High Precision Non-Destructive Test Method of Pt Loading and Distribution in Proton Exchange Membrane Fuel Cell Membrane Electrodes

doi:10.19894/j.issn.1000-0518.220379

Chinese Journal of Applied Chemistry ›› 2023, Vol. 40 ›› Issue (6): 845-852.DOI: 10.19894/j.issn.1000-0518.220379

• Full Papers • Previous Articles Next Articles

High Precision Non-Destructive Test Method of Pt Loading and Distribution in Proton Exchange Membrane Fuel Cell Membrane Electrodes

Xiao DUAN¹^,³, Feng CAO¹^,³, Yang ZHOU¹^,³, Bin ZHANG², Wei-Wen DONG², Ling-Li WEI², Jia LI¹(), Jian-Guo LIU¹()

^1.Institute of Energy Power Innovation, North China Electric Power University, Beijing 102206, China
^2.Heraeus Precious Metal Technology (China) Co. , Ltd. , Nanjing 211500, China )
^3.College of Engineering and Applied Sciences, Nanjing University, Nanjing 210093, China

Received:2022-11-21 Accepted:2023-03-27 Published:2023-06-01 Online:2023-06-27
Contact: Jia LI,Jian-Guo LIU
About author:jianguoliu@ncepu.edu.cn
lijia@ncepu.edu.cn；
Supported by:
the National Key R&D Program of China(2019YFB1504503)

Abstract

Abstract:

As the commercialization of proton exchange membrane fuel cells advances， non-destructive high-precision online inspection of Pt loading and distribution is needed in order to improve the reproducibility and product control of membrane electrode assemblies （MEA） fabrication. According to Joule's law and Ohm's law， the MEA resistance can be analyzed by using the heat distribution and current density signals generated under a DC excitation voltage. The inverse correlation between MEA resistance and Pt loading is demonstrated by current testing at different DC excitation voltages， and the accuracy of the non-destructive quantitative characterization of Pt loading is 0.0008~0.0025 mg/cm². The qualitative analysis of Pt loading distribution is successfully achieved by collecting thermal distribution information of MEA under DC excitation voltage using infrared thermography. Finally， comparison of MEA performance before and after DC excitation demonstrates that the method is non-destructive to membrane electrode performance. This method can improve the quality and manufacturing efficiency of MEA and reduce the cost of MEA manufacturing， which is of great significance to the large-scale commercialization of proton exchange membrane fuel cells.

Key words: DC excitation method, Non-destructive testing, Pt loading, Membrane electrode assemblies, Infrared thermography

CLC Number:

O657.9

Xiao DUAN, Feng CAO, Yang ZHOU, Bin ZHANG, Wei-Wen DONG, Ling-Li WEI, Jia LI, Jian-Guo LIU. High Precision Non-Destructive Test Method of Pt Loading and Distribution in Proton Exchange Membrane Fuel Cell Membrane Electrodes[J]. Chinese Journal of Applied Chemistry, 2023, 40(6): 845-852.

