Fabrication Method for Laboratory-Scale High Performance Membrane Electrode Assemblies for Fuel Cells

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1 Fabrication Method for Laboratory-Scale High Performance Membrane Electrode Assemblies for Fuel Cells Megan B. Sassin,,a* Yannick Garsany,,b Benjamin D. Gould, a and Karen E. Swider-Lyons a a U.S Naval Research Laboratory, Washington, DC b Excet inc, Springfield, VA Supporting Information The following information is contained within this document: Complete chemical/material/equipment list with part # and vendor Video showing ultrasonic deposition procedure G-code for the spray pattern Schematics of components with dimensions Photographs of the CCM hot-press and fuel cell assembly procedures

2 Figure S1. Schematic of porous aluminum vacuum plate with alignment pins, dimensions are in millimeters.

3 Figure S2. Schematic of CCM showing alignment holes in Nafion membrane, dimensions are in millimeters.

4 Figure S3. Schematic of acrylic mask used for defining deposition area, dimensions are in millimeters.

5 Figure S4. Schematic of in-house fabricated aluminum platens used for hot-pressing the CCMs, dimensions are in millimeters.

6 Figure S5. Photographs showing the steps of CCM hot-press procedure.

7 Figure S6. Schematic showing the 9 locations that thickness measurements are made on the GDM and the CCM, numbers represent typical measured values for each component in micrometers, for use in Eq. 3.

8 11 Figure S7. Schematic of Teflon gasket, dimensions are in millimeters.

9 Figure S8. Photograph of steps used in the assembly of a single fuel cell

10 Figure S9. Exploded view of the assembled cell and drawings of the carbon flow fields.

11 Figure S10. a) Representative cyclic voltammogram (CV) obtained from a single cell. b) Hydrogen adsorption/desorption region (corrected for double layer charging) used to determine the electrochemical surface area (ESCA) of the Pt electrocatalyst. CV recorded at a potential scan rate of 20 mv s -1, cell temperature of 30 C, gas temperatures of 50 C and gas flow rates are H 2 N 2 at 0.2 L H2 min -1 and 0.05 L N2 min -1, cell is at ambient pressure.

12 Figure S11. Representative hydrogen cross-over curve recorded for a single cell. Linear sweep voltammetry recorded at a potential scan rate of 1 mv s -1, cell temperature of 30 C, gas temperatures of 50 C and gas flow rates are H 2 N 2 at 0.2 L H2 min -1 and 0.05 L N2 min -1, cell is at ambient pressure.

13 Figure S12. Resistance and peak power density as a function of cell compression with scanning electron micrographs of the microporous layer after testing at a compression of 14% and 30%. Testing conditions: ambient pressure, 80 C cell, H 2 Air 79 C (RH100), stoichiometric flow of 2 2.

