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Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film

Transition metal oxides are promising electrocatalysts for water oxidation, i.e., the oxygen evolution reaction (OER), which is critical in electrochemical production of non-fossil fuels. The involvement of oxidation state changes of the metal in OER electrocatalysis is increasingly recognized in th...

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Autores principales: Pasquini, Chiara, Liu, Si, Chernev, Petko, Gonzalez-Flores, Diego, Mohammadi, Mohammad Reza, Kubella, Paul, Jiang, Shan, Loos, Stefan, Klingan, Katharina, Sikolenko, Vadim, Mebs, Stefan, Haumann, Michael, Beyer, Paul, D’Amario, Luca, Smith, Rodney D. L., Zaharieva, Ivelina, Dau, Holger
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Springer Berlin Heidelberg 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8405515/
https://www.ncbi.nlm.nih.gov/pubmed/34274992
http://dx.doi.org/10.1007/s00216-021-03515-0
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author Pasquini, Chiara
Liu, Si
Chernev, Petko
Gonzalez-Flores, Diego
Mohammadi, Mohammad Reza
Kubella, Paul
Jiang, Shan
Loos, Stefan
Klingan, Katharina
Sikolenko, Vadim
Mebs, Stefan
Haumann, Michael
Beyer, Paul
D’Amario, Luca
Smith, Rodney D. L.
Zaharieva, Ivelina
Dau, Holger
author_facet Pasquini, Chiara
Liu, Si
Chernev, Petko
Gonzalez-Flores, Diego
Mohammadi, Mohammad Reza
Kubella, Paul
Jiang, Shan
Loos, Stefan
Klingan, Katharina
Sikolenko, Vadim
Mebs, Stefan
Haumann, Michael
Beyer, Paul
D’Amario, Luca
Smith, Rodney D. L.
Zaharieva, Ivelina
Dau, Holger
author_sort Pasquini, Chiara
collection PubMed
description Transition metal oxides are promising electrocatalysts for water oxidation, i.e., the oxygen evolution reaction (OER), which is critical in electrochemical production of non-fossil fuels. The involvement of oxidation state changes of the metal in OER electrocatalysis is increasingly recognized in the literature. Tracing these oxidation states under operation conditions could provide relevant information for performance optimization and development of durable catalysts, but further methodical developments are needed. Here, we propose a strategy to use single-energy X-ray absorption spectroscopy for monitoring metal oxidation-state changes during OER operation with millisecond time resolution. The procedure to obtain time-resolved oxidation state values, using two calibration curves, is explained in detail. We demonstrate the significance of this approach as well as possible sources of data misinterpretation. We conclude that the combination of X-ray absorption spectroscopy with electrochemical techniques allows us to investigate the kinetics of redox transitions and to distinguish the catalytic current from the redox current. Tracking of the oxidation state changes of Co ions in electrodeposited oxide films during cyclic voltammetry in neutral pH electrolyte serves as a proof of principle. GRAPHICAL ABSTRACT: [Image: see text] SUPPLEMENTARY INFORMATION: The online version contains supplementary material available at 10.1007/s00216-021-03515-0.
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spelling pubmed-84055152021-09-09 Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film Pasquini, Chiara Liu, Si Chernev, Petko Gonzalez-Flores, Diego Mohammadi, Mohammad Reza Kubella, Paul Jiang, Shan Loos, Stefan Klingan, Katharina Sikolenko, Vadim Mebs, Stefan Haumann, Michael Beyer, Paul D’Amario, Luca Smith, Rodney D. L. Zaharieva, Ivelina Dau, Holger Anal Bioanal Chem Research Paper Transition metal oxides are promising electrocatalysts for water oxidation, i.e., the oxygen evolution reaction (OER), which is critical in electrochemical production of non-fossil fuels. The involvement of oxidation state changes of the metal in OER electrocatalysis is increasingly recognized in the literature. Tracing these oxidation states under operation conditions could provide relevant information for performance optimization and development of durable catalysts, but further methodical developments are needed. Here, we propose a strategy to use single-energy X-ray absorption spectroscopy for monitoring metal oxidation-state changes during OER operation with millisecond time resolution. The procedure to obtain time-resolved oxidation state values, using two calibration curves, is explained in detail. We demonstrate the significance of this approach as well as possible sources of data misinterpretation. We conclude that the combination of X-ray absorption spectroscopy with electrochemical techniques allows us to investigate the kinetics of redox transitions and to distinguish the catalytic current from the redox current. Tracking of the oxidation state changes of Co ions in electrodeposited oxide films during cyclic voltammetry in neutral pH electrolyte serves as a proof of principle. GRAPHICAL ABSTRACT: [Image: see text] SUPPLEMENTARY INFORMATION: The online version contains supplementary material available at 10.1007/s00216-021-03515-0. Springer Berlin Heidelberg 2021-07-17 2021 /pmc/articles/PMC8405515/ /pubmed/34274992 http://dx.doi.org/10.1007/s00216-021-03515-0 Text en © The Author(s) 2021 https://creativecommons.org/licenses/by/4.0/Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article's Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article's Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creativecommons.org/licenses/by/4.0/ (https://creativecommons.org/licenses/by/4.0/) .
spellingShingle Research Paper
Pasquini, Chiara
Liu, Si
Chernev, Petko
Gonzalez-Flores, Diego
Mohammadi, Mohammad Reza
Kubella, Paul
Jiang, Shan
Loos, Stefan
Klingan, Katharina
Sikolenko, Vadim
Mebs, Stefan
Haumann, Michael
Beyer, Paul
D’Amario, Luca
Smith, Rodney D. L.
Zaharieva, Ivelina
Dau, Holger
Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title_full Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title_fullStr Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title_full_unstemmed Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title_short Operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved X-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
title_sort operando tracking of oxidation-state changes by coupling electrochemistry with time-resolved x-ray absorption spectroscopy demonstrated for water oxidation by a cobalt-based catalyst film
topic Research Paper
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8405515/
https://www.ncbi.nlm.nih.gov/pubmed/34274992
http://dx.doi.org/10.1007/s00216-021-03515-0
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