H2NEW LTE: Durability and AST Development

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H2NEW Hydrogen (H2) from Next-generation Electrolyzers of Water: H2NEW LTE: Durability and AST Development Deborah Myers, ANL; Shaun Alia, NREL; Rangachary Mukundan, LANL Date: June 7-11, 2021 Project ID # P196a DOE Hydrogen Program 2021 Annual Merit Review and Peer Evaluation Meeting This presentation does not contain any proprietary, confidential, or otherwise restricted information.

Transcript of H2NEW LTE: Durability and AST Development

Page 1: H2NEW LTE: Durability and AST Development

H2NEW Hydrogen (H2) from Next-generation Electrolyzers of Water: H2NEW LTE: Durability and AST Development Deborah Myers, ANL; Shaun Alia, NREL; Rangachary Mukundan, LANL

Date: June 7-11, 2021 Project ID # P196a DOE Hydrogen Program 2021 Annual Merit Review and Peer Evaluation Meeting

This presentation does not contain any proprietary, confidential, or otherwise restricted information.

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Project Goals

Goal: H2NEW will address components, materials integration, and manufacturing R&D to enable manufacturable electrolyzers that meet required cost, durability, and performance targets, simultaneously, in order to enable $2/kg hydrogen.

Water

H2 production Low-Temperature target <$2/kg Electrolysis (LTE)

High-Temperature Electrolysis (HTE) Hydrogen

H2NEW has a clear target of establishing and utilizing experimental, analytical, and modeling tools needed to provide the scientific understanding of electrolysis cell performance, cost, and durability tradeoffs of electrolysis systems under predicted future operating modes

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H2NEW Task 1: Durability Overview

Timeline and Budget • Start date (launch): October 1, 2020• Awarded through September 30, 2025• FY21 DOE funding for Task 1: $2.9M• Annual budget adjustments anticipated

• Durability• Cost• Efficiency

Barriers

National Lab Consortium Task Team

Deputy Director: Deborah Myers (ANL) Task Liaisons: Shaun Alia (NREL)Rangachary Mukundan (LANL) Subtask Leads: David Cullen (ORNL) Nemanja Danilovic (LBNL)

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Relevance and Impact

Electrolyzer Stack Goals by 2025 LTE PEM

Capital Cost Electrical Efficiency (LHV)

Lifetime

$100/kW 70% at 3 A/cm2

80,000 hr

• Task 1 durability activities specifically focus on the lifetime target Primary focus of LTE efforts Identification of stressors leading to degradation and subsequent accelerated stress test (AST) development Ultimate goal is to mitigate degradation, meeting or exceeding degradation rate and lifetime goals while also

meeting efficiency and cost (e.g., Ir loading) targets

• The characterization sub-task cross cuts with Tasks 2 and 3

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Relevance and Impact

• Lifetime is perceived to be the mostcritical and the most difficult targetto achieve for LTE systems

• Primary focus of H2NEW LTE efforts

Nel Status Legacy > 40k h steady-state Nel Status Advanced: 1,400 h steady-state 2025 Target: 80,000 h Ultimate Target: 100,000 h Degradation rate target, 2025: 2.24 µV/h Ultimate degradation rate target: 1.56 µV/h PGM loading: 0.5 mg/cm2 (2025) Ultimate PGM loading target: as low as possible

while achieving durability and efficiency targets

N. Danilovic, ECS Transactions, 75 (2016) 395.K. Ayers, Nel, 2020 AMR, Project ID# P155

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Relevance and Impact

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Approach: Task 1 Breakdown

• Task 1a. Understanding component degradation Subtask i. Cell aging studies (NREL, LANL) Subtask ii. Mitigation efforts (NREL, LANL, LBNL)Subtask iii. Ex situ studies of MEA, components, and

interfaces (ORNL, ANL, NREL, LBNL, and LANL)

• Task 1b. Ex situ electrode durability and modeling(ANL, NREL)

• Task 1c. Ex situ membrane durability (LBNL, NREL)

• Task 1d. AST development (LANL, NREL)

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Approach: Task 1 Milestones

Milestone Name/Description Due Date Type Status

Finalize standard, state-of-the-art MEA material set, fabrication process, and/or source to be utilized in baseline studies including those for durability, performance, and scale-up/integration – All Labs

12/31/2020 QPM Complete

Identify parameter space and experimental matrix that support the model needs of the consortium with regards to in-situ, ex-situ, and in-operando experiments. Labs – NREL, LBNL, ANL. 3/30/2021 QPM Complete

Complete cell design and validation of a neutron imaging cell to be used with the high-resolution imaging detector at NIST. Cell performance in imaging hardware within ±10% of performance in a 25cm2 cell. Labs-LANL, NIST.

