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
- Institución
- Consejo Nacional de Investigaciones Científicas y Técnicas
- OAI Identificador
- oai:ri.conicet.gov.ar:11336/77012
Ver los metadatos del registro completo
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CONICET Digital (CONICET) |
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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 |
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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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score |
13.13397 |