failure or after two weeks, whichever was first. The molecular cells primarily degrade in conductivity and fill factor by various amounts (possibly due to introduction of an energetic barrier). Most polymer cells also exhibit significant conductivity degradation and lose their power conversion efficiency relatively rapidly. Further, all polymer cells with Ag electrodes shorted within 1 week, either before or after substantial conductivity decay (see IV curve of Polymer, Ag, Ambient in Figure 3-4). This indicates that Ag electrodes lead to device degradation that is not caused by environmental exposure and thus -if 62 4- 4-- 2- 2- C," E E -2- -2 Z0 -6--- 1 ___ -0.5 _ 0.0 0.5 Molecular Al, Initial At, Inert Al, Ambient Ag, Initial Ag, Inert Ag, Ambient Ambien 1.0 2 d Polymer Al, Initial Inert 6-Al, -8 Al, Ambient Ag, Initial Ag, Inert - 1__Ag,_Amb__ -6.5 nt 0.0 Voltage[ V ] Voltage [V ] 0.5 1.0 Figure 3-4: Representative current-voltage characteristics of devices initially and after failure or after 2 weeks (whichever cane first). utilized- necessitate strategies in addition to atmospheric encapsulation. [113] 3.3.3 Encapsulation with ALD Nanothin Film Effect of ALD Process on Device Performance ALD requires exposure of the device to elevated temperatures for an extended period of tinie, and additionally the device is exposed to precursors (e.g. water) during thin filn deposition. [109, 110] Chang et al optiniized their ALD process conditions for optimal annealing of a specific device architecture and conposition. [85] To investigate the impact of temperature vs precursor exposure, we separately annealed a batch of devices with no ALD film for the same length of time and temperature as the devices which had ALD fihn deposited on then (10 hours at 100 C). Figure 3-5 shows perforimance of polymer cells with aluminum electrode and small niolecule cells with silver electrode (1) initial perforniance, (2) after 10hours of annealing at 100'C, and (3) after encapsulant deposition (which includes 10 hours of annealing at 100 0 C). For the polymer cells, annealing at 100 0 C for 10 hours increases the Jsc by 12.5% but has no effect on overall PCE due to small decreases in FF (5%) and Voc (7%). For the nolecular cells, annealing at 100'C for 10 hours increases the fill factor by 6%, the Jsc by 4% and the PCE by 11%. However the ALD process had negligible effect on the performance parameters of either the polyner cells or the molecular 63 4- _______I 2- 0-2 - Polymer with At Initial --Annealed --ALD (inci annealing) Molecular with Ag C - 000_0_ -6- '7 S -. S- - - -- - Initial -- - -0.50 -0.25 0.00 0.25 0.50 Annealed ALD (inc annealing) 0.75 1,00 Voltage [ V I Figure 3-5: Impact of ALD encapsulation process on device performance of polymer cells with Al electrode and molecular cells with Ag electrode. Shown are representative current-voltage characteristics of: initial device, after 10 hour annealing, and after ALD process (includes 10 hour annealing). Polymer 1.0. - Molecular 1.0- ALD Inert 0.8- 0.8- *To 0.6. noALDlnert ...- M 0. - Z 0.4 - LD Ambient w a. 0.2- 0.0- .....-II.. SAmbe Z noALD, Ambient 0 200 400 0.4- a2. 0.2- 600 800 1000 1200 noALD, Ambient 0 Time (hours) 200 400 600 800 1000 1200 Time (hours) Figure 3-6: Effect of ALD encapsulation on lifetime of polymer cells and molecular cells, both with Al electrodes, stored in ambient environment or in inert environment. cells. Therefore, the annealing at 100'C for 10 hours slightly improves morphology of the organic active layers for device performance, [114,115] but either the effect of precursors during ALD counteracts whatever gains are caused by annealing, or the temperature of the devices during ALD or during annealing in inert atmosphere is not equal to the specified temperatures. In either case, the ALD process implemented here does not significantly affect the performance of the devices. 64 Effect of ALD on Device Shelflife Figure 3-6 shows the effect on shelflife of presence of encapsulation and exposure to ambient environment vs an inert environment of polymer cells and molecular cells with Al electrodes. Polymer cells with ALD encapsulation and stored in inert atmosphere have the same lifetime as the cells with no encapsulation and stored in inert atmosphere (11% decrease over 1200 hours), confirming that the ALD nanothin film is not a source of degradation. However, encapsulation does have a beneficial effect on shelflife of cells exposed to ambient atmosphere. Whereas polymer cells stored in ambient atmosphere with no encapsulation degrade to zero efficiency in less than 20 hours, ALD-encapsulated polymer cells retain >50% of its efficiency after 450 hours and continues to generate electrical power after 1200 hours. The molecular cell with ALD encapsulation shows negligible degradation due to ambient atmosphere exposure after 1150 hours. There is a small decrease in efficiency for molecular cells stored in inert atmosphere (whether encapsulated or unencapsulated) and for ALD-encapsulated molecular cells stored in ambient atmosphere after 1150 hours (8% vs. 13%). This demonstrates the effective encapsulation of ALD films, especially for molecular cells. 3.4 Conclusions III conclusion, our study indicates that Ag electrodes lead to shorting and significant decrease of device performance, regardless of atmospheric exposure, whereas Al electrodes lead to greater stability, for both polymeric and molecular cells. The ALD deposition process itself has negligible effect on device performance, although simply annealing at the same specifications slightly increases efficiency. Furthermore, we have shown that although device lifetime depends dramatically on the active materials choice as well as cathode choice, ALD nano-thin encapsulation is effective for organic solar cells of a variety of device architectures. Herein we demonstrated significant increases in shelf life (>50x) for polymer cells and molecular cells, and >1200 hours shelf life for molecular PVs stored in air due to a ianothin encapsulation film. 65 Part II Engineering Higher Efficiency Organic Photovoltaics 66 Chapter 4 Introduction to Nanostructures and Architectures Some of the greatest advances in nano-PV technology have been due to nanostructural engineering: Tang designed a cell with a exciton-dissociating interface within nanometers of the photoactive region. [17] Heeger et al designed a cell that further increased the surface area of this exciton-dissociating interface through a bulkheterojunction. [18] Matsuo et al designed a cell that kept a large exciton-dissociating interface while maintaining molecular order through nanopillars. [116] All of these nanostructural advances have brought the OPV field closer to the ideal 33%, as well as up to and beyond the supposed limit of commercial viability, 10%. Thus we can hope that further advances in nanostructuring will further push this technology to a status of serious impact on the world. This chapter provides a background on nanostructural engineering in OPVs. 4.1 Subcell Nanostructures 4.1.1 Bilayer/Planar (Tang) Cell One of the distinguishing features of small-molecule and polymer semiconductors is the presence of strongly bound excited states known as Frenkel excitons. These 67 b a C Gold Wire Conboct -BP -- n2O3 Cuft Gkos (Aor "'a Ligt ITO -PEDOT - - ITO MunWnOM wstate ---- glass 100 nm Figure 4-1: Historic Advances in Nanostructural Engineering of OPVs. a) The Tang cell (1985) introduced the photoactive interface on the nanoscale to achieve 1% PCE. [17] b) Heeger et al (1995) introduced the bulk heterojunction to achieve 1.5% PCE. [18] c) Matsuo et al (2009) fabricated a nanopillar structure that achieved 10.1% PCE. [116] excitons have significant impact on many of the processes in photovoltaic devices from photocurrent generation to characteristic absorption features. [117] For example, organic semiconductors typically exhibit static dielectric constants in the range of 25, [118] and accordingly, exhibit large exciton binding energies 0.2-0.8eV. To overcome this exciton binding energy, bilayer donor-acceptor architectures which have now become common to promote exciton separation to free carriers [17,119,120] as shown in Figure 4-2a. However, there still remains an inherent tradeoff between the absorption efficiency (a) and exciton diffusion efficiency (LD) to dissociating interfaces that results in thickness optima. The external quantum efficiency (EQE) can be described by constituent efficiencies as EQE = /AT/EDT/cTrlcc where TiA is the absorption efficiency, r/ED is the exciton diffusion efficiency, TICT is the charge- transfer or exciton dissociation efficiency, and r/cc is the charge collection efficiency. In the absence of optical interference, the absorption efficiency is, rjA = T(1 - exp(-ad)) (4.1) where T is the total transmission through the substrate and TCO to the active layer (typically limited to 75%), a is the absorption coefficient, and d is the active layer 68 In C 0.8 ----- 0.5 - 2 -100 0.6 3CP NCCEPTOR Uj wi A 0.41 = 100 -2 0.2 --00 - DONOR ITO Glass 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4 .0 dot Figure 4-2: Calculation of the external quantum efficiency (EQE) for donor-acceptor heterojunction as a function of aLo (change in line style) and aLD (change ini color), where LD is exciton diffusion length, a is absorption coefficient, and LC is carrier diffusion length, highlighting the exciton diffusion bottleneck. [5] thickness; the exciton diffusion efficiency is, d rlhD =CXP(- LD ) (4.2) offset; the charge transfer efficiency, qI-, is approximately 1 for a large donor-acceptor and the charge collection efficiency is, _ Lc d(1 - exp(- )) (4.3) where LC is the charge collection length. [5, 121, 122] This model for the EQE is plotted in Figure 4-2b as a function of ad for various values of aLj and aLc. Typical values for aLD are <<1 so that for planar structures, exciton diffusion is the limiting process. [117] 69 Figure 4-3: Left: Device structure of a planar heterojunction OPV. Right: Schematic showing the cross-section of the rrP3HT:PCBM BHJ device. Focused (c) and defocused (e) cross-sectional TEM images; inset: the magnified image of the rrP3HT:PCBM BHJ layer. [124] 4.1.2 Bulk Heterojunction and Planar-Mixed Heterojunction Bulk-heterojunction (BHJ) and planar-mixed heterojunction (PM-HJ) structures aim to decouple these two limiting efficiencies through the use of interpenetrating networks of donor and acceptor (shown in Figure 4-3), which enable the surface area of the dissociating interface to be dramatically increased. This manifests as an effective enhancement of the exciton diffusion length which, in turn, enables the optimal device thickness to be increased as shown in Figure ??. However, as the interdigitation of the donor-acceptor network increases the pathways for charge collection becomes hindered, which is also a common limitation even in planar structures where aGLc can be <<1. Indeed the mobility (p) of organic semiconductors is generally quite low 10- 7 101cm 2 /V - s. [123] Thus, there is a sensitive interplay between high photocharge generation and charge collection which requires careful morphology optimization. 4.1.3 Novel Nanostructures While solid state BHJ structures typically suffer from reduced carrier transport, [125 they nonetheless remain the highest performance solid-state solar cells to date. 70 Alternative approaches to simultaneously increase r/ED and T/cc include (1) long-range ordering which can increase both LD [126--128] and p [116,123,129] or (2) molecular design of highly absorptive materials reducing required thicknesses for high absorption efficiency. Most notable is the nanopillar architecture (Figure 4-1c) which in 2011 was the first OPV to surpass the 10% PCE mark and has recently been reported to produce a 11.1% PCE cell (the current world-record OPV cell). [7,116,129] 4.2 Multijunction Architecture Single junction solar cells are caught in a catch-22 of sorts: the larger the bandgap, the larger the Voc but the smaller the Jsc. The smaller the bandgap, the smaller the Voc but the larger the Jsc. This means that we can never quite utilize all of the energy of all the photons. One way around this is the multijunction architecture. (This architecture is also sometimes called "tandem" or "stacked".) A multifunction photovoltaic is comprised of two subcells in series (or in parallel). In this way, higher energy photons can be absorbed by a subcell with higher Voc, and lower energy photons are absorbed by a subcell with lower Voc. The first MJ-OPV was reported only a few years after the first SJ-OPV. [130] In this report they fabricated a lual-junction device with two of the same subeells stacked upon each other. The intention of this structure is simply to increase the amount of excitons dissociated, as the subcells were planar cells. The MJ device, however, exhibited significantly lower PCE than the SJ device (0.3% vs 1.0%) due to (1) an ineffective recombination zone and (2) unoptimized subcell thicknesses. With time the field moved to using complementary subcells [131] and empirical and computational optimization of subcell thicknesses. [132]. The current record holder MJ cell has a PCE of 10.6%. [7,133] 71 4.3 Nanostructural Engineering via Processing Thermal annealing of organic photovoltaics has been thoroughly studied in solutiondeposited organic films, to the effect of significant enhancements in OPV performance, however this technique has yet to be significantly implemented in vapor deposited materials systems. Herein we study the effect of thermal annealing on molecular thin films, covering multiple donor materials and nanostructures and devices comprising such. The nanostructure of OPVs is highly dependent on processing conditions. Through annealing the films, we enable the molecules to move towards and perhaps reach their most stable state. For most materials utilized in OPVs thus far, aggregation (longrange order) is the preferred state, which would thus lead to complete phase segregation. However the annealing is stopped before the material has reached equilibrium, trapping the photoactive film in a blend of aggregation leading to higher charge mobility but sufficiently close phase interfaces leading to effective exciton dissociation (see Figure 4-5). [114,115,134] This has been demonstrated in small-molecule mixed OPVs (see Figure 4-4) [65,135] and in polymer blends [115,136] to lead to significant enhancements in power conversion efficiency. However much research must be performed for each materials set to determine its ideal temperature and length of time for optimized PCE. Often the term "annealing" refers to thermal annealing, however that is not necessarily the case. Solvent annealing is also applicable to this field, and is used regularly in polymer blends through the use of low-boiling point solvents during deposition. [137] It has also been applied to fabrication of crystal needles of small molecules (see the next chapter), [138,139] and has only been sparsely experimented with in molecular OPVs. [140,141] Solvent annealing has the benefit of enabling the organic materials to move through unstable states into more stable states at low temperatures. Many substrates that are of interest to OPVs (particularly plastics) degrade quickly at high temperatures but are unaffected by solvent annealing. 72 100 0Tn 80 70 60 50 40 30 20 10 0 40 40 40 40 0 0 0 0 0 40 0 00 Figure 4-4: Effect of annealing on planar-mixed heterojunctions of CuPc-PTCBI. Top (a-d) shows SEM images and bottom (e-h) shows simulations of the morphology. Leftmost images are as deposited, images to right show increased aggregation due to increasing annealing temperatures. [65] 0 As Dep 7Q* '04 -6. -3 0 01 150.0: -10 0* 0.J nm 0.510 V Figure 4-5: Effect of annealing on bulk heterojunction polymer solar cells. Performance increases with annealing. SEM shows that this is due to increased phase separation of the polymers and fullerene materials. [115] 1.68110 Toluene Chlorobenzene Figure 4-6: Effect of solvent annealing with different solvents oil a polymer blend. [137] 73 74 Chapter 5 Practical Efficiency Limits of Organic Photovoltaics Five decades since Shockley and Queisser derived the power conversion efficiency limit of single-junction photovoltaic cells, researchers have still not demonstrated such high performance for any photovoltaic device system. [7] For example, the power con- version efficiency of the best single-crystal-Si single-junction PVs is q= 25% (without solar concentration), [7,142] which is only 76% of the SQ limit. Hence, in evaluating the achievable performance of a comparatively new PV technology, such as nano-PVs, it is prudent and necessary to inake an estimate of the upper limit of the achievable Herein we discuss the trends of the best demonstrations found in literature, and utilize this to determine the practical limits of nanomaterial-PVs. Further, we apply these trends to two standard material sets, to understand our expectations of their efficiency limits in single junction architecture as well as multijunction architecture. Using an optical model based on transfer-imatrix formalism [143], we can model the maximum Jsc accessible with the given materials set by varying the subcell thicknesses. We utilize this model to explore different nanostructures of these materials sets, namely: planar cells, ideal nanostructure cells, and tandem and mnultijunction cells. 75 5.1 Practical Limits Derived from Literature Here we report a numerical evaluation of trends of the best technical demonstrations. [5] Our literature survey of nano-PV technologies collects device data of the best experimentally reported performance in terms of EQE , FF , and VOC over the last two decades. From this data a semi-empirical estimate for the practical upper limit to the power conversion efficiency of nm-PVs is derived. The maximum demonstrated EQE across the spectrum is 75% with internal quantum efficiencies approaching 100%; the losses in EQE are due primarily to combined optical losses (~10% loss from transparent electrode absorption, ~5% reflection from substrate, and ~10% from internal reflections), which likely will be difficult to eliminate in a practical device structure. Assuming this maximum EQE of 75% at wavelengths extending to the band edge, upper limits of JSC are calculated as function of optical bandgap. Upper limits for the FF as a function of optical gap were similarly assumed to be that of the highest reported, i.e. FF = 0.75 across the spectrum. Deviations in FF from the SQ limit generally stem from a combination of large series resistance and low shunt resistance. While many empirical forms have been proposed for the functional form of VOC as a function of EG, [144, 145] it is found that maximum photovoltages follow a trend of reaching 80% of the value predicted by the SQ limit; the difference can be attributed to a number of recombination phenomena including internal conversion, interface recombination, and exciton binding losses as discussed below. Nonetheless, this threshold is consistent with the framework of the SQ limit. We combine the photo voltage trend with the limiting photocurrents and fillfactors to estimate the ultimate nanostructured efficiency limits as shown in Figure 51. We find that a semi-empirically derived maximum efficiency of 17% is achievable for a single-junction cell with a bandgap of approximately 1.1-1.4 eV. This maximum efficiency is lower than that reported in recent semi-theoretical studies in which practical considerations described above are not taken into account and which led to 76 CIAIPc DBP 30 - , - . - , - .