Operando X-ray Raman Studies of Oxide Derived Copper to Uncover the Carbon Dioxide Reduction Mechanism

This study aims to elucidate the operational mechanism of highly active electrocatalysts for CO2 reduction (CO2R) through operando X-ray Raman Scattering (XRS) at high current densities. By utilising the O K-edge and transition metal (TM) L-edges as probes of TM-O hybridisation, we seek to uncover the mechanism of the CO2R reaction. The short attenuation length of soft X-rays limits the operando studies with soft X-ray Absorption Spectroscopy; thus, we developed a novel cell to enhance gas mass transport at the electrode surface. Our investigations focuses on copper-based electrodes to understand operational mechanisms at high potentials linked to C2+ product formation. This research is crucial for improving the selectivity and stability of CO2R catalysts, promoting the industrial use of electrochemical processes for energy-dense products. We aim to utilise XRS for operando measurements of TM and O redox processes in CO2R to advance knowledge of the reaction mechanism.