CENTER FOR NANOSCALE SCIENCE AND ENGINEERING Standard Operating Procedures Large Sputtering Machine By Brian Wajdyk, Bonnie Cheng, Matt Deye Version 1.1 Page 1 of 15 Important • • • • • You can only use CeNSE laboratories and equipment if you have been approved by Brian or Chuck, reserved the tool on the calendar, and filled out a form. No Exceptions! If the equipment is acting unusual STOP! Please discuss with Brian or Chuck before proceeding and leave a note on the machine. Gloves should be worn while handling substrate and deposition to reduce contamination. Any accidental damage must be reported immediately. All CeNSE laboratories are protected by video surveillance. Version 1.1 Page 2 of 15 Machine exterior and chamber Figure 1a: Chambers Figure 1b: Left panel control Figure 2a: Right panel control Version 1.1 Page 3 of 15 Figure 2b: Deposition Monitor Version 1.1 Page 4 of 15 Other Parts of the Machine Figure 3a: Stage Figure 3b: Inside Load Lock Chamber Figure 3c: Motor controllers Version 1.1 Page 5 of 15 Operating Procedure 1. Preparation 1.1. Before beginning, be sure to wear gloves to reduce contamination and to protect the hands. 2. Start-up operations 2.1. Turn on compressed air cylinder. Check that regulator is set to 60 psi. 2.2. Turn on argon cylinder. Check that regulator is set to 30psi. 3. Load the sample 3.1. Remove the lid from load lock chamber. 3.1.1. If the chamber is under vacuum, turn on nitrogen gas to flood chamber to open it. Be sure to turn off nitrogen afterwards. 3.2. Use wrench from inside chamber to loosen clamps on the stage. Be sure to place the wrench back inside the chamber 3.3. Clamp the sample to the stage 3.4. Place the stage back in the chamber, with the sample facing down, aligning the slots on the pins 3.5. Replace the lid on the load lock chamber 3.6. Put the “on” button for the load lock vacuum located on the machine control cabinet 3.7. Turn on the load lock ion gauge. Press the “gauge” button on the display that says load lock ion gauge. Wait for the gauge to stabilize ( at least 5 e-6) 3.8. Turn on the main chamber ion gauge. Press the “IG1 button on the display that says main chamber ion gauge. 3.9. Wait for chamber to pressurize (About 30 minutes) 4. Transferring the holder 4.1. Turn gauges off. 4.2. Manually crank open the isolation valve in the counter-clockwise direction until the crank stops. 4.3. Slowly slide in your sample using the transfer handle. Push slowly add steadily until the handle rests against the stop ring. DO NOT TWIST THE HANDLE 4.4. Use controller to move the stage upwards to align the screw with the stage 4.5. Once the screw is aligned, press FWD on the controller to screw it on (or screw it on manually) 4.6. Once it us screwed on correctly, use controller to move the stage downwards to a measurement of 4 inches. 