3/30/2021 QPM Complete

Identify and prioritize needed in-situ, ex-situ, and in-operando diagnostic methods of interest to be developed in subsequent quarters potentially in future discretionary supported projects. Labs – NREL, LBNL, ANL, ORNL. 6/30/2021 QPM On Track

Assess the impact of the stress tests on electrode, membrane, and PTL through voltage loss breakdown and use ex-situ characterization to identify degradation mechanisms and support AST development. Determine initial stressors to be investigated in detail for potential to accelerate specific degradation mechanisms. Labs – NREL, LBNL, ANL, LANL.

6/30/2021 QPM On Track

Establish and validate single cell performance testing protocols on SOA MEAs with PGM loading of <0.8 mg/cm2 and membranes <100 µm demonstrating a minimum performance of 2 A/cm2 at 1.8 V and demonstrate ability to perform voltage loss breakdown modeling as verified by agreement within 10% across at least 3 labs.

9/30/2021 Milestone On Track

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Approach: Task 1 Operando cell studies Ex situ component studies Accelerated Stress Tests

Membrane 2 Determine key stressorsa)

1.9 Orders of magnitude acceleration Limits of durability and the impactaccelerating degradation of component degradation rates 1.8

0 15 30 45 60development, MEA integration, 1.4

of different membrane chemistry E [V

]

1.7

Assess cost and durability trade- Identify relevant degradation Variables: Side chain, equivalent 1.6

1.5 offs, accelerate materialsmechanisms at the component weight, pre-aging,level reinforcements, recombination

Understanding Understanding and Evaluation Solutions

Time [s]

2025 80,000 h

2.24 µV/h 0.5 mgPGM/cm2

and optimal operating strategieslayers and/or radical scavengingfor LTEs Impact of seal area/edges,

pressure

Mitigation Strategies Catalyst

Aqueous electrochemical cell coupled withICP-MS

Quantify losses associated with Potential and potential profile dependence ofthe dissolution of anode catalystsdifferent operating conditions

Correlation with oxidation state

Develop and implement operational, materials,and cell design-based degradation mitigationstrategies

Coordinate with AST development,technoeconomic analysis, and cell fabricationtasks

Voltage loss breakdown/modeling

Ex situ component characterization: SEM, TEM, X-ray spectroscopy, scattering, tomography, microelectrode studies

In-cell Diagnostics: I-V curves, impedance spectroscopy,cyclic voltammetry, fluoride emission

H2NEW: Hydrogen from Next generation Electrolyzers of Water S. M. Alia, S. Stariha, R. L. Borup, J. Electrochem. Soc. 2019, 166.; https://www.hydrogen.energy.gov/pdfs/review19/ta022 alia 2019 o.pdf 2019. 8

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Approach: Sub-Task 1ai Cell Aging Studies

Component-level Stressors/Variables Anode Membrane Porous transport layer

Catalyst loading Membrane Corrosion protection thickness material

Initial work plan: • Operating the rainbow stack and to

start studies evaluating lowerpotential limits to separate the

Hydrogen crossover rate Compression Thickness impact of sudden potential changesSteady-state potential Differential Structure from high potential in catalyst layer

pressure degradation.Voltage sweep rate/profile Pressure cycling Potential exposure • Continued upgrading of electrolysis

testing capability and increasedthroughput through new testequipment and expandingcapability of current equipment.

In-cell Diagnostics: I-V curves, impedance spectroscopy,cyclic voltammetry, fluoride emission

Voltage loss breakdown/modeling

-

Ex situ component characterization: SEM, TEM, X-ray spectroscopy, scattering, tomography, etc.

