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Improvement of electrochemical technologies is one of the most popular topicsin the field of renewable energy. However, this process requires a deepunderstanding of the electrode electrolyte interface behavior under operandoconditions. X-ray absorption spectroscopy (XAS) is widely employed tocharacterize electrode materials, providing element-selective oxidation stateand local structure. Several existing cells allow studies as close as possibleto realistic operating conditions, but most of them rely on the deposition ofthe electrodes on conductive and X-ray transparent materials, from where theradiation impinges the sample. In this work, we present a new electrochemicalflow-cell for operando XAS that can be used with X-ray opaque substrates, sincethe signal is effectively detected from the electrode surface, as the radiationpasses through a thin layer of electrolyte. The electrolyte can flow over theelectrode, reducing bubble formation and avoiding strong reactant concentrationgradients. We show that high-quality data can be obtained under operandoconditions, thanks to the high efficiency of the cell from the hard X-rayregime down to 4 keV. We report as a case study the operando XAS investigationat the Fe and Ni K-edges on Ni-doped maghemite films, epitaxially grown on Ptsubstrates. The effect of the Ni content on the catalytic performances for theoxygen evolution reaction is discussed.

A Novel Electrochemical Flow-Cell for Operando XAS Investigations On X-ray Opaque Supports