4.7. Pull the stage apparatus back all the way using the transfer handle 4.8. Use crank to close the isolation valve. It will be fully closed when you hear the valve click. 4.9. Turn off the load lock vacuum and turn on rotating stage. Version 1.1 Page 6 of 15 Operating Procedure, continued 5. Running the Sputtering Process (Completed on the computer) 5.1. Construct layers 5.1.1.Click “Program Layers” 5.1.2.Enter desired parameters 5.1.3.Name and save the layer 5.1.4.Repeat for as many layers as needed 5.2. Construct a Process 5.2.1.Click “Program Processes” 5.2.2.High light the desired layer and click “add” 5.2.3.Repeat until all desired layers are listed under process 5.2.4.Save the process list 5.3. Run the process 5.3.1.Click on “Run Process” 5.3.2.Enter the process name file or select “browse” 5.3.3.Other information on the screen is NOT necessary. 5.3.4. Click “next” 5.3.5.When the main chamber has reached the desired vacuum (best is in the -7 range), follow the instructions on the screen to start. 6. Unloading the substrate 6.1. Open the transfer gate valve 6.2. Push the transfer into the main chamber with the transfer handle. Push slowly and steadily until the handle rests against the stop ring. DO NOT TWIST THE HANDLE 6.3. While looking through the viewport, bring the hoist “in” using the pendant control 6.4. Bring the hoist in until the pins on the transfer ring are just in the slots on the substrate holder. Turn the screw with the knob on top of the hoist assembly to line the slots with the pins 6.5. Release the holder from the hoist. Turn the screw with the knob on top of the hoist assemble counter-clockwise to release the holder. Turn the knob until the holder drops from the hoist. 6.6. Bring the hoist” out until the holder is clear of the pins on the transfer 6.7. Push the transfer out of the chamber 6.8. Close the transfer gate valve. The valve will make a click when it is fully closed 7. Removing the substrate 7.1. Push the “off” button for the load lock vacuum. The button is on the machine control cabinet Version 1.1 Page 7 of 15 7.2. Turn on Nitrogen cylinder. 7.3. Put on gloves 7.4. Remove the lid from the load lock chamber 7.5. Turn off the nitrogen cylinder 7.6. Remove the substrate holder. 7.7. Remove the substrate from under the clips on the holder and re- tighten the screws 7.8. Place the holder on the ring of the transfer. The substrate side will be facing down and the pins on the ring will fit into the slots on the substrate holder 7.9. Place the lid on the load lock chamber Version 1.1 Page 8 of 15 Deposition material properties:1 Formula Ag AgBr AgCl Al Al2O3 Al4C3 AlF3 AlN AlSb As As2Se3 Au B B2O3 B4C BN Ba BaF2 BaN2O6 BaO BaTiO3 BaTiO3 Be BeF2 BeO Bi Bi2O3 Bi2S3 Bi2Se3 Bi2Te3 BiF3 C C C8H8 Ca CaF2 1 Density 10.5 6.47 5.56 2.70 3.97 2.36 3.07 3.26 4.36 5.73 4.75 19.3 2.37 1.82 2.37 1.86 3.5 4.886 3.244 5.72 5.999 6.035 1.85 1.99 3.01 9.8 8.9 7.39 6.82 7.7 5.32 2.25 3.52 1.1 1.55 3.18 Z-Ratio 0.529 1.18 1.32 1.08 0.336 ? ? ? 