Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station

A novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are...

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Autores: Salas, Eduardo, Muñoz-Noval, A., Heyman, C., Ovín Ania, María Concepción, Parra Soto, José Bernardo, García-Granda, Santiago, Calero, S., Rubio-Zuazo, J., Castro, Germán R.
Formato: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2015
País:España
Recursos:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/123294
Acesso em linha:http://hdl.handle.net/10261/123294
Access Level:acceso abierto
Palavra-chave:X-ray powder diffraction
Isobaric/isothermal environment
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spelling Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction stationSalas, EduardoMuñoz-Noval, A.Heyman, C.Ovín Ania, María ConcepciónParra Soto, José BernardoGarcía-Granda, SantiagoCalero, S.Rubio-Zuazo, J.Castro, Germán R.X-ray powder diffractionIsobaric/isothermal environmentA novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10−3 to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. Direct structure deformations by the adsorption of Ar and N2 gases have been observed in situ, demonstrating that this set-up is perfectly suitable for direct structural analysis under in operando conditions. The presented results prove the feasibility of this novel experimental station for the characterization in real time of solid–gas reactions and other solid–gas processes by SR-HRPD.The authors are grateful to the SpLine staff for their assistance. Financial support under grant PIE 201060E013 of the Consejo Superior de Investigaciones Científicas-CSIC and the Spanish Ministry of Economy and Competitiveness MINECO is also acknowledged.Peer reviewedWiley-VCHMinisterio de Economía y Competitividad (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]201520152015info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Postprintinfo:eu-repo/semantics/acceptedVersionhttp://hdl.handle.net/10261/123294reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Ingléshttp://dx.doi.org/10.1107/S1600577514021018Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/1232942026-05-22T06:33:51Z
dc.title.none.fl_str_mv Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
title Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
spellingShingle Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
Salas, Eduardo
X-ray powder diffraction
Isobaric/isothermal environment
title_short Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
title_full Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
title_fullStr Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
title_full_unstemmed Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
title_sort Design and development of a controlled pressure/temperature set-up for in situ studies of solid–gas processes and reactions in a synchrotron X-ray powder diffraction station
dc.creator.none.fl_str_mv Salas, Eduardo
Muñoz-Noval, A.
Heyman, C.
Ovín Ania, María Concepción
Parra Soto, José Bernardo
García-Granda, Santiago
Calero, S.
Rubio-Zuazo, J.
Castro, Germán R.
author Salas, Eduardo
author_facet Salas, Eduardo
Muñoz-Noval, A.
Heyman, C.
Ovín Ania, María Concepción
Parra Soto, José Bernardo
García-Granda, Santiago
Calero, S.
Rubio-Zuazo, J.
Castro, Germán R.
author_role author
author2 Muñoz-Noval, A.
Heyman, C.
Ovín Ania, María Concepción
Parra Soto, José Bernardo
García-Granda, Santiago
Calero, S.
Rubio-Zuazo, J.
Castro, Germán R.
author2_role author
author
author
author
author
author
author
author
dc.contributor.none.fl_str_mv Ministerio de Economía y Competitividad (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv X-ray powder diffraction
Isobaric/isothermal environment
topic X-ray powder diffraction
Isobaric/isothermal environment
description A novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid–gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10−3 to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. Direct structure deformations by the adsorption of Ar and N2 gases have been observed in situ, demonstrating that this set-up is perfectly suitable for direct structural analysis under in operando conditions. The presented results prove the feasibility of this novel experimental station for the characterization in real time of solid–gas reactions and other solid–gas processes by SR-HRPD.
publishDate 2015
dc.date.none.fl_str_mv 2015
2015
2015
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Postprint
info:eu-repo/semantics/acceptedVersion
format article
status_str acceptedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/123294
url http://hdl.handle.net/10261/123294
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv http://dx.doi.org/10.1107/S1600577514021018
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Wiley-VCH
publisher.none.fl_str_mv Wiley-VCH
dc.source.none.fl_str_mv reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC
instname:Consejo Superior de Investigaciones Científicas (CSIC)
instname_str Consejo Superior de Investigaciones Científicas (CSIC)
reponame_str DIGITAL.CSIC. Repositorio Institucional del CSIC
collection DIGITAL.CSIC. Repositorio Institucional del CSIC
repository.name.fl_str_mv
repository.mail.fl_str_mv
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score 15.228081

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