Phenyl siloxane hybrid xerogels: structure and porous texture

The aim of this research is to investigate the effect of phenyltriethoxysilane (PhTEOS) and tetraethoxysilane (TEOS) molar ratios as silicon precursors on the structure and porous texture of xerogels. We have prepared phenyl-silane hybrid xerogels from mixtures of PhTEOS and TEOS at pH 10 and 333 K,...

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Autores: Moriones, P., Echeverría, Jesús C., Parra Soto, José Bernardo, Garrido, J.J.
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2019
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/223516
Acceso en línea:http://hdl.handle.net/10261/223516
Access Level:acceso abierto
Palabra clave:Sol–gel
Phenyltriethoxysilane
Hybrid xerogels
Porous texture
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spelling Phenyl siloxane hybrid xerogels: structure and porous textureMoriones, P.Echeverría, Jesús C.Parra Soto, José BernardoGarrido, J.J.Sol–gelPhenyltriethoxysilaneHybrid xerogelsPorous textureThe aim of this research is to investigate the effect of phenyltriethoxysilane (PhTEOS) and tetraethoxysilane (TEOS) molar ratios as silicon precursors on the structure and porous texture of xerogels. We have prepared phenyl-silane hybrid xerogels from mixtures of PhTEOS and TEOS at pH 10 and 333 K, using ethanol as a solvent. Characterization techniques include 29Si NMR, FTIR, XRD, FE-SEM, HRTEM, TGA-DSC, helium density, and gas adsorption (N2 at 77 K and CO2 at 273 K). In order to assess the contribution of the quadrupolar moment of N2 and CO2 in the adsorption we obtained the adsorption–desorption isotherm of Ar at 87.3 K for the xerogel synthesized from 50% PhTEOS. The morphology of xerogels changed from aggregates of spherical particles for 20% PhTEOS to lamellae for samples obtained with PhTEOS percentages equal or larger that 60%. The incorporation of phenyl groups into the xerogel matrix caused an increase in the spacing bond between silicon atoms and led to an intramolecular reaction and the formation of lamellar domains. Increasing the PhTEOS molar ratio in the mixture of silicon precursors produced hybrid xerogels with lower specific surface area, pore volume and characteristic energy. The similarity between the isotherms of N2 at 77 K and Ar at 87.3 K indicates that the main retention mechanism is physisorption and that the variation in the surface chemistry with the incorporation of phenyl groups doesn’t inhibit the retention of N2.This work was backed by the “Ministerio de Ciencia y Tecnología” (Grant No. CTQ2009-07993) and by the “Ministerio de Economía, Industria y Competitividad” (Grant No. MAT2016-78155-C2-2-R). Paula Moriones is grateful to the “Departamento de Industria y Tecnología, Comercio y Trabajo” of the Navarre Government for the fellowships granted (Ref. Number 175/01/08 and 269/01/08, respectively).Kluwer Academic PublishersMinisterio de Economía, Industria y Competitividad (España)Ministerio de Ciencia y Tecnología (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]2020202020192020info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Postprintinfo:eu-repo/semantics/acceptedVersionhttp://hdl.handle.net/10261/223516reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/MINECO/Plan Estatal de Investigación Científica y Técnica y de Innovación 2013-2016/MAT2016-78155-C2-2-Rhttp://dx.doi.org/10.1007/s10450-019-00075-9Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/2235162026-05-22T06:33:51Z
dc.title.none.fl_str_mv Phenyl siloxane hybrid xerogels: structure and porous texture
title Phenyl siloxane hybrid xerogels: structure and porous texture
spellingShingle Phenyl siloxane hybrid xerogels: structure and porous texture
Moriones, P.
Sol–gel
Phenyltriethoxysilane
Hybrid xerogels
Porous texture
title_short Phenyl siloxane hybrid xerogels: structure and porous texture
title_full Phenyl siloxane hybrid xerogels: structure and porous texture
title_fullStr Phenyl siloxane hybrid xerogels: structure and porous texture
title_full_unstemmed Phenyl siloxane hybrid xerogels: structure and porous texture
title_sort Phenyl siloxane hybrid xerogels: structure and porous texture
dc.creator.none.fl_str_mv Moriones, P.
Echeverría, Jesús C.
Parra Soto, José Bernardo
Garrido, J.J.
author Moriones, P.
author_facet Moriones, P.
Echeverría, Jesús C.
Parra Soto, José Bernardo
Garrido, J.J.
author_role author
author2 Echeverría, Jesús C.
Parra Soto, José Bernardo
Garrido, J.J.
author2_role author
author
author
dc.contributor.none.fl_str_mv Ministerio de Economía, Industria y Competitividad (España)
Ministerio de Ciencia y Tecnología (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Sol–gel
Phenyltriethoxysilane
Hybrid xerogels
Porous texture
topic Sol–gel
Phenyltriethoxysilane
Hybrid xerogels
Porous texture
description The aim of this research is to investigate the effect of phenyltriethoxysilane (PhTEOS) and tetraethoxysilane (TEOS) molar ratios as silicon precursors on the structure and porous texture of xerogels. We have prepared phenyl-silane hybrid xerogels from mixtures of PhTEOS and TEOS at pH 10 and 333 K, using ethanol as a solvent. Characterization techniques include 29Si NMR, FTIR, XRD, FE-SEM, HRTEM, TGA-DSC, helium density, and gas adsorption (N2 at 77 K and CO2 at 273 K). In order to assess the contribution of the quadrupolar moment of N2 and CO2 in the adsorption we obtained the adsorption–desorption isotherm of Ar at 87.3 K for the xerogel synthesized from 50% PhTEOS. The morphology of xerogels changed from aggregates of spherical particles for 20% PhTEOS to lamellae for samples obtained with PhTEOS percentages equal or larger that 60%. The incorporation of phenyl groups into the xerogel matrix caused an increase in the spacing bond between silicon atoms and led to an intramolecular reaction and the formation of lamellar domains. Increasing the PhTEOS molar ratio in the mixture of silicon precursors produced hybrid xerogels with lower specific surface area, pore volume and characteristic energy. The similarity between the isotherms of N2 at 77 K and Ar at 87.3 K indicates that the main retention mechanism is physisorption and that the variation in the surface chemistry with the incorporation of phenyl groups doesn’t inhibit the retention of N2.
publishDate 2019
dc.date.none.fl_str_mv 2019
2020
2020
2020
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/10261/223516
url http://hdl.handle.net/10261/223516
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/MINECO/Plan Estatal de Investigación Científica y Técnica y de Innovación 2013-2016/MAT2016-78155-C2-2-R
http://dx.doi.org/10.1007/s10450-019-00075-9

dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Kluwer Academic Publishers
publisher.none.fl_str_mv Kluwer Academic Publishers
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
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repository.mail.fl_str_mv
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