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Voltage limits for cycling

Length of holds at voltage limits

Temperature

Mechanical stress

Local dehydration

Temperature

Cycling frequency

Redox cycling

Temperature

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Approach: Sub-Task 1ai Cell Aging Studies

Intermittent Operation Anode catalyst layer stressors: • Lower anode catalyst loading, higher a) 2

cycling frequency significantly increase 1.9

performance loss due to intermittent 1.8

operation 1.7

• Sweep rate less critical 1.6

• Simulated crossover reduces near- 1.5

surface iridium, dramatically increases 1.4

dissolution and loss i [A cm‒2]

Hydrogen Crossover

E [V

]

0 0.5 1 1.5 2 2.5 3

Catalyst aggregation, increased interfacial tearing

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Approach: Sub-Task 1ai Cell Aging Studies 4 2.08 2.2

Voltage

Current 2.06

3 2

2Vo

ltage

(V),

Cur

rent

Den

sity

(A/c

m

)

Conditioning Duration

2.04

1 day 2.02

2

1

Vol

tage

at 3

A (V

)

Volta

ge (V

) 1.8

1.6 2 20 mV

0 Mar 11 Mar 12 Mar 13

Time

Mar 14 Mar 15 1.98

Mar 11 Mar 13

Test Time

Mar 15

1.4 0 0.5 1 1.5

Current Density (A/cm

2 2.5

2 )

3

Conditioning Processes Baseline efforts: -3 1.7 V Hold

• Developing a consistent start point for 10

15 Kinetic

2C

urre

nt D

ensi

ty (A

/cm

),

Volta

ge (V

)

durability testing between users, labs• Evaluating variations in catalyst layer

formation and membrane preconditioning,

0.9

resistance 0.89 10 decreases

2 -Z

'' (

cm

)

5 0.88

0.87their impact on conditioning time andperformance Time = 64.1 min0

0.86 Voltage Time = 299.1 min

• Separating losses to evaluate howperformance changes occur during

Current Time = 534.0 min0.85 -5 Time = 769.0 min

HFR varies 0.84

conditioning 200 400 600 0.155 0.16 0.165 0.17 0.175 0.18 0.185

Time (min) 2Z' ( cm )

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pproach: Sub-Task 1aii Mitigation Efforts Operational strategies a)

2 Preventing start-stop, hydrogen crossover to minimize iridium 1.9

reduction/dissolution 1.8

0 15 30 45 60

Control over ramp rate and cycling frequency E [V

]

1.7

Limiting anode potential, dissolution rate at the catalyst layer 1.6

Evaluate trade-off between durability gains and production costs 1.5

• Materials mitigation strategies1.4

Time [s] Advanced catalysts, membranes, and PTLs Tradeoffs between load requirements and degradation rates 3

2.5 Catalyst dissolution rates

0 15 30 45 60 75 90

No Limit

1.9 V Limit

1.45

1.65

1.85

2.05

2.25

2.45

0 5

10 15 20 25 30

E [V

]

Win

d Sp

eed

[m s

‒1 ]

Jan 30, 2018 Time [h:mm]

‒2]

Membrane mechanical degradation and crossover

• Integration mitigation strategies 1.5

1

i 2.0

V [A

cm

elec

2 PTL corrosion and passivation

Vary components, structure (porosity, ionomer integration,0.5 uniformity), and configuration

i Lost (2 V) Utilized Wind Dissolution ‒2][A cm [m s‒1] [µg cm‒2]

No Limit 0.38 7.8 13.5 1.9 V Limit 0.28 7.4 11.5 ∆ [%] -26.0 -5.3 -15.0

• Manufacturing specific concerns will be incorporated and will assess the0

effects of defects on accelerating catalyst/interfacial and PTL loss Duration [days]

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Approach: Ex-situ characterization of MEAs/components/interfaces (Sub-Task 1aiii) • Summary: optical, electron microscopy, and X-ray

characterization techniques to assess changes in: Anode morphology, pore size, catalyst

aggregate/agglomerate size, ionomer distribution Anode catalyst oxidation state, atomic structure, and

migration PTL coating degradation and titanium passivationMembrane thinning, tearing and pinholes, interfacial

swelling, and delaminationMicroelectrode measurements of interface between catalyst

and ionomer to study ionomer degradation and effect on water transport

• First year characterization development efforts: Automated image acquisition and analysis methods for

tracking dissolved metal nanoparticles through themembrane

Absolute quantification of metal loss from electrodes usingthe Z-method

Identical location STEM

Technique Facility X ray Absorption Spectroscopy APS, ALS Ultra small, small, and wide angle X ray scattering

