In-situ STXM characterization of Cu/Cu₂O electrocatalysts for CO₂ reduction

Title data

Zhang, Chunyang ; Eraky, Haytham ; Ingino, Pablo ; Obst, Martin ; Wang, Jian ; Higgins, Drew ; Hitchcock, Adam P.:
In-situ STXM characterization of Cu/Cu₂O electrocatalysts for CO₂ reduction.
In: Chuang, Tzu-Hung ; Lin, Bi-Hsuan ; Shiu, Hung-Wei ; Wei, Der-Hsin (ed.): Proceedings of the 15th International Conference on X-ray Microscopy – XRM2022. - Melville, NY : AIP Publishing , 2023 . - 020011 . - (AIP Conference Proceedings ; 2990 )
ISBN 978-0-7354-4672-4
DOI: https://doi.org/10.1063/5.0168124

Project information

Abstract in another language

Scanning Transmission X-ray microscopy (STXM) is a synchrotron-based soft X-ray spectro-microscopic technique which provides chemically selective imaging via spatially resolved X-ray absorption spectroscopy. In-situ STXM of electrocatalysts provides imaging and spectroscopic information at different time / voltage points in the electrochemical process, which helps to understand the changes of morphology and chemistry that occur under reaction conditions. We have developed in-situ flow electrochemical devices with an electrolyte thickness < 2 μm which allow STXM measurements while controlling the electrochemical reaction environment, thus providing a platform for in-situ studies of electrochemical oxidation and reduction processes. Here we report results of in-situ STXM studies on electrochemically generated Cu based catalysts for the CO₂ reduction reaction (CO₂R). Cu 2p STXM spectromicroscopy was successfully used to monitor the morphology and oxidation state changes in the initially formed Cu/Cu₂O nano- particles as the potential was changed from open circuit to values where CO₂ reduction occurs. Ex-situ ptychography was also conducted on the same catalyst nanoparticles to provide spectro-microscopy images with similar chemical analysis but improved spatial resolution.