Figures/Tables 6

References 21

1	CHONG L， WEN J， KUBAL J， et al. Ultralow-loading platinum-cobalt fuel cell catalysts derived from imidazolate frameworks［J］. Science， 2018， 362（6420）： 1276-1281.
2	KONGKANAND A， SUBRAMANIAN N P， YU Y， et al. Achieving high-power PEM fuel cell performance with an ultralow-Pt-content core-shell catalyst［J］. ACS Catal， 2016， 6（3）： 1578-1583.
3	ZHAO Z， LIU Z， ZHANG A， et al. Graphene-nanopocket-encaged PtCo nanocatalysts for highly durable fuel cell operation under demanding ultralow-Pt-loading conditions［J］. Nat Nanotechnol， 2022， 17： 968-975.
4	CHOI J， LEE Y J， PARK D， et al. Highly durable fuel cell catalysts using crosslinkable block copolymer-based carbon supports with ultralow Pt loadings［J］. Energy Environ Sci， 2020， 13（12）： 4921-4929.
5	WANG G， HUANG B， XIAO L， et al. Pt skin on AuCu intermetallic substrate： a strategy to maximize Pt utilization for fuel cells［J］. J Am Chem Soc， 2014， 136（27）： 9643-9649.
6	TANG M， ZHANG S， CHEN S. Pt utilization in proton exchange membrane fuel cells： structure impacting factors and mechanistic insights［J］. Chem Soc Rev， 2022， 51（4）： 1529-1546.
7	YUAN X Z， NAYOZE-COYNEL C， SHAIGAN N， et al. A review of functions， attributes， properties and measurements for the quality control of proton exchange membrane fuel cell components‍［J］. J Power Sources， 2021， 491： 229540-229578.
8	ZENG Y C， GUO X Q， WANG Z Q， et al. Highly stable nanostructured membrane electrode assembly based on Pt/Nb₂O₅ nanobelts with reduced platinum loading for proton exchange membrane fuel cells‍［J］. Nanoscale， 2017， 9（20）： 6910-6919.
9	CHEN Z J， FU T， KONG X B， et al. A novel impregnation-reduction method combined with galvanic replacement for fabricating low cost MEA with high performance for PEM fuel cells‍［J］. J Electrochem Soc， 2021， 168（3）： 034522-034532.
10	PHILLIPS A， ULSH M， PORTER J， et al. Utilizing a segmented fuel cell to study the effects of electrode coating irregularities on PEM fuel cell initial performance［J］. Fuel Cells， 2017， 17（3）： 288-298.
11	RESHETENKO T V， BENDER G， BETHUNE K， et al. Application of a segmented cell setup to detect pinhole and catalyst loading defects in proton exchange membrane fuel cells［J］. Electrochim Acta， 2012， 76： 16-25.
12	WYON C， DELILLE D， GONCHOND J P， et al. In-line monitoring of advanced microelectronic processes using combined X-ray techniques［J］. Thin Solid Films， 2004， 450（1）： 84-89.
13	STOCKER M T， BARNES B M， SOHN M， et al. Development of large aperture projection scatterometry for catalyst loading evaluation in proton exchange membrane fuel cells［J］. J Power Sources， 2017， 364： 130-137.
14	SHARMA R， ANDERSEN S M. An opinion on catalyst degradation mechanisms during catalyst support focused accelerated stress test （AST） for proton exchange membrane fuel cells （PEMFCs）［J］. Appl Catal B， 2018， 239： 636-643.
15	BAKER A M， WILLIAMS S T D， MUKUNDAN R， et al. Zr-doped ceria additives for enhanced PEM fuel cell durability and radical scavenger stability［J］. J Mater Chem A， 2017， 5（29）： 15073-15079.
16	CAI Y， ZIEGELBAUER J M， BAKER A M， et al. Electrode edge cobalt cation migration in an operating fuel cell： an in situ micro-X-ray fluorescence study［J］. J Electrochem Soc， 2018， 165（6）： F3132-F3138.
17	PATRICK H J， ATTOTA R， BARNES B M， et al. Optical critical dimension measurement of silicon grating targets using back focal plane scatterfield microscopy［J］. J Micro-Nanolith Mem， 2008， 7（1）： 013012-013022.
18	BARNES B M， ATTOTA R， QUINTANILHA R， et al. Characterizing a scatterfield optical platform for semiconductor metrology［J］. Meas Sci Technol， 2011， 22（2）： 024003-024011.
19	DAS P K， WEBER A Z， BENDER G， et al. Rapid detection of defects in fuel-cell electrodes using infrared reactive-flow-through technique［J］. J Power Sources， 2014， 261： 401-411.
20	AIETA N V， DAS P K， PERDUE A， et al. Applying infrared thermography as a quality-control tool for the rapid detection of polymer-electrolyte-membrane-fuel-cell catalyst-layer-thickness variations［J］. J Power Sources， 2012， 211： 4-11.
21	VAN CLEVE T， KHANDAVALLI S， CHOWDHURY A， et al. Dictating Pt-based electrocatalyst performance in polymer electrolyte fuel cells， from formulation to application［J］. ACS Appl Mater Interfaces， 2019， 11（50）： 46953-46964.

