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聚偏氟乙烯/ N-甲基吡咯烷酮/[1-乙基-3-甲基咪唑][双(三氟甲基磺酰)亚胺]固体聚合物电解质的表面分析

Surface Analyses of PVDF/NMP/[EMIM][TFSI] Solid Polymer Electrolyte.

作者信息

Sedlak Petr, Sobola Dinara, Gajdos Adam, Dallaev Rashid, Nebojsa Alois, Kubersky Petr

机构信息

Faculty of Electrical Engineering and Communications, Brno University of Technology, Technicka 10, 616 00 Brno, Czech Republic.

Institute of Physics of Materials, Academy of Sciences CR, Zizkova 22, 616 62 Brno, Czech Republic.

出版信息

Polymers (Basel). 2021 Aug 11;13(16):2678. doi: 10.3390/polym13162678.

DOI:10.3390/polym13162678
PMID:34451218
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8401855/
Abstract

Thermal treatment conditions of solid polymer polymer electrolyte (SPE) were studied with respect to their impact on the surface morphology, phase composition and chemical composition of an imidazolium ionic-liquid-based SPE, namely PVDF/NMP/[EMIM][TFSI] electrolyte. These investigations were done using scanning electron microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy, differential scanning calorimetry as well as X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectroscopy. A thoroughly mixed blend of polymer matrix, ionic liquid and solvent was deposited on a ceramic substrate and was kept at a certain temperature for a specific time in order to achieve varying crystallinity. The morphology of all the electrolytes consists of spherulites whose average diameter increases with solvent evaporation rate. Raman mapping shows that these spherulites have a semicrystalline structure and the area between them is an amorphous region. Analysis of FTIR spectra as well as Raman spectroscopy showed that the β-phase becomes dominant over other phases, while DSC technique indicated decrease of crystallinity as the solvent evaporation rate increases. XPS and ToF-SIMS indicated that the chemical composition of the surface of the SPE samples with the highest solvent evaporation rate approaches the composition of the ionic liquid.

摘要

针对固态聚合物聚合物电解质(SPE)的热处理条件对基于咪唑鎓离子液体的SPE(即聚偏氟乙烯/ N - 甲基吡咯烷酮/ [EMIM][TFSI]电解质)的表面形态、相组成和化学成分的影响进行了研究。这些研究通过扫描电子显微镜、拉曼光谱、傅里叶变换红外光谱、差示扫描量热法以及X射线光电子能谱和飞行时间二次离子质谱来进行。将聚合物基体、离子液体和溶剂充分混合的共混物沉积在陶瓷基板上,并在特定温度下保持特定时间,以实现不同的结晶度。所有电解质的形态均由球晶组成,其平均直径随溶剂蒸发速率增加。拉曼映射表明这些球晶具有半结晶结构,它们之间的区域为非晶区。傅里叶变换红外光谱以及拉曼光谱分析表明,β相相对于其他相占主导地位,而差示扫描量热法技术表明随着溶剂蒸发速率增加结晶度降低。X射线光电子能谱和飞行时间二次离子质谱表明,溶剂蒸发速率最高的SPE样品表面的化学成分接近离子液体的成分。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/b3ad903bee65/polymers-13-02678-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/bd3c88a28ed2/polymers-13-02678-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/0968776548eb/polymers-13-02678-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/3f235eac69db/polymers-13-02678-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/e8b8a388b655/polymers-13-02678-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/d923fb7b734b/polymers-13-02678-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/26db7906b3a8/polymers-13-02678-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/b3ad903bee65/polymers-13-02678-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/bd3c88a28ed2/polymers-13-02678-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/0968776548eb/polymers-13-02678-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/3f235eac69db/polymers-13-02678-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/e8b8a388b655/polymers-13-02678-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/d923fb7b734b/polymers-13-02678-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/26db7906b3a8/polymers-13-02678-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d839/8401855/b3ad903bee65/polymers-13-02678-g007.jpg

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