- , - 25MJ 20 SJ W 15 10. 5- 0_ 0.75 - . 1.00 1.25 . 1.50 . . . 1.75 2.00 -. 2.25 2.50 Optical Bandgap (eV) Figure 5-1: Practical Limit PCE for a range of optical bandgaps. Black is for single junction architecture and purple is for multijunction architecture (plotted versus the top subcell bandgap). The bandgaps of DBP and CIAlPc are indicated. maximum exciton-limited efficiencies ranging from 2227%. [146] Further, Figure 5-1 also shows practical limits for dual-junction cells. We calculate a maximum efficiency of 24% for stacked, 2-cell, current-matched nanostructured tandems (compared to 43.4% predicted in the SQ limit [147,148]). 5.2 5.2.1 Computational Methods Materials Choice We study the DBP-C60 (DBC6) and ClAlPc-C60 (CAC6) subcells that are utilized throughout this thesis work. The single junction architecture is ITO/MoOx/subcell/BCP/Ag and the multijunction architecture is ITO/MoOx/subcell1/BCP/Ag*/MoOx/subcell2/BCP/Ag. These are standard materials sets and device architectures. Optical parameters have been derived from ellipsometry measurements of each of these materials. Exciton diffusion lengths (utilized in the modeling of the pla- nar architecture) are derived from EQE measurements of an array of active layer thicknesses. [149] 77 5.2.2 Planar Architecture Simply, we first computationally model the wavelength-resolved and spatiallyresolved optical intensity throughout the photoactive region of the device, via transfermatrix formalism. [143] Then we convolute this with the absorption spectra of the photoactive materials. For planar cells, any photons absorbed within an exciton diffusion length (which is experimentally determined) of the photoactive interface is assumed to contribute to the generated photocurrent. Here, we model the generated photocurrent for an array of total active layer thicknesses, assuming the ratio between donor and acceptor remains constant. 5.2.3 Ideal Nanostructured Architecture Herein we do not make any assumptions of what the ideal nanostructure would be except what is necessary for the model: (1) that both the donor and acceptor will be uniformly distributed throughout the thickness of the active layer, and (2) that every photon absorbed by the active layer will generate a photo charge that is collected by' the electrode. With these assumptions and the same materials optical properties and other device layers as selected above, we model the maximum Jsc. 5.2.4 Multijunction Architecture Building upon above, we simply add more layers to the device that is optically modeled as well as a second exciton dissociation interface. Note that, within our optical model, two "Jsc"s are generated: one for each subcell. For the sake of determining practical limits, we take the lowest subcell Jsc as the MJ Jsc, however we note that this is simply to acquire a general value. In chapters below, we will discuss the relationship between subcell Jsc and actual PCE. 78 20 18 160 1 CIAIPc-C60 - -' S 10. E . IQE =100% - -- -. DBP-C60 /- S6. 4 0 5; 2 50 10 10 20 Planar 25 30 160 1 50 200 250 300 Total Active Layer Thickness [nm ] Figure 5-2: Modeled Jsc for DBP-C60 and C1AlPc-C60 cells with either planar and ideal nanostructure. 5.3 5.3.1 Results and Discussion Single Junction: Planar Architecture We find DBC6 Planar to generate Jsc =6mA/cm2 and CAC6 Planar to generate Jsc= 10mA/cm2. Even though DBC6 has a longer exciton diffusion length and higher peak absorption coefficient, CAC6 has a lower optical bandgap (1.7eV vs 2.0eV) and thus is able to absorb a larger proportion of the solar spectrum. If we combine these Jsc's with best demonstrated FF and Voc of each materials set (FF= 0.55 and 0.75, and Voc= 0.74 and 0.92, respectively), we get a practical limit PCE of 4.1% for planar architectures of both CAC6 and DBC6. Interestingly, this has been experimentally attained for DBC6 but not for CAC6. [149] However it is clear that planar devices are limited by their exciton diffusion lengths. The active materials could absorb more light, but these extra excitons would be wasted because they are too distant from the photoactive interface to be converted to free photocharges. This limitation can be obviated through nano-structuring of the active layer. 79 7- MJ Planar SMJ BHJ 6- -Planar 2 1 -- BHJ 5- w 4- 5 BHJ: 70% inc Planar: DJ: 8% inc TJ: 10% inc PJ: 19% inc 3" 1 "2 321 0 500 1000 1500 2000 2500 3000 Total D+A thickness Figure 5-3: Calculated PCE of planar and ideal nanostructure single junctions (lines) and planar and ideal nanostructure tandems (squares) for DBP-C60 with current demonstrations of FF and Voc. 5.3.2 Single Junction: Ideal Nanostructured Architecture As discussed above, the "Ideal" nanostructure simply assumes that all excitons generated collected carriers. DBC6 Ideal generates Jsc = 11mA/cm2 and CAC6 ideal generates Jsc=19 mA/cm2. We find that Jsc is increased by 70% and 90%, respectively, over the maximal modeled planar cells of DBC6 and CAC6, respectively. If somehow the "ideal" nanostructure exhibited the empirical best FF and Voc rather than decaying (which has never been reported before, but we are imagining an ideal device), we get PCE of 7.6% and 7.3% for DBC6 and CAC6, respectively. These are on par with the highest bulk heterojunction device efficiencies currently demonstrated, but still fall short of the goal of 10% which is highly lauded for commercialization. Further, we apply the practical limit trends derived from literature: setting FF=0.75 (the highest reported, which is equal to that demonstrated for DBP-C60) and Voc equal to 80% of the SQ limit. The parameters derived from this are shown in Table 5.1. This leads to practical limit PCE values of 11% and 16% for DBC6 and CAC6 materials sets, respectively. The bandgap of ClAlPe, 1.7 eV, is closer to the ideal bandgap of 1.1eV to 1.4eV, leading to a significantly higher practical limit. [5] 80 Table 5.1: Current and Practical Limit Performance Parameters for SJ-OPVs of DBP-C60 and ClAlPc-C60 Jsc [mA/cm'] Voc [V] FF [frac] PCE [%] DBC6 Current DBC6 Practical Limit DBC6 Potential Gain 6.2 11 77% 0.70 0.75 6% 0.92 1.35 47% 4.0% 11.1% 178% CAC6 Current CAC6 Practical Limit CAC6 Potential Gain 7.1 19 167 0.51 0.75 47% 0.78 1.13 44% 2.8% 16.1% 475% In conclusion, realistic PCE increases of 70-90% can be achieved with these specific niaterials sets if the exciton diffusion length can be overcome via nano-structuring, and further PCE increases of up to 500% can be imagined if all PV parameters are enhanced to the practical limit. 5.3.3 Tandem Cells (with the Same Subcells) We further examine another approach to overcone the exciton diffusion limit: tandem cells. Tandem cells are a series of optically thin cells on top of each other. This increases the photoactive interface by adding one on top of the other, but this doesn't increase Jsc since the current of every subeell niust equal. Rather, the voltages add, so you get an increase in Voc. This can be useful in applications where high voltage is needed, such as water-splitting. [150] We model the maximal Jsc of tandemns for 2-, 3- and 5-junctions comprised of planar subcells, and we further calculate the maximal PCE by taking this Jsc and multiplying it by the empirical best FF and Voc and the number of junctions. We see that this tandem approach can lead to moderate improvements in PCE of approxiiately 20% over the planar single-junction architecture. Finally, we examine the approach of tandems comprised of "ideal rianostructure" subcells. This only serves to decrease PCE, according to our model, because of need of balancing the currents. If we were more thorough in the thickness intervals chosen for modeling, we should find that the PCE will niatch exactly that of the single junction, 81 but for this study we have chosen fairly big jumps in thickness (10nm) for the sake of computational time efficiency. 5.3.4 Multijunction Cells (with Different Subcells) In the following chapters we discuss the engineering and optimization of MJ cells, which achieve PCE of 5.5% utilizing these two materials sets. Ultimately, however we find that this structure is limited by the comprising subcells. If we calculate the MJOPV performance utilizing the practical limit subcells discussed above, we see that PCE could rise to 17.7%. This assumes current matching as well as implementation of the conventional subcell order. Note that the inverted subcell order discussed in the following chapters is beneficial only in MJ cells where the subcells are sub-100nm thickness. Table 5.2: Current and Practical Limit Performance DBP-C60 and ClAlPc-C60 Voc Jsc 2 [mA/cm ] [V] Current 4.9 0.68 Practical Limit 9.5 0.75 Potential Gain 94% 10% 5.4 Parameters for MJ-OPVs of FF PCE [frac] [%] 1.65 2.48 50% 5.5% 17.7% 222% Conclusions In conclusion: nanostructuring of these standard donor-acceptor materials sets could potentially double PCE, if only we can increase exciton dissociation efficiency while not decreasing the carrier collection efficiency nor increasing the series resistance. This would lead to PCE of 7-8% with the materials sets utilized in this thesis. If we could also achieve enhanced FF and Voc up to the practical limit for OPVs, we could see efficiencies up to 16% with materials sets utilized in this thesis. Furthermore, if combined in the multijunction architecture (as discussed below) PCE of up to 17.7% could be achieved. 82 Chapter 6 Materials and Architecture Design in Sub-100nm Multijunction Photovoltaics Organic photovoltaics (OPVs) have generated much interest due to their potential as flexible, semi-transparent solar cells. However low power conversion efficiency has A major limiting factor is the trade-off thus far limited their connercialization. between photon absorption and conversion to current and photon energy conversion to voltage, which can be manipulated by the choice of donor and acceptor energy levels. This trade-off can be minimized through implementation of a mnultijunction (MJ) architecture, [5, 147] in which multiple subcells of differing optical band gaps lower thermal losses. Organic semiconductors uniquely demonstrate structured absorption spectra, which enables MJ-OPVs in which donor materials are transparent to each other. [?, 151] This minimizes competitive absorption between subcells and enables facile optical device optimization. [152,153] Power conversion efficiencies up to 10.6% have now been reported for MJ-OPVs comprising complementary donor materials. [133] Herein [149] we present optical and electrical optimization of an MJ-OPV incorporating a near-infrared-absorbing visibly-transparent phthalocyaine-based donor (ClAlPc) and a complementary visible-absorbing perylene-based donor (DBP) (Fig- 83 2.0 *2 DBP CIAIPc IV 1.5 0 o 1.0 .: 0.51C 0.0 0 400 500 600 700 800 900 Wavelength ( nm ) Figure 6-1: Absorption spectra of C60 (green), DBP (blue) and ClAlPc (red) thin films, showing broad spectral response. Molecular structures are inset. ure 1). [100, 122,154] The two donor materials are transparent to one another, enabling the positioning of the narrower band-gap cell in front of the wider band-gap subcell in order to optimize optical absorption within the weak optical microcavity of the nanoscale PV. [152,153] The subcell thicknesses were computationally optimized for maximum generated photocurrent using T-matrix formalism. These subcells were connected with a variety of recombination zone (RZ) architectures to optimize subcell current recombination and thus minimize charge build-up and voltage loss. Optimization of the structure of the MJ cells leads to open-circuit voltage equal to near perfect summation of the subcell open-circuit voltages (1.65±0.02V), near maintenance of the high fill factor of the perylene-based subcell (0.685±0.002), broad spectral response (in the wavelength range of 350nm to 850nm), and OPV power conversion efficiencies of 5.5±0.2%. 6.1 Experimental Methods The MJ cells are fabricated monolithically entirely by vapor deposition and incorporate chloroaluminum phthalocyanine (ClAlPc) as a near-infrared-absorbing visiblytransparent donor and tetraphenyldibenzoperiflanthene (DBP) as a visible-absorbing 84 SC ITO MoOx CIAIPc-C60 3.2 RZ BCP Ag MoOx SC2 DBP-C60 3.5 4.0 BCP Ag 3.5 4.3 4.3 g4.8 .4m- 5.4 4.9 5.4 IRO... lease 6.5 6.5 Figure 6-2: Energy levels of each component layer of the multijunction cells. RZ BCP ITO| Glass Figure 6-3: Device cross-section of the mnultij unction cells. Thicknesses not to scale. 85 donor, with buckminsterfullerene (C6 0 ) as a wide bandgap acceptor in both subcells. The photovoltaic devices are fabricated via vacuum thermal evaporation on solvent cleaned, pre-patterned ITO-coated glass (Thin Film Devices, 20 Q/E). Prior to device growth, ClAlPc (TCI, C1167) and C 60 (Aldrich, sublimed 99.9%) are purified once by vacuum train sublimation, while DBP (Lumtec, LT-N4003), BCP (Lumtec, LT-E304), MoOx (Alfa, 99.9995%), and Ag (Alfa-Aesar, Premion 11357 99.9999%) are used as purchased. The subcell and RZ layers are blanket deposited, while the top Ag electrode is patterned via shadow masking in stripes orthogonal to the bottom ITO electrode to generate a device area of 0.0121 cm 2 . Each subcell and each RZ are fabricated without breaking high-vacuum (<10-- Torr), and all fabrication transfer and characterization is performed in the controlled environment of N2 -filled gloveboxes. The multijunction (MJ) cells structure consists of glass/ITO 150nm/MoOx 20nm/ (subcelli) / (RZ) / (subcell2) /BCP 6.5nm/Ag 1100nm. Single junction (SJ) cells with structure glass/ITO 150nm/MoOx 20nm/ (subcell) /BCP 6.5nm/Ag 1100nm are fabricated in parallel with MJ cells in order to characterize the opto-electrical response of individual subcells. A planar-mixed heterojunction of ClAlPc and C6 ocomprises subcell 1 (SCI) and a planar heterojunction of DBP and C60 comprises subcell 2 (SC2). The optimal SJ configuration (highest rqp in a SJ architecture) of subcelli (SC1) is ClAlPc 10nm/ClAlPc:C60 (1:1 ratio) 10nm/C 6 o20nm, and the SC1 in an optimal MJ cell consists of ClAlPc 11.4nm/ClAlPc:C 60 (1:1 ratio) 7.2nm/C 60 9.6nm. The optimal SJ configuration of subcell2 (SC2) is DBP 20nm/C 6 o40nm, and the SC2 in an optimal MJ cell is DBP 20nm/C 60 23.2nm. Film thicknesses are measured during film growth using a quartz-crystal monitor pre-calibrated by thin film measurement with a profiler (KLA Tencor, P-16+), leading to a film thickness error of <1nm. Current density-voltage characteristics are measured under dark conditions and under 1 sun illumination (100mW/cm 2. AM 1.5G), using a 150W solar simulator (Newport, 6255) illuminated through a AM1.5G filter (Newport, 81094) calibrated with an NREL-certified monocrystalline-Si photodiode (Newport, 91150V). Results 86 are not corrected for spectral mismatch. Electrical characteristics are measured with a picoammeter (Keithley, 6487) employing a switch mainframe (Keithley, 7001) for switching between cells. The external quantum efficiency (EQE) is measured with AC monochromatic light and DC light bias (Figure 6-4). For MJ cells, the measured photocurrent is equivalent to the response of the current-limiting subcell, thus the DC illumination wavelengths and intensities are selected such that the designated subcell is under isun conditions and the other subcell is over-illuminated so that its photocurrent is limited by the designated sub-cell. [155,156] The two subcells are complementary light absorbers (i.e. with limited absorption spectrum overlap) resulting in a distinct span of the excitation wavelengths for each subcell. The EQE shown here was taken while illuminating with AC monochromatic light signals scanned from wavelength A=350nm to 900nm at 2mW and 353Hz (using Oriel, 100W Xe arc lamp, 66921 and Princeton Instruments, SpectraPro 300i with a light chopper) and DC solar simulation light bias at 100 mW/cm 2 (Newport, 6255) and DC monochromatic light bias of A=532nm (absorbed predominately by DBP) at 50mW, CW (Extreme Lasers, GHQ-50 x1). The AC light intensity is calibrated with NREL-certified Si photodiode (Newport, 818-UV). Electrical characteristics are measured with a lock-in amplifier (Stanford Research Systems, SR830) employing a switch mainframe (Keithley, 7001) for switching between devices. We apply T-mnatrix formalism to model the wavelength-resolved optical field intensities within the full MJ cell structure and from these solve the ID exciton diffusion equations to calculate short-circuit currents as a function of layer configurations. [143] The optical properties of each material are measured via spectroscopic ellipsomnetry (J. A. Woollam, M-2000S). Ideal dissociation and charge collection efficiencies are assumed and exciton diffusion lengths are extracted from fitting single junction EQE thickness dependencies. Numerical optimization of tandem structures is performed by calculating the MJ photoresponse for cells over a series of SCI and SC2 donor and acceptor thicknesses (4 variables). 87 W Lamp Cho per Monochromator La sers 78 n 532nm Solar Si 4 ND Filter I- I I Figure 6-4: Schematic of the set up for external quantum efficiency measurement. 88 5.0 E 2.5 SJ 1SJ2 E -- MJ +-- 110.0 - -5.0 -7 -0.5 0.0 0.5 1.0 1.5 2.0 Voltage ( V ) Figure 6-5: Representative current density-voltage characteristics of MJ (green), SJ1 (red) and SJ2 (blue). Solid curves are taken under isun illumination (AM1.5G), and dashed curves are taken in (lark. Shown SJ1 and SJ2 were fabricated in parallel with the subcells of shown MJ. 6.2 Characteristics of Optimized Device Figure 6-5 shows the current density-voltage characteristics of the optimal MJ cell and SJ cells fabricated in parallel with the subcells of the shown MJ under dark conditions and under illumination of simulated solar spectrum (100 mW/cm 2 , AM1.5G, not corrected for spectral mismatch). The (Voc of the MJ cell (1.65±0.02 V) is equal to the sum of those of the SJ cells (1.64±0.01 V), and the FF (0.685±0.002) is within error of the average of those of the SJ cells (0.65±0.02). The Jsc 4.9±0.3 mA/cm 2 ) demonstrates the minimal loss of photocurrent, consistent with the coinplementary absorption of the subcells. The highest qp of SCI and SC2 are 2.8±0.1% and 4.0±0.1%, respectively, and the highest qp of the MJ cell is 5.5±0.2%. Figure 6-6 shows wavelength-resolved external quantum and efficiency (EQE) of a MJ cell with similar subcell thicknesses thicker RZ as the empirically optimized structure. The measured photocurrent is due to the photoresponse of the current-linmiting subcell, thus a subcell can be selected for EQE measurement via properly chosen optical bias. SCI (red) and SC2 (blue) were selected via optical bias of A=532nm 89 3 35-8 SCI 530 SC2 S25 E ** +:15e CV h 10 X 0 W 400 500 600 700 800 900 Wavelength ( nm ) Figure 6-6: Wavelength-resolved external quantum efficiency of SC1 (red) and SC2 (blue) selected via optical bias (A=532nm laser, 50mW; and AM 1.5G simulation, 100 mW/cm 2 ; respectively). 