本研究係以四乙氧基矽烷(TEOS)和甲基三乙氧基矽烷(MTES)作為二氧化矽的前驅物與離子熔液[BMIM-ClO4],並添加過氯酸鋰作為鋰離子的來源和甲酸做為催化劑,以溶膠-凝膠法(sol-gel method)合成出一系列的二氧化矽離子凝膠電解質。將所自製的離子熔液[BMIM-ClO4]以FT-IR與NMR作鑑定和線性掃描伏安法LSV測定其電化學視窗。而所製備之二氧化矽離子凝膠電解質藉由FT-IR、DSC、接觸角、29Si-solid state NMR與BET的量測探討其特性,再以導電度、電化學阻抗EIS、線性掃描伏安法LSV以及充放電測試進行電化學性質量測。由FT-IR 光譜與29Si-solid state NMR圖譜證實 TEOS與MTES成功經由水解縮合形成二氧化矽的骨架。而從DSC 結果證實二氧化矽骨架與離子熔液之間有相互作用力。導電度結果顯示,其最高的離子導電度(1.65×10-3S/cm)幾乎與離子熔液(2.41×10-3)相同。最後充放電測試結果顯示,在0.2充放電速率與55℃下,首圈之放電電容量最高可達108.7 mAh/g。
A series of silica ionogel electrolyte (SIE) were prepared by sol-gel method with tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) as silica precursor and ionic liquid (1-butyl-3-methylimidazolium perchlorate [BMIM][ClO4]). In the process, lithium perchlorate was used as the lithium source and formic acid as the catalyst. The ionic liquid was synthesized and identified by Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance (NMR) and linear sweep voltammetry (LSV) was measured for its electrochemical window. The SIEs were characterized with FT-IR, DSC, contact angle,29Si-Solid state NMR and Brunauer-Emmett-Teller (BET).The electrochemical properties of the SIEs prepared were studied by the measurements of ionic conductivity, electrochemical impendence spectroscopy (EIS) and linear sweep voltammetry (LSV) and charge-discharge performance as well. The results of FT-IR and NMR spectra indicated that the silica networks were formed by the reaction of TEOS and MTES. The DSC result confirmed the interaction between silica network and ionic liquid. The best ionic conductivities (1.65×10-3 S/cm)of the silica ionogel electrolytes prepared were close to the order of that of the ionic liquid(2.41×10-3 S/cm).The best first-cycle discharge capacity of the SIE-based half-cells (Li/LiFePO4) fabricated at 0.2Crate and 55℃was 108.7 mAhg-1. The result of his study indicated that the SIE can be potential gel electrolytes for lithium ion battery.
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