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

© Sara Frank et al. 2024.

Bibliographische Detailangaben
Veröffentlicht in:Journal of applied crystallography. - 1998. - 57(2024), Pt 5 vom: 01. Okt., Seite 1489-1502
1. Verfasser: Frank, Sara (VerfasserIn)
Weitere Verfasser: 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: Online-Aufsatz
Sprache:English
Veröffentlicht: 2024
Zugriff auf das übergeordnete Werk:Journal of applied crystallography
Schlagworte:Journal Article X-ray absorption spectroscopy X-ray scattering cell design electrocatalysis operando studies structure–property relationships
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520 |a 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 
650 4 |a Journal Article 
650 4 |a X-ray absorption spectroscopy 
650 4 |a X-ray scattering 
650 4 |a cell design 
650 4 |a electrocatalysis 
650 4 |a operando studies 
650 4 |a structure–property relationships 
700 1 |a Ceccato, Marcel  |e verfasserin  |4 aut 
700 1 |a Jeppesen, Henrik S  |e verfasserin  |4 aut 
700 1 |a Marks, Melissa J  |e verfasserin  |4 aut 
700 1 |a Nielsen, Mads L N  |e verfasserin  |4 aut 
700 1 |a Lu, Ronghui  |e verfasserin  |4 aut 
700 1 |a Gammelgaard, Jens Jakob  |e verfasserin  |4 aut 
700 1 |a Quinson, Jonathan  |e verfasserin  |4 aut 
700 1 |a Sharma, Ruchi  |e verfasserin  |4 aut 
700 1 |a Jensen, Julie S  |e verfasserin  |4 aut 
700 1 |a Hjelme, Sara  |e verfasserin  |4 aut 
700 1 |a Friberg Klysner, Cecilie  |e verfasserin  |4 aut 
700 1 |a Billinge, Simon J L  |e verfasserin  |4 aut 
700 1 |a Just, Justus  |e verfasserin  |4 aut 
700 1 |a Gjørup, Frederik H  |e verfasserin  |4 aut 
700 1 |a Catalano, Jacopo  |e verfasserin  |4 aut 
700 1 |a Lock, Nina  |e verfasserin  |4 aut 
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