The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

Frank, Sara; Ceccato, Marcel; Jeppesen, Henrik S.; Marks, Melissa J.; Nielsen, Mads L. N.; Lu, Ronghui; Gammelgaard, Jens Jakob; Quinson, Jonathan; Sharma, Ruchi; Jensen, Julie S.; Hjelme, Sara; Friberg Klysner, Cecilie; Billinge, Simon J. L.; Just, Justus; Gjørup, Frederik H.; Catalano, Jacopo; Lock, Nina

doi:10.1107/S1600576724007817

The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

Journal Article · Fri Sep 20 00:00:00 EDT 2024 · Journal of Applied Crystallography (Online)

DOI:https://doi.org/10.1107/S1600576724007817· OSTI ID:2447508

; Ceccato, Marcel; Jeppesen, Henrik S.; Marks, Melissa J.; Nielsen, Mads L. N.; ; Gammelgaard, Jens Jakob; Quinson, Jonathan; Sharma, Ruchi; Jensen, Julie S.; ; Friberg Klysner, Cecilie; ; ; ; Catalano, Jacopo; Lock, Nina

Understanding the structure–property relationship in electrocatalysts under working conditions is crucial for the rational design of novel and improved catalytic materials. This paper presents the Aarhus University reactor for electrochemical studies using X-rays (AUREX) operando electrocatalytic flow cell, designed as an easy-to-use versatile setup with a minimal background contribution and a uniform flow field to limit concentration polarization and handle gas formation. The cell has been employed to measure operando total scattering, diffraction and absorption spectroscopy as well as simultaneous combinations thereof on a commercial silver electrocatalyst for proof of concept. This combination of operando techniques allows for monitoring of the short-, medium- and long-range structure under working conditions, including an applied potential, liquid electrolyte and local reaction environment. The structural transformations of the Ag electrocatalyst are monitored with non-negative matrix factorization, linear combination analysis, the Pearson correlation coefficient matrix, and refinements in both real and reciprocal space. Upon application of an oxidative potential in an Ar-saturated aqueous 0.1 M KHCO ₃ /K ₂ CO ₃ electrolyte, the face-centered cubic (f.c.c.) Ag gradually transforms first to a trigonal Ag ₂ CO ₃ phase, followed by the formation of a monoclinic Ag ₂ CO ₃ phase. A reducing potential immediately reverts the structure to the Ag (f.c.c.) phase. Following the electrochemical-reaction-induced phase transitions is of fundamental interest and necessary for understanding and improving the stability of electrocatalysts, and the operando cell proves a versatile setup for probing this. In addition, it is demonstrated that, when studying electrochemical reactions, a high energy or short exposure time is needed to circumvent beam-induced effects.

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Sponsoring Organization:: USDOE

Grant/Contract Number:: SC0019212

OSTI ID:: 2447508

Journal Information:: Journal of Applied Crystallography (Online), Journal Name: Journal of Applied Crystallography (Online) Journal Issue: 5 Vol. 57; ISSN 1600-5767; ISSN JACGAR

Publisher:: International Union of Crystallography (IUCr)Copyright Statement

Country of Publication:: Denmark

Language:: English

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