Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis

Institute of Catalysis Research and Technology (IKFT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz Platz 1, 76344 Eggenstein-Leopoldshafen, Germany

Paul Scherrer Institut (PSI), 5252 Villigen, Switzerland

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Deutsches Elektronen-Synchrotron DESY, Notkestrasse 85, 22607 Hamburg, Germany

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European Synchrotron Radiation Facility (ESRF), 71 Avenue des Martyrs, 38000 Grenoble, France

Author to whom correspondence should be addressed.

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Current affiliation: [email protected] Sector 20, Advanced Photon Source, Argonne National Laboratory, 9700 S. Cass Avenue, Argonne, IL 60439, USA.

^‡

Current affiliation: Canadian Light Source Inc., 44 Innovation Boulevard, Saskatoon, SK S7N 2V3, Canada.

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Current affiliation: European XFEL GmbH, Holzkoppel 4, 22869 Schenefeld, Germany.

Academic Editor: Gloria Berlier

Catalysts 2021, 11(4), 459; https://doi.org/10.3390/catal11040459

Received: 13 March 2021 / Revised: 28 March 2021 / Accepted: 29 March 2021 / Published: 1 April 2021

(This article belongs to the Special Issue 2020s Vision on Catalysts: Operando Characterization Methods)

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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 CO₂ 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. View Full-Text

Keywords: in situ; operando; synchrotron radiation; X-ray tomography

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MDPI and ACS Style

Becher, J.; Weber, S.; Ferreira Sanchez, D.; Doronkin, D.E.; Garrevoet, J.; Falkenberg, G.; Motta Meira, D.; Pascarelli, S.; Grunwaldt, J.-D.; Sheppard, T.L. Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis. Catalysts 2021, 11, 459. https://doi.org/10.3390/catal11040459

AMA Style

Becher J, Weber S, Ferreira Sanchez D, Doronkin DE, Garrevoet J, Falkenberg G, Motta Meira D, Pascarelli S, Grunwaldt J-D, Sheppard TL. Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis. Catalysts. 2021; 11(4):459. https://doi.org/10.3390/catal11040459

Chicago/Turabian Style

Becher, Johannes, Sebastian Weber, Dario Ferreira Sanchez, Dmitry E. Doronkin, Jan Garrevoet, Gerald Falkenberg, Debora Motta Meira, Sakura Pascarelli, Jan-Dierk Grunwaldt, and Thomas L. Sheppard. 2021. "Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis" Catalysts 11, no. 4: 459. https://doi.org/10.3390/catal11040459

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Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis

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