Journal Article

PUBDB-2021-02756

http://join2-wiki.gsi.de/foswiki/pub/Main/Artwork/join2_logo100x88.png Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis

Becher, J.Extern* ; Weber, S.Extern* ; Ferreira Sanchez, D. ; Doronkin, D.Extern* ; Garrevoet, J.DESY* ; Falkenberg, G.DESY* ; Motta Meira, D. ; Pascarelli, S.XFEL.EU* ; Grunwaldt, J.-D.Extern* ; Sheppard, T. L. (Corresponding author)Extern*

2021
MDPI Basel

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Please use a persistent id in citations: doi:10.3390/catal11040459  doi:10.3204/PUBDB-2021-02756

Abstract: Structure–activity relations in heterogeneous catalysis can be revealed through in situ and operando measurements of catalysts in their active state. While hard X-ray tomography is an ideal method for non-invasive, multimodal 3D structural characterization on the micron to nm scale, performing tomography under controlled gas and temperature conditions is challenging. Here, we present a flexible sample environment for operando hard X-ray tomography at synchrotron radiation sources. The setup features are discussed, with demonstrations of operando powder X-ray diffraction tomography (XRD-CT) and energy-dispersive tomographic X-ray absorption spectroscopy (ED-XAS-CT). Catalysts for CO$_2$ methanation and partial oxidation of methane are shown as case studies. The setup can be adapted for different hard X-ray microscopy, spectroscopy, or scattering synchrotron radiation beamlines, is compatible with absorption, diffraction, fluorescence, and phase-contrast imaging, and can operate with scanning focused beam or full-field acquisition mode. We present an accessible methodology for operando hard X-ray tomography studies, which offer a unique source of 3D spatially resolved characterization data unavailable to contemporary methods.

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Contributing Institute(s):

1. FS-PETRA (FS-PETRA)
2. FS-Photon Science (FS-PS)
3. externe Institute im Bereich Photon Science (KIT)
4. Experimentebetreuung PETRA III (FS-PET-S)

Research Program(s):

1. 632 - Materials – Quantum, Complex and Functional Materials (POF4-632) (POF4-632)
2. 6G3 - PETRA III (DESY) (POF4-6G3) (POF4-6G3)
3. FS-Proposal: I-20191105 (I-20191105) (I-20191105)
4. FS-Proposal: I-20190299 (I-20190299) (I-20190299)

Experiment(s):

1. PETRA Beamline P06 (PETRA III)

Appears in the scientific report 2021

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