2 laser, 50mW; and simulated AM 1.5G, 100 mW/cm ; respectively; such that the selected subcell generates a photocurrent within an order of magnitude of the measured photocurJsc under 1sun and the deselected subcell generates a significantly larger rent. With application of the optical model described above, we calculate that under A=532nm laser illumination SC2 generates 412% more photocharges than SCI and under simulated AM1.5G illumination SC1 generates 28% more photocharges than SC2. Through varying optical bias intensity and spectra, we find that this level of photocharge generation unbalance is sufficient to clearly select SC2 for EQE measurement (data not shown). The EQE spectrum of SC1 corresponds to the optical absorption spectrum of ClAlPc thin film (over the spectral range A=600nm-850nm) with a small response corresponding to C60 film (A <500nm), and the EQE spectrum of SC2 corresponds to a summation of the optical absorption spectrums of C60 (A <500nm) and DBP (A=500nm-650nm). Comparison of the SJ and MJ cell current density-voltage characteristics demonstrates effective opto-electrical optimization of the MJ cell structure. The MJ cell 90 ,t/p is 5.5±0.2%, a nearly 40% improvement over the most efficient SJ cell made with these materials. The minimal loss of V oc from the two subeells confirms the efficient operation of the RZ. The similarity of the Jsc of the SJ cell and MJ cell as well as the spectral response of the MJ subcells shown in Figure 2b demonstrate the complementary absorption of the subcells and the broad utilization of the solar spectrum from A=350nm to A=850nm. Integrating the EQE spectra of each subeell with the AM1.5G spectrum gives a generated Jsc for SCI of 3.6+0.4 mA/cm [5] and for SC2 of 3.2±0.3 mA/cm2 , as compared to the measured MJ cell Jsc of 3.9+0.2 mA/cm2 . Both integrated subcell Jsc are low by 10-20%, possibly due to spectral aberration of the calibration spectrum and/or of the solar simulated illumination. It is expected that if each subcell peak EQE was increased from the present 25±5% to 70%, a 2 practical limit already achieved in the best OPVs, then the Jsc and rpwould be additionally enhanced up to three-fold, suggesting a practically-achievable potential r/p of >10% with these organic materials and the MJ device architecture. 6.3 Recombination Zone Development A key component in advancing from fabrication of single junction cells to multijunction cells is the selection and deposition of an efficient recombination zone. Figure 6-7 shows the dependence of MJ cell performance on the recombination zone (RZ) composition and layer thicknesses. Figure 6-7a compares the i-V charac- teristics under 1 sun of MJ cells with either no RZ (i.e. SCI in direct contact with SC2) or RZ compositions of: Ag 0.5mn/BCP 5nn/MoOx 5nm, or BCP 5mn/Ag 0.5nrn/MoOx 5nm. Comparing the MJ cell with no RZ and the MJ cell with the full RZ, the FF increases by 40% (from 0.40±0.002 to 0.56±0.002) and the T/p increases by 160% (from 1.9±0.2% to 5.0±0.2%). MJ cells fabricated without aiy recombination zone or with just BCP/MoOx or just Ag nanoclusters exhibit S-shaped current density characteristics, suggesting a build-up of space-charge [157] due to inefficient recombination of subcell currents of opposing charge. However the complete 3-layer RZ (BCP/Ag/MoOx) has clear 91 Ag thickness ( nm) 0.6 f"---no RZ 4- ...Ag nanoclusters BCP/MoOx -Full RZ: BCP/Ag/MoOx / 2 -- 2.0 1.5 1.0 0.5 0.64 3.2 0.62 3.0 0.60 C 0. 0.58- -2- LL0.56 0.54 . C-) C 2.8 o 0--. 2.6 0 -2.40 0.52 -6 -1.0 a 0.50 -0.5 0.0 0.5 1.0 1.5 2.0 2 3 4 5 6 7 8 9 2.2 1lul BCP, MoOx Thickness ( nm) Voltage ( V ) Figure 6-7: (Left) Current Density-Voltage characteristics of MJ cells with either no RZ (dash-dot) or RZ of: Ag 0.5nm (short dash), BCP 5nm/MoOx 5nm (long dash), BCP 5nm/Ag 0.5nm/MoOx 5nm (solid). (Right) Fill factor of MJ cells with BCP x nm/Ag 0.5nm/MoOx 5nm (solid circles) or BCP 5nm/Ag 0.5nm/MoOx x nm (open circles) as the RZ. And short-circuit current of MJ cells with BCP x nm/Ag 0.5nm/MoOx 5nm (squares) as the R.Z . Measurements were performed under 100 mW/cm2, AM1.5G. rectification, resulting in high FF and Voc. The RZ can be further optimized by tuning each layer thickness. In Figure 67b, the thickness of each layer of the RZ was varied while keeping all other layers constant. Solid circles correspond to BCP x nm/Ag 0.5nm/MoOx 5nm, open circles correspond to BCP 5nm/Ag 0.5nm/MoOx x nm, and squares correspond to BCP 5nm/Ag x nm/MoOx 5nm. By increasing the BCP and MoOx thicknesses from 5nm to 7.5nm and 5nm to 10nm, respectively, the FF decreases by 5% and 11%, respectively. By increasing the Ag thickness, the J sc decreases by 22%. Other photovoltaic parameters were negligibly affected. For BCP and MoOx film thicknesses >5nm, the FF is sub-optimal. Since BCP and MoOx are semiconducting thin films, the series resistance of the cell increases with the thickness of either layer, consequently decreasing FF while maintaining a high Voc. Furthermore, Jsc decreases with increasing Ag thickness. This is due to the non-negligible absorption of Ag nanoclusters, decreasing the optical intensity in the subcells. Due to these effects, the optimized RZ is BCP 2.5nm/Ag 0.5nm/MoOx 2.5nm and is used in devices throughout this work unless otherwise indicated. 92 1.6- TO . . . Aq 1.4~ 1.2 1.0- 1. 85nm 530nm L.8 -0.6- 0.4- 0 50 100 150 200 250 300 Position (nm ) Figure 6-8: Optical fields for wavelengths absorbed by SCI (A=785nm) and SC2 (A=530nm) within the MJ cell modeled via T-matrix formalism. 6.4 Optical Optimization of Sub-100nm Subcells Figure 6-8 shows the calculated optical field distribution within the empiricallyoptimized MJ cell for two wavelengths (A=530nm, absorbed primarily by DBP, and A=785nm, absorbed only by ClAlPc). The optical interference due to the reflective top electrode and the nanoscale-thickness of the MJ cell is evident in the spatially- oscillating optical intensity. The optical intensity of A=785nm light (which is primarily absorbed by the ClAlPc film) peaks farther from the reflective electrode than A=530nm light (which is primarily absorbed by the DBP film). This suggests that a greater photocurrent would be generated if the NIR-absorbing subcell (SC1) is placed further from the reflective electrode than the visible-absorbing subcell (SC2) (see modeled EQE shown in Figure 6-10.). This is contrary to tandem stacking of typical inorganic or organic solar cells where the largest bandgap sub-cell must be positioned closest to the incident light [143,147] for best MJ performance. However the structured absorption spectrum of our NIR cell (SCI) which has minimal absorption of visible light, enables us to place the SC1 in front of SC2 and optimize our MJ design for the peaks in the optical fields of different colors of light. Modeled EQE of devices either conventional or inverted structure is shown below. 93 Inverted MJ structure: Small bandgap in front Conventional MJ structure: large bandgap in front BCP RZ BCP ITO Glass ITO Glass Enabled by complementary absorption Figure 6-9: Architectures of conventional and inverted subcell order. Thicknesses not to scale. We calculate that a Jsc enhancement of 20% can be achieved by inverting the subcell order. Indeed, experimental data confirms this enhancement, as shown in figure 6-10. For series-connected MJ cells, an equal current density must flow through both of the subcells, which leads to a dependence of the overall photovoltaic performance on the relative photocurrent generated in each subcell. Therefore the photocurrent generation of each subcell was modeled for a range of subcell donor:acceptor thickness ratios and total thicknesses. By numerically varying the four free variables, we find the modeled-maximum-Jsc for MJ structure with SC1: ClAlPc 9.5nm/ClAlPc:C6 o6nm/C 6o 8nm and SC2: DBP 25nm/C 6o29nm, which closely matches the empirically optimized structure, SCI: ClAlPc 11.4nm/ClAlPc:C 6o 7.2nm/C 60 9.6nm and SC2: DBP 20nm/C 60 23.2nm. Figure 4b shows the calculated Jsc for an array of SCI and SC2 total thicknesses varying from 19nm to 28nm and from 43nm to 65nm, respectively, and with donor:acceptor thickness ratios restrained to those of the modeled-maximum-Jsc MJ cell. The overlaid text is the empirical data of MJ cells fabricated with the designated pair of subcell thicknesses. Over this range, the simulated Jsc are within error of the experimental Jsc. Additionally, the trend of the simulated Jsc closely follows 94 1.0 L) 0.8 04 E E 0.6 Ej Inverted MJ - - Conventional MJ ai) w E 0 2- 0 SC1 SC2 0.4 C 5 II C / -2 -3 -- Conventional MJ l,=2.9% 0 0.2 Inverted MJ U (D 0.0 wr 400 500 600 700 800 -5-0.5 900 0.0 0.5 3,=3.3% 1.0 1.5 2.0 Voltage ( V) Wavelength (nm) Figure 6-10: (Left) Modeled external quantum efficiency and (right) experimental current density-voltage characteristics of conventional and inverted subcell order. 64 62 48*0.2 5.3± E 60 C 58 O56 42 5.6±0.2 5.5*0.2 5.4d .r 52 F- C%4 50 ( 48 ~46 44 ± 4 4.9±0.2 4 20 22 18 a -- .9: 24 _T I 26 28 Subcell1 Thickness ( nm ) Figure 6-11: Simulated short-circuit currents for an array of thicknesses of subcell 1 and 2 with fixed donor-acceptor ratios. Overlaid is text of experimental JSC for nine samples corresponding to the thicknesses specified by their position. Experimental Jsc error is ±0.3 mA/cm 2 and thickness error is ±1nm. 95 that of the experimental Jsc, confirming the model's validity when used for optical optimization. 6.5 Conclusions In conclusion, we demonstrated a multijunction cell with Tp of 5.5±0.2% by incorporating near-infrared-absorbing visibly-transparent ClAlPc and visible-absorbing DBP, with all layers fabricated via vapor deposition. These devices are enabled by an efficient hybrid tunnel junction RZ and optimized optically for maximum photocurrent generation. The MJ cells shown here are ultimately limited by the low EQEs of the component subcells (of between 20% and 30%), thus further enhancement of subcell EQE to practical limits [5] (e.g. EQE between 70% and 80%) could lead to OPVs with Tp of > 10%. Multijunction architectures are an important approach to reduce thermal losses and improve overall efficiencies of PVs composed of nanostructured and organic materials and will likely be important to their commercial viability. 96 Chapter 7 Subcell Photocurrent Balance in Multijunction Photovoltaics 7.1 Introduction Multijunction (MJ) cells are a key approach to enhancing photovoltaic power conversion efficiency, surpassing the Shockley-Queisser limit and potentially advanc- ing OPVs into the range of commercial viability. [5, 24, 147, 158] There has been much work in the field regarding this architecture, primarily focusing on rmaterials selection and architecture optimization to maximize short circuit current (Jsc). [133,143,149, 151-153, 159] However, there has been little discussion on utilizing the imbalance of subcell photocurrents for efficiency optimization. Recently, Forrest et al reported analytical calculations of MJ organic photovoltaic (OPV) device parameters and their dependence on the ratio of subcell photocurrents. [160] They conclude that for MJ cells made with subcells with very similar fill factors (FF) power generation is maximized when subcell photocurrents are balanced, confirming popular thought. But for MJ cells with subcells with very dissimilar FFs, power generation can be max- imized when the higher-FF subcell is slightly current-limiting. Most MJ-OPV reports thus far have utilized subcells with similar FF, and thus where subcell balance has been explored, the most balanced device architecture was found to be optimized. [133] However there has not yet been a report of an MJ-OPV architecture that exhibits 97 (a) 7 (a) 8 7 6 6 .. - -Sub-cell ... ..... 3 2 (b) 2 (b) 7 6 5 0 0 Balanced Z3 I 0 5. ...... 4......... .............. (C) 2 5. 3 iL oss 5 Least Loss 53 2 Least A ..... FF .. -Tandem Dissimilar... --- sub-cell I -- 8 7. Tandem B Sub-coll I Sub-cell 2 %. (c) 46 I SCI 0 :10 gre -An=9.0% Z3 . -0.5 0.0 52 0.5 1.0 1.5 -1.0 2.0 Applied bas (V) -0.5 0:0 0.5 1.0 Applied bias (V) 1.5 2.0 Figure 7-1: Theoretical dependence of PCE loss on subcell balance for MJs with similar FF subcells and dissimilar FF subcells. [160] maximum efficiency when the subcells are imbalanced. Herein we present an MJ-OPV architecture comprising subcells with dissimilar FFs, for which the maximum reported PCE cell is comprised of imbalanced subcells. For this materials set, we report that FF gain from subcell imbalance dominates over Jsc loss, and the highest Jsc cell is not the highest PCE cell. Further, we introduce a highly accessible technique to determine subcell photocurrent balance simply from the reconstruction of 3-V curves of the MJ device from representative SJ devices. Finally we simulate this specific MJ architecture under a broad range of subcell photocurrent balances to further explore the dependence of Jsc, FF and PCE on subcell photocurrent balance. 7.2 Experimental Methods The subcells in this report are: (subcell 1) CIAlPc/ClAlPc:C60/C60, and (subcell 2) DBP/C60. The bottom contact is ITO/MoOx, the top contact is BCP/Ag, and the recombination zone is BCP/Ag*/MoOx. The contacts and recombination zone 98 are kept constant throughout this work. Single junction (SJ) architectures are also fabricated in parallel with the MJ subcells, with the same bottom and top contacts as the MJ cell. Current-voltage characteristics are performed under AM1.5G 1 sun, not corrected for spectral mismatch. A more in depth description of the materials and methods are described elsewhere. [149] 7.3 7.3.1 Calculation and Simulation Subcell Photocurrent Fitting Subcell photocurrents for each MJ cell were determined by utilizing two fitting parameters while re-constructing the MJ current-voltage (JV) curve from the two SJ curves. The method of constructing an MJ JV curve from two SJ curves is proposed and described elsewhere. [156,161] Briefly: for two subeells in series, the current going through each of the subcells must be equal, i.e., JAI = JcI = Jsc2 (7.1) Furthermore, the voltage across the entire MJ cell equals the sui of the voltage across each subeell, i.e. VAIJ = Vsc1 + VsC 2 (7.2) Therefore, at any given current magnitude, we add the voltages of each subcell, and that voltage sum is equivalent to the voltage of the MJ cell at that current magnitude. The photocurrents (i.e., effective short circuit currents) for the two subcells are used as fitting parameters for matching the constructed MJ curve to the empirical MJ curve. 7.3.2 Subcell Photocurrent Balance After identifying each of the subcell photocurrents within the MJ cell, we then quantify their balance within the MJ cell with a parameter identified as subcell pho99 RsI lPr2 R=10 Ohm SC2 D2 12 ls=8e-16A N=1.2 VI=1.2 V Rshl R=2000 Ohm Rs R=11 Ohm V1 P 11 i=z 4' Ash R=550 Ohm U=Uce DI Is=6e-1OA ZSN=1.8 vj=o.e v Figure 7-2: Circuit diagram for the MJ-OPV model. tocurrent balance, SPB, which equals the difference between the two subcell photocurrents divided by the sum of the two subeell photocurrents: SPB = 7.3.3 ± SF2 SP1 + SP2 (7.3) Circuit Simulations We simulate our MJ-OPV circuit via the Quite-Universal Circuit Simulator. [162, 163] The MJ-OPV is modeled as two SJ-OPVs in series. Each SJ-OPV has a series resistance in parallel with a diode, a DC current source, and a shunt resistance. The diode characteristics and shunt resistance are varied to match each of the fabricated subcells in single junction architecture. The recombination zone is not considered as a separate component, since it has been confirmed as a lossless interconnection. [149] The circuit structure and its parameters are reported in Figure 7-2. Current-Voltage characteristics of fabricated SJ cells and simulated SJ cells are compared in Figure 7-3. 100 Experimental & Simulated 0 E.. -1 L - E -2(D) -3E3 - --S ' -4- - (0 -5SC2- -6-7-0.5 1.0 0.5 0.0 Voltage [ V ] Figure 7-3: Experimental (solid lines) and simulated (dashed) current density-voltage characteristics of single junction devices comprising SCI (red) and SC2 (blue). N 42-I E 0 / - -2. SJ1 U) -4-3% SJ2 -6-8 -10- -0.5 0.0 0.5 1.0 1.5 Voltage (V) Figure 7-4: Current Density-Voltage Characteristics of single junction cells with the SC1 and SC2. 7.4 7.4.1 Results Subcells with Dissimilar Fill Factors We utilize two subcells with complementary absorption and dissimilar FF. [149] SCI has FF of approximately 0.55 and SC2 has FF of approximately 0.73. Over a thickness range of ± 20% of the optically modeled-optimal MJ cell, the FF of SC1 and SC2 in the SJ architecture vary by only 3±1% and 5±3%, respectively. This data is reported in Table 7.1. 101 Table 7.1: Pe rformance parameters for SJ-OPVs of varying SCI and SC 2 thicknesses. SC T SC2 T Jsc Voc FF PCE 2 [%] [V] [frac] [mA/cm ] [nm] [nm] 18.9 - 3.4 0.66 0.54 1.2 23.5 28.2 - - 4.1 4.9 5.8 6.4 6.4 0.71 0.74 0.91 0.92 0.92 0.55 0.55 0.75 0.73 0.71 1.6 2.0 3.9 4.3 4.2 43.2 54.0 64.8 Table 7.2: Performance parameters for MJ-OPVs of varying SCI and SC2 thicknesses. Fitted photocurrents and calculated SPB are included. SC1 T SC2 T SPi SP2 SPB Jsc Voc FF PCE 2 2 2 [%] [V] [frac] ] [mA/cm [mA/cm ] [mA/cm ] [nm] [nm] 18.9 43.2 5.3 5.3 0.00 5.3 1.56 0.63 5.2 18.9 54.0 4.9 6.3 -0.13 5.8 1.61 0.56 5.2 18.9 64.8 4.4 5.4 -0.10 5.1 1.59 0.57 4.6 23.5 43.2 5.6 5.0 +0.06 5.1 1.63 0.67 5.6 23.5 54.0 5.55 5.7 -0.01 5.7 1.65 0.60 5.7 23.5 64.8 4.9 6.1 -0.11 5.7 1.65 0.55 5.2 28.2 43.2 6.0 5.0 +0.09 5.1 1.66 0.69 5.8 28.2 54.0 5.3 5.7 -0.04 5.7 1.66 0.59 5.6 28.2 64.8 5.1 6.2 -0.10 5.9 1.66 0.54 5.3 102 Reconstructed & Experimental Reconstructed & Experimental E 0 -1E 0 E -2- E 0-4 0 -2-3-- -5 6- -0.5 1 50O 0.0 0.5 1.0 Voltage [ V 1.5 -0.5 2.0 0.0 0.5 1.0 1.5 2.0 Voltage [ V ] ] Figure 7-5: Representative reconstructed current density-voltage characteristics of multijunction devices either balanced (left) or unbalanced (right). The device on right is the maximal-PCE cell. 7.4.2 Subcell Photocurrents First, we determine the photocurrent generated by each of the subcells within each fabricated MJ cell. Two methods previously proposed for determining the subcell photocurrent balance are (1) utilizing optical models of the subcells [156] or (2) integrating the subcell EQEs under solar simulation [133]. Optical models can exhibit significant variation from experimental results (see Figure 7-6). [149] Furthermore, accurate EQE measurements of subcells are difficult to perfect and may also lead to significant error [133].Therefore here we utilize a simple method to quantify each subcell photocurrent and calculate the subcell photocurrent balance, SPB of each fabricated MJ-OPV, based on the re-construction of the MJ cell JV curve from SJ JV curves. Subcell photocurrents for each MJ cell were determined by utilizing two fitting parameters while re-constructing the MJ JV curve from the two SJ curves. Two examples are shown in Figure 7-5. The fitted subcell photocurrents and calculated SPB for each MJ-OPV are listed in Table 7.2. The array of devices formed by fabricating subcells equal to, 20% thicker or 20% thinner than those of the modeledoptimal structure (SCI T = 23.5nim, SC2 T = 54.Onm) leads to SPB between -0.13 and +0.09. To simulate the MJ-OPV circuit, the subeell current sources must be programmed 103 8 - SIP1 Modeled C~4 U7 - E E SP1 Exp 6p SP2 Exp U 1W 0 5 SP2 Modeled 4 11 40 60 50 SC2 Thickness [nm] 70 Figure 7-6: Fitted photocurrent for an array of fabricated cells with the same SCi thickness and varying SC2 thickness. Black lines are fits to the data. Red and Blue lines are modeled subcell photocurrents. with an array of realistic subcell photocurrents. The tradeoff between the photocurrent of one subcell and that of the other is complex and depends both on absorption spectra as well as the weak micro-cavity effect formed by the silver electrode. The optical model utilized in our previous publication is highly useful for initial selection of subcell order and thickness, but contains inherent sources of error, such as assumptions of unity carrier collection efficiency and potential discrepancies in thickness and in optical behavior (especially of the silver nanoparticle layer). Therefore, we fit our fitted subcell photocurrent data to trend lines to estimate subcell photocurrents outside of the range of our fabricated devices. Even though this may not lead to accurate models of photocurrent values for real devices, it enables us to visualize PCE dependence on SPB to a larger range. The data and their fits alongside the optical model results are shown in Figure 7-6. 