In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating

A plug-flow fixed-bed cell for synchrotron powder X-ray diffraction (PXRD) and X-ray absorption fine structure (XAFS) idoneous for the study of heterogeneous catalysts at high temperature, pressure and under gas flow is designed, constructed and demonstrated. The operating conditions up to 1000°C an...

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Main Authors: Benjamin Bischoff, Maged F. Bekheet, Emiliano Dal Molin, Sebastian Praetz, Birgit Kanngießer, Reinhard Schomäcker, Martin Etter, Henrik S. Jeppesen, Akhil Tayal, Aleksander Gurlo, Albert Gili
Format: Article
Language:English
Published: International Union of Crystallography 2024-01-01
Series:Journal of Synchrotron Radiation
Subjects:
Online Access:http://scripts.iucr.org/cgi-bin/paper?S1600577523009591
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author Benjamin Bischoff
Maged F. Bekheet
Emiliano Dal Molin
Sebastian Praetz
Birgit Kanngießer
Reinhard Schomäcker
Martin Etter
Henrik S. Jeppesen
Akhil Tayal
Aleksander Gurlo
Albert Gili
author_facet Benjamin Bischoff
Maged F. Bekheet
Emiliano Dal Molin
Sebastian Praetz
Birgit Kanngießer
Reinhard Schomäcker
Martin Etter
Henrik S. Jeppesen
Akhil Tayal
Aleksander Gurlo
Albert Gili
author_sort Benjamin Bischoff
collection DOAJ
description A plug-flow fixed-bed cell for synchrotron powder X-ray diffraction (PXRD) and X-ray absorption fine structure (XAFS) idoneous for the study of heterogeneous catalysts at high temperature, pressure and under gas flow is designed, constructed and demonstrated. The operating conditions up to 1000°C and 50 bar are ensured by a set of mass flow controllers, pressure regulators and two infra-red lamps that constitute a robust and ultra-fast heating and cooling method. The performance of the system and cell for carbon dioxide hydrogenation reactions under specified temperatures, gas flows and pressures is demonstrated both for PXRD and XAFS at the P02.1 (PXRD) and the P64 (XAFS) beamlines of the Deutsches Elektronen-Synchrotron (DESY).
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spelling doaj.art-9cd954164d9a4fa78723d6590acfda092024-01-08T14:34:54ZengInternational Union of CrystallographyJournal of Synchrotron Radiation1600-57752024-01-01311778410.1107/S1600577523009591vl5016In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heatingBenjamin Bischoff0Maged F. Bekheet1Emiliano Dal Molin2Sebastian Praetz3Birgit Kanngießer4Reinhard Schomäcker5Martin Etter6Henrik S. Jeppesen7Akhil Tayal8Aleksander Gurlo9Albert Gili10Technische Universität Berlin, Faculty III Process Sciences, Institute of Materials Science and Technology, Chair of Advanced Ceramic Materials, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty III Process Sciences, Institute of Materials Science and Technology, Chair of Advanced Ceramic Materials, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty III Process Sciences, Institute of Materials Science and Technology, Chair of Advanced Ceramic Materials, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty III Process Sciences, Institute for Optic and Atomic Physics, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty III Process Sciences, Institute for Optic and Atomic Physics, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty II Mathematik und Naturwissenschaften, Institut für Chemie, Straße des 17 Juni 135, 10623 Berlin, GermanyDeutsches Elektronen-Synchrotron (DESY), Notkestrasse 85, 22607 Hamburg, GermanyDeutsches Elektronen-Synchrotron (DESY), Notkestrasse 85, 22607 Hamburg, GermanyDeutsches Elektronen-Synchrotron (DESY), Notkestrasse 85, 22607 Hamburg, GermanyTechnische Universität Berlin, Faculty III Process Sciences, Institute of Materials Science and Technology, Chair of Advanced Ceramic Materials, Straße des 17 Juni 135, 10623 Berlin, GermanyTechnische Universität Berlin, Faculty II Mathematik und Naturwissenschaften, Institut für Chemie, Straße des 17 Juni 135, 10623 Berlin, GermanyA plug-flow fixed-bed cell for synchrotron powder X-ray diffraction (PXRD) and X-ray absorption fine structure (XAFS) idoneous for the study of heterogeneous catalysts at high temperature, pressure and under gas flow is designed, constructed and demonstrated. The operating conditions up to 1000°C and 50 bar are ensured by a set of mass flow controllers, pressure regulators and two infra-red lamps that constitute a robust and ultra-fast heating and cooling method. The performance of the system and cell for carbon dioxide hydrogenation reactions under specified temperatures, gas flows and pressures is demonstrated both for PXRD and XAFS at the P02.1 (PXRD) and the P64 (XAFS) beamlines of the Deutsches Elektronen-Synchrotron (DESY).http://scripts.iucr.org/cgi-bin/paper?S1600577523009591plug-flow fixed-bed cellultra-fast infra-red heatinggas–solid interactionsin situ x-ray diffractionin situ x-ray absorption fine structure
spellingShingle Benjamin Bischoff
Maged F. Bekheet
Emiliano Dal Molin
Sebastian Praetz
Birgit Kanngießer
Reinhard Schomäcker
Martin Etter
Henrik S. Jeppesen
Akhil Tayal
Aleksander Gurlo
Albert Gili
In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
Journal of Synchrotron Radiation
plug-flow fixed-bed cell
ultra-fast infra-red heating
gas–solid interactions
in situ x-ray diffraction
in situ x-ray absorption fine structure
title In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
title_full In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
title_fullStr In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
title_full_unstemmed In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
title_short In situ/operando plug-flow fixed-bed cell for synchrotron PXRD and XAFS investigations at high temperature, pressure, controlled gas atmosphere and ultra-fast heating
title_sort in situ operando plug flow fixed bed cell for synchrotron pxrd and xafs investigations at high temperature pressure controlled gas atmosphere and ultra fast heating
topic plug-flow fixed-bed cell
ultra-fast infra-red heating
gas–solid interactions
in situ x-ray diffraction
in situ x-ray absorption fine structure
url http://scripts.iucr.org/cgi-bin/paper?S1600577523009591
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