矽氧烷改質有機無機複合式高分子電解質之結構鑑定與動力學研究

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陳育修(Yu-hsiu Chen) 查詢紙本館藏

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論文名稱

矽氧烷改質有機無機複合式高分子電解質之結構鑑定與動力學研究
(Structural characterization and dynamic properties of organic-inorganic hybrid electrolytes based on alkoxysilane modification)

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摘要(中)

本研究著重於製備與鑑定有機/無機複合式高分子電解質根據poly(propylene glycol)-block-poly(ethylene glycol)-block-poly(propylene glycol) bis(2-aminopropyl ether) (ED600、ED900、ED2000) 和過氯酸鋰共混合經由 TEOS 和 3-(Triethoxysilyl)propyl isocyanate 共水解。乾燥的有機/無機複合式高分子電解質經過以重量比 1:1 的 EC/PC 電解液混合液，然後獲得塑化。離子導電度經由塑化後上升2個級數，達到室溫最高導電度 2.11×10-3 S/cm。由 DSC、TGA、FT-IR、SEM、XRD、AC-Impedance 和 Solid State NMR光譜用來鑑定複合式高分子電解質結構和動力學特性和離子遷移率。根據熱差式掃描卡計儀結果，玻璃轉化溫度隨著鋰鹽的增加而上升。用 2D 1H-13C WISE (WIdeline SEparation) NMR 技術，複合式高分子電解質系統的動力學能夠被定量的確定由測量在 F1 dimension 上的 1H 的譜寬和在 F2 dimension 上結構相關連的碳譜，而且，乾式複合式高分子電解質的 7Li 擴散係數由 Pulse Gradient Spin- Echo 和離子導電度相關。

摘要(英)

This research focus on the preparation and characterization of organic–inorganic hybrid electrolytes based on poly(propylene glycol)-block-poly(ethylene glycol)-block-poly(propylene glycol) bis(2-aminopropyl ether) (ED600、ED900、ED2000) complexed with LiClO4 via the co-condensation of tetraethoxysilane (TEOS) and 3-(triethoxysilyl)propyl isocyanate. The dry organic–inorganic hybrid electrolytes thus obtained were also plasticized by a solution of ethylene carbonate (EC)/propylene carbonate (PC) mixture (1:1 by volume). The ionic conductivity of the dry hybrid electrolyte films was enhanced by two orders of magnitude via plasticization, reaching a maximum conductivity value of 2.11×10-3 S/cm of the polymer molecule weight 2000 at 30℃. A variety of techniques such as DSC、TGA、FT-IR、SEM、XRD、AC Impedance and solid state NMR spectroscopy are performed to elucidate the realtionship between the structural and dynamic properties of the hybrid electrolyte and the ion mobility. According to DSC results, the glass transition temperature (Tg) raised with increasing the lithium salt content. By means of 2D 1H-13C WISE (WIdeline SEparation) NMR, the dynamic information within such a hybrid system can be qualitatively assessed by examining the proton line shapes in the F1 dimension that are directly related to structural elements resolved in the 13C CP/MAS NMR spectrum in the F2 dimension. Furthermore, the 7Li diffusion coefficients of the dry hybrid electrolytes were determined by pulsed gradient spin-echo (PGSE) experiment to correlate with the behavior of the ion conductivity.

關鍵字(中)

★ 玻璃轉換溫度
★ 擴散係數
★ 離子導電度
★ 有機/無機複合式高分子電解質

關鍵字(英)

★ Organic-inorganic hybrid electrolytes
★ ion conductivity
★ glass transition temperature
★ self-diffusion coefficients