7.4.3 Dependence of Multijunction Performance on Subcell Photocurrent Balance Table 7.2 reports the performance parameters for the array of 9 MJ cells as well as their fitted subcell photocurrents (SP) and calculated SPB. The dependence of 104 6.5- 0.75070- 0 6,5- 6.5- 0.70 . 5 C 4.5 5 PC 5.5 5.5- LL ' T 0.65 A. 4 5 .5 0.50 -0.15 6 - JSC 0.00 0.05 0.10 Subcell Photocurrent Balance -0.10 -0.05 40 4.5 0.15 L- 0 4 0C. 0.0 0.1 0.2 0.3 0.4 0.5 Subcell Photocurrent Balance -0.5 -0.4 -0.3 -0.2 -0.1 Figure 7-7: Dependence of FF, Jsc arid PCE on SPB for an array of simulated MJOPVs. Left arid Right show different ranges of SPB. Lines are simulated values and points are experimental values. FF, Jsc, and PCE on SPB are shown in Figure 7-7. Within this range of data, there is a clear monotonic trend of increasing FF with increasing SPB, with a change of 28% of the maximnal-FF. Jsc decreases slightly with SPB, with a change of 14% of the maximal-Jsc. Voc (not shown) has no dependence on SPB, and varies over a range of 6% of the maxinmal-Voc. PCE increases with SPB, with a change of 21% of the maximal-PCE. The maximal PCE cell shown here is the highest PCE cell we have reported for this materials set. To have a more detailed look at a larger range of SPB, we simulate our MJ- OPV circuit via the quite-universal circuit simulator, [162, 163] and set the subeell photocurrents to follow the fits shown in Figure 7-6. Figure 7-7 shows the dependence of FF and PCE on SPB for an array of sirmulated MJ-OPVs. For 0 <SPB <0.2, FF increases while Jsc decreases, leading to an inflection point of maximum PCE. For SPB >0.2, FF stabilizes as Jsc continues to decrease rapidly, leading to rapid decrease in PCE. For SPB <0.2, both FF arid Jsc decrease, leading to decrease of PCE. At SPB =±0.06, FF is increased by 8% arid Jsc has decreased by 5% versus the balanced device. This has the maximum PCE which is 3% greater than the balanced device (SPB=0) and 16% greater than the maximal-Jsc device (SPB= -0.15). 105 7.5 7.5.1 Discussion PCE Optimization in Multijunctions The increase in FF with SPB in this array of devices experimentally confirms empirical observations stated elsewhere that the FF of a MJ-OPV depends on the balance of subeell photocurrents, particularly noting that FF seems to be dominated by the current-limiting subcell [132, 156,164]. Further, we note that this relatively small change in FF in the single-junctions indicates that the significantly larger change in FF in the multijunctions is not simply due to any increase in series resistance of the subcells. Jsc varies without a clear dependence on PCB due to its dependence primarily on absorption efficiency (and thus optical environment) rather than electrical characteristics of MJ architecture. Voc varies minimally over this thickness range because with the optimized hybrid tunnel junction RZ the Voc is equivalent to the sum of the SJ cells, and the Voc of the SJ cells are essentially independent of subcell thickness. PCE shows variation due to Jsc, but the trend of increasing PCE with increasing PCB (due to increasing FF) is evident. Figure 7-8a shows current-voltage characteristics for MJ-OPV devices with constant SCI thickness (28.2 nm) but three different SC2 thicknesses: 43.2, 54.0, 64.8 nm. Simulated current-voltage characteristics for multijunctions with SPB = 0 (balanced), -. 15, and +.06 (optimal) are shown in Figure 7-8b. The dominance of FF over Jsc in maximizing PCE is evident. Thus, even though optical models are useful for initial optimization of subcell order and thickness, [143,149] further PCE gains are made by utilizing imbalanced subcell photocurrents. We note, however, that the tradeoff of Jsc and FF will vary for each materials set. [158,160] Ultimately, the gains (and losses) in FF can be probed via adding any two SJ JVs with varying PCB, as explained above. 106 Simulated Experimental E _-2 E -2 -3- -3 CD-4- a) -4- 5 Max-PCE -5 -- 07 -0.5 -Matched Max-Jsc - 70.0 0.5 1.0 1.5 , -0.5 2.0 0.0 0.5 Voltage [ V Voltage [ V , , 1.5 1.0 2.0 ] Figure 7-8: (Left) Experimental Current Density-Voltage Characteristics of multijunction devices with increasing SC2 thickness and constant SCI thickness. (Right) Simulated Current Density-Voltage Characteristics of multijunction devices with balanced subcell photocurrents, large negative imbalance, or positive (optimal) imbalance. 7.5.2 Dependence of Subcell Photocurrent Balance on NonStandard Conditions Illumination We further note that herein we vary SPB with subcell thickness, but SPB also depends on spectrum of illumination and on light intensity. Therefore, effects of SPB on PCE should be considered for all solar cells that will be under natural solar illumination, which indeed exhibits significant intensity and spectral shifts throughout the day and year. [165] Power Output Dependence on Load Resistance Often within the research lab we focus solely on power conversion efficiency, however out in the field power generation and utilization is not so simple. In Figure 7-10 we plot the power output of three simulated MJ cells (max-Jse, balanced, and maxPCE cells) versus the load resistance. The maximal-PCE cell (with slight positive SPB) produces the highest power output at a load resistance of approximately 300 , 3% higher than the balanced cell and 16% greater than the max-Jsc cell. However this advantage in power output decreases as the load resistance is varied from the 107 0.07 - . .. , . . ... . ... 0.06 ,0.06 0.8 0.75 . . ... T - 0.05' ::,0.04 0 ! J2 't- S J1 Qf 0.01 0.00 .. .!.7 ---. 6 . . 4 '45 0.5- 0.03 r.0 , .. S. 0.1 ioU1 0 3 0.2 . 0.1 100 0 1 ]*- 0. Intensity [mW/cm2] 0c 0.3 0.4- 0 0.1 10 1 Intensity [mW/cm2] 100 D 3: 0 Figure 7-9: (Left) Experimental responsivities of max-PCE MJ and corresponding SJ cells versus illumination intensity. (Right) Calculated subcell photocurrent balance and experimental power conversion efficiency for the max-PCE MJ cell versus illumination intensity. maximum power point. The balanced subcell produces greater power for load resishas tances less than 200 Ohms (towards short circuit). Furthermore, the max-Jsc cell the advantage of having a significantly smaller variance in power output in the region of maximum power point (a change of 1% in power output for a change in 10% of load resistance versus a change of 3% for the maximal-PCE cell). This is an unexpected advantage of the lower FF and higher shunt resistance of the max-Jsc cell. Therefore, for systems without sophisticated MPP tracking systems or seeking higher flexibility in load resistance may choose to utilize the max-Jsc cell with lower FF and lower PCE. Likewise, for applications seeking lower load resistance, the balanced cell may be preferable to the maximal-PCE cell. 7.6 Conclusions We first demonstrate the importance of fill factor in optimizing MJ-OPVs. We then show a simple method for calculating subcell photocurrent balance, SPB, from current-voltage characteristics and find that the fill factor for multijunctions comprised of this materials set show a linear dependence on SPB within a limited thickness range. Finally, we simulate a broad array of subcell thicknesses and confirm that is a MJ FF can be adjusted via subcell photocurrent imbalance, and that when there 108 7 6 E S5 Ea I-4 0~ '53 -.15 -SPB= -SPB= 0 -SPB= +.06 . 0 -------- 0 200 600 400 Load Resistance [Ohm] 800 1000 Figure 7-10: Simulated MJ cell power output versus load resistance. large difference in FF of the subcells then the gain in MJ FF can dominate losses in Jsc. These methods are broadly applicable to multijunction photovoltaics and should be utilized to fully optimize power conversion efficiency. 109 110 Chapter 8 Vapor-Processed Crystals and Aggregates of Organic Semiconductors As discussed above, high long-range order can lead to increased short circuit current within OPVs. The highest possible ordered nano-structure is the crystal. Herein we explore two novel processes for fabricating organic micro-crystals: via solvent annealing (first demonstrated by Mascaro et al [166] and here analyzed and modeled [167]) and via low vacuum thernial evaporation. Both of these processes are compatible with conventional device fabrication techniques. 8.1 Organic Semiconductor Needles Formed via Solvent Annealing Mascaro et al [166] produced extremely high-aspect-ratio Alq3 needles up to a centimeter long, with characteristic cross-sectional dimensions of less than a micron. After evaporating thin (10-20 nim) filis of amorphous Alq3 onto silicon and glass substrates, Mascaro et al annealed these filns in a solvent vapor (chloroform or methanol) at room temperature and atmospheric pressure to promote the growth of single-crystal 111 Glass substrate i Amorphous Alq 3 film Alq 3 deposition . I Alq3 crystals and droplets Methanol annealing Figure 8-1: Process flow for growth of Alq3 needles. [167] Alq3 needles. This process is shown in Fig. 8-1. They demonstrate that the rate of Alq3-needle growth and its morphology depended on substrate topography, substrate properties, and solvent properties. Motivated by Mascaro et al we examine the growth of needle-like crystals from a binary fluid mixture. Through experiments, numerical modeling, and analytic scaling laws, we characterize the general growth process on planar substrates. 8.1.1 Experimental Results A few minutes into the solvent annealing process, images of the substrate as viewed through a microscope darken, and later the substrate develops a speckled texture. This visual transformation corresponds to an initially-uniform film breaking up into small drops driven by either spinodal dewetting or hole nucleation [168]. The first Alq3 crystals begin to appear during this transformation. These crystal needles tend to grow in clusters surrounding a common nucleation point, as shown in figure 82. For thicker films, these points of nucleation appeared as large splotches (see the micrograph for HAlq3=60nm in figure 8-2) that were tens of microns in diameter; the periphery of those splotches acted as nucleation sites for crystal needles. These nucleation sites were not seeded; instead it appears the came form imperfections during deposition, or, possible, form particulate contamination during handling. It is interesting to note that the morphology and thickness dependence of these splotches 112 (a) (b) HAtq, = 10 nm HAlq3 = 15 nm H Alq = 30 nm H441q = 60 nm Figure 8-2: (a) Optical micrographs of needles for different thicknesses of Alq3 films after annealing for 1-5 hours. (b) SEM micrograph of rectangular needles going from a common nucleation site after solvent annealing a fihn with HAIq3=15nm. [167] resembles hole formation in nucleation-driven dewetting (e.g. [169]). The thick rims of such holes could serve as nucleation sites, which is in agreement with our observations. In experiments, Alq3 tends to solidify into single-crystal, high-asp ect-ratio needles. Note that Alq3-needle formation is not specific to these experiments; needle formation is also observed in crystals grown from physical-vapor deposition [170] and liquid solutions of Alq3 and solvent [171]. Thus, it is likely that Alq3 has an anisotropy in the growth due to an anisotropic surface energy, which favors needle-like morphologies [172]. Nevertheless, the rectangular geometry breaks down for large Alq3 thicknesses. The needles for HAq3=60 nmni are tapered and have a sharp (as opposed to flat) tip. In addition, these tapered needles grow along slightly curved paths, in contrast to the straight paths observed in thinner filns. For rectangular needles, we track their lengths in experiments by taking a onedimensional slice of pixels along the needle's long axis. When sequential pixel slices are placed side-by-side, they form a simple visualization of the evolution of the needle length, as shown in figure 8-3. The dark curved line in figure 8-3b gives the position of the needle tip as a function of time and corresponds to the length of the needle, since the pixel slices start at the base of the needle. 113 (a) 5 min 20 min 60 min 120 min (b) 5 30 5 ptm 120 90 60 Time (min) 150 180 4 pm Figure 8-3: (a) Successive snapshots of a cluster of needles growing during solvent annealing. The top-left needle from the cluster is tracked over time in (b). (b) Slice of micrograph pixels along the axis of a needle as a function of time. [167] Needle growth appeared to exhibit a power-law behavior over one decade, such that the needle length grows like Lneedle ~ T' (8.1) where T is time and y is the growth exponent. In our experiments, To was taken to be the start of the experiment. Needle growth slows down over time, such that 0 < -y < 1. Simulations, discussed below, suggest that this slowing of growth is due to the depletion of liquid Alq3: at late times, growth saturates as nearby liquid Alq3 solidifies, thus reducing the availability of mobile material. 8.1.2 Physical Picture In these experiments, methanol vapor interacts with solid Alq3 film to produce a liquid mixture. Thus, the evolution of the Alq3-methanol film is governed by the dynamics of thin liquid films. Furthermore, we neglect condensation and evaporation of solvent during needle growth. In what follows, we consider a time after a needle has nucleated from the binary mixture. 114 Alq 3 needle Wetting layer \ | Droplets / Figure 8-4: (a) Schematic of a needle growing into a fluid fih. (b) Optical micrograph of the area surrounding an Alq3 needle after solvent annealing for 3 hours. [167] The mixture of Alq3 and methanol forms a thin, liquid film with characteristic film thickness H and characteristic length L in the plane of the fihn. For filns that are approximately 100nn thick or less, intermolecular interaction between liquid, substrate, and surrounding vapor become important. For van der Waals interactions, the interaction strength is given by the combined Hamaker constant for the solidliquid-vapor system, ASLV. In addition to the intermolecular pressure, surface tension produces a pressure juimp across a curved liquid/vapor interface. Thus the total fluid pressure is a sum of the surface tension as well as van der Waals interactions between liquid, substrate, and surrounding vapor. The competition between surface tension and intermolecular forces causes the initially-uniform film to break up into drops through either spinodal or nucleation-driven deleting. Note that the short-range repulsive force in the molecular interactions prevents formation of dry spots. Although the term 'dewetting' suggests complete removal of fluid, here and in the literature it describes progression toward an ultra-thin filn rather than film rupture. After dewetting, the drops coarsen, during which capillary pressure denominates in drops, while internolecular pressure dominates in the ultra-thin film forming a slowly-evolving quasi steady configuration. In our system, the fluid film is composed of a binary mixture of Alq3 and solvent molecules, lience a second equation is required to track motion of solvent relative to mixture. Solvent is advocated by fluid flow and driven down concentration gradients 115 ([- 1=0 (b)L r=256 (c) IA A A A ~ ~ A A t= 1000 (d) -ineedle A t= 1000000 A 5 0 Figure 8-5: Evolving Thin Film. A solid needle grows from the left. [167] by diffusion. Furthermore, at the solid/liquid interface of a growing crystal needle, we assume local equilibrium at the needle tip, such that the solvent concentrations at the tip are fixed.These fixed values provide the relevant boundary condition at the needle tip if solidification is limited by transport of Alq3, not by interface kinetics. 8.1.3 Mathematical Model and Numerical Results Based upon this physical picture of Alq3 crystal growth, my collaborators in the Hosoi group developed a mathematical model [167]. Then, these governing equations were solved numerically using centered finite differences and fully implicit time steps. At each time step, the system was solved using a two-step procedure: first they solved for film hight and concentration while holding the needle tip position fixed; next they advanced the needle tip. The result of this simulation is shown in figure 8-5. At time t=0, the fluid film has a uniform, but rough, thickness. At a characteristic time (here at t=256), the uniform film becomes unstable and breaks up into small drops (t=1000). At late times, drops collapse and coalesce to form a larger, more coarsely-spaced drops. The growth exponent could be manipulated by varying the thickness of the Alq3 film. The measured growth exponents were consistent with the predicted range, and increased with increasing film thickness, as predicted by the model. 116 8.1.4 Conclusions Although these experiments were conducted on a single system, Alq3-methanolglass, the results should be applicable to many molecule-solvent-substrate systems. In particular, the behavior of the system is governed by a set of dimensionless parameters, which could be tuned using different molecules, solvents, and substrates. 