Year: 2026
Type: preprint
Abstract: Operando characterization techniques allow the understanding of electrochemical energy materials under operating conditions, which is essential to design high-performance electrocatalysts. Here, we present a novel operando electrochemical cell designed for X-ray absorption spectroscopy (XAS), enabling the simultaneous acquisition of electrochemical data, real-time oxygen detection, and XAS spectra on X-ray opaque electrodes. The incident X-ray beam reaches the sample through the electrolyte rather than through the substrate in contrast to the majority of other cells. This configuration removes constraints related to substrate transparency and thickness, thereby broadening the range of compatible electrode materials and samples that can be analyzed. The cell was commissioned using a well-characterized CoOx catalyst for the oxygen evolution reaction in alkaline media. Reversible shifts in the Co K-edge position were observed under applied potential steps, directly correlating electronic structure changes with electrochemical activity and oxygen production. The modular and adaptable design provides a versatile platform for advanced spectroelectrochemical investigations and can be extended to a wide range of electrochemical systems and complementary spectroscopic techniques.
Source: ChemRxiv
Language: English
Subfield: Radiation
Field: Physics and Astronomy
Domain: Physical Sciences
Open Access status: green
OpenAlex ID: W7223178628