0.743 0.966 ? 0.381 0.389 ? ? ? 2.1 0.793 1.261 ? 0.464 0.412 0.543 ? ? 0.79 ? ? ? ? ? 3.26 0.22 ? 2.62 0.775 Acoustic Impedance 16.69 7.48 6.69 8.18 26.28 11.88 9.14 23.18 22.70 4.20 11.13 7.00 19.03 21.43 16.26 11.18 2.71 40.14 3.37 11.39 SQM-160 User’s Guide, Version 4.06. Sigma Instruments, Inc. 2000-2008. Version 1.1 Page 9 of 15 Material Name Silver Silver Bromide Silver Chloride Aluminum Aluminum Oxide Aluminum Carbide Aluminum Fluoride Aluminum Nitride Aluminum Antimonide Arsenic Arsenic Selenide Gold Boron Boron Oxide Boron Carbide Boron Nitride Barium Barium Fluoride Barium Nitrate Barium Oxide Barium Titanate (Tetr) Barium Titanate (Cubic) Beryllium Beryllium Fluoride Beryllium Oxide Bismuth Bismuth Oxide Bismuth Trisuiphide Bismuth Selenide Bismuth Telluride Bismuth Fluoride Carbon (Graphite) Carbon (Diamond) Parlyene (Union Carbide) Calcium Calcium Fluoride Formula CaO CaO-SiO2 CaSO4 CaTiO3 CaWO4 Cd CdF2 CdO CdS CdSe CdTe Ce CeF3 CeO2 Co CoO Cr Cr2O3 Cr3C2 CrB Cs Cs2SO4 CsBr CsCl CsI Cu Cu2O Cu2S Cu2S CuS Dy Dy2O3 Er Er2O3 Eu EuF2 Fe Fe2O3 FeO FeS Version 1.1 Density 3.35 2.9 2.962 4.1 6.06 8.64 6.64 8.15 4.83 5.81 6.2 6.78 6.16 7.13 8.9 6.44 7.2 5.21 6.68 6.17 1.87 4.243 4.456 3.988 4.516 8.93 6 Cu2S Cu2S CuS Dy Dy2O3 Er Er2O3 Eu EuF2 7.86 5.24 5.7 4.84 Z-Ratio ? ? 0.955 ? ? 0.682 ? ? 1.02 ? 0.98 ? ? ? 0.343 0.412 0.305 ? ? ? ? 1.212 1.41 1.399 1.542 0.437 ? 5.6 5.8 4.6 8.55 7.81 9.05 8.64 5.26 6.5 0.349 ? ? ? Acoustic Impedance 9.25 12.95 8.66 9.01 25.74 21.43 28.95 7.29 6.26 6.31 5.73 20.21 1.58 1.52 1.92 1.03 1.13 0.98 1.02 1.68 1.36 25.30 Page 10 of 15 Material Name Calcium Oxide Calcium Silicate (3) Calcium Sulfate Calcium Titanate Calcium Tungstate Cadmium Cadmium Fluoride Cadmium Oxide Cadmium Sulfide Cadmium Selenide, Cadmium Telluride Cerium Cerium (III) Fluoride Cerium (IV) Dioxide Cobalt Cobalt Oxide Chromium Chromium (III) Oxide Chromium Carbide Chromium Boride Cesium Cesium Sulfate Cesium Bromide Cesium Chloride Cesium Iodide Copper Copper Oxide Copper (I) Sulfide (Alpha) Copper (I) Sulfide (Beta) Copper (II) Sulfide Dysprosium Dysprosium Oxide Erbium Erbium Oxide Europium Europium Fluoride Iron Iron Oxide Iron Oxide Iron Sulphide Formula Ga Ga2O3 GaAs GaN GaP GaSb Gd Gd2O3 Ge Ge3N2 GeO2 GeTe Hf HfB2 HfC HfN HfO2 HfSi2 Hg Ho Ho2O3 In In2O3 In2Se3 In2Te3 InAs InP InSb Ir K KBr KCl KF KI La La2O3 LaB6 LaF3 Li LiBr Version 1.1 Density 5.93 5.88 5.31 6.1 4.1 5.6 7.89 7.41 5.35 5.2 6.24 6.2 13.09 10.5 12.2 13.8 9.68 7.2 13.46 8.8 8.41 7.3 7.18 5.7 5.8 5.7 4.8 5.76 22.4 0.86 2.75 1.98 2.48 3.128 6.17 6.51 2.61 5.94 0.53 3.47 Z-Ratio 0.593 ? 