8.2 Low Vacuum Thermal Evaporation of Organic Semiconductors 8.2.1 Theory It is well established that the vacuum pressure of a deposition chamber has significant effects on purity of a thin film. The "air" molecules (or whatever else might be floating around in a dirty chamber) will land on a substrate at a uniform rate. The time for a monolayer of "air" to form on a surface is given by: tmoflo = 3.61 P (8.2) where tmOO is the monolayer formation time in seconds, and P is the pressure in pascals (1 pascal = .0075Torr). (Note: the constant value will depend on the chemistry of the "air" molecules, but the possible variance is negligible for our consideration.) Since we typically deposit organic thin films at 1 Angstrom/second and at a pressure of 10-' Torr, an typical active layer of 60nm (roughly 60 monolayers of molecules) will include approximately 200 monolayers of "air". (Air is made primarily of Nitrogen, which has a covalent atomic radius of 71 pmn, thus we can roughly approximate 200 monolayers of air as 14nm thick, or >20% of the thickness of the active layer.) This, apparently, is not too bad. If we lower the pressure to 10' Torr, we can get down to only 2 monoloayers of air, but if we increase the pressure to 1 mTorr (10' Torr), the thin film will contain 200,000 monolayers of air.1 We see here that pressure has 'Note that our quartz thickness monitor stops working at approximately 10-4 Torr. 117 1E+04 G1E+03 IE+02 - E 1E+02 1E+03 0 E 1E+01 - 0 IE+OO U- 1E-02 o - 1E-02 0 S1E-03 1E-09 ____ 1E-06 1E-07 1E-08 1E-05 1E-04 1E-03 Chamber Pressure [Torr] Figure 8-6: Relation of "air" molecule's monolayer formation time and chamber pres- sure. The typical length of an active layer deposition is identified with the red line. a significant influence on thin film purity. However, vacuum pressure also affects the mean free path (i.e. line-of-sight flight distance) of an evaporant. At higher pressures, there are more "air" molecules floating around in the chamber, and thus, as an evaporant shoots off towards the substrate, it may be subject to collisions with these "air" molecules. The mean free path, 1 between collisions for a molecule is given by: I = kBT BT (8.3) 23 J/K), T is the temwhere kB is the Boltzmann constant in J/K (1.3806488x10- perature in K (here, 300K), P is pressure in pascals , and d is the diameter of the molecules in meters (typically 10' m). For the situation described here, we can simplify this equation to: 1- 0.00125 P (8.4) The number of collisions depends both on the vacuum pressure as swell as the throw distance of the chamber. Both of ONE Lab's vacuum thermal evaporation chambers have a throw distance of approximately 50cm. The comparison of mean free path and ONE Lab's throw distance is shown in figure 8-7. We see that for pressures lower than 1 mTorr there is very low probability of an evaporant colliding 118 1E+03 - E 1E+02 ) 1E+01 C 1E+00 1lE-01 1E-02 .L 1E-03 1E-04 1E-05 1E-06 - - - - 1E-06 1E-05 1E-04 1E-03 1E-02 1E-01 1E+00 1E+01 1E+02 1E+03 Chamber Pressure [Torr] Figure 8-7: Relation of evaporate molecule's mean free path and chamber pressure. The throw distance of our chamber is identified with the red line. before landing on the substrate. However, for pressures higher than 1 mTorr there is high probability of scattering events. At atmospheric pressure (760 Torr) we can anticipate > 105 collisions before deposition on the substrate surface. This is definitely no longer line-of-sight and we anticipate will result in a conformal coating. 8.2.2 Results and Discussion However, what we anticipate is usually not what actually happens. In experiment, we find that pressures of 1 mTorr result in aggregation of the evaporant (in this case, CuPc) in mid-"air", and deposition of huge (>1 micron) clusters of crystalline CuPc. In the field, this is called "snowing". An image of a snowy thin film is shown in Figure 8-8. In an attempt to utilize our CuPc snow, we soak the snowed-on substrate in methanol to dissolve the CuPc. (CuPc is nearly insoluble, but methanol is the best attempt.) We then fabricate a solution-processed solar cell with dissolved CuPc snow (a donor) blended with PCBM (an acceptor), capped with conventional electrodes and interlayers. In current density-voltage characteristics, the snowy PV exhibits an extremely low shunt resistance, such that diode behavior is non-existent. We propose that the 'gigantic' CuPc nanocrystals (micron-scale versus the sub-100nm-scale of the device) allowed shorting from the bottom electrode to the top electrode, bypassing 119 Figure 8-8: SEM image of CuPc "snow" formed by LVTE. any potential heterojunction interface. Further work should include intentionally varying the size of the CuPc snow-likely through vacuum pressure control- as well as development of more suitable device architectures. 8.3 Conclusions The novel processes reported here for generation of long range order in molecular systems are highly accessible due to their utilization of conventional capital equipment and materials in the organic optoelectronics field. We propose that these processes will be compliant with current OPV fabrication, however demonstration of efficient solar cells with the organic crystals demonstrated in this thesis is not yet completed. Furthermore, the micron- and centimeter-scale crystals reported here would also be of interest in pairing with a vapor-processed, conformally deposited semiconductor material, such as oCVD semiconducting polymers (e.g. [173]). The macro-scale molecular ordering presented here holds potential to produce solar cells with enhanced Jsc, Voc, and FF due to extended exciton and polar diffusion lengths in molecular semiconductors. 120 Chapter 9 Conclusions 9.1 Summary With the development of the first "efficient" organic photovoltaic, Tang kicked off an era of rapid development in nanostructured solar energy. Significant improvements have been made to the point of near-connercialization in niche markets today. However continued improvements in power conversion efficiency, enhancements to device lifetime, and better processability and mechanical properties are still needed to realize broad market presence in both developing and developed nations. In this thesis we tackle the problems of processability and module mechanical properties via implementation and development of Mapor-processed carbon-based electrodes and nano-thin encapsulant. We further tackle the problem of power conversion efficiency with two approaches: first through development of optimization guildelines for sub-100nm multijunction photovoltaics and secondly through novel methods for formation of molecular semiconductor crystals. Firstly, we investigated novel robust electrode materials with the Kong and Gleason groups and have reported: " development of vapor-processed organic conductors and integration with organic semiconductors * demonstration of monolithic organic solar cell arrays with carbon-based elec- 121 trodes e first ever solar cell fabricated directly on paper In addition we investigated the device lifetime of our array of standard OPV structures and materials and explore the implementation of nano-thin ALD encapsulants. We report: * distinguishment between shelflife decay due to atmospheric exposure and to materials aging * >50 times improvement in device shelflife via <30nm-thin encapsulation The combination of this nano-thin encapsulant and carbon-based electrodes, enabled by their ease of processing and earth abundance, will lead to solar cells empowered for vast impact and distribution throughout developing nations. Furthermore, we advanced power conversion efficiency through development of sub-100nm multijunction photovoltaics. Specifically, we report: " Demonstration of simple recombination zone with negligible electrical loss * Investigation of optical interference in nano-thin photovoltaics, leading to photocharge generation enhancement via inversion of subcell order We also reported on the rarely explored impact of subcell photocurrent balance on multijunction photovoltaic optimization, including, " empirical demonstration of fill factor dominating over short-circuit current in efficiency maximization of multijunctions comprising subcells with dissimilar fill factor * development of a highly accessible technique for determining subcell photocurrent balance Multijunction photovoltaics enable surpassing of the SQ limit, and these reports will enable significant steps towards practical devices. Finally, we report on nano-structuring of organic semiconductors for utilization in photovoltaics, including, 122 " modeling of potential enhancement via nanostructuring for two standard materials sets. These results suggest that an ideal nanostructure of either DBP-C60 or ClAlPc-C60 would lead to approximately doubling of efficiency compared to the planar nano-architecture. " demonstration of low-temperature thermal annealing of completed devices for enhancement of power conversion efficiency " formation of organic semiconductor crystals via (1) atmospheric thermal evap- oration and (2) solvent annealing These unconventional applications of conventional processing methods suggest a path to development of efficient OPVs. 9.2 Looking to the Future While considerable progress towards efficient solar cells on every surface is reported in this thesis, that goal is by no means yet achieved. The wide-ranging and practical demonstrations in Part 1 illustrate the near-termn potential for the design and implementation of low-cost solar energy conversion on non-traditional substrates, without mechanical or processing limitations. However the tradeoff of conductivity and transparency in these carbon-based electrodes continues to be a limitation for their utilization as transparent electrodes of large area devices. Further improvements in transparency and/or conductivity or implementation of metallic grids (such as that found in conventional solar cells) could expand the practicality of these novel electrode materials. Furthermore, the enhancement in lifetime via a sub-30nm thin film shown here is significant, but is still impractical for long term (>2 months) applications. Further work exploring new chemistries of encapsulation layers as well as more stable active layers and electrode materials will enable robust, ultra-lightweight solar arrays for long term deployment to the ends of the earth. 123 The demonstration of organic photovoltaics with mechanical properties that can be utilized in developing countries are highly motivating, however their current status of low efficiency continues to limit their actual utility. However, the tools and guidelines for enhanced power conversion efficiency reported here present significant steps towards useful operation of organic photovoltaics. Multijunction architectures are an important approach to reduce thermal losses and can significantly increase the ultimate performance of these relatively low efficiency organic materials. Further work should be performed on implementing the multijunction guidelines reported in this work with higher efficiency active layer materials. One should note, however, that some of the methods presented here will be less beneficial with better performance subcells, namely: (1) as OPV nano-structuring enables more absorbant and/or thicker subcells, conventional subcell order will likely give higher efficiencies than the inverted subeell order presented here. And (2) optimization via subcell photocurrent balance is most beneficial with subcell sets wherein at least one of the subeells has very low FF. As subcells are all brought to similarly high FF (>0.75), the optimal SPB will likely draw closer to zero (i.e. current matched). However these optimization methods will ocntinue to be useful as we work towards "practical limit" efficiency subeells. In addition, the novel processes reported here for formation of organic semiconductor crystals should be compatible with current solar cell fabrication processes, however demonstration of efficient solar cells with the organic crystals demonstrated in this thesis is yet be completed. Thus, our hypothesis that molecular ordering will concurrently produce greater Jsc, Voc, and FF is left for confirmation via experimental work and/or simulation. Ultimately, incorporation of these high efficiency approaches with the flexible, processable electrodes and encapsulants demonstrated in this work may lead to functional solar technologies for both developing and developed nations. The field of organic photovoltaics is rapidly advancing, yet these very real limitations are inhibiting their broad distribution. The impact of developing countries' lack of electricity as well as developed countries' dependence on polluting electricity generation schemes should motivate our field towards advancing the production and utilization of robust, 124 ultra-lightweight, efficient solar arrays. I hope and pray that this work has sped the coming of clean electricity generation to those in need around the world. 125 126 Appendix A Photovoltaic Primer for U.S. Policy Makers The word photovoltaic comes from the Latin words for light and electricity. The function of a photovoltaic (PV) device is to convert optical power into electrical power. Light is comprised of photons (i.e. chunks of light), each with a specified energy. Our eyes identify the different photon energies as different colors. Sunlight looks white because it is comprised of photons with energies ranging from 0.5 to 4 electronVolts (e-V). When light is incident on a material, it can be reflected, absorbed, or transmitted. Only light that is absorbed by the PV device can be used to make electricity. Semiconductors are the essential building blocks of modern day electronics (e.g. transistors, flash memory, LED displays). In semiconductor materials, electrons reside in energy states that are grouped in bands, and each of the bands is either completely filled or completely empty of electrons. The highest energy band that is completely filled when the material has received no optical or other energy is called the valence band (VB), and the lowest energy band that is completely empty is the conduction band (CB). If an electron in the VB is given enough energy, it can be excited to al empty state in the CB, where it is mobile and may thus conduct electricity. The energy difference between the VB and CB is called the bandgap (EG). Bandgap energies of semiconductors range from 1 to 5 eV. Coincidentally, this energy range 127 Wavelength [nm] 1.75 1.50 C 1.25 C14 1.00 9 0.75 0 50 S0.25 0.00 0 0.5 1 15 2 2.5 3 3.5 4 4.5 5 Energy [eV] Figure A-1: Solar power per area separated by photon energy. Energy CB Energy EG VB Position Color Figure A-2: Energy levels of photons and electrons in semiconductors. overlaps with the energy range of sunlight, and thus situates semiconductors to be efficiently utilized as the primary component of PV devices. Excitation energy for an electron can be supplied by photons. If a photon with energy of exactly EG is incident on a VB electron, then the photon is absorbed and the energy excites the electron to the CB. An excited positive charge (i.e. a hole) is formed simultaneously and also becomes mobile. If the photon has energy greater than EG, then the electron will still be excited to the CB but the extra light energy is wasted as heat. If the incident photon has energy lower than EG, it will not be absorbed and the electron will not be excited. (Note that more complex behavior can occur in some unconventional semiconductors.) Excited electrons must then be expelled from the semiconductor by energetic asymmetry within the device. This asymmetry can be generated either by introducing a p-n junction (a boundary or 128 Excited Excited +Heat Not Excited CB Energy VB Figure A-3: Excitement of electrons by photons in semiconductors interface between two types of semiconductor material p-type and n-type inside a single crystal of semiconductor, achieved by incorporating impurities/dopants) or a junction between the semiconductor and another material. Excited electrons are then removed via electrical contacts. A single PV device is called a solar cell. It is comprised of semiconductor(s), electrical contacts and, potentially, optical and/or encapsulation material(s). Semiconductors can be comprised either of a single element (e.g. Silicon (Si)) or of an alloy of two or more elements (e.g. Cadmium Telluride (CdTe) or Copper Zinc Tin Sulfide (CZTS)). The semiconductor component can either be fabricated as a wafer (i.e. a slab of crystalline semiconductor that is hundreds of microns thick) and then cut to size with the other layers deposited upon it (wafer based); or it can be fabricated as a micron-scale thin film upon a substrate with other layers also deposited inunediately preceding or subsequent (thin filn based). Electrical contacts are utilized to output the generated electricity from the semiconductor. Optical materials may be added to enhance light absorption in the semiconductor (most commonly by reducing reflection). Encapsulation materials may be added to minimize environmental exposure of the semiconductor and contacts, therefore increasing operational lifetime of the solar cell. A solar cell generates electricity only when light is shining on it. The amount of electricity generated is characterized by the number of electrons flowing as well as 129 the potential energy of those electrons. Each photon absorbed in the semiconductor can excite one electron: this translates to current. Each electron volt (1eV) of energy of the bandgap converts to IV of electrostatic potential energy of the electrons: this translates to voltage. However, there are losses for both current and voltage, so generated electricity is significantly lower than potential generation. The actual electrical output of the solar cell is characterized by the power conversion efficiency (PCE), which is the ratio of the electric power outputted to the optical power inputted. PCE is dominated not only by the opto-electrical properties of the semiconductor but also incorporates gain and loss mechanisms within the optical and/or conductive materials. PCE is typically reported under standard test conditions, e.g. light with an intensity of 1000 W/m2 and a spectrum of AM1.5G (the lighting condition representing the yearly average solar light intensity and spectrum at sea level in global mid-latitudes (e.g. the United States, Europe, China, and Australia)). The total power output of a solar cell is calculated by multiplying the PCE by the total incident optical power. The theoretical maximal PCE for the conversion of sunlight to electricity on Earth (calculated from fundamental thermodynamic principles) is 89% (the Carnot limit). However, if we account for the physics of single semiconductor junction PV devices, the theoretical maximal PCE is 33% (the Shockley-Queisser (SQ) Limit). This is due to (1) the non-utilization of photons with energy less than the semiconductor bandgap, (2) the loss of photonic energy greater than the bandgap, and (3) fundamental recombination losses within semiconductors. Currently, the maximal reported PCE for a single junction solar cell is 29%, nearly the theoretical limit. However, most solar cells commercially available today are single junctions with PCEs ranging from 12-23%. However there are multiple methods for exceeding the SQ Limit. First is the implementation of multi-junction solar cells, in which multiple solar cells with semiconductors of differing bandgaps are fabricated on top of each other to better utilize the solar spectrum. A triple-junction solar cell could theoretically achieve 49% PCE. This approach has produced the highest reported solar cell thus far, with a PCE of 44.4%. However, fabrication of such a complex cell is cost prohibitive for most appli130 cations. The second method is usage of optics and/or imechanical tracking systems to concentrate the intensity of light incident on the solar cell. For most (but not all) semiconductors, this increases efficiency while decreasing overall cost. The third method is utilization of semiconductors with unconventional opto-electronic physics, however such PV technologies are still in the R&D stage. Solar cells are connected mechanically and electrically to form PV modules (also known as solar panels). The typical mechanical connection is adherence to a glass pane and mounting on an aluminum frame. The cells are connected either in series and/or in parallel with thin wires to provide the desired voltage and current output. Typical PV modules output voltages of 5V to 30V. A full PV system further includes electrical components. PV modules gener- ate DC electric power, which is the unidirectional flow of electrons. DC power is useful primarily for charging batteries and powering personal electronics, ideal for residential-scale applications. However, the electric grid runs on AC power, where the flow of electrons periodically switches direction (in the US, at a frequency of 60 Hz). Household AC power in the US is at 120V, and transmission line power is at 110,000 V or above (to reduce the energy lost when transmitting over long distances). Therefore, for grid-scale applications, an inverter is necessary to convert between DC power and AC power in addition to other electronics for modification of voltage output. 