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Title: Best Practices and Testing Protocols for Benchmarking ORR Activities of Fuel Cell Electrocatalysts Using Rotating Disk Electrode

Abstract

Thin-film-rotating disk electrodes (TF-RDEs) are the half-cell electrochemical system of choice for rapid screening of oxygen reduction reaction (ORR) activity of novel Pt supported on carbon black supports (Pt/C) electrocatalysts. It has been shown that the magnitude of the measured ORR activity and reproducibility are highly dependent on the system cleanliness, evaluation protocols, and operating conditions as well as ink formulation, composition, film drying, and the resultant film thickness and uniformity. Accurate benchmarks of baseline Pt/C catalysts evaluated using standardized protocols and best practices are necessary to expedite ultra-low-platinum group metal (PGM) catalyst development that is crucial for the imminent commercialization of fuel cell vehicles. We report results of evaluation in three independent laboratories of Pt/C electrocatalysts provided by commercial fuel cell catalyst manufacturers (Johnson Matthey, Umicore, Tanaka Kikinzoku Kogyo - TKK). The studies were conducted using identical evaluation protocols/ink formulation/film fabrication albeit employing unique electrochemical cell designs specific to each laboratory. Furthermore, the ORR activities reported in this work provide a baseline and criteria for selection and scale-up of novel high activity ORR electrocatalysts for implementation in proton exchange membrane fuel cells (PEMFCs).

Authors:
 [1];  [1];  [1];  [2];  [2];  [2];  [2];  [2];  [2];  [3]
  1. National Renewable Energy Lab. (NREL), Golden, CO (United States)
  2. Argonne National Lab. (ANL), Argonne, IL (United States)
  3. U.S. Dept. of Energy, Washington, D.C. (United States)
Publication Date:
Research Org.:
National Renewable Energy Lab. (NREL), Golden, CO (United States)
Sponsoring Org.:
USDOE Office of Energy Efficiency and Renewable Energy (EERE)
OSTI Identifier:
1371530
Report Number(s):
NREL/JA-5900-68538
Journal ID: ISSN 1868-2529
Grant/Contract Number:
AC36-08GO28308
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Electrocatalysis
Additional Journal Information:
Journal Volume: 8; Journal Issue: 4; Journal ID: ISSN 1868-2529
Publisher:
Springer
Country of Publication:
United States
Language:
English
Subject:
30 DIRECT ENERGY CONVERSION; RDE; ORR activity; benchmark; PEMFC; best practices; standard method

Citation Formats

Kocha, Shyam S., Shinozaki, Kazuma, Zack, Jason W., Myers, Deborah J., Kariuki, Nancy N., Nowicki, Tammi, Stamenkovic, Vojislav, Kang, Yijin, Li, Dongguo, and Papageorgopoulos, Dimitrios. Best Practices and Testing Protocols for Benchmarking ORR Activities of Fuel Cell Electrocatalysts Using Rotating Disk Electrode. United States: N. p., 2017. Web. doi:10.1007/s12678-017-0378-6.
Kocha, Shyam S., Shinozaki, Kazuma, Zack, Jason W., Myers, Deborah J., Kariuki, Nancy N., Nowicki, Tammi, Stamenkovic, Vojislav, Kang, Yijin, Li, Dongguo, & Papageorgopoulos, Dimitrios. Best Practices and Testing Protocols for Benchmarking ORR Activities of Fuel Cell Electrocatalysts Using Rotating Disk Electrode. United States. doi:10.1007/s12678-017-0378-6.
Kocha, Shyam S., Shinozaki, Kazuma, Zack, Jason W., Myers, Deborah J., Kariuki, Nancy N., Nowicki, Tammi, Stamenkovic, Vojislav, Kang, Yijin, Li, Dongguo, and Papageorgopoulos, Dimitrios. Tue . "Best Practices and Testing Protocols for Benchmarking ORR Activities of Fuel Cell Electrocatalysts Using Rotating Disk Electrode". United States. doi:10.1007/s12678-017-0378-6. https://www.osti.gov/servlets/purl/1371530.
@article{osti_1371530,
title = {Best Practices and Testing Protocols for Benchmarking ORR Activities of Fuel Cell Electrocatalysts Using Rotating Disk Electrode},
author = {Kocha, Shyam S. and Shinozaki, Kazuma and Zack, Jason W. and Myers, Deborah J. and Kariuki, Nancy N. and Nowicki, Tammi and Stamenkovic, Vojislav and Kang, Yijin and Li, Dongguo and Papageorgopoulos, Dimitrios},
abstractNote = {Thin-film-rotating disk electrodes (TF-RDEs) are the half-cell electrochemical system of choice for rapid screening of oxygen reduction reaction (ORR) activity of novel Pt supported on carbon black supports (Pt/C) electrocatalysts. It has been shown that the magnitude of the measured ORR activity and reproducibility are highly dependent on the system cleanliness, evaluation protocols, and operating conditions as well as ink formulation, composition, film drying, and the resultant film thickness and uniformity. Accurate benchmarks of baseline Pt/C catalysts evaluated using standardized protocols and best practices are necessary to expedite ultra-low-platinum group metal (PGM) catalyst development that is crucial for the imminent commercialization of fuel cell vehicles. We report results of evaluation in three independent laboratories of Pt/C electrocatalysts provided by commercial fuel cell catalyst manufacturers (Johnson Matthey, Umicore, Tanaka Kikinzoku Kogyo - TKK). The studies were conducted using identical evaluation protocols/ink formulation/film fabrication albeit employing unique electrochemical cell designs specific to each laboratory. Furthermore, the ORR activities reported in this work provide a baseline and criteria for selection and scale-up of novel high activity ORR electrocatalysts for implementation in proton exchange membrane fuel cells (PEMFCs).},
doi = {10.1007/s12678-017-0378-6},
journal = {Electrocatalysis},
number = 4,
volume = 8,
place = {United States},
year = {Tue May 02 00:00:00 EDT 2017},
month = {Tue May 02 00:00:00 EDT 2017}
}