APS: USAXS, SAXS, WAXS ALS: SAXS and WAXS

Micro and Nano X ray computed tomography

ALS, APS

Micro X ray computed tomography LANL, NREL Benchtop

ALS, APS Neutron imaging Tomography NIST Focused ion beam and scanning electron microscopy

LANL, ORNL

Scanning transmission electron microscopy

ORNL

Scanning electron microscopy ANL, LANL, ORNL

X ray photoelectron spectroscopy ORNL Optical microscopy ANL, ORNL

Brunauer Emmett Teller ANL, LANL, NREL, ORNL

Mercury intrusion porosimetry LANL

X ray fluorescence spectroscopy ANL, LANL, NREL

Ion Chromatography LANL

Inductively couple plasma mass spectrometry

ANL, NREL

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Progress: Ex-situ characterization of MEAs/components/interfaces (Sub-Task 1aiii)

Identical-Location Scanning Transmission Electron Microscopy Capability Developed and Demonstrated Test conditions: Protocol: 30s 0.5s

2.00 VvsRHE• Catalyst: Alfa Aesar IrO2 provided by NREL 420 cycles • 0.05M H2SO4, Ar-saturated, Room temperature

1.45 VvsRHE30s

Area 1: BOL 420 cycles BOL 420 cycles

IrO2 IrO2

80

60

40

20

0

-20

-40

-60

EDS analysis: O/Ir atomic ratio

BOL 420 Cycles

-

1.2 1.8

Electrochemical performance of cell

validated

Cur

rent

/µA

IrOx_CV_BOL

0 0.3 0.6 0.9 1.2

E vs. RHE /V

Ar-saturated 0.05M H2SO4, 50mV/s, 5th cycle. Preconditioning: 0.05-1.3 VRHE, 200 mV/s, 40 cycles

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Approach: Ex-situ characterization of MEAs/components/interfaces (Sub-Task 1aiii)

Microelectrode for water and O2 transport measurements in Nafion films Approach 1: polycrystalline surface

Ir Microelectrode data

Microelectrode Cell

Approach 2: Microcavity with nanoparticles

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Approach: Ex-situ catalyst durability (Task 1b)

• Determine the potential and potential profiledependence of the dissolution of the metalliccomponents of OER catalysts

• Aqueous electrochemical cell coupled with ICP-MS• Correlate dissolution rates with catalyst type and

oxidation state• Correlate with in-situ studies performed under

Task 1a• Used to develop models that can be used to

explain and predict catalyst losses over time

Work Plan (Year 1 focus) O2

Catalyst type conc.

% Steady-state

voltage Voltage sweep

profile/rate bal. Ar

• Triangle

• Alfa AesarIrO2

• UmicoreIrO2/TiO2

• TKK IrO2• Johnson

Matthey Ir• Umicore Ir

0 50

100

• 1.6 V to2.0 V

• 50, 100,200, 350mVincrements

• Duration:3, 5, 10mins

(5, 10, 20mV/s)

• Square• Potential

stepping• Trapezoid • Sawtooth

up/down(50, 100,200, 350mV/s)

Voltage limits for voltage

cycling

• Trianglecyclingstarting at0.05 V to various UPL starting at 0.9 V and increasing at 0.1 V to 2.0V.

• 10, 20, 50,100 mV/s

• Year 1: Alfa Aesar IrO2, room temp., O2 conc. 0%• Beyond Year 1: Other catalysts, elevated temp, effect of O2 conc.

