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Student Number 942203058
Author Feng-shien Wu(吳豐賢)
Author's Email Address No Public.
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Department Chemistry
Year 2006
Semester 2
Degree Master
Type of Document Master's Thesis
Language zh-TW.Big5 Chinese
Title 具有星狀有機無機高分子電解質之結構與動力學研究
Date of Defense 2007-07-12
Page Count 134
Keyword
  • cyanuric chloride
  • electrolyte
  • GLYMO
  • Abstract 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 onto the first two chlorides of the triazine ring in a stepwise manner at 0 and 25 oC, and then (3-aminopropyl)trimethoxysilane (APTMS) cross-linking to the third chloride site at 130 oC. Afterwards, (3-glycidyloxypropyl)
    -trimethoxysilane (GLYMO) react with the NH2 end groups of 
    oligo(oxyalkylene)amines (Jeffamine-ED serious) and co-condensation with APTMS to form an organic-inorganic hybrid electrolyte system.
    The effects of several variables on conductivity were investigated, such as length of PEO chain, percentage of EO/PO segments, extent of cross-linking, and salt concentration (LiClO4). A full characterization was made by Solution NMR, X-ray Diffraction Spectrometer (XRD), Thermo Gravimetric Analyzer (TGA), differential scanning calorimetry (DSC), ionic conductivity, IR spectroscopy, and multinuclear solid-state NMR spectroscopy. The optimal lithium ionic conductivity for the hyperbranched copolymer electrolytes thus obtained reaches 6.80 x 10-5 S/cm at 30 °C with the composition of cc: ED2000: GLYMO = 1:3:3.
    Table of Content 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……………..………………………………..2
    1-2-3. 固態高分子電解質 (Solid Polymer Electrolytes)………....3
    1-2-4. 膠態 (gelled-type) 高分子電解質…………………………5
    1-2-5. 含有三氮環之高分子………………………………………7
    1-2-6. 有機矽高分子………………………………………………9
    第貳章 研究方向………………………………………………………10
    2-1. 研究目的………………………………………………………..10
    2-2. 研究架構………………………………….…………………….10
    第叁章 實驗部分與原理………………………………………………12
    3-1. 實驗藥品………………………………………………………..12
    3-2. 儀器設備………………………………………………………..13
    3-3. 高分子電解質膜之製備………………………………………..13
    3-3-1. 含有 APTMS 之星狀高分子…………………………….13
    3-3-2. 相同手臂的星狀高分子 ( homoarm star polymer )……...14
    3-4. 儀器分析原理…………………………………………………..16
    3-4-1. 液態核磁共振儀 (Solution NMR)…………….……….…16
    3-4-2. X光繞射儀 (X-ray Diffraction Spectrometer)…………....18
    3-4-3. 微差掃瞄熱卡計 (Differential Scanning Calorimeter)…...20
    3-4-4. 熱重量分析儀 (Thermo Gravimetric Analyzer)……….....22
    3-4-5. 傅立葉紅外線吸收光譜儀………………………………..23
    3-4-6. 交流阻抗分析儀…………………………………………..23
    3-4-7. 固態核磁共振光譜儀……………………………………..27
     3-4-7-1. 原理簡介……………………………………………...27
       3-4-7-2. 常用固態核磁共振技術……………………………...32
    第肆章 結果與討論…………………………………………………..37
    4-1. 乾式星狀固態高分子電解質……………………………………..37
    4-2. 液態核磁共振 (Solution NMR) 光譜分析……...………………38
    4-3. X-ray 粉末繞射 (Powder X-ray Diffraction) 圖譜分析…..…...45
    4-4. 微差掃瞄熱卡計 ( Differential Scanning Calorimeter) 分析.…...48
    4-5. 熱重量分析……………………………………………...………...56
    4-6. 紅外吸收光譜之鑑定……………………………………………..58
    4-7. 固態高分子電解質之導電度量測………………………………..75
    4-8. 固態核磁共振光譜分析….………………..……………………...99
    4-8-1. 29Si MAS NMR………………………..…………...…......100
    4-8-2. 13C MAS NMR……………………………..……….…….102
    4-8-3. 13C CP/MAS NMR ……………………...….………..……106
    4-8-4. 7Li 譜寬分析………………………………………….…..113
    4-8-5. 7Li-{1H} MAS NMR………...............................................122
    第伍章 結 論…………………………………………………………128
    參考文獻………………………………………………………………131
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    Advisor
  • Hsien-Ming Kao(高憲明)
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    Date of Submission 2007-07-23

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