14 Chemicals, Materials, and Equipment List Chemicals Isopropanol, Analytical Grade, Sigma Aldrich Carbon-supported Pt catalyst powder, 50 wt. % Pt, Ion Power Aqueous Nafion ionomer solution, 1100 equivalent weight, 15 wt. %, Ion Power Water, 18 MΩ cm, Barnstead purification system Nitrogen or Argon, Alpha Gaz-2 grade ( %), Air-Liquide Hydrogen, Alphagas-2 grade, ( %), Air-Liquide Oxygen, Alphagas-2 grade, ( %), Air-Liquide Air, Alphagas-2 grade, ( %), Air-Liquide Materials Qorpack Graduated Glass Bottle Beaker, 60 ml, part# GH , Cole-Parmer Disposable glass pipets, part# B, VWR Stir bars, 20x20 cross, part# SBM-2020-CRO, stirbar.com HP Nafion membrane, H + form, Ion Power Acrylic sheet, part# 8560K172, McMaster-Carr Fiber-reinforced Teflon, 5 mils thick, part# PC-5, Precision Coating Sigracet 25BC gas diffusion media, part# 25BC, Fuel Cells Etc., cut into 3.56 cm x 3.56 cm pieces Spec-Wipe, part# , VWR Skived PTFE sheet, 1, 2, 3, 4, and 5 mils thick, part# N/A, ENFLO Power Duster by Skillcraft, part# 2RRD2, Grainger Equipment High shear mixer, T10 Basic, Ultra Turrax Stir plate, model Big Squid white, IKA CNC router table, model VR-1414, Velox CNC Heated vacuum table, mm mm 50.4 mm, part # HVT50, Nuvant Systems Inc. Porous aluminum plate, Metapor, 250 mm 250 mm 30 mm, part #819K31, McMaster-Carr Syring pump, model NX-1000, syringepump.com PTFE tipped plunger and dispenser syringe, part# , SGE Analytical Science Ultrasonic narrow spray atomizer nozzle, 316SS model# NS60K316, Sonaer Inc Sonozap ultrasonic generator, Sonaer Inc Single micro-feed tube (Model SMF-20), Sonaer Inc Pin point spray shaper, Sonaer Inc Balance, model M-220D, Denver Instrument Hot-press, model , Carver Digimatic Micrometer, Model MDC-1 PX, Mitutoyo Aluminum platens, 76.2 mm 76.2 mm 12.8 mm Thermocouple, part TMTSS , Omega Digital thermocouple reader, Omegaette HH303 Type KJ, Omega Laser Mini engraver/cutter, Helix Model 8000, Epilog

15 Electronic torque wrench, model Proto J6345, Company Test fixture, 10 cm 2, Fuel Cell Technologies Fuel cell test stand, model 850e, Scribner Potentiostat/galvanostat, model 1287, Solartron Analytical Software MACH3 control software, Newfrangled Solutions LLC ( ) Solidworks 2015 FlashCut CNC (Demo Version ), G-code used for spray pattern: Below is the G-code written to spray Spray path#1 through Spray path#4. The code was written has a loop. L corresponds to number of loops. One loop correspond to 4 layers (Spray path#1 through Spray path#4 deposited), two loops correspond to 8 layers. % O0001 (File created using FlashCut CNC DXF Import) (Import File: MASK-10cm 2 and Patterns_YG_ DXF) (Import Date: 8/19/2015) G90 G54 G00 X0 Y0 Z0 T1 M06 M98 P002 L2 (L IS THE NUMBER OF LOOPS) M30 O002 G90 G54 N10 G00 X Y N20 G01 X Y F40.00 N30 G03 X Y I J N40 G01 X Y N50 G02 X Y I J N60 G01 X Y

16 N70 G03 X Y I J N80 G01 X Y N90 G02 X Y I J N100 G01 X Y N110 G03 X Y I J N120 G01 X Y N130 G02 X Y I J N140 G01 X Y N150 G03 X Y I J N160 G01 X Y N170 G02 X Y I J N180 G01 X Y N190 G03 X Y I J N200 G01 X Y N210 G02 X Y I J N220 G01 X Y N230 G03 X Y I J N240 G01 X Y N250 G02 X Y I J N260 G01 X Y N270 G03 X Y I J N280 G01 X Y N290 G02 X Y I J N300 G01 X Y N310 G03 X Y I J N320 G01 X Y N330 G02 X Y I J N340 G01 X Y N350 G03 X Y I J N360 G01 X Y N370 G02 X Y I J N380 G01 X Y N390 G03 X Y I J N400 G01 X Y N410 G02 X Y I J N420 G01 X Y N430 G03 X Y I J N440 G01 X Y N450 G02 X Y I J N460 G01 X Y N470 G03 X Y I J N480 G01 X Y N490 G02 X Y I J0.0000

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Facile and Gram-scale Synthesis of Metal-free Catalysts: Toward Realistic Applications for Fuel Cells

Supplementary Information Facile and Gram-scale Synthesis of Metal-free Catalysts: Toward Realistic Applications for Fuel Cells Ok-Hee Kim 1, Yong-Hun Cho 2, Dong Young Chung 3,4, Minjeong Kim 3,4, Ji