131 132 Appendix B Fabrication of Vapor-Processed Organic Photovoltaics B.1 Introduction There are many variables that impact on device performance. Figure B-1 are all the same photoactive materials and device structure, and all are optimal performances for an experimental run, yet PCE range from 0.6%-4.0%. Note: typical standard deviation 10%. Thickness of the photoactive layers is a key factor in planar OPVs. Too thin and the electrodes/interlayers may short through the device. Too thick and they will add too much series resistance and optical absorption losses. (Figure B-2 shows devices with two different batches of DBP.) B.2 Dominance of DBP Why do we mostly focus on DBP optimization? materials, we get a significantly smaller effect. Because when we vary other (Note: this doesnt hold for every material set and device structure. But it does here, and is the foundation of the research presented in this chapter.) From the circuit model we note that lower series resistance, Rs, is better for fill 133 4- 2 i - - 20110309 20120328 20120918 20120925 20121003 20121121 20130124 4.0% 2.7% 1.2% 1.6% 0.6% 1.8% 2.7% 1, 0 -2 - -- -4 -6 -1.0 -0.5 0.0 0.5 1.0 Voltage [V] Figure B-1: Current Density-Voltage Characteristics of a variety of devices with nominally the same architecture and materials. factor as well as short circuit current density. Whereas lower shunt resistance, RSH, is worse for fill factor as well as short circuit current density. B.3 Donor Layer B.3.1 Manufacturer DBP material purchased from Sigma Aldrich shows a 40-50% improvement in PCE over material purchased from Lumtec. The SA batch shown here is purified once whereas the Lumtec batch shown here is purified two times. These two JVs are from two separate device runs. The improvement in PCE is due to increases in both Jsc and FF. This may be due to differences in impurity concentration or impurity chemistry. Note that we should further experiment with comparing different purities of the different manufactures. However also note that our evaporator is only capable of 134 4- ---- 3.- ;: - 2- - 1- Onm DBP DBP DBP DBP DBP 4- 2.5nm 5nm 10nm 20nm 2- ~/i'1I'I E -2 -1 20nm 2-3 -5 -050 -0.25 0.00 0,25 0.50 0.75 10nm -4t 4 DBP 1.00 DBP 00 oa5 -1V0 Voltage [ V I 05 1.0 1.5 Voltage (V) 2.5 I I*I*I * I -U-- 20130130 -U- 20121003 2.0U 1.5- IR 0L. 0 U 1.0- U 0.5U 0.00 5 10 15 20 25 30 35 40 Donor Thickness (nm) Figure B-2: Current Density-Voltage Characteristics of a thickness optimization run for two different batches of donor material. TOR RS - Glass Figure B-3: Left: Schematic of device architecture highlighting the various layers for optimization. Right: Device circuit model. 135 U U U IvPCE -, 2 0 R81 tVPCE - 2 0 - ivPCF 8 500- s50- 500 U I E I 200- 15 20 . 5 10 25 30 40 35 - 05 I W I 100- Ii i,., o 45 U U 100, - 0 0 300 200- U I I10W 2 200 0-. . 20 400U E 300- a E300 - 1,5 400- 1 5 400 20 10 50 30 40 50 60 70 U! 80 IW 20 40 C60 DBP [nm 60 MoOx Figure B-4: Thickness optimization of various layers. 10000, jINI 1000 E * Rs @1.25V Rsh @-1.25V N I * iv PCE iv Jsc Siv FF RshU Jsc 1 - IL IL 0 100- LU -Ci It FF INe Rs PCE 10U 0 5 I 0.1 15 10 20 25 35 30 40 45 50 DBP [nm] Figure B-5: Thickness optimization of DBP showing various parameters. 2- 2- 1 - I E t 0 0 f I - Lumtec 2x SA 1x I 2.8 3.2 0.89 0.90 0.52 0.67 1.3 2.0 -1.1 -3 (D2 -3 - -0.50 -0.25 0.00 20121121 3.1 0.90 0.65 1.8% 20130124 3.9 0,90 0.70 2.5% 0.25 0.50 0.75 1.00 -0.5 0 5 0.0 Voltage [V I 1.25 Voltage [ V ] Figure B-6: JVs with DBP from two manufacturers. 136 1.0 80 100 05 OU 120 -- 2- as purch DBP 20120925 3.4 1x pur DBP 20120925 3.4 2x pur DBP 20130107 3.2 0.89 0.90 0.88 0.45 0.53 0.64 2- 1.4% 1.6% 18% --- 0- E ---- E 1 I unpur DBP 1x pur DBP -1 - U -2- -2 .3 - :3 -3 -0.5 -0.50 -025 0.00 0.25 0.50 Voltage [ V ] 05 1.00 0.0 0.5 1.0 Voltage [ V I 1.25 Figure B-7: JVs with DBP as purchased or purified once or purified twice. holding two donor materials at once. (So, to experiment with more batches of donor material, the evaporator would have to be re-loaded midst a device run.) B.3.2 Purity For the specific manufacturer Lumtec, we explored the effect of purity via comparison of different purification runs on device performance. We note that higher purity led to higher fill factors, resulting in a 30% increase in PCE. We speculate that the higher FF is due to lower concentration of traps and thus higher mobility within the donor layer. We also note that higher purity led to higher yield and stability of devices on a given substrate (each substrate has 10 devices). This is evident in the graph with JV curves from every device pad on a substrate from either unpurified DBP or once- purified DBP. B.3.3 Growth Rate Optimizing the growth rate of the DBP layer results in PCE enhancements of up to 20%. Growth rate is well known to cause changes in nanostructure, which of course effects performance. We hypothesize that the higher growth rate either results in a more disordered film which thus is missing grain boundaries that are sources of traps, 137 22-- E -1 01 -2- 0 7 - -. -I -1 -3 0 -4 e -1.0 , -0,5 , --- , 0.0 .5 DBP 0.2N/s -- 1.7%, 0.5 -1.0 1.0 DBP A/s - 1.1% -DBP 1A/s - 1.4% DBPO0.5A/s - 1.5% __________ -0.5 0.0 0.5 1.0 Voltage [ V Voltage LVI Figure B-8: JVs with DBP grown at variety of rates. - C60 C70 35 40 075 0.75 0.37 0.36 1.1% 1 .2% 5.02.5E0. 0 -2.5 -5.0 -7.5 -0.5 0.0 Voltage ( V ) 05 1.0 Figure B-9: JVs comparing C60 and C70 as acceptor, with the donor material ClAlPc. or it results in a more ordered film, the bulk of which has less traps and thus higher mobility. Further experiments must be performed to confirm either option. B.4 Acceptor Layer B.4.1 Materials Choice Note that this data is for a different donor material: CIAlPe. We have not yet successfully performed this experiment with DBP. (Each attempt coincided with issues with the evaporator.) Substituting C70 for C70 led to a 30% increase in short circuit current, and a 9% increase in PCE. We note that C70 has stronger and broader absorption than C60 yet very similar in other characteristics, thus explaining the focused improvement in Jsc. 138 2010-11-16 20- 10 _ MoOx+C60 -- MoOx+C60 Oxpur 1xpur 87 8- >10 ( 0 -2- 201011 16 -oOxoC6O Ipur MoOxvC6O Oxpur 060 1ixpur -10 s -05 _ 00 060 Oxpur 0 05 300 400 500 600 700 800 Wavelength [nm] Voltage [VI Figure B-10: JV and EQE for various C60 purities. B.4.2 Purity Purer C60 leads to an increase in incident photon to electron efficiency for C60 absorption range, and additionally increases FF. This is likely due to decrease in trap states which could lead to recombination. B.5 Anode Interlayer B.5.1 Materials Choice PEDOT shows a 10-40% PCE improvement over MoOs as an anode interlayer. We speculate that this is due to a smnoother/more favorable contact between DBP and PEDOT vs DBP and MoOx. However it may also be due to PEDOT leading DBP to grow in a more power conversion efficient morphology. Note that PEDOT is also more sensitive to age etc. The double-diode JV in blue is due to an old batch of PEDOT. The rest of these experiments are performed with a more recently purchased bottle of PEDOT. (The manufacturer tells us that PEDOT expiration is at approximately 6 months.) B.5.2 Thickness Thicker MoOx decreases PCE but increases yield. Thus we utilize 50nmn as our standard thickness, which is a blanace between shorting (yield) and resistance (PCE). 139 1.0- 4- MoOx 20130124 MoOx 20130130 PEDOT 20130124 PEDOT 20130130 - 3- - 2- - 0.5 E -- 0C-- -- - -+ -+ E '- - E -' C -2- -0.5 -MoOx - - -1.0 -1.5 PEDOT PEDOT/MoOx - -2.0 - -3- - -4- -2.5 -3.0 -0.50 -5 -0.50 -0.25 0.00 0.25 0.50 Voltage [ V 1.00 0.75 -0.25 ] 0.00 0.25 0.50 0.75 1.00 Voltage [V Figure B-11: JV for various anode interlayers: MoOx and PEDOT. 1.0- MoOx -- 0.5- - Yield 4/10 8/10 S00nm 9/10 20nm 50nm E E -0.5 C 0D -1.0 -1.5-2.0 -2.5 -0.50 - -0.25 0.00 0.25 0.50 0.75 1.00 Voltage [ V I Figure B-12: JV for various MoOx thicknesses. B.6 Cathode Interlayer B.6.1 Materials Choice BCP is the conventional cathode interlayer for vapor-processed molecular PVs, however we experiment with Alq3, a conventional electrode transport layer. We find a 21% increase in PCE, due to the lower resistivity of the Alq3 film. Note that the thicknesses shown here have each been optimized for this particular donor-acceptor device structure. 140 4. 1- BCP .- 0- - I 2. E E Onm - 3. E - 1- 2.5nm 6.5nm 10nm 18nm 18nm 0- -1 C -2- -2 - - none BCP 6.5nm -3- Alq 10nm -0.5 0.5 0.0 1.0 1.0 -0,5 0.0 0.5 10 1.5 Voltage [V ] Voltage [ V] Figure B-13: Left: JV comparing various cathode interlayers: BCP and Alq3. Right: JVs of various thicknesses of BCP. Due to the significant enhancement in Alq3, we recounend that further experiments be employed to explore the change in "ONE Lab conventional OPV" from BCP to Alq3. B.6.2 Thickness In optinzing the thickness of BCP layer, we find that there is a narrow optninum point. We speculate that this is due to the combination of Ag traps (thus necessitating a thicker BCP layer) and high inherent resistance (necessitating a thinner BCP layer). B.7 Substrates and Substrate Treatments B.7.1 Substrate Choice We find that although substrate choice has significant effect on as-purchased Lumtec DBP, there is negligible difference in devices grown with purified DBP. This suggests the growth morphology of as-purchased DBP is highly sensitive to surface conditions. Note that Jill's devices are most commonly grown on "current large ITO" and Andrea's devices are most commonly grown on "current small ITO", simply as a matter of preference. 141 as purch DBP 1x pur DBP . - 2- - . - 1 - - - --- current large ITO old large ITO old small ITO 0E -1 . C -2 - -3 - II -0.5 e a I 0.5 0.0 1.0 Voltage [ V ] Figure B-14: JVs of various substrates with either purified DBP or as-purchased DBP. However, due to the clear dependence of substrate effects on the DBP batch, this experiment should be repeated with every new batch of DBP. B.7.2 Substrate Treatments We first compare depositing devices on ITO substrates just solvent cleaned vs ITO substrates that are solvent cleaned plus exposed to oxygen plasma. We find that 30 seconds of 02 plasma has no effect on device performance. Thus the plasma either does not effect the ITO, or the MoOx interlayer minimizes any effects. We further explore the effect of 5 minutes 02 plasma or 6 minutes of UV-Ozone (a slightly gentler technique). We see a slight decline ( 10%) in PCE in both devices exposed to long 02 plasma and long UV-Ozone. For less conventional techniques of influencing the ITO, we also rinse the ITO with dhilte HCl (in an attempt to slightly etch it and remove rough spots), which results in a slight decrease in Jsc. Further, we fabricated devices utilizing ITO sputter deposited in ONE Lab (rather than purchased pre-deposited), and find that all devices utilizing our ITO are shorted, suggesting production of a very rough ITO film. 142 1.0- 1- no plasma 30s 02 plasma 0.5- CN. E E E E -0.5-1.0- -1 0D -1.5 -------- - -02 - -2.0 -2.5- - 0.0 0.5 Voltage [V 1 ,U I 0 -0.50 I -0.25 0.00 0.25 0.50 plasma 30" 2 plasma 5' UV-Ozone 6' dilute HCI sputtered ITO 0.75 1.00 Voltage [ V ] Figure B-15: JVs of various substrates with various substrate treatments. B.8 Conclusions " More pure -+ higher FF -+ 30%X larger PCE " Lunitec -+ SA -- 40-50% larger PCE " DBP higher Growth Rate -4 6-20% larger PCE " MoOx -+ PEDOT -+ 10-40%X larger PCE " BCP -+ A 1 3 -a 20% larger PCE " Substrates have no effect on PVs with stable DBP " Plasma or UV- Ozone -* largest change is 8% decrease in PCE 143 144 Appendix C Contributions Associated with This Thesis 1. Macko, J. A., Lunt, R. R., Osedach, T. P., Brown, P. R., Barr, M. C., Gleason, K. K., & Bulovic, V. (2012). Multijunction organic photovoltaics with a broad spectral response. Physical Chmistry Chemical Physics. doi: 10. 1039/c2cp43000b 2. Lunt, R. R., Osedach, T. P., Brown, P. R., Rowehl, J. A., & Bulovic, V. (2011). Practical Roadmap and Limits to Nanostructured Photovoltaics. Advanced Materials, 23(48), 57125727. doi:10.1002/adnia.201103404 3. Barr, M. C., Rowehl, J. A., Lunt, R. R., Xu, J., Wang, A., Boyce, C. M., In, S. G., Bulovic, V., & Gleason, K. K. (2011). Direct monolithic integration of organic photovoltaic circuits on unmodified paper. Advanced Materials, 23(31), 34993505. doi:10.1002/adma.201101263 4. Park, H., Rowehli, J. A., Kim, K. K., Bulovic, V., & Kong, J. (2010). Doped graphene electrodes for organic solar cells. Nanotcchnology, 21, 505204. doi:10.1088/0957- 4484/21/50/505204 145 146 Bibliography [1] International Energy Agency, "World Energy Outlook," International Energy Agency, Tech. Rep., 2012. Grid the From Far Huts "African Rosenthal, [2] E. 2010. [Online]. Available: Glow with Renewable Power," http://www.nytimes.coim/2010/12/25/science/earth/25fossil.html?hpw&_r=0 "Switching on to soProperty Organization, [3] World Intellectual Available: 2011. [Online]. Sep. goodbye kerosene," lar http://www.wipo.int/wipo-magazie/en/211/05/article_0002.html [4] FAO Agricultural Services Bulletin, Renewable Biological Systems for Alternative Sustainable Energy Production, 1997. [5] R. R. Lunt, T. P. Osedach, P. R. Brown, J. A. Rowehl, and V. Bulovid, "Practical Roadmnap and Limits to Nanostructured Photovoltaics," Advanced Materials, vol. 23, no. 48, pp. 5712 5727, Nov. 2011. [Online]. Available: http://www.ncbi.nlnm.nih.gov/pubimed/22057647 [6] N. National Renewal Energy Laboratory, "Best Research-Cell Efficiencies," Tech. Rep., 2014. [Online]. Available: littp://www.lnrel.gov/ncpv/ [7] M. A. Green, K. Emery, Y. Hishikawa, W. Warta, and E. D. Dunlop, "Solar cell efficiency tables (version 43)," Progress in Photovoltaics: Research and Applications, vol. 22, pp. 1-9, 2014. [8] L. Gross, F. Mohn, N. Moll, P. Liljeroth, and G. Meyer, "The chemical structure of a molecule resolved by atomic force microscopy," Science, vol. 325, no. 5944, pp. 1110--4, Aug. 2009. [Online]. Available: http://www.ncbi.niliii.nif.gov/pubnmed/19713523 [9] I. F. Almuog, M. S. Bradley, and V. Bulovic, "The Lorentz Oscillator and its Applications," Tech. Rep., 2008. [10] B. P. Rand, D. Burk, and S. R. Forrest, "Offset energies at organic semiconductor heterojunctions and their influence on the open-circuit voltage of thin-film solar cells," Physical Review B, vol. 75, no. 11, pp. 1-11, Mar. 2007. [Online]. Available: http://liiik.aps.org/doi/10.1103/PhysRevB.75.115327 147 [11] R. H. Bube, Photoelectronic Properties of Semiconductors. Cambridge University Press, 1992. Cambridge, UK: [12] M. Knupfer, "Exciton binding energies in organic semiconductors," Applied Physics A, vol. 77, no. 5, pp. 623-626, http://dx.doi.org/10.1007/s00339-003-2182-9 2003. [Online]. Available: [13] S. F. Alvarado, P. F. Seidler, D. G. Lidzey, and D. D. C. Bradley, "Direct determination of the exciton binding energy of conjugated polymers using a scanning tunneling microscope," Physical Review Letters, vol. 81, no. 5, p. 1082, 1998. [14] I. Hill, A. Kahn, Z. Soos, and R. Pascal, Jr, "Charge-separation energy in films of r-conjugated organic molecules," Chemical Physics Letters, vol. 327, no. 3-4, pp. 181-188, Sep. 2000. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S0009261400008824 [15] G. Chamberlain, "Organic solar cells: A review," Solar Cells, vol. 8, no. 1, pp. 47-83, Feb. 1983. [Online]. Available: http://www.sciencedirect.com/science/article/pii/037967878390039X [16] B. D. Wohrle and D. Meissner, "Organic Solar Cells," Advanced Materials, vol. 3, pp. 129-138, 1991. [17] C. W. Tang, "Two-layer organic photovoltaic cell," Applied Physics Letters, vol. 48, no. 5, pp. 183-185, 1985. [18] G. Yu, J. Gao, J. C. Hummelen, F. Wudl, and A. J. Heeger, "Polymer Photovoltaic Cells: Enhanced Efficiencies via a Network of Internal Heterojunctions," Science, vol. 270, no. 5243, pp. 1789-1791, 1995. [19] H. Spanggaard and F. C. Krebs, "A brief history of the development of organic and polymeric photovoltaics," Solar Energy Materials and Solar Cells, vol. 83, no. 2-3, pp. 125-146, Jun. 2004. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S0927024804000923 [20] P. Peumans and S. R. Forrest, "Very-high-efficiency double-heterostructure copper phthalocyanine C60 photovoltaic cells," Applied Physics Letters, vol. 79, no. 1, pp. 126-128, 2001. [21] A. C. Arango, "High open-circuit voltage in heterojunction photovoltaics containing a printed colloidal quantum-dot photosensitive layer," PhD, MIT, 2010. [22] S. Olthof, S. Mehraeen, S. K. Mohapatra, S. Barlow, V. Coropceanu, J.-L. Bredas, S. R. Marder, and A. Kahn, "Ultralow Doping in Organic Semiconductors: Evidence of Trap Filling," Physical Review Letters, vol. 109, no. 17, p. 176601, Oct. 2012. [Online]. Available: http://link.aps.org/doi/10.I103/PhysRevLett.109.176601 148 [23] C. F. Madigan, "Theory and Simulation of Amorphous Organic Electronic Devices," PhD, MIT, 2006. [24] W. Shockley and H. J. Queisser, "Detailed Balance Limit of Efficiency of p-n Junction Solar Cells *," Journal of Applied Physics, vol. 32, no. 3, pp. 510-519, 1961. [25] B. M. C. Scharber, D. Miihlbacher, M. Koppe, P. Denk, C. Waldauf, A. J. Heeger, and C. J. Brabec, "Design Rules for Donors in Bulk-Heterojunction Solar Cells Towards 10 % Energy-Conversion Efficiency," Advanced Materials, vol. 18, pp. 789-794, 2006. [26] A. C. Arango, D. C. Oertel, Y. Xu, M. G. Bawendi, "Heterojunction photovoltaics using printed colloidal and V. BuloviL, quantum dots as a photosensitive layer." Nano letters, vol. 9, no. 2, pp. 860--3, Feb. 2009. [Online]. Available: http://www.ncbi.nlrm.nih.gov/pubiiied/19161261 EnCrqy 6 "Organic photovoltaics," [27] B. Kippelen and J.