Progress in the Understanding of PEFC Degradation related to Liquid Water interactions

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1 Progress in the Understanding of PEFC Degradation related to Liquid Water interactions K. Andreas Friedrich, German Aerospace Center (DLR), Institute of Technical Thermodynamics

2 Outline Introduction to the issue of degradation in PEFC fuel cells Short description of Project Selected examples of degradation and mitigation results of: Catalytic layer and membrane Gas diffusion layers (GDL) Bipolar Plates Modeling

3 Development und Research Challenges for Polymer Electrolyte Fuel Cells Costs For high volume production noble metal cost will dominate the system stem cost. Therefore, loading of <0.2g Pt /kw with power density >0.9 W/cm 2 (stack size) at >0.60V (heat removal) required. Durability 5500 h operation with only 50 to 75 mv voltage loss at 0.6 A cm ,000 load cycles with humidity changes 30,000 start / stop cycles transient potentials of > 1.5 V Water management critical operation with compromise of high conductivity and formation of liquid water ~2500 starts at subzero temperatures with transformation from ice e to liquid water dimension changes of membrane

4 Polymer Electrolyte Fuel Cells State of the Art Function of Operation Source: Ballard 2009

5 EU Project Understanding of Degradation Mechanisms to Improve Components and Design of PEFC Electrode Membrane Bipolar Plates Gas diffusion layers

6 Objective of : Assessment of the different degradation processes with focus on liquid water interactions Flooding may lead to severe degradation of catalysts, gas diffusion layers and bipolar plates

7 Key Degradation Mechanisms Mechanical interaction interaction Thermal Edge failure Fiber puncture Membrane wear/tear due to shrinkage expansion Damage by abrasion or contact pressure Higher temperature exarcebates degradation Freezing leads to volume expansion of water Catalyst corrosion (support, Pt dissolution) Catalyst deactivation and surface loss (Pt sintering) (Electro)chemical Membrane thinning, pin hole formation (Functionality impaired by contaminants) Bipolar plate corrosion Levers for mitigation: Operating Conditions - Design - Materials

8 Mechanical + Chemical Stress: Edge Failure Simple gasket design: Degradation issues: Gas X-over on the edges leads to chemical degradation Mechanical shear stress during dynamic operation (membrane expansion/shrinkage) Membrane exposed to GDL fiber puncture Suitable edge/gasket designs will avoid these failure modes

9 Current Density Distribution with a Membrane a Membrane Pinhole OCV Current Density Fluctuations Current Density Distribution at under load (approx. 100 ma/cm 2 )

10 Cycling Conditions / Dry-Wet Transitions of the Cell Testing of Aquivion TM (Solexis)) based MEA - Durability tests: Dynamic cycles protocol: 40 s at 0.12 A/cm² 20 s at 0.6 A/cm² Stationary protocol: fixed j = 0.6 A/cm² - Conditioning in stationary conditions: 60 C, 1.5 bars, 0/100%RH i = 0.6 A/cm² 1,2 1 0,8 0,6 0,4 0, t (s)

11 Cycling Conditions / Dry-Wet Transitions of the Cell Enhanced durability by preventing edge failure Dynamic cycles with the Aquivion membrane during ~1000 hours (60000 cycles) before membrane failure in the active zone Polarization curves test 130-A41 (E79-03S edge protected) Voltage [V] 1 0,9 0,8 0,7 0,6 0,5 0,4 0,3 0,2 0,1 130-A41 BOL 130-A41 hour A41 hour A41 hour A41 hour A41 hour A41 hour A41 hour A41 hour A41 hour ,2 0,4 0,6 0,8 1 1,2 Current Density [A/cm²]

12 Comparison Cycling and Stationary Operation OCV still not affected for this duration Important performance degradation from low to high current densities with an acceleration for the cycling operation compared to the stationary test due to electrode degradation 1000 MAqPP C 40/60%RH 900 MAqPP C 40/60% 245h Cycling stationary U (mv) MAqPP C 40/60%RH MAqPP C 40/60%RH 306h i (ma/cm²)

13 Effect of membrane thickness on degradation HGF Voltage (V) N117 N115 NR212 NR211 Computer update Time (Hour) Air compressor shutdown Significant degradation occurred for NR211 cell during 600 to 800hours; Significant degradation occurred for NR212 cell during 800 to 1000hours. Devastating degradation for NR211 cell during 800 to 1000hours. Potential decay trend of individual cells for 1000 hours

14 Structure of MEA before and after OCV ageing before after Micro-structure Change of the MEA cross section before and after OCV degradation

15 Structure of Catalyst before and after OCV ageing (a) TEM of as-received MEA (b) TEM of anode catalyst after degradation. (c) TEM of cathode catalyst after degradation

16 Stabilized Aquivion TM Membrane OCV at 75 C C 50 % RH std Hydrogen Crossover (ma/cm²) standard grades 70 C 50 % RH stab 90 C 50 % RH std 90 C 50 % RH stab stabilized grades 1,00 0,90 Polarisation curves E79-03S + LT250EW (25cm² cell) 0.6 V constant (=~1A/cm²) 100% reactant humidification - 75 C Bar abs OCV 250 duration (hrs) 300 Cell Voltage (V) 0,80 0,70 0,60 0,50 0,40 0,00 0,20 0,40 0,60 0,80 1,00 1,20 1,40 Current Density (A/cm²) BOL Hour 1000 Hour 2000 Hour 3000 Hour 4000