論文目次

中文摘要……………………………………………………………………………………….I
英文摘要………………………………………………………………………………………II
謝誌……………………………………………………………………………………….. …IV
目錄…………………………………………………………………………………………....V
圗目錄………………………………………………………………………………………VIII
表目錄………………………………………………………………………………………....X
第壹章緒論…………………………………………………………………………………..1
1-1. 前言…………………………………………………………………………………...1
1-2 鋰電池與鋰二次電池簡介…………………………………………………………..2
1-3. 高分子電解質簡介…………………………………………………………………...6
1-4. 固態高分子電解質…………………………………………………………………...6
1-4-1. 交聯高分子電解質………………………………………………………………7
1-4-2. 共聚高分子電解質………………………………………………………………8
1-4-3. 接枝高分子電解質………………………………………………………………9
1-4-4. 混摻高分子電解質………………………………………………………………9
1-4-5. 複合高分子電解質………………………………………………………………9
1-4-6. 單離子高分子電解質…………………………………………………………..10
1-4-7. Polymer-in-Salt Polymer Electrolyte……………………………………………11
1-4-8. Ormolytes / Ormocer……………………………….……………………………11
1-5. 膠態高分子電解質………………………………………………………………….12
1-6. 微孔型高分子電解質……………………………………………………………….13
1-7. 溫度效應對高分子電解質導電度的影響………………………………………….16
1-8. 研究動機與目的…………………………………………………………………….17
第貳章文獻回顧…………………………………………………………………………....19
2-1. 高分子電解質之發展……………………………………………………………….19
2-2. 奈米複合高分子電解質發展……………………………………………………….22
2-3. 聚氨基甲酸酯……………………………………………………………………….23
2-4. 聚氨基甲酸酯熱性質……………………………………………………………….27
第參章實驗部分與原理……………………………………………………………………28
3-1. 實驗藥品…………………………………………………………………………….28
3-2. 儀器設備…………………………………………………………………………….29
3-3. 高分子電解質薄膜之製備………………………………………………………….30
3-3-1. 固態高分子電解質薄膜之製備………………………………………………..30
3-3-2. 膠態高分子電解質膜之製備…………………………………………………..32
3-4. 儀器分析原理及操作條件………………………………………………………….33
3-4-1. 微差掃瞄熱卡計 (DSC)…....………………………………………………….33
3-4-1-1. 原理…………………………………………………..................................33
3-4-1-2. 樣品製備……………………………………………..................................34
3-4-2. 熱重量分析儀 (TGA)………..………….....……………..................................35
3-4-2-1. 原理…………………………………………………..................................35
3-4-2-2. 樣品製備……………………………………………..................................35
3-4-3. 傅立葉紅外線吸收光譜儀 (FT-IR) ……………………..................................35
3-4-3-1. 原理………………………………………………………………………..35
3-4-3-2. FT-IR之操作程序………………………………………….........................38
3-4-4. 掃瞄式電子顯微鏡 (SEM)....…………………………………………………39
3-4-2-1. 原理…………………………………………………...................................39
3-4-2-2. 樣品製備……………………………………………...................................40
3-4-5. X光繞射儀 (XRD)……………………………………………………………..40
3-4-5-1. 原理…………………………………………………..................................40
3-4-5-2. 樣品製備…………...……………………………………………………...41
3-4-6. 交流阻抗儀 (AC-Impedance)...………………………………………………41
3-4-6-1. 原理…………………………………………………...................................41
3-4-6-2. 操作程序……………………………………………...................................45
3-4-7. 液態核磁共振光譜儀 (Solution NMR)………………………………………..45
3-4-7-1. 原理…………………………………………………..................................45
3-4-7-2. 樣品製備……………………………………………..................................46
3-4-8. 固態核磁共振光譜儀 (Solid State NMR)……………………………………..46
3-4-8-1. 原理簡介……………………………………………...................................46
3-4-8-2. 常用固態核磁共振技術……………………………...................................57
3-4-8-3. 樣品製備……………………………………………...................................62
第肆章結果與討論………………………………………………………………………..63
4-1. 固態高分子電解質………………………………………………………………….63
4-1-1. 微差式掃瞄熱卡計儀 (DSC) 圖譜分析X-ray 粉末繞射圖譜分析…………64
4-1-2. 熱重量分析 (TGA)…………………………………………………………….69
4-1-3. 紅外吸收光譜之鑑定 (FT-IR)…..……………………………………………..73
4-1-4. 掃瞄式電子顯微鏡 (SEM) 電解質薄膜表面分析…………………………...83
4-1-5. X-ray 粉末繞射 (Power X-ray Diffraction) 分析.….…………………………90
4-1-6. 固態高分子電解質之導電度量測……………………………………………..92
4-1-7. 液態核磁共振光譜分析………………………………………………………..99
4-1-8. 固態核磁共振光譜分析………………………………………………………102
4-1-8-1. 13C CP / MAS NMR……………………………………………………….……………….102
4-1-8-2. 2D 1H - 13C WISE (WIdeline SEparation) NMR………………………..110
4-1-8-3. 29Si CP / MAS……….….……………………………………………….113
4-1-8-4. 29Si MAS NMR……………………….…………………………………114
4-1-8-5. 7Li譜寬分析……….………………………………................................119
4-1-8-6. 7Li-{1H} MAS NMR….………..…………………................................126
4-1-8-7. 7Li 擴散常數 (Diffusion Constant) 測量…..……................................131
第伍章結論………………………………………………………………………………138
參考文獻……………………………………………………………………………………140

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指導教授

高憲明(Hsien-ming Kao)

審核日期

2007-7-23

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