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研究生： 林紀昌
Chi-Chang Lin
論文名稱： 複合高分子電解質
指導教授： 諸柏仁
Po-Jen Chu
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： 94
語文別： 中文
論文頁數： 189
相關次數： 點閱：11  下載：0 
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    • 有機-無機奈米複合材料為高分子電解質帶來許多電性與熱性質上的改善，除了優越的機械穩定性、高離子導電度、大的電化學穩定區間之外，尚能提供與電極良好的介面穩定性。
    針對本研究所製備之二氧化鈦奈米管以及經過高分子表面修飾的二氧化鈦奈米管，使用XRD、NMR、XPS、TEM、TGA等儀器進行鑑定。將修飾後的二氧化鈦奈米管進一步製備成複合高分子電解質，由SEM表面型態觀察到相容性的提升，由離子導電度的分析也證實經修飾後，相較於僅只是摻合的方式，能有效提升導電度超過一個級數（order）。XPS及FT-IR的分析則指出鋰鹽在電解質系統中能有效的解離，減少離子對的情形。
    藉由AC-Impedance與DSC的研究，顯示在不同製備條件的複合高分子電解質中，不僅二氧化鈦奈米管能有效藉由短暫交聯結構的形成，使高分子重組作用降低、增加非結晶區塊，並延緩剩餘高分子結晶區塊的結晶速率；同時也發現發現，小分子量高分子的採用能有效提高離子導電度；適當的成膜溶劑選擇，除了能提供高介電常數促使鹽類解離外，還能利用奈米管的特殊表面微結構或是管徑中空的位置做溶劑儲存（retain）的功用，即使在高溫（90°C）也不會逸失；不同鋰鹽的使用，也能從導電度行為上觀察到二氧化鈦、高分子與鋰鹽之間的作用是否於一開始就已達平衡狀態，亦或需要做一高溫的熱催化，來促使三者間的作用或配對情形達平衡狀態；使用不同合成製備方式的二氧化鈦奈米管，也能觀察到由於其表面結構缺陷濃度的不同，而影響導電度及高分子熱性質的行為。最後，發現在複合交聯型高分子電解質的系統中，酚醛樹酯與高分子所形成相互貫穿的網狀區塊，能有效限制高分子的結晶行為，交聯劑的添加則大幅提昇的薄膜的機械穩定性，而二氧化鈦奈米管的使用，則避免了結構交聯過度所帶來導電度的大幅衰退。

    Organic-inorganic nano-composite bring lots of improvements in electric and thermal properties, such as excellent mechanical stability, higher ionic conductivity and wide electrochemical stability, and also provide better interface stability with electrode.
    This research focus on the preparation of TiO2 nano-tube and surface modification of TiO2 nano-tube with polymer which can be characterized by using XRD, NMR, XPS, TEM and TGA etc. Composite polymer electrolyte made by surface modified TiO2 nano-tube exhibit better compatibility from SEM surface morphology observation and an increase in ionic conductivity more than one order than that of blending ones. XPS and FT-IR also indicated polymer electrolyte containing TiO2 nano-tube can efficaciously dissociate the lithium salt and decrease the ion-pairing occurring.
    Composite polymer electrolyte made with a number of variable components were systematically study to find their impact upon the electrochemical properties of the resulting materials. TiO2 nano-tube surface group can act as a cross-linking center for the polymer segments, which reduced the polymer reorganization, increased amorphous domain and delay the rate of recrystallization. It’s generally observed the lower molecular weight samples yielded the higher ionic conductivity. A proper choice of solvent will not only increase the order of salt dissociation but also can be stored in TiO2 tubular microstructure. Conductivity behavior suggested specific salt will re-distribute between TiO2 nano-tube and polymer chain to reach equilibrium state. TiO2 nano-tube with different `concentration of surface defect will be a critical factor affect the conductivity and thermal proper of polymer electrolyte.
    In the composite/cross-linking polymer electrolyte, the interpenetrating network structure between phenolic and polymer chain can be efficiently hindered polymer crystallization, the cross-linker promoted mechanical stability, and the using of TiO2 nano-tube avoid the dramatically fadedness of conductivity came from over cross-linking.