Voltage/V	1# MEA		2# MEA		3# MEA		4# MEA		5# MEA		6# MEA
Voltage/V	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）
0.1	0.052 04	0.143	0.095 46	0.239	0.033 13	0.101	0.077 35	0.199	0.121 86	0.298	0.169 03	0.402
0.2	0.104 08	0.143	0.190 3	0.239	0.066 34	0.101	0.154 62	0.199	0.243 58	0.297	0.337 66	0.402
0.3	0.156 1	0.143	0.284 81	0.238	0.099 49	0.101	0.231 81	0.199	0.365 34	0.298	0.506 41	0.402
0.4	0.208 1	0.143	0.379 01	0.238	0.132 70	0.101	0.308 99	0.199	0.487 13	0.298	0.675 02	0.402
0.5	0.260 21	0.143	0.472 88	0.237	0.165 99	0.101	0.386 42	0.199	0.609 27	0.298	0.843 91	0.402
0.6	0.312 51	0.143	0.567	0.237	0.199 32	0.101	0.463 92	0.199	0.731 56	0.298	1.012 84	0.402
0.7	0.365 11	0.143	0.661 17	0.237	0.232 81	0.101	0.541 78	0.199	0.853 91	0.298	1.181 92	0.402
0.8	0.418 03	0.143	0.755 4	0.237	0.266 47	0.101	0.619 81	0.199	0.976 55	0.298	1.351 48	0.402
0.9	0.471 28	0.143	0.850 46	0.237	0.300 18	0.101	0.698 45	0.199	1.099 78	0.298	1.521 62	0.402
1.0	0.524 95	0.143	0.946 12	0.237	0.334 04	0.101	0.777 65	0.199	1.223 64	0.298	1.692 45	0.402
1.1	0.579 11	0.144	1.042 46	0.237	0.368 04	0.101	0.857 34	0.199	1.348 19	0.298	1.864 06	0.401
1.2	0.633 8	0.144	1.139 27	0.237	0.402 29	0.101	0.937 65	0.199	1.473 26	0.298	2.036 52	0.402
μ		0.000 8		0.002 5		0.001 0		0.001 0		0.002 1		0.001 9

Voltage/V	1# MEA		2# MEA		3# MEA		4# MEA		5# MEA		6# MEA
Voltage/V	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）	Current density/（mA·cm^-2）	Pt loading/（mg·cm^-2）
0.1	0.052 04	0.143	0.095 46	0.239	0.033 13	0.101	0.077 35	0.199	0.121 86	0.298	0.169 03	0.402
0.2	0.104 08	0.143	0.190 3	0.239	0.066 34	0.101	0.154 62	0.199	0.243 58	0.297	0.337 66	0.402
0.3	0.156 1	0.143	0.284 81	0.238	0.099 49	0.101	0.231 81	0.199	0.365 34	0.298	0.506 41	0.402
0.4	0.208 1	0.143	0.379 01	0.238	0.132 70	0.101	0.308 99	0.199	0.487 13	0.298	0.675 02	0.402
0.5	0.260 21	0.143	0.472 88	0.237	0.165 99	0.101	0.386 42	0.199	0.609 27	0.298	0.843 91	0.402
0.6	0.312 51	0.143	0.567	0.237	0.199 32	0.101	0.463 92	0.199	0.731 56	0.298	1.012 84	0.402
0.7	0.365 11	0.143	0.661 17	0.237	0.232 81	0.101	0.541 78	0.199	0.853 91	0.298	1.181 92	0.402
0.8	0.418 03	0.143	0.755 4	0.237	0.266 47	0.101	0.619 81	0.199	0.976 55	0.298	1.351 48	0.402
0.9	0.471 28	0.143	0.850 46	0.237	0.300 18	0.101	0.698 45	0.199	1.099 78	0.298	1.521 62	0.402
1.0	0.524 95	0.143	0.946 12	0.237	0.334 04	0.101	0.777 65	0.199	1.223 64	0.298	1.692 45	0.402
1.1	0.579 11	0.144	1.042 46	0.237	0.368 04	0.101	0.857 34	0.199	1.348 19	0.298	1.864 06	0.401
1.2	0.633 8	0.144	1.139 27	0.237	0.402 29	0.101	0.937 65	0.199	1.473 26	0.298	2.036 52	0.402
μ		0.000 8		0.002 5		0.001 0		0.001 0		0.002 1		0.001 9

High Precision Non-Destructive Test Method of Pt Loading and Distribution in Proton Exchange Membrane Fuel Cell Membrane Electrodes

RichHTML

PDF

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 6

References 21

Related Articles 0

Recommended Articles

Metrics

Comments