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研究生： 潘育麒
Yu-chi Pan
論文名稱： 固態有機無機星狀高分子電解質之結構與動力學研究
Structural characterization and dynamic properties of star-like organic-inorganic hybrid electrolytes
指導教授： 高憲明
Hsien-ming Kao
口試委員:
學位類別： 碩士
Master
系所名稱： 理學院 - 化學學系
Department of Chemistry
畢業學年度： 96
語文別： 中文
論文頁數： 116
中文關鍵詞： 高分子電解質 、固態核磁共振
外文關鍵詞： solid state polymer electrolyte, sold state NMR
相關次數： 點閱：6  下載：0 
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    • 此篇論文主要是利用 jeffamine-ED serious 與三聚氯氰反應形成具有星狀結構之高分子，進一步藉由添加3-Glycidyloxypropyl trimeth- oxysilane (GLYMO) 使其固化，觀察在不同 Lithium perchloride (LiClO4) 濃度下對導電行為的影響。
    此篇論文的是藉由X光繞射儀 (XRD) 、微差掃描卡計 (DSC) 、紅外吸收光譜儀 (FTIR) 、交流阻抗分析儀 (AC-Impedance) 以及固態核磁共振光譜儀 (Solid State NMR) 等儀器對具有星狀結構之的固態高分子電解質加以分析研究。藉由交流阻抗分析儀的分析結果，發現於乾式固態高分子電解質中，其導電度隨高分子鏈段運動性增加而上升。在30 ?C 時的最佳導電度可達4.36 × 10-5 S/cm。

    A sol-gel synthetic route for preparing poly(oxyalkylene) block copolymers has been developed by using 2,4,6-trichloro-1,3,5-triazine (cyanuric chloride, cc) as the coupling core. The coupling reaction involves the selective substitutions of oligo(oxyalkylene)-amines at 0?C, 25?C and 130?C. Afterwards, (3-glycidyloxypropyl)-trimethoxysilane (GLYMO) reacts with the NH2 end groups of oligo(oxyalkylene)amines (Jeffamine-ED serious), and then the Si-OCH3 will condensation with other GLYMO.
    The effects of several variables on ionic conductivity were investigated, such as length of PEO chain, percentage of EO/PO segment, extent of cross-linking, and salt concentration (LiClO4). Characterization was made by solid-state NMR, Differential scanning calorimetry (DSC), AC-Impedance and IR spectroscopy. The optimal lithium conductivity for the copolymer electrolytes thus obtained reaches 4.3 x 10-5 S/cm at 30?C.

    第壹章 緒論……………………………………………………………..1 1-1. 簡介………………………………………………………………1 1-2. 文獻回顧…………………………………………………………2 1-2-1. 鋰電池的發展..……………………………………………..2 1-2-2. 高分子電解質……………..………………………………..6 1-2-3. 固態高分子電解質 (Solid Polymer Electrolytes)……….....7 1-2-4. 膠態 (gelled-type) 高分子電解質…………………………9 1-2-5. 含有三氮環之高分子……………………………………..11 1-2-6. 有機矽高分子……………………………………………..12 第貳章 研究方向………………………………………………………13 2-1. 研究目的………………………………………………………..13 2-2. 研究架構………………………………….…………………….14 第叁章 實驗部分與原理………………………………………………15 3-1. 實驗藥品………………………………………………………..15 3-2. 儀器設備………………………………………………………..16 3-3. 高分子電解質膜之製備………………………………………..16 3-4. 儀器分析原理…………………………………………………..19 3-4-1. X光繞射儀…………………………………...………….....19 3-4-2. 熱重量分析儀………………………………………...…...21 3-4-3. 微差掃瞄熱卡計……………………………………...…...21 3-4-4. 傅立葉紅外線吸收光譜儀………………………………..23 3-4-5. 掃描式電子顯微鏡………………………………………..24 3-4-6. 交流阻抗分析儀…………………………………………..23 3-4-7. 固態核磁共振光譜儀……………………………………..30 3-4-7-1. 原理簡介……………………………………………...30 3-4-7-2. 常用固態核磁共振技術……………………………...35 第肆章 結果與討論…………………………………………………..46 4-1. 固態星狀高分子電解質…………………………………………..46 4-2. 熱重量分析 (Thermal Gravimetric Analysis)...………...…..…...47 4-3. X-ray 粉末繞射 (Powder X-ray Diffraction) 圖譜分析…..…...49 4-4. 微差掃瞄熱卡計 ( Differential Scanning Calorimeter) 分析.…...51 4-5. 紅外吸收光譜之鑑定……………………………………………..56 4-6. 固態電解質膜之表面分析………………………………………..63 4-7. 固態高分子電解質之導電度量測………………………………..65 4-8. 固態核磁共振光譜分析….………………..……………………...77 4-8-1. 13C MASNMR………………………..…………...…..........78 4-8-2. 13C CP/MASNMR……………………………..……….…..81 4-8-3. 29Si MASNMR …............…………………...….………..…88 4-8-4. 1H/13C 2D WISE NMR..........................................................90 4-8-5. 7Li 譜寬分析………………………………………….……93 4-8-6. 7Li-{1H} MAS NMR………...............................................101 4-8-7. 7Li 擴散常數之量測……………………………………...105 第伍章 結 論…………………………………………………………109 參考文獻………………………………………………………………111

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