Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)

Autores
Abad, María J.; Barral, Luis; Fasce, Diana Patricia; Williams, Roberto Juan Jose
Año de publicación
2003
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
A polyhedral oligomeric silsesquioxane (POSS) containing one epoxy group and seven isobutyl groups per molecule was incorporated into an epoxy network following a two-stage process. In the first stage, POSS was reacted with an aromatic diamine, employing a 1:1 molar ratio of both reactants. The distribution of species at the end of reaction, determined by size exclusion chromatography (SEC), was close to the ideal one. In a second step, this precursor was reacted with the stoichiometric amount of an aromatic diepoxide to generate an organic-inorganic hybrid material containing 51.8 wt% POSS. A primary liquid-liquid phase separation process occurred at the time of adding the diepoxide to the POSS-diamine precursor. This led to a macrophase separation into epoxy-rich and POSS-rich regions, possibly derived from the incompatibility of the isobutyl groups attached to the POSS with the aromatic epoxy-amine network. A secondary phase separation occurred in the epoxy-rich phase in the course of polymerization, producing a dispersion of small POSS domains. Both modulated local thermal analysis (LTA) and differential scanning calorimetry (DSC) showed that most POSS-rich domains were amorphous. A small fraction of POSS crystals was also detected. A postcure cycle led to an increase in the glass transition temperature and the disappearance of crystallinity. A reference network was synthesized by replacing POSS by phenyl glycidyl ether (PGE) in equimolar amounts. The resulting network was homogeneous but exhibited a lower glass transition temperature than the POSS-modified network. As both networks had the same topology, the higher Tg observed for the POSS-modified epoxy may be associated with the hindering of polymer chain motions by their covalent bonding to POSS clusters. The most important concept arising from these results is that a phase separation process may take place when employing a POSS bearing organic groups that are not compatible with the epoxy network.
Fil: Abad, María J.. Universidad da Coruña; España
Fil: Barral, Luis. Universidad da Coruña; España
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Materia
Polyhedral Oligomeric Silsesquioxane
Epoxy Network
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/77012

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network_name_str CONICET Digital (CONICET)
spelling Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)Abad, María J.Barral, LuisFasce, Diana PatriciaWilliams, Roberto Juan JosePolyhedral Oligomeric SilsesquioxaneEpoxy Networkhttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1A polyhedral oligomeric silsesquioxane (POSS) containing one epoxy group and seven isobutyl groups per molecule was incorporated into an epoxy network following a two-stage process. In the first stage, POSS was reacted with an aromatic diamine, employing a 1:1 molar ratio of both reactants. The distribution of species at the end of reaction, determined by size exclusion chromatography (SEC), was close to the ideal one. In a second step, this precursor was reacted with the stoichiometric amount of an aromatic diepoxide to generate an organic-inorganic hybrid material containing 51.8 wt% POSS. A primary liquid-liquid phase separation process occurred at the time of adding the diepoxide to the POSS-diamine precursor. This led to a macrophase separation into epoxy-rich and POSS-rich regions, possibly derived from the incompatibility of the isobutyl groups attached to the POSS with the aromatic epoxy-amine network. A secondary phase separation occurred in the epoxy-rich phase in the course of polymerization, producing a dispersion of small POSS domains. Both modulated local thermal analysis (LTA) and differential scanning calorimetry (DSC) showed that most POSS-rich domains were amorphous. A small fraction of POSS crystals was also detected. A postcure cycle led to an increase in the glass transition temperature and the disappearance of crystallinity. A reference network was synthesized by replacing POSS by phenyl glycidyl ether (PGE) in equimolar amounts. The resulting network was homogeneous but exhibited a lower glass transition temperature than the POSS-modified network. As both networks had the same topology, the higher Tg observed for the POSS-modified epoxy may be associated with the hindering of polymer chain motions by their covalent bonding to POSS clusters. The most important concept arising from these results is that a phase separation process may take place when employing a POSS bearing organic groups that are not compatible with the epoxy network.Fil: Abad, María J.. Universidad da Coruña; EspañaFil: Barral, Luis. Universidad da Coruña; EspañaFil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaAmerican Chemical Society2003-05info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/77012Abad, María J.; Barral, Luis; Fasce, Diana Patricia; Williams, Roberto Juan Jose; Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS); American Chemical Society; Macromolecules; 36; 9; 5-2003; 3128-31350024-9297CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/doi/10.1021/ma021539finfo:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/10.1021/ma021539finfo:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-03T10:07:26Zoai:ri.conicet.gov.ar:11336/77012instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-03 10:07:26.714CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
title Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
spellingShingle Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
Abad, María J.
Polyhedral Oligomeric Silsesquioxane
Epoxy Network
title_short Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
title_full Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
title_fullStr Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
title_full_unstemmed Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
title_sort Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS)
dc.creator.none.fl_str_mv Abad, María J.
