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.