Versatile spectroscopic cell for operando studies in heterogeneous catalysis using tender X‐ray spectroscopy in fluorescence mode

Author:

Suarez Orduz H. A.12ORCID,Heck S.‐L.2ORCID,Dolcet P.2ORCID,Watier Y.1ORCID,Casapu M.2ORCID,Grunwaldt J.‐D.23ORCID,Glatzel P.1ORCID

Affiliation:

1. ESRF – The European Synchrotron 71 Avenue des Martyrs 38000 Grenoble France

2. Institute for Chemical Technology and Polymer Chemistry (ITCP) Karlsruhe Institute of Technology (KIT) Engesserstr. 18/20 76131 Karlsruhe Germany

3. Institute of Catalysis Research and Technology (IKFT) Karlsruhe Institute of Technology (KIT) 76344 Eggenstein-Leopoldshafen Germany

Abstract

AbstractThe design and commissioning of a cell suitable for operando studies using high‐energy‐resolution fluorescence‐detected X‐ray absorption near‐edge structure (HERFD‐XANES) spectroscopy in the tender X‐ray regime is reported. The cell is optimized for measurements within the energy range of 1.5 keV to 4.5 keV. It has a plug‐flow geometry and can be used for sieved powder samples, analogous to reactors employed for laboratory tests. The functionality of the spectroscopic cell is demonstrated in the area of emission control using CO oxidation as target reaction over 1 wt.% Rh/γ‐Al2O3 as catalyst. We show how HERFD‐XANES at the Rh L3‐edge captures variations in the noble metal structure resulting from the interaction with the support material and reactant molecules. Moreover, distinct structural changes were identified along the catalyst bed as a function of temperature and local gas mixture.

Publisher

Wiley

Subject

Materials Science (miscellaneous)

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