Barral, Luis
Fasce, Diana Patricia
Williams, Roberto Juan Jose
author Abad, María J.
author_facet Abad, María J.
Barral, Luis
Fasce, Diana Patricia
Williams, Roberto Juan Jose
author_role author
author2 Barral, Luis
Fasce, Diana Patricia
Williams, Roberto Juan Jose
author2_role author
author
author
dc.subject.none.fl_str_mv Polyhedral Oligomeric Silsesquioxane
Epoxy Network
topic Polyhedral Oligomeric Silsesquioxane
Epoxy Network
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv A polyhedral oligomeric silsesquioxane (POSS) containing one epoxy group and seven isobutyl groups per molecule was incorporated into an epoxy network following a two-stage process. In the first stage, POSS was reacted with an aromatic diamine, employing a 1:1 molar ratio of both reactants. The distribution of species at the end of reaction, determined by size exclusion chromatography (SEC), was close to the ideal one. In a second step, this precursor was reacted with the stoichiometric amount of an aromatic diepoxide to generate an organic-inorganic hybrid material containing 51.8 wt% POSS. A primary liquid-liquid phase separation process occurred at the time of adding the diepoxide to the POSS-diamine precursor. This led to a macrophase separation into epoxy-rich and POSS-rich regions, possibly derived from the incompatibility of the isobutyl groups attached to the POSS with the aromatic epoxy-amine network. A secondary phase separation occurred in the epoxy-rich phase in the course of polymerization, producing a dispersion of small POSS domains. Both modulated local thermal analysis (LTA) and differential scanning calorimetry (DSC) showed that most POSS-rich domains were amorphous. A small fraction of POSS crystals was also detected. A postcure cycle led to an increase in the glass transition temperature and the disappearance of crystallinity. A reference network was synthesized by replacing POSS by phenyl glycidyl ether (PGE) in equimolar amounts. The resulting network was homogeneous but exhibited a lower glass transition temperature than the POSS-modified network. As both networks had the same topology, the higher Tg observed for the POSS-modified epoxy may be associated with the hindering of polymer chain motions by their covalent bonding to POSS clusters. The most important concept arising from these results is that a phase separation process may take place when employing a POSS bearing organic groups that are not compatible with the epoxy network.
Fil: Abad, María J.. Universidad da Coruña; España
Fil: Barral, Luis. Universidad da Coruña; España
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
description A polyhedral oligomeric silsesquioxane (POSS) containing one epoxy group and seven isobutyl groups per molecule was incorporated into an epoxy network following a two-stage process. In the first stage, POSS was reacted with an aromatic diamine, employing a 1:1 molar ratio of both reactants. The distribution of species at the end of reaction, determined by size exclusion chromatography (SEC), was close to the ideal one. In a second step, this precursor was reacted with the stoichiometric amount of an aromatic diepoxide to generate an organic-inorganic hybrid material containing 51.8 wt% POSS. A primary liquid-liquid phase separation process occurred at the time of adding the diepoxide to the POSS-diamine precursor. This led to a macrophase separation into epoxy-rich and POSS-rich regions, possibly derived from the incompatibility of the isobutyl groups attached to the POSS with the aromatic epoxy-amine network. A secondary phase separation occurred in the epoxy-rich phase in the course of polymerization, producing a dispersion of small POSS domains. Both modulated local thermal analysis (LTA) and differential scanning calorimetry (DSC) showed that most POSS-rich domains were amorphous. A small fraction of POSS crystals was also detected. A postcure cycle led to an increase in the glass transition temperature and the disappearance of crystallinity. A reference network was synthesized by replacing POSS by phenyl glycidyl ether (PGE) in equimolar amounts. The resulting network was homogeneous but exhibited a lower glass transition temperature than the POSS-modified network. As both networks had the same topology, the higher Tg observed for the POSS-modified epoxy may be associated with the hindering of polymer chain motions by their covalent bonding to POSS clusters. The most important concept arising from these results is that a phase separation process may take place when employing a POSS bearing organic groups that are not compatible with the epoxy network.
publishDate 2003
dc.date.none.fl_str_mv 2003-05
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/77012
Abad, María J.; Barral, Luis; Fasce, Diana Patricia; Williams, Roberto Juan Jose; Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS); American Chemical Society; Macromolecules; 36; 9; 5-2003; 3128-3135
0024-9297
CONICET Digital
CONICET
url http://hdl.handle.net/11336/77012
identifier_str_mv Abad, María J.; Barral, Luis; Fasce, Diana Patricia; Williams, Roberto Juan Jose; Epoxy networks containing large mass fractions of a monofunctional Polyhedral Oligomeric Silsesquioxane (POSS); American Chemical Society; Macromolecules; 36; 9; 5-2003; 3128-3135
0024-9297
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/doi/10.1021/ma021539f
info:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/10.1021/ma021539f
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv American Chemical Society
publisher.none.fl_str_mv American Chemical Society
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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