1.59 ? ? ? 0.67 ? 0.516 ? ? ? 0.36 ? ? ? ? ? 0.74 0.58 ? 0.841 ? ? ? ? ? 0.769 0.129 10.189 1.893 2.05 ? 2.077 0.92 ? ? ? 5.9 1.23 Acoustic Impedance 14.89 5.55 13.18 17.11 24.53 11.93 15.22 10.50 11.48 68.45 0.87 4.66 4.31 4.25 9.60 1.50 7.18 Page 11 of 15 Material Name Gallium Gallium Oxide (B) Gallium Arsenide Gallium Nitride Gallium Phosphide Gallium Antimonide Gadolinium Gadolinium Oxide Germanium Germanium Nitride Germanium Oxide Germanium Telluride Hafnium Hafnium Boride, Hafnium Carbide Hafnium Nitride Hafnium Oxide Hafnium Silicide Mercury Holminum Holminum Oxide Indium Indium Sesquioxide Indium Selenide Indium Telluride Indium Arsenide Indium Phosphide Indium Antimonide Iridium Potassium Potassium Bromide Potassium Chloride Potassium Fluoride Potassium Iodide Lanthanum Lanthanum Oxide Lanthanum Boride Lanthanum Fluoride Lithium Lithium Bromide Formula LiF LiNbO3 Lu Mg MgAl2O4 MgAl2O6 MgF2 MgO Mn MnO MnS Mo Mo2C MoB2 MoO3 MoS2 Na Na3AlF6 Na5AL3F14 NaBr NaCl NaClO3 NaF NaNO3 Nb Nb2O3 Nb2O5 NbB2 NbC NbN Nd Nd2O3 NdF3 Ni NiCr NiCrFe NiFe NiFeMo NiO P3N5 Version 1.1 Density 2.638 4.7 9.84 1.74 3.6 8 3.18 3.58 7.2 5.39 3.99 10.2 9.18 7.12 4.7 4.8 0.97 2.9 2.9 3.2 2.17 2.164 2.558 2.27 8.578 7.5 4.47 6.97 7.82 8.4 7 7.24 6.506 8.91 8.5 8.5 8.7 8.9 7.45 2.51 Z-Ratio 0.778 0.463 ? 1.61 ? ? 0.637 0.411 0.377 0.467 0.94 0.257 ? ? ? ? 4.8 ? ? ? 1.57 1.565 0.949 1.194 0.492 ? ? ? ? ? ? ? ? 0.331 ? ? ? ? ? ? Acoustic Impedance 11.35 19.07 5.48 13.86 21.48 23.42 18.91 9.39 34.36 1.84 5.62 5.64 9.30 7.40 17.95 26.68 Page 12 of 15 Material Name Lithium Fluoride Lithium Niobate Lutetium Magnesium Magnesium Aluminate Spinel Magnesium Fluoride Magnesium Oxide Manganese Manganese Oxide Manganese (II) Sulfide Molybdenum Molybdenum Carbide Molybdenum Boride Molybdenum Trioxdide Molybdenum Disulfide Sodium Cryolite Chiolite Sodium Bromide Sodium Chloride Sodium Chlorate Sodium Fluoride Sodium Nitrate Niobium (Columbium) Niobium Trioxide Niobium (V) Oxide Niobium Boride Niobium Carbide Niobium Nitride Neodynium Neodynium Oxide Neodynium Fluoride Nickel Nichrome Inconel Permalloy Supermalloy Nickel Oxide Phosphorus Nitride Formula Pb PbCl2 PbF2 PbO PbS PbSe PbSnO3 PbTe Pd PdO Po Pr Pr2O3 Pt PtO2 Ra Rb Rbl Re Rh Ru S8 Sb Sb2O3 Sb2S3 Sc Sc2O3 Se Si Si3N4 SiC SiO SiO2 Sm Sm2O3 Sn SnO2 SnS SnSe SnTe Version 1.1 Density 11.3 5.85 8.24 9.53 7.5 8.1 8.1 8.16 12.038 8.31 9.4 6.78 6.88 21.4 10.2 5 1.53 3.55 21.04 12.41 12.362 2.07 6.62 5.2 4.64 3 3.86 4.81 2.32 3.44 3.22 2.13 2.648 7.54 7.43 7.3 6.95 5.08 6.18 6.44 Z-Ratio 1.13 ? 