Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes

A solvent-free method that allows thermoplastic solid electrolytes based on poly(ethylene oxide) PEO to be obtained under controlled atmosphere conditions is presented. This method comprises two steps, the first one being the melt compounding of PEO with a filler, able to physically crosslink the po...

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Autores: Miguel, Álvaro, González González, Francisco José, Gregorio, Víctor, García, Nuria, Tiemblo, Pilar
Tipo de recurso: artículo
Estado:Versión publicada
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:10261/178946
Acceso en línea:http://hdl.handle.net/10261/178946
Access Level:acceso abierto
Palabra clave:Polymer electrolytes
Thermoplastic electrolytes
Solid electrolytes
Ionic liquids
Energy storage
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spelling Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer ElectrolytesMiguel, ÁlvaroGonzález González, Francisco JoséGregorio, VíctorGarcía, NuriaTiemblo, PilarPolymer electrolytesThermoplastic electrolytesSolid electrolytesIonic liquidsEnergy storageA solvent-free method that allows thermoplastic solid electrolytes based on poly(ethylene oxide) PEO to be obtained under controlled atmosphere conditions is presented. This method comprises two steps, the first one being the melt compounding of PEO with a filler, able to physically crosslink the polymer and its pelletizing, and the second the pellets’ swelling with an electroactive liquid phase. This method is an adaptation of the step described in previous publications of the preparation of thermoplastic electrolytes by a single melt compounding. In comparison to the single step extrusion methodology, this new method permits employing electroactive species that are very sensitive to atmospheric conditions. The two-step method can also be designed to produce controlled phase-segregated morphologies in the electrolyte, namely polymer-poor and polymer-rich phases, with the aim of increasing ionic conductivity over that of homogeneous electrolytes. An evaluation of the characteristics of the electrolytes prepared by single and two-step procedures is done by comparing membranes prepared by both methods using PEO as a polymeric scaffold and a solution of the room-temperature ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl) imide (EMI TFSI) and the bis(trifluoromethanesulfonyl) imide lithium salt (Li TFSI) as liquid phase. The electrolytes prepared by both methods have been characterized by Fourier transform infrared spectroscopy and optic microscopy profilometry, differential scanning calorimetry, self-creep experiments, and dielectric spectroscopy. In this way, the phase separation, rheology, and ionic conductivity are studied and compared. It is striking how the electrolytes prepared with this new method maintain their solid-like behavior even at 90 °C. Compared to the single step method, the two-step method produces electrolytes with a phase-separated morphology, which results in higher ionic conductivity.This research was funded by H2020-FETOPEN-1-2016-2017 project SALBAGE, Grant Agreement nº766581. F.G. is grateful to CONACYT-SENER for the scholarship granted (CVU 559770/Registro 297710 and S2013/MAE-2800)We acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI)Peer reviewedMultidisciplinary Digital Publishing InstituteConsejo Superior de Investigaciones Científicas (España)European CommissionConsejo Nacional de Ciencia y Tecnología (México)Secretaría de Energía (México)Comunidad de MadridConsejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]2019201920192019info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/178946reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/EC/H2020/766581S2013/MAE-2800/LIQUORGAShttp://dx.doi.org/10.3390/polym11030406Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/1789462026-05-22T06:33:51Z
dc.title.none.fl_str_mv Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
title Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
spellingShingle Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
Miguel, Álvaro
Polymer electrolytes
Thermoplastic electrolytes
Solid electrolytes
Ionic liquids
Energy storage
title_short Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
title_full Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
title_fullStr Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
title_full_unstemmed Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
title_sort Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes
dc.creator.none.fl_str_mv Miguel, Álvaro
González González, Francisco José
Gregorio, Víctor
García, Nuria
Tiemblo, Pilar
author Miguel, Álvaro
author_facet Miguel, Álvaro
González González, Francisco José
Gregorio, Víctor
García, Nuria
Tiemblo, Pilar
author_role author
author2 González González, Francisco José
Gregorio, Víctor
García, Nuria
Tiemblo, Pilar
author2_role author
author
author
author
dc.contributor.none.fl_str_mv Consejo Superior de Investigaciones Científicas (España)
European Commission
Consejo Nacional de Ciencia y Tecnología (México)
Secretaría de Energía (México)
Comunidad de Madrid
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Polymer electrolytes
Thermoplastic electrolytes
Solid electrolytes
Ionic liquids
Energy storage
topic Polymer electrolytes
Thermoplastic electrolytes
Solid electrolytes
Ionic liquids
Energy storage
description A solvent-free method that allows thermoplastic solid electrolytes based on poly(ethylene oxide) PEO to be obtained under controlled atmosphere conditions is presented. This method comprises two steps, the first one being the melt compounding of PEO with a filler, able to physically crosslink the polymer and its pelletizing, and the second the pellets’ swelling with an electroactive liquid phase. This method is an adaptation of the step described in previous publications of the preparation of thermoplastic electrolytes by a single melt compounding. In comparison to the single step extrusion methodology, this new method permits employing electroactive species that are very sensitive to atmospheric conditions. The two-step method can also be designed to produce controlled phase-segregated morphologies in the electrolyte, namely polymer-poor and polymer-rich phases, with the aim of increasing ionic conductivity over that of homogeneous electrolytes. An evaluation of the characteristics of the electrolytes prepared by single and two-step procedures is done by comparing membranes prepared by both methods using PEO as a polymeric scaffold and a solution of the room-temperature ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl) imide (EMI TFSI) and the bis(trifluoromethanesulfonyl) imide lithium salt (Li TFSI) as liquid phase. The electrolytes prepared by both methods have been characterized by Fourier transform infrared spectroscopy and optic microscopy profilometry, differential scanning calorimetry, self-creep experiments, and dielectric spectroscopy. In this way, the phase separation, rheology, and ionic conductivity are studied and compared. It is striking how the electrolytes prepared with this new method maintain their solid-like behavior even at 90 °C. Compared to the single step method, the two-step method produces electrolytes with a phase-separated morphology, which results in higher ionic conductivity.
publishDate 2019
dc.date.none.fl_str_mv 2019
2019
2019
2019
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/10261/178946
url http://hdl.handle.net/10261/178946
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
#PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/EC/H2020/766581
S2013/MAE-2800/LIQUORGAS
http://dx.doi.org/10.3390/polym11030406
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Multidisciplinary Digital Publishing Institute
publisher.none.fl_str_mv Multidisciplinary Digital Publishing Institute
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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