This article reviews progress in the study of materials using X-ray-based techniques from an electrochemistry perspective. We focus on in situ/in operando surface X-ray scattering, X-ray absorption spectroscopy, and the combination of both methods. The background of these techniques together with key concepts is introduced. Key examples of in situ and in operando investigation of liquid–solid and liquid–liquid interfaces are presented. X-ray scattering and spectroscopy have helped to develop an understanding of the underlying atomic and molecular processes associated with electrocatalysis, electrodeposition, and battery materials. We highlight recent developments, including resonant surface diffraction and time-resolved studies.

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