-L. Brddas, Environmental Science, vol. 2, no. 3, p. 251, 2009. [Online]. Available: http://xlink.rsc.org/'?DOI=b812502n [28] R. Gaudiana and C. Brabec, "Organic materials: Fantastic plastic," Nature Photonics, vol. 2, pp. 287 289, 2008. [29] M. C. Barr, J. A. Rowehl, R. R. Lunt, J. Xu, Boyce, S. G. Inn, V. Bulovid, and K. K. Gleason, A. Wang, C. M. "Direct Monolithic Integration of Organic Photovoltaic Circuits oii Unmodified Paper," Advanced Materials, vol. 23, no. 31, pp. 3500--3505, Aug. 2011. [Online]. Available: http://www.inebi.nlliii.nih.gov/pubimed/21739489 [30] M. Kaltenbrunner, M. S. White, E. D. Gowacki, T. Sekitani, T. Somneya, N. S. Sariciftei, and S. Bauer, "Ultrathin and lightweight organic solar cells with high flexibility." Nature CoMmunications, vol. 3, p. 770, Jan. 2012. [31] Sharp World, "Sharp Concentrator Develops Highest Conversion Efficiency of 44.4%," Solar Jun. 2013. Cell with [Online]. World's Available: http://sharp-world.coin,/corporate/news/130614.html H. [32] Y. Yongbo, Organic Tandem [Online]. Available: and Jinsong, Solar Cells," G. Li, Green, "Intermediate vol. 1, p. Layers in 65, 2011. http://www.degruyter.com/view/j/gree.2011.1.issue- 1/green.2011.009/green.2011.009.xil [33] M. Jo rgensen, J. E. Carl6, R. R. So ndergaard, M. Lauritzen, N. a. Dagnm s Hansen, S. L. Byskov, T. R. Andersen, T. T. Larsen-Olsen, A. P. B6ttiger, B. Andreasen, L. Fu, L. Zuo, Y. Liu, E. Bundgaard, X. Zhan, H. Chen, and F. C. Krebs, "The state of organic solar cellsA iieta analysis," Solar Energy Materials and Solar Cells, vol. 119, pp. 84--93, Dec. 2013. [Online]. Available: http://liikiiigliub.elsevier.coi/retrieve/pii/S0927024813002559 149 [34] R. Po, A. Bernardi, A. Calabrese, C. Carbonera, G. Corso, and A. Pellegrino, "From lab to fab: how must the polymer solar cell materials design change? an industrial perspective," Energy & Environmental Science, pp. 925-943, 2014. [Online]. Available: http://xlink.rsc.org/?DOI=c3ee43460e [35] K. Zweibel, "Thin Film PV manufacturing : Materials costs and their optimization," Solar Energy Materials and Solar Cells, vol. 63, pp. 375-386, 2000. [36] A. L. Roes, E. A. Alsema, K. Blok, and M. K. Patel, "Ex-ante environmental and economic evaluation of polymer photovoltaics," Progress in Photovoltaics: Research and Applications, vol. 17, no. 6, pp. 372-393, 2009. [Online]. Available: http://dx.doi.org/10.1002/pip.891 [37] E. Fortunato, D. Ginley, H. Hosono, and D. C. Paine, "Transparent Conducting Oxides for Photovoltaics," MRS Bulletin, vol. 32, no. March, pp. 242-247, 2007. [38] M. C. Barr, J. A. Rowehl, R. R. Lunt, J. Xu, A. Wang, C. M. Boyce, S. G. Im, V. Bulovid, and K. K. Gleason, "Direct Monolithic Integration of Organic Photovoltaic Circuits on Unmodified Paper," Advanced Materials, vol. 23, pp. 3500-3505, Jul. 2011. [Online]. Available: http://doi.wiley.com/10.1002/adma.201101263 [39] J. D. Goede, P. Bouten, L. Medico, Y. Leterrier, J.-a. Ma nson, and G. Nisato, "Failure of brittle functional layers in flexible electronic devices," Materials Research Society Symposium Proceedings, vol. 854E, pp. 1-6, 2005. [40] D. R. Cairns, R. P. Witte, D. K. Sparacin, S. M. Sachsman, D. C. Paine, G. P. Crawford, and R. R. Newton, "Strain-dependent electrical resistance of tin-doped indium oxide on polymer substrates," Applied Physics Letters, vol. 76, no. 11, p. 1425, 2000. [Online]. Available: http://scitation.aip.org/content/aip/journal/apl/76/11/10.1063/1.126052 [41] S. K. Park, J. I. Han, D. G. Moon, and W. K. Kim, "Mechanical Stability of Externally Deformed IndiumTinOxide Films on Polymer Substrates," Japanese Journal of Applied Physics, vol. 42, no. Part 1, No. 2A, pp. 623-629, Feb. 2003. [Online]. Available: http://jjap.jsap.jp/link?JJAP/42/623/ [42] J. Lewis, "Material challenge for flexible organic devices," Materials Today, vol. 9, no. 4, pp. 38-45, Apr. 2006. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S1369702106714468 [43] A. Kumar and C. Zhou, "The race to replace tin-doped indium oxide: which material will win?" ACS nano, vol. 4, no. 1, pp. 11-4, Jan. 2010. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/20099909 [44] D. Angmo and F. C. Krebs, "Flexible ITO-free polymer solar cells," Journal of Applied Polymer Science, vol. 129, no. 1, pp. 1-14, Jul. 2013. [Online]. Available: http://doi.wiley.com/10.1002/app.38854 150 [45] R. Po, C. Carbonera, A. Bernardi, F. Tinti, and N. Camaioni, "Polymer- and carbon-based electrodes for polymer solar cells: Toward low-cost, continuous fabrication over large area," Solar Energy Materials and Solar Cells, vol. 100, pp. 97-114, May 2012. [Online]. Available: http://likinglib.elsevier.com/retrieve/pii/S0927024811007185 [46] H. Park, J. A. Rowehl, K. K. Kim, V. Bulovic, and J. Kong, "Doped graphene electrodes for organic solar cells," Nanotechnology, vol. 21, p. 505204, 2010. [47] J. W. McClure, "Band Structure of Graphite and de Haas-van Alphen Effect," Phys. Rev., vol. 108, no. 3, pp. 612-618, Nov. 1957. [Online]. Available: http://link.aps.org/doi/10.1103/PhysRev.108.612 Phys. Rev., "The Band Theory of Graphite," [48] P. R. Wallace, Available: [Online]. May 1947. 9, pp. 622-634, no. vol. 71, http://link.aps.org/doi/10.1103/PhysRev.71.622 [49] K. S. Novoselov, D. Jiang, F. Schedin, T. J. Booth, V. V. Khotkevich, S. V. Morozov, and A. K. Geim, "Two-dimensional atomic crystals," Proceedings of the National Academy of Sciences of the United States of America, vol. 102, no. 30, pp. 10451-10453, Jul. 2005. [Online]. Available: littp://www.pias.org/content/102/30/10451.abstract [50] C. Berger, Z. Song, X. Li, X. Wu, N. Brown, C. Naud, D. Mayou, T. Li, J. Hass, A. N. Marchermkov, E. H. Conrad, P. N. First, and W. A. de Heer, "Electronic Confinement and Coherence in Patterned Epitaxial Graphene," Science, vol. 312, no. 5777, pp. 1191 1196, May 2006. [Online]. Available: http://www.scienceiag.org/coitent/312/5777/1191.abstract [51] K. Bolotin, K. Sikes, Z. Jiang, M. Klimna, G. Fudenberg, J. Hone, P. Kim, and H. Stormer, "Ultrahigh electron mobility in suspended graphene," Solid State Communications, vol. 146, no. 9-10, pp. 351-355, Jun. 2008. [Online]. Available: http://www.sciemcedirect.coim/scieie/article/pii/S0038109808001178 "CurrentBachtold, A. and Barreiro, A. Moser, induced cleaning of graphene," Applied Physics Letters, Available: [Online]. , 2007. pp. 16, 91, no. vol. http://scitation.aip.org/content/aip/jourmal/apl/91/16/10.1063/1.2789673 [52] J. [53] J. S. Bunch, A. M. van der Zande, S. S. Verbridge, I. W. Frank, D. M. Tanenbaum, J. M. Parpia, H. G. Craighead, and P. L. McEuen, "Electromechanical Resonators from Graphene Sheets," Science, vol. 315, no. 5811, pp. 490--493, Jan. 2007. [Online]. Available: http://www.scieincemag.org/coitent/315/5811/490.abstract [54] G. Eda, films of electronic "Large-area ultrathin and M. Chhowalla, G. Fanchini, and flexible oxide as a transparent reduced graphene imaterial," Nat Nano, vol. 3, no. 5, pp. 270-274, 151 May 2008. [Online]. Available: http://dx.doi.org/10.1038/nnano.2008.83 http://www.nature.com/nnano/journal/v3/n5/suppinfo/nnano.2008.83_S1.html [55] R. R. Nair, P. Blake, A. N. Grigorenko, K. S. Novoselov, T. J. Booth, T. Stauber, N. M. R. Peres, and A. K. Geim, "Fine Structure Constant Defines Visual Transparency of Graphene," Science, vol. 320, no. 5881, p. 1308, Jun. 2008. [Online]. Available: http://www.sciencemag.org/content/320/5881/1308.abstract [56] K. K. Kim, A. Reina, Y. Shi, H. Park, L.-J. Li, Y. H. Lee, and J. Kong, "Enhancing the conductivity of transparent graphene films via doping," Nanotechnology, vol. 21, no. 28, p. 285205, 2010. [Online]. Available: http://stacks.iop.org/0957-4484/21/i=28/a=285205 [57] H. Park, R. M. Howden, M. C. Barr, V. Bulovic, K. K. Gleason, and J. Kong, "Organic Solar Cells with Graphene Electrodes and Vapor PrintedPoly(3,4ethylenedioxythiophene) as the Hole Transporting Layers," ACS Nano, vol. 6, no. 7, pp. 6370-6377, 2012. [58] L. G. P. Martins, Y. Song, T. Zeng, M. S. Dresselhaus, J. Kong, and P. T. Araujo, "Direct transfer of graphene onto flexible substrates," Proceedings of the National Academy of Sciences, vol. 110, p. 44, 2013. [59] M. E. Alf, A. Asatekin, M. C. Barr, S. H. Baxamusa, H. Chelawat, G. Ozaydin-Ince, C. D. Petruezok, R. Sreenivasan, W. E. Tenhaeff, N. J. Trujillo, S. Vaddiraju, J. Xu, and K. K. Gleason, "Chemical vapor deposition of conformal, functional, and responsive polymer films." Advanced materials (Deerfield Beach, Fla.), vol. 22, no. 18, pp. 1993-2027, May 2010. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/20544886 [60] S. H. Baxamusa, S. G. Im, and K. K. Gleason, "Initiated and oxidative chemical vapor deposition: a scalable method for conformal and functional polymer films on real substrates." Physical chemistry chemical physics : PCCP, vol. 11, no. 26, pp. 5227-40, Jul. 2009. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/19551189 [61] B. r. Winther-Jensen and K. West, "Vapor-Phase Polymerization of 3,4Ethylenedioxythiophene: A Route to Highly Conducting Polymer Surface Layers," Macromolecules, vol. 37, no. 12, pp. 4538-4543, May 2004. [Online]. Available: http://dx.doi.org/10.1021/ma498641 [62] S. Admassie, F. Zhang, A. Manoj, M. Svensson, M. R. Andersson, and 0. Inganis, "A polymer photodiode using vapour-phase polymerized PEDOT as an anode," Solar Energy Materials and Solar Cells, vol. 90, no. 2, pp. 133-141, Jan. 2006. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S0927024805000425 152 [63] V. ent, Scardaci, R. conductive Coull, carbon and J. nanotube N. films Coleman, "Very on flexible thin transpar- substrates," Physics Letters, vol. 97, no. 2, P. 023114, 2010. [Online]. http://link.aip.org/link/APPLAB/v97/i2/p023114/s1&Agg=doi Applied Available: [64] Y. H. Kim, C. Sachse, M. L. Machala, C. May, L. Miiller-Meskamp, and K. Leo, "Highly Conductive PEDOT:PSS Electrode with Optimized Solvent and Thermal Post-Treatment for ITO-Free Organic Solar Cells," Advanced Functional Materials, vol. 21, no. 6, pp. 1076-1081, 2011. [Online]. Available: littp://dx.doi.org/10.1002/adfm.201002290 [65] P. Peumans, S. Uchida, and S. R. Forrest, "Efficient bulk heterojunction photovoltaic cells using small- molecular-weight organic thin films," Nature, vol. 425, 2003. [66] S. Schultes, P. Sullivan, S. Heutz, B. Sanderson, and T. Jones, "The role of molecular architecture and layer composition on the properties and performance of CuPc-C60 photovoltaic devices," Materials Science and Engineering: C, vol. 25, no. 5-8, pp. 858 -865, Dec. 2005. [Online]. Available: http://www.sciencedirect. com/science/article/pii/S0928493105001311 [67] B. F. Yang, K. Sun, and S. R. Forrest, "Efficient Solar Cells Using All-Organic Nanocrystalline Networks," Advanced Materials, vol. 19, pp. 4166--4171, 2007. [68] N. Li and S. R. Forrest, "Tilted bulk heterojunction organic phoApplied Physics tovoltaic cells grown by oblique angle deposition," Available: no. 12, p. 123309, 2009. [Online]. Letters, vol. 95, littp://liik.ail).org/liik/APPLAB/v95/i12/p123309/sI&Agg=doi [69] N. R. Armstrong, C. Carter, C. Donley, A. Simmuonds, P. Lee, M. Bruibach, B. Kippelen, B. Domercq, and S. Yoo, "Interface modification of ITO thin films: organic photovoltaic cells," Thin Solid Films, vol. 445, no. 2, pp. 342--352, Dec. 2003. [Online]. Available: http://www.sciencedirect.coin/science/article/pii/S0040609003011830 [70] H. J. Snaith, H. Kenrick, M. Chiesa, and R. H. Friend, "Morphological and electronic consequences of modifications to the polymer anode PEDOT:PSS," Polymer, vol. 46, no. 8, pp. 2573--2578, Mar. 2005. [Online]. Available: http://www.scieicedirect.coi/scielice/article/pii/S0032386105001291 [71] M. W. Rowell, M. A. Topinka, M. D. McGehee, H.-J. Prall, G. Dennler, N. S. Sariciftei, L. Hu, and G. Gruner, "Organic solar cells with carbon nanotube network electrodes," Applied Physics Available: 2006. [Online]. no. 23, p. 233506, Letters, vol. 88, http://link.aip.org/liik/APPLAB/v88/i23/p233506/s1&Agg=doi [72] S.-I. Na, S.-S. Kim, J. Jo, and D.-Y. Kim, "Efficient and Flexible ITO-Free Organic Solar Cells Using Highly Conductive Polymer Anodes," 153 Advanced Materials, vol. 20, no. 21, pp. 4061-4067, 2008. [Online]. Available: http://dx.doi.org/10.1002/adma.200800338 [73] M. W. Rowell and M. D. McGehee, "Transparent electrode requirements for thin film solar cell modules," Enerqy & Environmental Science, vol. 4, no. 1, p. 131, 2011. [Online]. Available: http://xlink.rsc.org/?DOI=c0ee00373e [74] U. Zschieschang, T. Yamamoto, K. Takimiya, H. Kuwabara, M. Ikeda, T. Sekitani, T. Someya, and H. Klauk, "Organic Electronics on Banknotes," Advanced Materials, vol. 23, pp. 654-658, 2011. [75] M. Jorgensen, K. Norrman, and F. C. Krebs, "Stability/degradation of polymer solar cells," Solar Energy Materials and Solar Cells, vol. 92, no. 7, pp. 686-714, Jul. 2008. [Online]. Available: http://inkinghub.elsevier.com/retrieve/pii/S0927024808000056 [76] X. Xi, F. Li, Q. Meng, Y. Ding, J. Ji, Z. Shi, and G. Li, "The investigation of the stability and optimal encapsulation time for ITO/CuPc/C60/Al bilayer cells," Solar Energy Materials and Solar Cells, vol. 94, no. 5, pp. 924-929, May 2010. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S0927024810000036 [77] K. Kawano, R. Pacios, D. Poplavskyy, J. Nelson, D. Bradley, and J. Durrant, "Degradation of organic solar cells due to air exposure," Solar Energy Materials and Solar Cells. vol. 90, no. 20, pp. 3520-3530, Dec. 2006. [Online]. Available: http://inkinghub.elsevier.com/retrieve/pii/S0927024806002960 [78] W. J. Potscavage, S. Yoo, B. Domercq, and B. Kippelen, "Encapsulation of pentacene/C[sub 60] organic solar cells with Al[sub 2]O[sub 3] deposited by atomic layer deposition," Applied Physics Letters, vol. 90, no. 25, p. 253511, 2007. [Online]. Available: http://link.aip.org/link/APPLAB/v90/i25/p253511/s1&Agg=doi [79] R. Franke, B. Maennig, A. Petrich, and M. Pfeiffer, "Long-term stability of tandem solar cells containing small organic molecules," Solar Energy Materials and Solar Cells, vol. 92, no. 7, pp. 732-735, Jul. 2008. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S0927024807004412 [80] M. Jorgensen, K. Norrman, S. a. Gevorgyan, T. Tromholt, B. Andreasen, and F. C. Krebs, "Stability of polymer solar cells." Advanced Materials, vol. 24, pp. 580-612, Feb. 2012. [Online]. Available: http://www.ncbi.nlml.nili.gov/pibmed/22213056 [81] R. Tipnis, J. Bernkopf, S. Jia, J. Krieg, S. Li, M. Storch, and D. Laird, "Largearea organic photovoltaic moduleFabrication and performance," Solar Energy Materials and Solar Cells, vol. 93, no. 4, pp. 442-446, 2009. 154 [82] B. Zimmermann, U. Wirfel, and M. Niggemann, "Longterin stability of efficient inverted P3HT:PCBM solar cells," Solar Eneryy Materials and Solar Cells, vol. 93, no. 4. pp. 491 496, 2009. [83] P. E. Burrows, V. Bulovic, S. R. Forrest, L. S. Sapochak, D. M. McCarty, and M. E. Thompson, "Reliability and degradation of organic light emnitting devices," Applied Physics Letters, vol. 65, no. 23, p. 2922, 1994. [Online]. Available: http://link.ail).org/link/APPLAB/v65/i23/p2922/s1&Agg=doi [84] C. H. Peters, I. T. Sachs-Quintana, J. P. Kastrop, S. Beaupr6, M. Leclerc, and M. D. McGehee, ",High Efficiency Polymer Solar Cells with Long Operating Lifetimes," Advanced Energy Materials, vol. 1, no. 4, pp. 491-494, Jul. 2011. [Online]. Available: http://doi.wiley.coi/10.1002/aeni.201100138 [85] C.-Y. Chang, C.-T. Tsai, "Thin-filrn photovoltaic cells Chou, encapsulation by atomic Y.-J. Lee, M.-J. of polymer-based layer deposition," Chen, and F.-Y. bulk-heterojunction Organic Electron- zcs, vol. 10, no. 7. pp. 1300--1306, Nov. 2009. [Online]. http://linkinghub.elsevier.com/retrieve/pii/S1566119909001979 Available: [86] M. Schaer, F. Niiesch, D. Berner, W. Leo, and L. Zuppiroli, "Water Vapor and Oxygen Degradation Mechanisms in Organic Light Emitting Diodes," Advanced FunctionalMaterials, vol. 11, no. 2, pp. 116-121, 2001. [87] N. Grossiord, J. M. Kroon, R. Andriessen, dationi mechanisms in organic photovoltaic and P. W. Blom, devices," OrYanic ics, vol. 13, no. 3, pp. 432--456, Mar. 2012. [Online]. http://liikinghub.elsevier.coi/retrieve/pii/S1566119911004046 "DegraElectron- Available: [88] E. Vorosliazi, B. Verreet, T. Aernouts, and P. Heremans, "Long-term operational lifetime and degradation analysis of P3HT:PCBM photovoltaic cells," So- lar Energy Materials and Solar Cells, vol. 95, pp. 1303-1307, May 2011. [Online]. Available: http://likinghiib.elsevier.coin/retrieve/pii/S927024810005295 [89] M. P. Nikiforov, J. Strzalka, and S. B. Darling, "Delineation of the effects of water and oxygen on the degradation of organic photovoltaic devices," Solar Energy Materials and Solar Cells, vol. 110, pp. 36 42, Mar. 2013. [Online]. Available: http://linkinghub.elsevier.coi/retrieve/pii/S927024812003315 [90] D. M. Tanenbaum, M. Herinenau, E. Voroshiazi, M. T. Lloyd, Y. Galagan, B. Zimmermann, M. H6sel, H. F. Dam, M. Jorgensen, S. a. Gevorgyan, S. Kudret, W. Maes, L. Lutsen, D. Vanderzande, U. Wirfel, R. Andriessen, R. Rosch, H. Hoppe, G. Teran-Escobar, M. Lira-Cantu, A. Rivaton, G. Y. Uzunolu, D. Gerimack, B. Andreasen, NI. V. Madsen, K. Norrman, and F. C. Krebs, 'The ISOS-3 inter-laboratory collaboration focused on the stability of a variety of organic photovoltaic devices," RSC Advances, vol. 2, no. 3, p. 882, 2012. [Online]. Available: http://xlink.rse.org/?DOI=c1ra00686j 155 [91] B. Zimmermann, U. Wurfel, A. Gombert, and M. Niggemann, "STABILITY OF EFFICIENT ITO-FREE INVERTED ORGANIC SOLAR CELLS," in 23rd European Photovoltaic Solar Energy Conference, no. September, Valencia, Spain, 2008, pp. 235-237. [92] M. 0. Reese, M. S. White, G. Rumbles, D. S. Ginley, and S. E. Shaheen, "Optimal negative electrodes for poly(3-hexylthiophene): [6,6]-phenyl C61-butyric acid methyl ester bulk heterojunction photovoltaic devices," Applied Physics Letters, vol. 92, p. 053307., 2008. [93] R. de Bettignies, J. Leroy, M. Firon, C. Sentein, S. Bailly, and S. Guillerez, "Ageing process in organic photovoltaic solar cell," in European Conference on Hybrid and Organic Solar Cells, 2006. [94] S. Ghorashi, a. Behjat, and R. Ajeian, "The effect of a buffer layer on the performance and optimal encapsulation time of ITO/CuPc/C60/buffer/Cu bilayer cells," Solar Energy Materials and Solar Cells, vol. 96, no. 1, pp. 50-57, Jan. 2012. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/SO927024811004934 [95] M. Wang, F. Xie, J. Du, Q. Tang, S. Zheng, Q. Miao, J. Chen, N. Zhao, and J. Xu, "Degradation mechanism of organic solar cells with aluminum cathode," Solar Energy Materials and Solar Cells, vol. 95, no. 12, pp. 3303--3310, Dec. 2011. