Design and application of an electrochemical cell for operando X-ray diffraction and absorption studies for electrocatalysts.

The development of advanced catalysts for various electrochemical reactions necessitates precise characterization of their structure and dynamic evolution. This study introduces an innovative electrochemical cell tailored for operando X-ray characterizations, including X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS). The cell features an adjustable aqueous electrolyte window to reduce X-ray signal absorption and an integrated flow system for efficient removal of gas products. This design enables simultaneous XRD and XAFS measurements in both fluorescence and transmission modes. Using LiCoO(2) as a model oxygen evolution reaction catalyst, operando measurements reveal structural transformations during the reaction. This device will aid in the exploration of catalyst mechanisms and the development of high-performance catalysts.