0.661 ? 0.566 ? ? 0.651 0.357 ? ? ? ? 0.245 ? ? 2.54 ? 0.15 0.21 0.182 2.29 0.768 ? ? 0.91 ? 0.864 0.712 *1000 ? 0.87 1 0.89 ? 0.724 ? ? ? ? Acoustic Impedance 7.81 13.36 15.60 13.56 24.73 36.04 3.48 58.87 42.05 48.52 3.86 11.50 9.70 10.22 12.40 10.15 8.83 9.92 12.20 Page 13 of 15 Material Name Lead Lead Chloride Lead Fluoride Lead Oxide Lead Sulfide Lead Selenide Lead Stannate Lead Telluride Palladium Palladium Oxide Polonium Praseodymium Praseodymium Oxide Platinum Platinum Oxide Radium Rubidium Rubidium Iodide Rhenium Rhodium Ruthenium Sulphur Antimony Antimony Trioxide Antimony Trisulfide Scandium Scandium Oxide Selenium Silicon Silicon Nitride Silicon Carbide Silicon (II) Oxide Silicon Dioxide Samarium Samarium Oxide Tin Tin Oxide Tin Sulfide Tin Selenide Tin Telluride Formula Sr SrF2 SrO Ta Ta2O5 TaB2 TaC TaN Tb Tc Te TeO2 Th ThF4 ThO2 ThOF2 Ti Ti2O3 TiB2 TiC TiN TiO TiO2 Tl TlBr TlCl TlI U U3O8 U4O9 UO2 V V2O5 VB2 VC VN VO2 W WB2 WC Version 1.1 Density 2.6 4.277 4.99 16.6 8.2 11.15 13.9 16.3 8.27 11.5 6.25 5.99 11.694 6.32 9.86 9.1 4.5 4.6 4.5 4.93 5.43 4.9 4.26 11.85 7.56 7 7.09 19.05 8.3 10.969 10.97 5.96 3.36 5.1 5.77 6.13 4.34 19.3 10.77 15.6 Z-Ratio ? 0.727 0.517 0.262 0.3 ? ? ? 0.66 ? 0.9 0.862 0.484 ? 0.284 ? 0.628 ? ? ? ? ? 0.4 1.55 ? ? ? 0.238 ? 0.348 0.286 0.53 ? ? ? ? ? 0.163 ? 0.151 Acoustic Impedance 12.15 17.08 33.70 29.43 13.38 9.81 10.24 18.24 31.09 14.06 22.08 5.70 37.10 25.37 30.87 16.66 54.17 58.48 Page 14 of 15 Material Name Strontium Strontium Fluroide Strontium Oxide Tantalum Tantalum (V) Oxide Tantalum Boride Tantalum Carbide Tantalum Nitride Terbium Technetium Tellurium Tellurium Oxide Thorium Thorium (IV) Fluoride Thorium Dioxide Thorium Oxyfluoride Titanium Titanium Sesquioxide Titanium Boride Titanium Carbide Titanium Nitride Titanium Oxide Titanium (IV) Oxide Thallium Thallium Bromide Thallium Chloride Thallium Iodide (B) Uranium Tri Uranium Octoxide Uranium Oxide Uranium Dioxide Vanadium Vanadium Pentoxide Vanadium Boride Vanadium Carbide Vanadium Nitride Vanadium Dioxide Tungsten Tungsten Boride Tungsten Carbide Formula WO3 WS2 WSi2 Y Y2O3 Yb Yb2O3 Zn Zn3Sb2 ZnF2 ZnO ZnS ZnSe ZnTe Zr ZrB2 ZrC ZrN ZrO2 Version 1.1 Density 7.16 7.5 9.4 4.34 5.01 6.98 9.17 7.04 6.3 4.95 5.61 4.09 5.26 6.34 6.49 6.08 6.73 7.09 5.6 Z-Ratio ? ? ? 0.835 ? 1.13 ? 0.514 ? ? 0.556 0.775 0.722 0.77 0.6 ? 0.264 ? ? Acoustic Impedance 10.57 7.81 17.18 15.88 11.39 12.23 11.47 14.72 33.45 Page 15 of 15 Material Name Tungsten Trioxide Tungsten Disulphide Tungsten Suicide Yttrium Yttrium Oxide Ytterbium Ytterbium Oxide Zinc Zinc Antimonide Zinc Fluoride Zinc Oxide Zinc Sulfide Zinc Selenide Zinc Telluride Zirconium Zirconium Boride Zirconium Carbide Zirconium Nitride Zirconium Oxide