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/SO927024811004235 [96] N. Kim, W. J. Potscavage, B. Domercq, B. Kippelen, and S. Graham, "A hybrid encapsulation method for organic electronics," Applied Physics Letters, vol. 94, no. 16, p. 163308, 2009. [Online]. Available: http://link.aip.org/link/APPLAB/v94/i16/p163308/sI&Agg=doi [97] C. J. Brabec, S. Gowrisanker, J. J. M. Halls, D. Laird, S. Jia, and S. P. Williams, "Polymer-Fullerene Bulk-Heterojunction Solar Cells," Advanced Materials, vol. 22, pp. 3839-3856, Aug. 2010. [Online]. Available: http://doi.wiley.com/10.1002/adma.200903697 [98] M. D. Irwin, D. B. Buchholz, a. W. Hains, R. P. H. Chang, and T. J. Marks, "p-Type semiconducting nickel oxide as an efficiency-enhancing anode interfacial layer in polymer bulk-heterojunction solar cells," Proceedings of the National Academy of Sciences, vol. 105, no. 8, pp. 2783-2787, Feb. 2008. [Online]. Available: http://www.pnas.org/cgi/doi/10.1073/pnas.0711990105 [99] J. Xue, B. P. Rand, S. Uchida, and S. R. Forrest, "A Hybrid Planar-Mixed Molecular Heterojunction Photovoltaic Cell," Advanced Materials,vol. 17, no. 1, pp. 66-71, 2005. [100] R. R. Lunt and V. Bulovic, "Transparent, near-infrared organic photovoltaic solar cells for window and energy-scavenging applications," Applied Physics 156 Letters, vol. 98, no. 11, p. 113305, Mar. Iittp://link.aip.org/link/'?APPLAB/98/113305/1 2011. [Online]. Available: Sariciftci, N. Neugebauer, H. Lungenschnied, C. Dennler, [101] G. "A new enand M. Wertheimer, M. Latreche, G. Czereniuszkin, Thin Solid capsulation solution for flexible organic solar cells," Available: Jul. 2006. [Online]. pp. 349--353, Films, vol. 511-512, http://linkinghub.elsevier.coim/retrieve/pii/S0040609005023680 [102] F. C. Krebs, J. Fyenbo, D. M. Tanenbaum, S. a. Gevorgyan, R. Andriessen, B. van Remoortere, Y. Galagan, and M. Jorgensen, "The OE-A OPV demonstrator anno domini 2011," Energy & EnvironrrrentalScience, vol. 4, no. 10. p. 4116, 2011. [Online]. Available: littp://xlink.rsc.org/?DOI=clee01891d [103] P. Madakasira, K. Inoue, R. Ulbricht, S. B. Lee, M. Zhou, J. P. Ferraris, and A. a. Zakhidov, "Multilayer encapsulation of plastic photovoltaic devices," Synthetic Metals, vol. 155, no. 2, pp. 332-335, Nov. 2005. [Online]. Available: http://inkinghub.elsevier.com/retrieve/pii/S0379677905007745 [104] M. R. Cavallari, C. 1. Cuppoletti, G. Pucker, F. J. Fonseca, A. M. Andrade, S. Carturan, G. Maggioni, A. Quaranta, M. Buffa, and M. Tonezzer, "Degradation studies of rigid and flexible rr-P3HT : PCBM bulk heterojunction solar cells encapsulated with a parylene polymeric coating," in 11th International Conference on Advanced Materials, vol. 15, no. 1, 2009. [105] S. P. Subbarao, M. E. Balilke, and I. Kynissis, "Laboratory Thin-Fihn Encapsulation of Air-Sensitive Organic Semiconductor Devices," IEEE TRANSACTIONS ON ELECTRON DEVICES, vol. 57, no. 1, pp. 153-156, 2010. [106] C. Lungenschmnied, G. Derinler, G. Czerenuzskin, M. Latreche, H. Neugebauer, and N. S. Sariciftci, "Flexible Encapsulation for Organic Solar Cells." Proceedings of SPIE, vol. 6197, p. 619712, Apr. 2006. [107] J. a. Hauch, P. Schilinsky, S. a. Choulis, R. Childers, M. Biele, and C. J. Brabec, "Flexible organic P3HT:PCBM bulk-heterojunction modules with more than 1 year outdoor lifetime," Solar Energy Materials and Solar Cells, vol. 92, no. 7, pp. 727 731, Jul. 2008. [Online]. Available: http://liikinghub.elsevier.coi/retrieve/pii/S0927024808000196 [108] M. Hosel, R. R. Sondergaard, M. Jorgensen, and F. C. Krebs, "Comparison of UV-Curing, Hotmelt, and Pressure Sensitive Adhesive as Roll-to-Roll Encapsulation Methods for Polyner Solar Cells," Advanced Engineering Materials, pp. n/a n/a, Jul. 2013. [Online]. Available: http://doi.wiley.com/10.1002/adei.201300172 [109] J. C. Hackley and T. Gougousi, "Properties of atonic layer deposited HfO2 thin films," Thin Solid Fillms, vol. 517, no. 24, pp. 6576 6583, Oct. 2009. [Online]. Available: http://linkinghub.elsevier..com/retrieve/pii/S0040609009008384 157 [110] T. 0. Kaariainen, P. Maydannik, D. C. Cameron, K. Lahtinen, P. Johansson, and J. Kuusipalo, "Atomic layer deposition on polymer based flexible packaging materials: Growth characteristics and diffusion barrier properties," Thin Solid Films, vol. 519, no. 10, pp. 3146--3154, Mar. 2011. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S0040609010018201 [111] C.-Y. Chang and F.-Y. Tsai, "Efficient and air-stable plastics-based polymer solar cells enabled by atomic layer deposition," Journal of Materials Chemistry, vol. 21, pp. 5710-5715, 2011. [112] M. 0. Reese, S. a. Gevorgyan, M. Jorgensen, E. Bundgaard, S. R. Kurtz, D. S. Ginley, D. C. Olson, M. T. Lloyd, P. Morvillo, E. a. Katz, A. Elschner, 0. Haillant, T. R. Currier, V. Shrotriya, M. Hermenau, M. K. Riede, K. R. Kirov, G. Trimmel, T. Rath, 0. Ingands, F. Zhang, M. Andersson, K. Tvingstedt, M. Lira-Cantu, D. Laird, C. McGuiness, S. J. Gowrisanker, M. Pannone, M. Xiao, J. Hauch, R. Steim, D. M. DeLongchamnp, R. RB6sch, H. Hoppe, N. Espinosa, A. Urbina, G. Yaman-Uzunoglu, J.-B. Bonekamp, A. J. van Breemen, C. Girotto, E. Voroshazi, and F. C. Krebs, "Consensus stability testing protocols for organic photovoltaic materials and devices," Solar Energy Materials and Solar Cells, vol. 95, no. 5, pp. 1253-1267, May 2011. [Online]. Available: http://inkinghub.elsevier.com/retrieve/pii/S092702481100050X [113] M. 0. Reese, A. J. Morfa, M. S. White, N. Kopidakis, S. E. Shaheen, G. Rumbles, and D. S. Ginley, "Pathways for the degradation of organic photovoltaic P3HT:PCBM based devices," Solar Energy Materials and Solar Cells, vol. 92, no. 7, pp. 746-752, Jul. 2008. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S0927024808000305 [114] L. K. Wagner, K. M. Colwell, and J. C. Grossman, "Morphology optimization in bulk heterojunction photovoltaics," unpublished, pp. 1-7, 2009. [115] W. Ma, C. Yang, X. Gong, K. Lee, and A. J. Heeger, "Thermally Stable, Efficient Polymer Solar Cells with Nanoscale Control of the Interpenetrating Network Morphology," Advanced Functional Materials, vol. 15, no. 10, pp. 1617-1622, Oct. 2005. [Online]. Available: http://doi.wiley.com/10.1002/adfm.200500211 [116] Y. Matsuo, Y. Sato, T. Niinomi, I. Soga, H. Tanaka, and E. Nakamura, "Columnar structure in bulk heterojunction in solution-processable three-layered p-i-n organic photovoltaic devices using tetrabenzoporphyrin precursor and silylmethyl[60]fullerene." Journal of the American Chemical Society, vol. 131, no. 44, pp. 16048--50, Nov. 2009. [Online]. Available: http://pubs.acs.org/doi/abs/10.1021/ja9048702 [117] S. R. Forrest, "The Limits to Organic Photovoltaic Cell Efficiency," MRS Bulletin, vol. 30, pp. 28-32, 2005. 158 [118] M. Pope and C. E. Swenberg, "Electronic processes in organic crystals and polymers," Oxford University Press, Oxford, 1999. [119] P. Peumans and S. R. Forrest, "Separation of geminate charge-pairs at donor acceptor interfaces in disordered solids," Chemrical Physics Letters, vol. 398, pp. 27-31, 2004. [120] P. Peumans, A. Yakimov, and S. R. Forrest, "Small molecular weight organic thin-film photodetectors and solar cells," Journal of Ap- plied Physics, vol. 93, no. 7, p. 3693, 2003. [Online]. http://link.aip.org/link/JAPIAU/v93/i7/p3693/s1&Agg=doi Available: [121] R. S. Crandall, "Modeling of thin film solar cells: Uniform field approximation," Journal of Applied Physics, vol. 54, no. 12, p. 7176, 1983. [Online]. Available: http://scitation.aip.org/content/aip/journal/jap/54/12/10.1063/1.331955 [122] J. Xue, B. P. Rand, S. Uchida, and S. R. Forrest, "Mixed donor-acceptor nolecular heterojunctions for photovoltaic applications . II . Device performance," Journal of Applied Physics, vol. 98, p. 124903, 2005. [123] N. Karl, "Charge carrier transport in organic semiconductors," Synthetic Metals, vol. 133-134, pp. 649 657, Mar. 2003. [Online]. Available: Ittp://www.sciencedirect. coim/science/article/pii/S0379677902003983 [124] J. S. Moon, J. K. Lee, S. Cho, J. Byun, and A. J. Heeger, ""Columnlike" structure of the cross-sectional morphology of bulk heterojunction materials." Nano letters, vol. 9, no. 1, pp. 230-4, Jan. 2009. http://www.ncbi.nllm.nih.gov/pubmed/19035768 [Online]. Available: [125] J. Wagner, M. Gruber, A. Hinderhofer, A. Wilke, B. Br6ker, J. Frisch, P. Amnsalen, A. Vollmer, A. Opitz, N. Koch, F. Schreiber, and W. Britting, "High Fill Cells with Factor and Open Circuit Voltage in Diindenoperylene as Donor Material," Organic Photovoltaic Advanced Functional Materials, vol. 20, no. 24, pp. 4295- 4303, Dec. 2010. [Online]. Available: http://doi.wiley.coli/10.1002/adfim.201001028 [126] R. R. Lunt, J. B. Benziger, and S. R. Forrest, "Relationship between crystalline order and exciton diffusion length in molecular organic semiconductors." Advanced Materials,vol. 22, no. 11, pp. 1233 6, Mar. 2010. [Online]. Available: lttp://www.micl)i. nln.nih.gov/pubmed/20437510 [127] R. R. Lunt, N. C. Giebink, A. A. Belak, J. B. Benziger, Forrest, "Exciton diffusionmlengths of organic semiconductor measured by spectrally resolved photoluiniescence quenching" and S. R. thin filns Journal of Applied Physics, vol. 105, no. 5, p. 053711, 2009. [Online]. Available: http://scitation.aip.org/content/aip/journal/jap/105/5/10.1063/1.3079797 159 [128] H. Najafov, B. Lee, Q. Zhou, L. C. Feldman, and V. Podzorov, "Observation of long-range exciton diffusion in highly ordered organic semiconductors." Nature materials, vol. 9, no. 11, pp. 938-43, Nov. 2010. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/20935655 [129] S. Aramaki, "Solution-Processible Crystalline Organic Semiconductors for Photovoltaic Application," in Materials Research Society Fall Meeting, 2011. [130] M. Hiramoto, M. Suezaki, and M. Yokoyama, "Effect of Thin Gold Interstitiallayer on the Photovoltaic Properties of Tandem Organic Solar Cell," Chemistry Letters, pp. 327-330, 1990. [131] a. Hadipour, B. deBoer, J. Wildeman, F. Kooistra, J. Hummelen, M. Turbiez, M. Wienk, R. A. J. Janssen, and P. Blom, "Solution-Processed Organic Tandem Solar Cells," Advanced Functional Materials, vol. 16, no. 14, pp. 1897-1903, Sep. 2006. [Online]. Available: http://doi.wiley.com/10.1002/adfm.200600138 [132] J. Y. Kim, K. Lee, N. E. Coates, D. Moses, T.-Q. Nguyen, M. Dante, and A. J. Heeger, "Efficient tandem polymer solar cells fabricated by all-solution processing." Science, vol. 317, no. 5835, pp. 222-5, Jul. 2007. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubned/17626879 [133] J. You, L. Don, K. Yoshimura, T. Kato, K. Ohya, T. Moriarty, K. Emery, C.-C. Chen, J. Gao, G. Li, and Y. Yang, "A polymer tandem solar cell with 10.6% power conversion efficiency." Nature communications, vol. 4, p. 1446, Jan. 2013. [Online]. Available: http://www.pubmedcentral.nih.gov/articlerender.fcgi?artid=3660643&tool=pmcentrez&rende: [134] B. Ray and M. a. Alam, "Random vs regularized OPV: Limits of performance gain of organic bulk heterojunction solar cells by morphology engineering," Solar Energy Materials and Solar Cells, pp. 1-9, Jan. 2012. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/SO927024811006568 [135] J. Sakai, T. Taima, T. Yamanari, and K. Saito, "Annealing effect in the sexithiophene:C70 small molecule bulk heterojunction organic photovoltaic cells," Solar Energy Materials and Solar Cells, vol. 93, no. 6-7, pp. 1149-1153, Jun. 2009. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S092702480900052X [136] H. Hoppe and N. S. Sariciftci, "Organic solar cells: An overview," Journal of Materials Research, vol. 19, no. 7, pp. 1924-1945, 2004. [Online]. Available: http://www.mrs.org/publications/jnr/jmra/2004/jul/0252.html [137] H. Hoppe, M. Niggemann, C. Winder, J. Kraut, R. Hiesgen, a. Hinsch, D. Meissner, and N. S. Sariciftci, "Nanoscale Morphology of Conjugated Polymer/Fullerene-Based Bulk- Heterojunction Solar Cells," Advanced Functional Materials, vol. 14, no. 10, pp. 1005---1011, Oct. 2004. [Online]. Available: http://doi.wiley.com/10.1002/adfm.200305026 160 [138] D. J. L. Mascaro, "Formation of In-Plane Crystals of Molecular Organic Seniconductors," Ph.D. dissertation, MIT, 2004. [139] T. S. Yu., "Solidification in a thin liquid film: Growing Alq3 needles via methanol-vapor annealing," Ph.D. dissertation, MIT, 2011. [140] J. C. Conboy, E. J. C. Olson, D. M. Adams, J. Kerino, A. Zaban, B. A. Gregg, and P. F. Barbara, "Impact of Solvent Vapor Annealing on the Morphology and Photophysics of Molecular Semiconductor Thin Films," Journal of Physical Chemistry B, vol. 102, no. 23, pp. 4516-4525, Jun. 1998. [Online]. Available: http://pubs.acs.org/doi/abs/10.1021/jp980969y [141] J. D. Zimmerman, X. Xiao, C. K. Renshaw, S. Wang, V. V. Diev, M. E. Thompson, and S. R. Forrest, "Independent control of bulk and interfacial morphologies of small molecular weight organic lieterojunction solar cells." Nano letters, Jul. 2012. [Online]. Available: http://www.ncbi.nliii.nih.gov/pubmed/22809215 [142] J. Zhao, A. Wang, M. A. Green, and F. Ferrazza, "19.8% efficient honeycomb textured nmulticrystalline and 24.4% ionocrystalline silicon solar cells," Applied Physics Letters, vol. 73, no. 14, pp. 1991-1993, 1998. [143] L. A. Pettersson, L. S. Roman, and 0. Inganas, "Modeling photocurrent action spectra of photovoltaic devices based on organic thin films," Journal of Applied Physics, vol. 86, no. 1, pp. 487-496, 1999. [Online]. Available: http://link.aip.org/link/JAPIAU/v86/il/1)487/s1&Agg=doi [144] A. Luque and S. Hegedus, Handbook of Photovoltaic Science and Enginecring. John Wiley & Sons, 2011. [145] M. D. Perez, C. Borek, S. R. Forrest, and M. E. Thompson. "Molecular and Morphological Influences on the Open Circuit Voltages of Organic Photovoltaic Devices," Journal of Anerican Chemical Society, vol. 131, no. 26, pp. 92819286, 2009. [146] N. C. Giebink, G. P. Wiederrecht, M. R. Wasielewski, and S. R. Forrest, "Thermodynamic efficiency limit of excitonic solar cells," Physical Review B, vol. 83, no. 19, p. 195326, May 2011. [Online]. Available: http://link.aps.org/doi/10.1103/PhysRevB.83.195326 [147] C. H. Henry, "Limiting efficiencies of ideal single and multiple energy gap terrestrial solar cells," Joqrnal of Applied Physics, vol. 51, no. 8, pp. 4494-4500, 1980. [148] A. J. Nozik, "Nanoscience and nanostructures for phiotovoltaics and solar fuels." Nano letters, vol. 10, no. 8, pp. 2735--41, Aug. 2010. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/20597472 161 [149] J. A. Macko, R. R. Lunt, T. P. Osedach, P. R. Brown, M. C. Barr, K. K. Gleason, and V. Bulovic, "Multijunction organic photovoltaics with a broad spectral response." Physical Chemistry Chemical Physics, Sep. 2012. [Online]. Available: http://www.ncbi.nln.nih.gov/pubined/23014483 [150] M. T. Winkler, C. R. Cox, D. G. Nocera, and T. Buonassisi, "Modeling integrated photovoltaic electrochemical devices using steady-state equivalent circuits," Proceedings of the National Academy of Sciences, vol. 110, no. 12, 2013. [151] L. Dou, J. You, J. Yang, C.-c. Chen, Y. He, S. Murase, T. Moriarty, K. Emery, G. Li, and Y. Yang, "Tandem polymer solar cells featuring a spectrally matched low-bandgap polymer," Nature Photonics, vol. 6, pp. 180-185, 2012. [Online]. Available: http://dx.doi.org/10.1038/nphoton.2011.356 [152] D. Cheyns, B. P. Rand, and P. Heremans, "Organic tandem solar cells with complementary absorbing layers and a high open-circuit voltage," Applied Physics Letters, vol. 97, no. 3, p. 033301, 2010. [Online]. Available: http://link.aip.org/link/APPLAB/v97/i3/p33301/s1&Agg=doi [153] M. K. Riede, C. L. Uhrich, J. Widmer, R. Timmreck, D. Wynands, G. Schwartz, W.-M. Gnehr, D. Hildebrandt, A. Weiss, J. Hwang, S. Sudharka, P. Erk, M. Pfeiffer, and K. Leo, "Efficient Organic Tandem Solar Cells based on Small Molecules," Advanced Functional Materials, pp. n/a--n/a, Jun. 2011. [Online]. Available: http://doi.wiley.com/10.1002/adfm.201002760 [154] D. Fujishima, H. Kanno, T. Kinoshita, E. Maruyama, M. Tanaka, M. Shirakawa, and K. Shibata, "Organic thin-film solar cell employing a novel electron-donor material," Solar Energy Materials and Solar Cells, vol. 93, no. 6-7, pp. 1029-1032, Jun. 2009. [Online]. Available: http://linkinghiib.elsevier.coin/retrieve/pii/S092702480800442X [155] G. Meusel, C. Baur, G. Letay, A. W. Bett, W. Warta, and E. Fernandez, "Spectral Response Measurements of Monolithic GaInP/Ga(In)As/ Ge TripleJunction Solar Cells: Measurement Artifacts and their Explanation," Progress in Photovoltaics: Research and Applications, vol. 11, pp. 499-514, 2003. [156] J. Gilot, M. M. Wienk, and R. A. J. Janssen, "Optimizing polymer tandem solar cells." Advanced Energy Materials, vol. 22, no. 8, pp. E67-71, Feb. 2010. [Online]. Available: http://www.ncbi.nlm.nih.gov/pubmed/20217802 [157] J. Wang, X. Ren, S. Shi, C. Leung, and P. K. Chan, "Charge accumulation induced S-shape JV curves in bilayer heterojunction organic solar cells," Organic Electronics, vol. 12, no. 6, pp. 880-885, Jun. 2011. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S1566119911000668 [158] a. Hadipour, B. deBoer, and P. Blom, "Organic Tandem and Multi-Junction Solar Cells," Advanced Functional Materials, vol. 18, no. 2, pp. 169-181, Jan. 2008. [Online]. Available: http://doi.wiley.com/10.1002/adfm.200700517 162 [159] B. E. Lassiter, J. D. Zimnmerman, A. Panda, X. Xiao, and S. R. Forrest, "Tandem organic photovoltaics using both solution and vacuum deposited small molecules," Applied Physics Letters, vol. 101, no. 6, p. 063303, 2012. [Online]. Available: http://link.aip.org/link/APPLAB/vI01/i6/p063303/s1&Agg=doi [160] B. E. Lassiter, C. Kyle Renshaw, and S. R. Forrest, "UnderstandJournal of Aping tandem organic photovoltaic cell performance," plied Physics, vol. 113, no. 21, P. 214505, 2013. [Online]. Available: http://link.aip.org/link/JAPIAU/v113/i21/p214505/si&Agg=doi [161] A. Hadipour, B. de Boer, and P. Bloin, "Device operation of organic tandem solar cells," Organic Electronics, vol. 9, no. 5, pp. 617--624, Oct. 2008. [Online]. Available: http://linkinghub.elsevier.com/retrieve/pii/S1566119908000633 Simulator," Universal Circuit [162] "Quite htt)://qucs.sourceforge.net/index.html 2014. [Online]. Available: [163] M. P. Aparicio, J. Pelegri-Sebastin, T. Sogorb, and V. Llario, "Modeling of Photovoltaic Cell Using Free Software Application for Training and Design Circuit in Photovoltaic Solar Energy," New Developments in Renewable Enerqy 2013. [Online]. Available: http://www.i tehopen.com/books/inewdevelopmnents-in-renewable-energy [164] M. Meusel, R. Adelhelm, F. Dimroth, a.W. Bett, and W. Warta, "Spectral mismatch correction and spectrometric characterization of monolithic IIIV multi-junction solar cells," Progress in Photovoltaics: Research and Applications, vol. 10, no. 4, pp. 243--255, Jun. 2002. [Online]. Available: http://doi.wiley.coin/10.1002/pip.407 [165] A. Nakajima, M. Ichikawa, T. Sawada, M. Yoshimi, and K. Yamamoto, "Optimization of Device Design for Thin-Film Stacked Tandem Solar Modules in Terms of Outdoor Performance," Japanese Journal of Applied Physics, vol. 43, no. No. 9A/B, pp. L1162 L1165, Aug. 2004. [Online]. Available: http://jjap.ipap.jp/link?JJAP/43/L1162/ [166] D. J. Mascaro, M. E. Thompson, H. I. Smith, and V. Bulovid, "Forming oriented organic crystals from amorphous thin films on Organic ElectTronpatterned substrates via solvent-vapor annealing," ics, vol. 6, no. 5-6, pp. 211-220, Dec. 2005. [Online]. Available: lttp://linkinglhub.elsevier.com/retrieve/pii/S1566119905000546 "Coarsening and soV. Bulovid, and a. E. Hosoi, [167] T. S. Yu, Journal of lidification via solvent-annealing in thin liquid filhs," Fluid Mechanics, vol. 723, pp. 69-90, Apr. 2013. [Online]. Available: http://www.journals.cambridge.org/abstractS0022112013001158 [168] S. H. driven Lee, P. J. Yoo, S. J. Kwon, iim instability." and dewetting 163 and H. H. Lee, The Journal of "Solventchemical physics, vol. 121, no. 9, pp. 4346-51, Sep. 2004. [Online]. http://www.ncbi.nlm.nih.gov/pubmed/15332985 Available: [169] J. Becker, G. Grun, R. Seemann, H. Mantz, K. Jacobs, K. R. Mecke, and R. Blossey, "Complex dewetting scenarios captured by thin-film models," Nat Mater, vol. 2, no. 1, pp. 59-63, Jan. 2003. [Online]. Available: http://dx.doi.org/10.1038/nmat788 [170] X. Tian, J. Fei, Z. Pi, C. Yang, D. Luo, F. Pei, and L. Zhang, "Selective temperature physical vapor deposition route to tri (8-hydroquinoline) aluminum nanowires, nanowalls, nanoclusters and micro-spherical chains," Solid state communications, vol. 138, no. 10, pp. 530--533, 2006. [171] W. Chen, Q. Peng, and Y. Li, "Alq3 Nanorods: Promising Building Blocks for Optical Devices," Advanced Materials, vol. 20, no. 14, pp. 2747-2750, 2008. [Online]. Available: http://dx.doi.org/10.1002/adma.200702809 [172] L. Grinaisy, T. Pusztai, T. B6rzs6nyi, J. A. Warren, and J. F. Douglas, "A general mechanism of polycrystalline growth," Nature materials, vol. 3, no. 9, pp. 645-650, 2004. [173] D. C. Borrelli, M. C. Barr, V. Bulovid, and K. K. Gleason, "Bilayer heterojunction polymer solar cells using unsubstituted polythiophene via oxidative chemical vapor deposition," Solar Energy Materials and Solar Cells, vol. 99, pp. 190-196, Apr. 2012. [Online]. Available: http://www.sciencedirect.com/science/article/pii/S0927024811006544 164