Length of holds

at voltage limits

• 3, 5, 10min

• Lowerlimitdependon ICP-MSresponsedelay time

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Progress: Ex-situ catalyst durability (Task 1b)

On-going Activites • Performing time-resolved measurements of Ir dissolution from Alfa-Aesar IrO2

catalyst as a function of electrocatalyst potential using an aqueous flow cellcoupled with on-line inductively-coupled plasma mass spectrometry

• Validated ability to detect dissolved Ir and to maintain integrity of IrO2 layer• Mitigating effects of bubble formation using ionomer film and shaker• Established matrix of dissolution measurements needed for modeling efforts

(potential hold staircase with hold time as long as needed to reach steady-statedissolution rate)

Future Work • Formulate models for formation of surface oxides and dissolution of Ir and Ir oxides

using time-resolved ICP-MS dissolution data in an electrochemical flow cell• In situ X-ray absorption spectroscopy for oxidation state as a function of potential

(Summer beam time cycle)

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Approach: Ex-situ membrane durability (Task 1c)

Initial Test Matrix • Fundamental understanding of the limits ofNo reinforcements, no recombination layers, no radical scavengers durability and the impact of different

membrane chemistry• Membrane variables: Side chain, equivalent

weight, extent of pre-aging, and membrane lifeextension strategies, such as reinforcements,recombination layers and/or radical scavenging

• Impact of seal area/edges, pressure, etc. oncreep

• Coordinate with Task 1a and provide data toTask 1d and to Task 2 modeling

Membrane type/ thickness

Side chain

EW Extent of pre-

aging Test /Creep Condition

N117 175 micron Long 1100 Pretreated in

water at 100◦C 25◦C, 50◦C

Creep at 2 pressures

N117 175 micron Long Pretreated in 25◦C

1100 water at 50◦C Creep at 2 pressures

N115 125 micron Long 1100 Pretreated in

water at 100◦C 25◦C

Creep at 2 pressures

Solvay 90 micron Short Pretreated in 25◦C, 50◦C

980 water at 100◦C Creep at 2 pressures

Solvay 90 micron Short 980 Pretreated in water at 50◦C

25◦C Creep at 2 pressures

3M Medium EW and thickness match to matrix, if available Chemours Long Varying EW, fixed thickness, if available

• Longer term scope: reinforced membranes,recombination layers, alternative membranes, and highertemperatures.

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Progress: Ex-situ membrane durability (Task 1c)

• Completed the compression creep procedure at room temperature and drafted a paper on the technique

• Prepared a summary for comparison of compression creep response for Nafion 117, 115, and Nafion 1110in liquid water at 25 °C (all samples pretreated)

• Completed the required pressure load cell and thickness measurement calibration for setup andequipment

• Repeating measurements on Nafion 117 membrane to check reproducibility before moving on to otherinvestigations with this setup

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Approach: Accelerated Stress Test Development (Task 1d)

• Goals Develop ASTs to predict 80,000 hours of life in desired application Develop additional ASTs to rapidly evaluate different PEM electrolyzer components Recommend to DOE protocols and targets related to PEM electrolyzers

• Methods Establish AST Working Group (ASTWG) comprised of stakeholders and researchers to develop

ASTs that reflect degradation modes encountered in deployed electrolyzers Utilize understanding of degradation mechanisms to develop ASTs

Electrolyzer Stack Goals by 2025 LTE PEM

Capital Cost Electrical Efficiency (LHV)

Lifetime

$100/kW 70% at 3 A/cm2

80,000 hr

Data from ASTs using different material sets will inform cost/performance/durability trade-offs and techno economic analysis

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Approach: Accelerated Stress Test Development (Task 1d)

Utilize understanding of degradation mechanisms to develop ASTs for Electrolyzers • Develop a duty cycle representative of electrolyzer operation while capturing all degradation mechanisms

Dynamic load cycling Open circuit testing (Load off) going through Ir/IrOx redox High current operation (> 3A/cm2) High voltage operation (> 2.5V) Pressure cycling Presence of contaminants (like Fe)

• Develop component specific ASTs to evaluate the durability of individual components in a reasonable timeperiod (1 week to 1 month) Define conditions; Set targets based on correlation with duty cycle Catalysts : Suitability for dynamic operation. Ability to go through redox.Membranes : Durability under dynamic conditions; effect of pressure differentials and contaminants PTLs : Resistance to oxidation (Interface resistance and hydrophobicity changes)

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Progress: Accelerated Stress Test Development (Task 1d)

