Electrochemical flow cell enabling operando probing of electrocatalyst surfaces by X-ray spectroscopy and diffraction

Physical Chemistry Chemical Physics : PCCP
Maryam FarmandWalter S Drisdell

Abstract

The rational improvement of current and developing electrochemical technologies requires atomistic understanding of electrode-electrolyte interfaces. However, examining these interfaces under operando conditions, where performance is typically evaluated and benchmarked, remains challenging, as it necessitates incorporating an operando probe during full electrochemical operation. In this study, we describe a custom electrochemical flow cell that enables near-surface-sensitive operando investigation of planar thin-film catalysts at significant hydrogen evolution reaction (HER) rates (in excess of -100 mA cm-2) using grazing incidence X-ray methods. Grazing-incidence X-ray spectroscopy and diffraction were implemented on the same sample under identical HER conditions, demonstrating how the combined measurements track changing redox chemistry and structure of Cu thin-film catalyst surfaces as a function of electrochemical conditions. The coupling of these methods with improved mass transport and hydrodynamic control establishes a new paradigm for operando measurement design, enabling unique insights into the key fundamental processes occurring at the catalyst-electrolyte interface.

References

May 4, 2005·Nature Materials·Antonino Salvatore AricòWalter van Schalkwijk
Apr 7, 2007·The Review of Scientific Instruments·Frank Uwe RennerJörg Zegenhagen
Feb 11, 2015·Journal of the American Chemical Society·Charles C L McCroryThomas F Jaramillo
Sep 1, 2016·Nature Communications·Marco FavaroEthan J Crumlin
Sep 10, 2016·ACS Central Science·Anna WuttigYogesh Surendranath
Dec 21, 2016·Nature Materials·Joseph H MontoyaJens K Nørskov
Mar 9, 2018·Journal of Electron Spectroscopy and Related Phenomena·Benedikt Lassalle-KaiserJunko Yano

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Citations

Jan 1, 2021·Journal of the American Chemical Society·Soo Hong LeeWalter S Drisdell
Jan 28, 2022·Chemical Communications : Chem Comm·Liu YanShi-Gang Sun

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Methods Mentioned

BETA
X-ray

Software Mentioned

GIXAS
PowderCell
Protocafe

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