TY - JOUR

T1 - Shedding Light on Electrocatalysts

T2 - Practical Considerations for Operando Studies with High-Energy X-Rays

AU - Pittkowski, Rebecca K.

N1 - Funding Information: This work was supported by the Danish National Research Foundation Center for High Entropy Alloy Catalysis (DNRF 149). Publisher Copyright: © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH.

PY - 2024/6/17

Y1 - 2024/6/17

N2 - Operando studies using high-energy X-rays from synchrotron sources are essential for unraveling the complex material transformation that electrocatalysts undergo under operating conditions. This article explores key considerations to perform these experiments and the insights gained from such studies on nanostructured electrocatalysts. Critical factors include optimizing electrochemical performance while obtaining high-quality X-ray signals, which often require compromises. The electrochemical operando cell design is crucial, and several different cells are discussed here. Working electrode geometries parallel to the X-ray beam, probed with a microfocused beam, are emerging as promising solutions for realistic electrochemical performance in operando cells. Careful attention must also be paid to the electrochemical measuring conditions, electrode loading, and beam damage to ensure reliable experiments. When carefully performed and by combining multiple characterization techniques, operando studies with high-energy X-rays offer the unique possibility to fully understand the structure of the active electrocatalyst.

AB - Operando studies using high-energy X-rays from synchrotron sources are essential for unraveling the complex material transformation that electrocatalysts undergo under operating conditions. This article explores key considerations to perform these experiments and the insights gained from such studies on nanostructured electrocatalysts. Critical factors include optimizing electrochemical performance while obtaining high-quality X-ray signals, which often require compromises. The electrochemical operando cell design is crucial, and several different cells are discussed here. Working electrode geometries parallel to the X-ray beam, probed with a microfocused beam, are emerging as promising solutions for realistic electrochemical performance in operando cells. Careful attention must also be paid to the electrochemical measuring conditions, electrode loading, and beam damage to ensure reliable experiments. When carefully performed and by combining multiple characterization techniques, operando studies with high-energy X-rays offer the unique possibility to fully understand the structure of the active electrocatalyst.

KW - electrocatalysis

KW - in situ

KW - nanoparticles

KW - operando

KW - X-ray absorption spectroscopy

KW - X-ray scattering

UR - http://www.scopus.com/inward/record.url?scp=85193685822&partnerID=8YFLogxK

U2 - 10.1002/celc.202400171

DO - 10.1002/celc.202400171

M3 - Journal article

AN - SCOPUS:85193685822

VL - 11

JO - ChemElectroChem

JF - ChemElectroChem

SN - 2196-0216

IS - 12

M1 - e202400171

ER -