Procedure for Performing PEM Single Cell Testing - Energy

1 FSEC s Procedures For Performing PEM Single Cell Testing Test protocol for Cell Performance Tests Work Performed Under DOE Contract # DE FC36 06GO16028 April 8, 2009 EXECUTIVE SUMMARY This document defines, in detail, a test protocol for Performing proton exchange membrane (PEM) Single cell Testing . Development of this test protocol is a part of the requirements of FSEC s Task 5, Characterize MEA Performance, under DOE Contract #DE FC36 06GO16028.

2 This test protocol has been evaluated and is used at FSEC for Single cell Testing . Under this contract, FSEC will perform Single cell tests to assess the relative merits of the candidate membranes that are submitted by the Task 1 team members. These tests will be conducted at operating conditions that are of interest to the DOE and, where appropriate, will be run using identical procedures on all tested cells. Task 1 team members that are continuing beyond the Go No Go milestone are requested to review this document and identify conditions that are of concern. FSEC will iterate with these Task 1 team members to resolve these concerns Researchers following the test protocol will be able to reproduce results that have been obtained by FSEC. Contents 1.

3 Overview of FSEC s Procedures for Performing PEM Single Cell Testing .. 6 Introduction To The Test Protocol for PEM Cell Screening 6 Components to be Delivered .. 6 Details of the Cell .. 6 Membrane, CCM, and GDL Thickness 8 Cell Assembly.. 9 Pre Test Integrity 10 Tests Performed on Each Cell .. 10 Linear Sweep Voltammetry, Cyclic Voltammetry, And Cell Conditioning .. 10 Performance Verification Test .. 13 Post test Integrity 15 Post test Analysis .. 15 Cell Data Report .. 16 Fuel Cell Hydrogen Safety Plan .. 16 2. Day by Day PEM MEA Test Sequence .. 19 Assemble the 19 Day 19 Day 20 Day 20 Day 4 (at atm).. 20 Days 5, 6, and 7 (at atm) .. 21 Day 8 (at atm).. 21 Day 22 Appendix A: Gurley Number Procedure .. 23 A1 Reference 23 A2 Introduction .. 23 A3 Materials and Equipment .. 24 Materials .. 24 24 Quality 25 A4 Main Gasket 25 A5 Preparation of 25 A6 Preparation of Gas Diffusion Layer Samples.

4 26 A7 Cleaning of Fuel Cell Components .. 26 A8 Assembly Procedure .. 26 A9 Leaking Check 29 A10 Data 29 Data Sheet Gurley Number Calculations .. 30 A11 30 2 Appendix B: PEM Fuel Cell Unit Cell Assembly Procedure .. 31 B1 Reference 31 B2 Bill of Materials .. 31 Materials .. 31 31 B3 32 B4 General 32 B5 Preparation for Cell 32 B6 Assembling the Cell Fuel Cell Technology (FCT) Hardware Set.. 32 Appendix C Procedure for Leak Testing a Single Cell After Assembly .. 34 C1 External Leak Test.

5 34 34 C2 Internal Leak 35 Procedure for Internal Leak 35 Appendix D PEMFC Unit Cell 37 D1 Reference Materials .. 37 D2 Bill of 37 Materials .. 37 37 D3 Objectives .. 37 D4 General Instructions .. 38 Fuel Cell System 38 Explanation of the Test 38 Hardware Specifications .. 39 Data Filing Naming 39 Nomenclature of Test Condition 39 Handling of Gas 40 D5 Day 1 Test .. 40 Setup Cell Hardware on the Test 40 Preparation of Cell Test on the Test 40 Operation of computer to Start Up 40 Crossover and Cyclic Voltammetry Tests at 25/25/25 .. 42 Humidification of the 44 Operation of the Cell in Break In 45 Cool Down 45 D6 Day 2 Test .. 46 Crossover and Cyclic Voltammetry Tests at 25/25/25 .. 46 Polarization Curve Measurement at 80/80/73 (Air/O2 Alternating) .. 46 Crossover and Cyclic Voltammetry Tests at 80/80/73.

6 48 Hold at 400 mA/cm2 Overnight .. 49 D7 Day 3 Test .. 49 Performance Measurement at 80/80/73 (Air/O2 Alternating, atm) .. 49 3 Performance Measurement at 100/90/90 (Air, atm) .. 49 Hold Overnight at 400 mA/cm2 .. 49 D8 Day 4 Test .. 49 Performance Measurement at 100/90/90 (O2/Air Alternating, atm).. 49 Crossover and Cyclic Voltammetry Tests at 120/90/90 .. 49 Performance Measurement at 120/90/90 (Air/O2 Alternating, atm) .. 49 Hold Overnight at 400 mA/cm2.

7 49 D9 Day 5 Test .. 49 Crossover and Cyclic Voltammetry Tests at 100/90/90 .. 49 Performance Measurement at 100/90/90 (Air/O2 Alternating, atm).. 49 Stability Test (Days 5,6, and 7).. 50 D10 Day 8 50 Crossover and Cyclic Voltammetry Tests at 100/90/90 .. 50 Performance Test at 100/90/90 (Air/O2 Alternating, atm).. 50 Cool 50 D11 Day 9 Test .. 51 Crossover and Cyclic Voltammetry Tests at 25/25/25 .. 51 Leak Test .. 51 Resistance Test .. 51 Shut Down and Remove from Test 51 Post Test Analysis .. 51 D15 Troubleshooting: Hardware Problems .. 51 D16 Chart Summarizing Day to Day 53 Appendix E Fluoride Concentration Measurements Test 54 E1 Checking Electrode 54 Suggested 54 Procedure .. 54 E2 Fluoride Concentration 54 Direct 54 Calibration 55 Measuring Samples with Concentrations Greater than 1 ppm .. 56 Measuring Samples with Concentrations Less than 1 ppm.

8 57 E3 Electrode Cleaning and Storage .. 58 Electrode Cleaning 58 Electrode Cleaning 58 Electrode Storage I .. 58 Electrode Storage II .. 58 Appendix F Safety Plan .. 59 F1 Scope of Work .. 60 F2 Identification of Safety 61 F3 Risk Mitigation 62 Organic Vapor 62 4 Catalyst 62 Hydrogen Leaks .. 62 Standard Operating 63 Previous Experience With 64 Safety Performance Measurement and Management of Change 64 Employee 64 Equipment 65 Maintenance of Safety Documentation .. 65 F4 Communication Plan .. 66 Emergency Response 66 Incident Reporting and Lessons Learned .. 66 F5 Sample Handling and 67 F6 67 Appendix G Facilities and Instrumentation .. 68 G1 Membrane 68 G2 Membrane Electrode Assembly Fabrication.

9 68 G3 Electrochemical 68 G4 Materials Characterization .. 68 5

10 Introduction to the Test Protocol for PEM Cell Tests PEM Single cell Testing for performance, durability and accelerated stress is conducted on a Fee for Service basis at a number of government as well as commercial laboratories. These services are available for the individual Task 1 team members with customer specific protocols to meet their individual Testing requirements. This document defines the PEM test procedures that will be used at FSEC for conducting the screening tests that are required under FSEC s Task 5 Characterize performance of MEA of the DOE program DE PS36 6095020.