Operando Laboratory‐Based Multi‐Edge X‐Ray Absorption Near‐Edge Spectroscopy of Solid Catalysts

Abstract Laboratory‐based X‐ray absorption spectroscopy (XAS) and especially X‐ray absorption near‐edge structure (XANES) offers new opportunities in catalyst characterization and presents not only an alternative, but also a complementary approach to precious beamtime at synchrotron facilities. We successfully designed a laboratory‐based setup for performing operando, quasi‐simultaneous XANES analysis at multiple K‐edges, more specifically, operando XANES of mono‐, bi‐, and trimetallic CO2 hydrogenation catalysts containing Ni, Fe, and Cu. Detailed operando XANES studies of the multielement solid catalysts revealed metal‐dependent differences in the reducibility and re‐oxidation behavior and their influence on the catalytic performance in CO2 hydrogenation. The applicability of operando laboratory‐based XANES at multiple K‐edges paves the way for advanced multielement catalyst characterization complementing detailed studies at synchrotron facilities.