Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization

Composites based on an L-rich poly(lactic acid), PLA, and different contents in mesoporous SBA-15 silica have been prepared by extrusion in order to evaluate the influence of incorporation of mesoporous particles on the structural PLA features and on their ultimate mechanical performance. For that,...

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Autores: Díez-Rodríguez, Tamara M., Blázquez-Blázquez, Enrique, Martínez, Juan C., Pérez, Ernesto, Cerrada, María L.
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2022
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/267163
Acceso en línea:http://hdl.handle.net/10261/267163
Access Level:acceso abierto
Palabra clave:PLA
SBA-15 composites
α′ and α forms
Cold crystallization
Microhardness
Long spacing
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spelling Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallizationDíez-Rodríguez, Tamara M.Blázquez-Blázquez, EnriqueMartínez, Juan C.Pérez, ErnestoCerrada, María L.PLASBA-15 compositesα′ and α formsCold crystallizationMicrohardnessLong spacingComposites based on an L-rich poly(lactic acid), PLA, and different contents in mesoporous SBA-15 silica have been prepared by extrusion in order to evaluate the influence of incorporation of mesoporous particles on the structural PLA features and on their ultimate mechanical performance. For that, the samples have been isothermally cold crystallized for relatively long times at different temperatures, ranging from 65 to 120 °C. The results from DSC, X-ray diffraction and Raman spectroscopy show that the pure α′ modification is obtained at the lower annealing temperatures, while the α form is in majority above 85 °C. The temperature range at which α′ and α polymorphs were developed is somewhat atypical, being associated with the particular D stereoisomer content of the PLA used. Furthermore, several phase transitions are observed depending on the crystallinity reached and the polymorphs developed during the isothermal crystallization from the glass: an additional cold crystallization, the α′/α transformation and the subsequent melting processes. These transitions have been evaluated thoroughly by DSC measurements and real-time variable temperature experiments with synchrotron radiation. It was also found that rigidity of these materials is influenced by both the presence of SBA-15 particles and by the amount and perfection of crystallites. Thus, the relative reinforcement effect of SBA-15 particles is importantly reduced by differences in long spacing PLA values for the materials crystallized between 85 and 120 °C, mainly in the composites with the lowest SBA-15 content. Those are the temperatures where the α polymorph is the major existing crystalline structure.This research was funded by AEI, Spain/FEDER, EU (grant numbers MAT2016-79869-C2-1-P and PID2020-114930GB-I00), by CSIC, Spain (grant number 2020AEP129) and by ALBA Synchrotron Light Facility, Spain. TMDR is also grateful for her pre-doctoral funding (contract number BES-2017-082284). The FESEM, Raman and TGA measure- ments were carried out in the Characterization Service at ICTP-CSIC and authors are grateful for the help and advices received. The synchrotron experiments were performed in the beamline BL11-NCD-SWEET at ALBA Synchrotron Light Facility and authors would like to thank the collaboration and help of ALBA stafElsevierEuropean CommissionMinisterio de Ciencia e Innovación (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]2022202220222022info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/267163reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2020-114930GB-I00http://dx.doi.org/10.1016/j.polymer.2022.124515Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/2671632026-05-22T06:33:51Z
dc.title.none.fl_str_mv Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
title Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
spellingShingle Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
Díez-Rodríguez, Tamara M.
PLA
SBA-15 composites
α′ and α forms
Cold crystallization
Microhardness
Long spacing
title_short Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
title_full Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
title_fullStr Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
title_full_unstemmed Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
title_sort Composites of a PLA with SBA-15 mesoporous silica: Polymorphism and properties after isothermal cold crystallization
dc.creator.none.fl_str_mv Díez-Rodríguez, Tamara M.
Blázquez-Blázquez, Enrique
Martínez, Juan C.
Pérez, Ernesto
Cerrada, María L.
author Díez-Rodríguez, Tamara M.
author_facet Díez-Rodríguez, Tamara M.
Blázquez-Blázquez, Enrique
Martínez, Juan C.
Pérez, Ernesto
Cerrada, María L.
author_role author
author2 Blázquez-Blázquez, Enrique
Martínez, Juan C.
Pérez, Ernesto
Cerrada, María L.
author2_role author
author
author
author
dc.contributor.none.fl_str_mv European Commission
Ministerio de Ciencia e Innovación (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv PLA
SBA-15 composites
α′ and α forms
Cold crystallization
Microhardness
Long spacing
topic PLA
SBA-15 composites
α′ and α forms
Cold crystallization
Microhardness
Long spacing
description Composites based on an L-rich poly(lactic acid), PLA, and different contents in mesoporous SBA-15 silica have been prepared by extrusion in order to evaluate the influence of incorporation of mesoporous particles on the structural PLA features and on their ultimate mechanical performance. For that, the samples have been isothermally cold crystallized for relatively long times at different temperatures, ranging from 65 to 120 °C. The results from DSC, X-ray diffraction and Raman spectroscopy show that the pure α′ modification is obtained at the lower annealing temperatures, while the α form is in majority above 85 °C. The temperature range at which α′ and α polymorphs were developed is somewhat atypical, being associated with the particular D stereoisomer content of the PLA used. Furthermore, several phase transitions are observed depending on the crystallinity reached and the polymorphs developed during the isothermal crystallization from the glass: an additional cold crystallization, the α′/α transformation and the subsequent melting processes. These transitions have been evaluated thoroughly by DSC measurements and real-time variable temperature experiments with synchrotron radiation. It was also found that rigidity of these materials is influenced by both the presence of SBA-15 particles and by the amount and perfection of crystallites. Thus, the relative reinforcement effect of SBA-15 particles is importantly reduced by differences in long spacing PLA values for the materials crystallized between 85 and 120 °C, mainly in the composites with the lowest SBA-15 content. Those are the temperatures where the α polymorph is the major existing crystalline structure.
publishDate 2022
dc.date.none.fl_str_mv 2022
2022
2022
2022
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/267163
url http://hdl.handle.net/10261/267163
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/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2020-114930GB-I00
http://dx.doi.org/10.1016/j.polymer.2022.124515
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
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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