Abstract
AbstractSoft X‐ray spectroscopy is a powerful method to investigate materials on an element selective level with respect to their atomic and electronic structure. However, its application is technically challenging for in situ or operando investigations of materials for electrochemical applications. Herein, we present a spectroelectrochemical flow‐cell designed to enable state‐of‐the‐art electrochemical characterization while being installed in a vacuum chamber for the direct accessibility of the electroactive sample to soft X‐rays. An overview of the application of soft X‐ray photon‐in–photon‐out spectroscopic studies to electromaterials is provided, along with discussions of experimental and technical considerations specific to this highly sensitive mode of analysis. Application of the cell for the in situ spectroelectrochemical characterization of an electrodeposited nickel oxide water electrooxidation catalyst is demonstrated.
Highlights
The development of materials for energy conversion and storage to facilitate the usage of sustainable energy remains a prominent scientific challenge
The counter electrode (CE) is placed into a compartment separated by e.g. a proton conductive polymer, such as Nafion, to avoid interference of dissolved material or products generated at the CE with the processes of interest occurring at the working electrode (WE)
The cell design is applicable for any suitable type of spectrometer/endstation, though the mounting points shown are adapted for the LiXEdrom endstation[16] of the synchrotron radiation light source BESSY II, Berlin
Summary
The development of materials for energy conversion and storage to facilitate the usage of sustainable energy remains a prominent scientific challenge. We present a vacuum compatible cell for in situ and operando soft X-ray photon-in–photon-out spectroelectrochemical studies, that was designed to provide optimized and mutually balanced spectroscopic and electrochemical conditions This includes a balancing of the electrochemically active and the spectroscopically accessible area, conventional arrangement of the working-referencecounter electrodes, an optimized flow pathway for the electrolyte solution and bubble removal, increased volume (compared to other cells), and spatial separation of the working and counter electrode compartments by an ion conductive polymer separator. Taken together, these and other features of the cell design discussed below avoid instrumental challenges of the electrochemical measurements, while enabling collection of soft X-ray spectroscopic data in situ. Its capabilities are demonstrated by an in situ TFY study on an electrodeposited NiOx thin film as an anode material for the oxygen evolution reaction (OER)
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