17 Spectroscopic Characterization of Stabilized Aquivion TM Membranes No evidence for loss of any functional groups whereas already observed in other studies Apparent promising chemical stability of the Aquivion membrane But no OCV and < 600 hours other analyses after > 1000 hours to be discussed C-F (backbone) After 600h of cycling operation C-S (Sulfonic acid group) C-O-C (ether side chain) Confocal Raman microscopy (Chalmers University) C-S (Sulfonic acid group) Vibrational modes visible with Raman spectroscopy

18 AFM Characterization of Stabilized Aquivion TM Membranes Conductive Atomic Force Microscopy (DLR) large conductive areas composed of small conductive channel features with sizes limited by the spatial resolution of the tip. No changes upon fuel cell operation detected so far. Superior water retention capabilities than Nafion 112 under similar conditions na Conductivity measurements image nm

19 Decomposition of Polymer in Electrode and GDL Partial decomposition of PTFE identified by XPS PTFE decomposition mainly on the anode Decrease of hydrophobicity Changed water balance Reversible loss of performance

20 Force - Separation Curve as measured by AFM ( HarmoniX -Mode Veedo) x/nm F/nN Peak Force Surface 0 Adhesion Force Stiffness ΔF/ Δx Dissipation Energy x/nm

21 AFM measurement of Gas Diffusion Layer (GDL) GDL with Micro Porous Coating at ambient conditions / Dissipation distribution after 12 h operation before operation after operation Anode after operation Cathode 1 μm Z-Range: 768 mev Z-Range: 768 mev Z-Range: 768 mev Overall decrease in dissipation area - at cathode more than at anode less PTFE at cathode

22 Experimental Ageing of BPP: 5 Stacks tested Durability run of 600 ma/cm 2 0,9 0,8 0,7 0,6 cell voltage in V 0,5 0,4 0,3 0,2 0,1 0,0 6 Uave SS904L at CEA 6 Uave SS316L with Au at DANA 4 Uave SS904L at ZSW 8Uave SS316L with Au at ZSW time in h 3 Uave SS316L at DANA

23 Task 5.2: Long term testing Task 5.3 experimental determination of ageing BPP: corrosion analysis 40 No obvious correlation between contamination from metallic ions and degradation within a Stack 20 Degradation Rate in V/h Cell 4 Cell 5 0

24 Task 5.2: Long term testing Task 5.3 experimental determination of ageing BPP: corrosion analysis 40 Correlation between contamination from water ions and degradation within a Stack? 20 Degradation Rate in V/h 0

25 Comparison of Corrosion and CFD modeling Results 3 Cathode 4 Inlet Inlet Outlet Relative humidity in the middle of the channel Outlet Areas (channel and landing) with a few traces of corrosion which has in the simulation a lower velocity of the gas. Areas with stronger traces of corrosion which has no different velocity in the simulation.

26 Modeling of Liquid Water in Channels Volume Of Fluid Numerical method (JRC) VOF method: developed in the 1980s a volume fraction indicator C is used to determine the location of the interface Cair = 1 Cwater = 0 Cair = 0.08 Cwater = 0.92 Cair = 0 Cwater = 1

27 Modelling of Liquid Water in Channels Geometry

28 WP 5: Simulation Results (JSR) Influence of the bipolar plate contact angle: Initial conditions:

29 Influences of (liquid) Water on Degradation Acknowledgement: Liquid water lead to enhanced catalyst layer degradation Wet-dry cycles lead to mechanical stress on membranes Liquid water plays a role in loss of hydrophobicity of GDLs and other porous media Liquid water is important for corrosion of biploar plates Partners of : Acknowledgement: Partners of NRC-HGF PEFC Durability Project: Riny Yuan, Shengsheng Zhang, Cheng Huang, Shuai Ban, Jun Shen, Haijiang Wang, Institute for Fuel CellInnovation, National Research Council, Canada R. Hiesgen, University of Applied Sciences Esslingen, talk on Wednesday at 9:45

30

31 Fiber Penetration into Catalytic Layer Layer and Membrane

32 Comparison of normal and fast GDL Degradation Force/nN 28 E/meV GDL 1 7 GDL GDL 3 GDL GDL 3 GDL 2 14 H 2 O 2 Before Anode Cathode H 2 O 2 Before Anode Cathode Adhesion GDL 1: after 650 h decrease at cathode twice of anode GDL 2: after 12 h smaller decrease at anode than at cathode hole in membrane leads to very large degradation and failure Dissipation GDL 1 BC25: after 650 h decrease at cathode small increase at anode GDL 2 DC35: after 12 h large decrease at anode and larger decrease at cathode GDL 3 BC25: after 1 h cooking with H 2 O 2

33 HarmoniX -Mode for Tapping Mode AFM Force-distance-curve reconstructed by Fourier synthesis from a pulse applied by the tip at every image point Evaluation of adhesion force, phase shift, stiffness, maximal force, and dissipation energy HarmoniX -Mode (Multimode, Veeco Instr.) AFM tip for sensing higher harmonic vibrations

34 Technical results / Task Task Ex-situ characterization (DLR) Progress & Results - Conductive Atomic Force Microscopy (DLR) First characterization of Aquivion membrane Topography of Aquivion E79-03S indicates some 03S indicates some nanoscale roughness and some occasional holes. In general topography images indicate a smooth polymer surface nm Topography µ

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