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  • Abstract Thin-film-rotating disk electrodes (TF-RDEs) are the half-cell electrochemical system of choice for rapid screening of oxygen reduction reaction (ORR) activity of novel Pt supported on carbon black supports (Pt/C) electrocatalysts. It has been shown that the magnitude of the measured ORR activity and reproducibility are highly dependent on the system cleanliness, evaluation protocols, and operating conditions as well as ink formulation, composition, film drying, and the resultant film thickness and uniformity. Accurate benchmarks of baseline Pt/C catalysts evaluated using standardized protocols and best practices are necessary to expedite ultra-low-platinum group metal (PGM) catalyst development that is crucial for themore » imminent commercialization of fuel cell vehicles. We report results of evaluation in three independent laboratories of Pt/C electrocatalysts provided by commercial fuel cell catalyst manufacturers (Johnson Matthey, Umicore, Tanaka Kikinzoku Kogyo—TKK). The studies were conducted using identical evaluation protocols/ink formulation/film fabrication albeit employing unique electrochemical cell designs specific to each laboratory. The ORR activities reported in this work provide a baseline and criteria for selection and scale-up of novel high activity ORR electrocatalysts for implementation in proton exchange membrane fuel cells (PEMFCs).« less
  • The rotating disk electrode (RDE) technique is being extensively used as a screening tool to estimate the activity of novel PEMFC electrocatalysts synthesized in lab-scale (mg) quantities. Discrepancies in measured activity attributable to glassware and electrolyte impurity levels, as well as conditioning, protocols and corrections are prevalent in the literature. Moreover, the electrochemical response to a broad spectrum of commercially sourced perchloric acid and the effect of acid molarity on impurity levels and solution resistance were also assessed. Our findings reveal that an area specific activity (SA) exceeding 2.0 mA/cm 2 (20 mV/s, 25°C, 100 kPa, 0.1 M HClO 4)more » for polished poly-Pt is an indicator of impurity levels that do not impede the accurate measurement of the ORR activity of Pt based catalysts. After exploring various conditioning protocols to approach maximum utilization of the electrochemical area (ECA) and peak ORR activity without introducing catalyst degradation, an investigation of measurement protocols for ECA and ORR activity was conducted. Down-selected protocols were based on the criteria of reproducibility, duration of experiments, impurity effects and magnitude of pseudo-capacitive background correction. In sum, statistical reproducibility of ORR activity for poly-Pt and Pt supported on high surface area carbon was demonstrated.« less
  • In this paper a new cell configuration for use with the rotating disk electrode (RDE), the inverted rotating disk electrode (IRDE), is outlined. The IRDE faces upwards in solution and rotates without electrolyte leakage, even in highly corrosive solutions. This facilitates gas evolution and free convection studies. Mass transfer characteristics obtained by limiting current measurements agree well with literature for the RDE.