• AST Working Group Established• Two Meetings of AST Working Group completed

• Survey of Needs/Protocols Completed and Summarized• Importance of Various Stressors Ranked• Durability Evaluation Underway

Leads: Rangachary (Mukund) Mukundan (LANL), Shaun Alia (NREL), Dave Peterson (DOE)

Industry: Corky Mittelsteadt (Plug) Kathy Ayers (NEL) Richard Ancimer (Cummins) Andrew Smeltz (DeNora)

DOE: Dave Peterson Will Gibbons

University: Svitlana Pylypenko (CSM) Iryna Zenyuk (UCI)

National Labs: NREL : Bryan Pivovar, Shaun Alia, Guido Bender, Mike Ulsh LANL : Rangachary (Mukund) Mukundan, Siddharth Komini Babu LBNL : Nemanja Danilovic, Ahmet Kusoglu ANL. : Debbie Myers, Rajesh Ahluwalia ORNL : Haoran Yu

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Progress: Accelerated Stress Test Development (Task 1d)

ASTWG Priority list (1=highest priority) Task Name Average Std Dev

Develop Electrolyzer Duty cycle that captures all relevant stressors at the MEA level 1.375 0.484 Anode Catalyst AST 1.875 0.599 PTL AST 3.9375 0.634 Membrane AST 3.125 0.927 Catalyst layer ionomer AST 5.5 1.118 Cathode Catalyst AST 6.375 1.494 Bi-polar plate AST 6.1875 1.058

Stressor Name

Dynamic load cycling 2.625 1.932 Shut down/Start up. Allowing Ir/IrOx redox 2.25 1.713 High current operation (> 3A/cm2) 4.3125 1.919 High voltage operation (> 2.5V) 3.3125 1.434 Pressure cycling 5.25 1.089 Presence of contaminants (like Fe) 4.25 1.198 Hydrogen cross-over 5.875 1.615

• Electrolyzer duty cycle identified as #1 priority• Needs to incorporate dynamic load cycling and

Ir/IrOx redox cycling• Completing baseline materials and testing protocols• Initiating testing matrix for AST development

• Establish degradation rate at 80 oC: Square wavepotential from 0V (no load, ambient) to 1.6V (up to30 bar). 15mins at each potential. Both pressureand Redox cycling to capture all degradation modes

• Monitor pol curves, CVs, and EIS during test andalso fluoride emission from both anode andcathode

• BOL and EOL particle sizes, membrane thickness,membrane mechanical properties, PTL hydrophobicity and porosity

Future Work: • Parametric study to quantify influence of individual

stressors• Working to incorporate other loss mechanisms in

conjunction with the AST working groupH2NEW: Hydrogen from Next generation Electrolyzers of Water 23

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Responses to Previous Year Reviewers’ Comments

• Not Applicable, first year of project

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Collaboration and Coordination

NREL Team Members: Shaun Alia, Elliott Padgett, Jason Zack, Tobias Schuler LBNL Team Members: Claire Arthurs, Grace Anderson, Nemanja Danilovic, Ahmet Kusoglu ANL Team Members: Rajesh Ahluwalia, C. Firat Cetinbas, Nancy Kariuki, Debbie Myers, Jaehyung Park, Jui-Kun Peng, Xiaohua Wang, Andrew Star LANL Team Members: Siddharth Komini Babu, Rangachary Mukundan, Xiaoxiao Qiao ORNL Team Members: Jefferey Baxter, David Cullen, Harry Meyer, Shawn Reeves, Haoran Yu

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Summary of Proposed Future Work

• Subtask 1a.i: LTE Aging Studies Cycle baseline MEAs through load-off, full power cycles to identify degradation and quantify degradation rates Cycle through shutdowns and probe the impact of crossover, water starvation, and cycled backpressure on component degradation Assess membrane loss through chemical and mechanical degradation, including cycled backpressure, water input, and temperature Assess relevancy of catalyst layer degradation at low loading and lab-level coating processes with comparisons to manufacturing and

moderate loading Evaluate PTL coating durability through catalyst layer defects and the impact of coating and sub-coating properties on interfacial contact

and performance loss

• Subtask 1a.ii : Mitigation Strategies Develop materials-based mitigation strategies, probing how component development can be used to minimize loss through lower load

requirements Develop and prioritize operational strategies to limit performance loss, including potential/load and cycling limits

