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

Nina S Genz; Antti-Jussi Kallio; Ramon Oord; Frank Krumeich; Anuj Pokle; Øystein Prytz; Unni Olsbye; Florian Meirer; Simo Huotari; Bert M Weckhuysen

doi:10.1002/anie.202209334

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

Angew Chem Int Ed Engl. 2022 Nov 25;61(48):e202209334. doi: 10.1002/anie.202209334. Epub 2022 Oct 26.

Authors

Affiliations

¹ Inorganic Chemistry and Catalysis group, Department of Chemistry, Utrecht University, Universiteitsweg 99, 3584 CG, Utrecht, The Netherlands.
² Department of Physics, University of Helsinki, P. O. Box 64, 00014, Helsinki, Finland.
³ Laboratory of Inorganic Chemistry, Department of Chemistry, ETH Zürich, Vladimir-Prelog-Weg 1, 8093, Zürich, Switzerland.
⁴ Department of Physics, Center for Materials Science and Nanotechnology, University of Oslo, P.O. Box 1048, 0316, Oslo, Norway.
⁵ Department of Chemistry, University of Oslo, P.O. Box 1033, 0315, Oslo, Norway.

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.

Keywords: Alloys; CO2 Hydrogenation; Heterogeneous Catalysis; Multielement Catalysts; X-Ray Absorption Spectroscopy.

Abstract

Grants and funding