The electrochemical reduction of CO2 is an indispensable choice under the carbon peak and neutrality goal. It is of great significance to clarify the structure-performance relationship of catalysts at atomic and electronic dimensions. Synchrotron radiation X-ray spectroscopy (SRXS), including X-ray absorption fine structure (XAFS) and X-ray emission spectroscopy (XES), is a unique method to study the local atomic and electronic structure of materials. Toward this end, the speaker has developed synchrotron radiation high-resolution X-ray spectroscopy methods based on the von Hamos spectrometer built on BL14W1 at Shanghai Synchrotron Radiation Facility. The high-resolution X-ray spectroscopy could break the broadening lifetime limitation of traditional XAFS spectroscopy and measure the occupied orbitals directly. Using operando measurement technology combined with difference spectra analysis and spectroscopy simulation, the dynamic changes of local atomic and electronic structures of Cu-based catalysts during CO2 reduction was monitored. Accordingly, the electron spin, charge transfer and other fine electron structure information of the catalyst surface sites in the key steps was obtained. Exploring the origin of intrinsic structure that determines the kinetics of CO2 reduction reaction facilities the full-dimensional exploration of the process of high-performance and high-stability catalysts promoting CO2 reduction to olefin and alcohol. The high-energy-resolution SRXS methods, characterizing the active-site geometry and dynamic structural change, is a novel and powerful technique to elucidate complex catalytic mechanisms and is expected to contribute to the rational design of highly effective catalysts.

Exploring the mechanism of carbon dioxide electroreduction based on synchrotron radiation high-energy-resolution X-ray spectroscopy methods

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ACS Fall 2022

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