• Subtask 1a.iii: Ex-situ Characterization of MEAs/components/interfaces Utilize identical location STEM to characterize the effects of potential holds and cycling on IrOx composition and structure Utilize microelectrode apparatus to measure effects of ionomer degradation and effect on transports properties

Any proposed future work is subject to change based on funding levels

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Summary of Proposed Future Work (continued)

• Subtask 1b: Ex-situ Catalyst Durability Formulate models for formation of surface oxides and dissolution of Ir and Ir oxides using time-resolved dissolution data In situ X-ray absorption spectroscopy for catalyst oxidation state as a function of potential

• Subtask 1c: Ex-situ Membrane Durability Perform membrane creep measurements for water-soaked membranes as a function of membrane properties Quantify chemical degradation rates for membranes of different thickness (different cross-over) under electrolyzer relevant conditions

• Subtask 1d: Accelerated Stress Test Development Further define stress test protocols Parametric study to quantify influence of individual stressors

Any proposed future work is subject to change based on funding levels

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Task 1 Summary

• The Task 1 effort focuses on cell durability/lifetime and mitigation of degradation processes• Task 1 work areas includes

– Operando studies of cells to determine key stressors coupled with in-cell diagnostics, ex situ beginning-of-life and post-test characterization of components, coupled with voltage loss breakdown and modeling

– Ex situ studies of components and interfaces to determine materials and operating stressors, to develop predictivedegradation models and inform mitigation strategies

– Accelerates stress test development and validation to assess cost and durability trade-offs and inform mitigation strategyeffort

• Early accomplishments include– Standardization of cell preparation, assembly, and testing (with Task 2)– Durability demonstration experiments on degradation test stands using a rainbow stack– Adaptation and demonstration of on-line ICP-MS capability to study and quantify potential dependence Ir dissolution

from anode catalyst– Development and demonstration of identical location scanning transmission electron microscopy capability to study

degradation processes of anode catalyst– Implementation of microelectrode capability to study catalyst-membrane interface and membrane/ionomer properties– Establishment of accelerated stress test working group and definition of initial stressors for evaluation

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Technical Backup and Additional Information Slides

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Technology Transfer Activities

• No current patent or licensing sought• H2NEW website and marketing material being developed• Interactions with the following OEMs:

– Mott– Bekaert– JM– Heraeus– Chemours– Pajarito Powder– 3M

• IP generation mechanism through CRADAs with industry to be sought during the course ofthe project

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Progress Towards DOE Targets or Milestones

*Table 3.1.4 in MYRD&DElectrolyzer Stack Goals by 2025

LTE PEM MYRD&D 2020* Capital Cost

Electrical Efficiency (LHV)

Lifetime

$100/kW 70% at 3 A/cm2

80,000 hr

$300/kW 77% (n/a current

density) n/a

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Publications and Presentations

• Capuano C.B., Ayers K., Manco J., Wiles L., Errico S., Zenyuk I.V., Weber A.Z., Kusoglu A.,Danilovic N., Ulsh M., Mauger S.A., Pfeilsticker J., Alia S.M. “High Efficiency PEM WaterElectrolysis Enabled By Advanced Catalysts, Membranes and Processes.” Invited oralpresentation at the Fall ESC Meeting (virtual); October 2020.

• Park J., Kang Z., Bender G., Ulsh M., Mauger S.A. “Direct roll-to-roll coating of catalyst-coatedmembranes for low-cost PEM water electrolyzers.” Oral presentation at the Fall ESC Meeting(virtual); October 2020.

• M.R. Gerhardt, L.M. Pant, J.C.M. Bui, A. R. Crothers, V.M. Ehlinger, J.C. Fornaciari, J. Liu andA.Z. Weber, “Methods—Practices and Pitfalls in Voltage Breakdown Analysis ofElectrochemical Energy-Conversion Systems”, JES, DOI:10.1149/1945-7111/abf061.

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Special Recognitions and Awards

• Bryan Pivovar was awarded the 2021 Energy Technology Division Research Award ofthe Electrochemical Society and the 2021 US Department of Energy Secretary’sHonor Award.

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