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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...
Autores principales: | , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
MDPI
2019
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6473492/ https://www.ncbi.nlm.nih.gov/pubmed/30960390 http://dx.doi.org/10.3390/polym11030406 |
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author | Miguel, Álvaro González, Francisco Gregorio, Víctor García, Nuria Tiemblo, Pilar |
author_facet | Miguel, Álvaro González, Francisco Gregorio, Víctor García, Nuria Tiemblo, Pilar |
author_sort | Miguel, Álvaro |
collection | PubMed |
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. |
format | Online Article Text |
id | pubmed-6473492 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2019 |
publisher | MDPI |
record_format | MEDLINE/PubMed |
spelling | pubmed-64734922019-05-03 Solvent-Free Procedure for the Preparation under Controlled Atmosphere Conditions of Phase-Segregated Thermoplastic Polymer Electrolytes Miguel, Álvaro González, Francisco Gregorio, Víctor García, Nuria Tiemblo, Pilar Polymers (Basel) Article 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. MDPI 2019-03-01 /pmc/articles/PMC6473492/ /pubmed/30960390 http://dx.doi.org/10.3390/polym11030406 Text en © 2019 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Article Miguel, Álvaro González, Francisco Gregorio, Víctor García, Nuria Tiemblo, Pilar 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 |
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_short | 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 |
topic | Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6473492/ https://www.ncbi.nlm.nih.gov/pubmed/30960390 http://dx.doi.org/10.3390/polym11030406 |
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