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Updated: Feb 13, 2026

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy
Published on: September 12, 2018
In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy
Benedikt Lassalle-Kaiser1, Sheraz Gul2, Jan Kern2,3
1Synchrotron SOLEIL, L'Orme des Merisiers, Saint-Aubin, 91191 Gif-sur-Yvette, France.
Abstract:
This review focuses on the use of X-ray absorption and emission spectroscopy techniques using hard X-rays to study electrocatalysts under in situ/operando conditions. We describe the importance and the versatility of methods in the study of electrodes in contact with the electrolytes, when being cycled through the catalytic potentials during the progress of the oxygen-evolution, oxygen reduction and hydrogen evolution reactions. The catalytic oxygen evolution reaction is illustrated with examples using Co, Ni and Mn oxides, and Mo and Co sulfides are used as an example for the hydrogen evolution reaction. A bimetallic, bifunctional oxygen evolving and oxygen reducing Ni/Mn oxide is also presented. The various advantages and constraints in the use of these techniques and the future outlook are discussed.
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