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

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

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 fl...

Full description

Saved in:
Bibliographic Details
Published in:Journal of applied crystallography Vol. 57; no. 5; pp. 1489 - 1502
Main Authors: 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
Format: Journal Article
Language:English
Published: 5 Abbey Square, Chester, Cheshire CH1 2HU, England International Union of Crystallography 01-10-2024
Blackwell Publishing Ltd
International Union of Crystallography (IUCr)
Subjects:
Absorption spectroscopy
cell design
Chemical reactions
Correlation coefficient
Correlation coefficients
Diffraction
electrocatalysis
Electrocatalysts
Electrochemical cells
Electrochemistry
Electrode polarization
Electrolytes
Environmental monitoring
Gas formation
operando studies
Phase transitions
Potassium carbonate
Research Papers
Scattering
Silver
Spectrum analysis
structure–property relationships
Uniform flow
Working conditions
X-ray diffraction
X‐ray absorption spectroscopy
X‐ray scattering
operando studies
X-ray scattering
structure–property relationships
X-ray absorption spectroscopy
cell design
electrocatalysis
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary: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 KHCO3/K2CO3 electrolyte, the face‐centered cubic (f.c.c.) Ag gradually transforms first to a trigonal Ag2CO3 phase, followed by the formation of a monoclinic Ag2CO3 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. The AUREX operando electrocatalytic cell is demonstrated to be a versatile setup for elucidating structure–property relations by means of X‐ray total scattering and multimodal absorption and diffraction techniques using an Ag electrocatalyst for proof of concept.
Bibliography:ObjectType-Article-1
SourceType-Scholarly Journals-1
ObjectType-Feature-2
content type line 23
USDOE
ISSN:1600-5767
0021-8898
1600-5767
DOI:10.1107/S1600576724007817