    中文摘要………………………………………………………….………I 英文摘要……………………………………………………………......III 謝誌……………………………………………………………………...V 目錄……………………………………………………………………..VI 表目錄…………………………………………………………….……. X 圖目錄…………………………………………………………......….. XII 第一章 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（Cross-link Polymer Electrolyte）…....…7 1-4-2 共聚高分子電解質（Block-Copolymer Electrolyte）……..…8 1-4-3 接枝高分子電解質（Graft/Comb Polymer Electrolyte）….…8 1-4-4 混摻高分子電解質（Blend Polymer Electrolyte）…………9 1-4-5 複合高分子電解質（Composite Polymer Electrolyte）…....9 1-4-6 單離子高分子電解質（Single-ion Polymer Electrolyte）…..10 1-4-7 Polymer - in – Salt Polymer Electrolyte………………….….11 1-4-8 Ormolytes/Ormocer（Organically Modified CERamics）……11 1-5 膠態高分子電解質……………………………………………...…12 1-6 微孔型高分子電解質………………………………………...……14 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 1-9 第一章參考文獻…………………………………………...………19 第二章 文獻回顧…………………………………………..………24 2-1 高分子電解質之發展………………………………………….…..24 2-2 奈米複合（nano-composite）高分子電解質發展…………….……27 2-3 二氧化鈦之發展…………………………………………...………30 2-3-1 二氧化鈦奈米管之製備……………………….…...………33 2-4 Novolac type酚醛樹酯…………………………………….……..37 2-4-1 酚醛樹酯的特性…................................................................37 2-4-2 Novolac type酚醛樹酯與聚氧化乙烯摻合之研究探討…38 2-5 交聯劑六甲烯基四胺的特性……………….…………...………...39 2-6 第二章參考文獻…………………………………………...………40 第三章 實驗及儀器原理……………………………………..……47 3-1 樣品製備………………………………………………………...…47 3-1-1 二氧化鈦奈米管之合成（TiO2 nano-tube）………...………47 3-1-2 修飾型二氧化鈦奈米管之複合高分子電解質……………47 3-1-3 混摻型二氧化鈦奈米管之複合高分子電解質……………48 3-1-4 不同製備條件之複合高分子電解質………………………49 3-1-5 三相複合高分子電解質……………………………………49 3-2 實驗藥品……………………………………………………...……50 3-3 實驗儀器設備………………………………………………...……52 3-4 分析儀器應用理論……………………………………………...…53 3-4-1 微差掃瞄熱卡計（DSC）……………………………………53 3-4-2 熱重分析儀（TGA）…………………………………..……..54 3-4-3 傅立葉式紅外線吸收光譜儀（FT-IR）……………….…….55 3-4-4 掃瞄式電子顯微鏡（SEM）………………………..………..56 3-4-5 交流阻抗分析儀（AC Impedance）…………………………57 3-4-6 電化學穩定度量測（LSV）……………………………...….68 3-4-7 電池組裝與充放電量測（charge / discharge capacity）……70 3-4-8 X光繞射儀（XRD）………………………………….…….71 3-4-9 氮氣等溫吸附/脫附儀(ASAP)………………………..……72 3-4-10 核磁共振儀(Solid-state NMR)……………………………75 3-4-11 射線光電子能譜儀（XPS）…………………………..…….77 第四章 結果與討論…………………………………………...……79 4-1 二氧化鈦奈米管結構分析…………………………………...……81 4-1-1 X光繞射結構分析（XRD）………………………..………81 4-1-2 氮氣等溫吸附/脫附測量（ASAP）………………………83 4-1-3 熱重損失分析（TGA）……………………………………85 4-1-4 傅立葉紅外線（FT-IR）光譜分析………………………..87 4-1-5 穿透式電子顯微鏡分析（TEM）………………….……..88 4-1-6 掃瞄式電子顯微鏡分析（SEM）…………………..……..90 4-1-7 1H固態核磁共振儀分析（solid-state NMR）……………92 4-1-8 X光射線光電子光譜分析（XPS）……………………….94 4-2 二氧化鈦奈米管之修飾及其複合高分子電解質探討……...……99 4-2-1 掃瞄式電子顯微鏡分析（SEM）……………………….100 4-2-2 熱重損失分析（TGA）……….…………………….……102 4-2-3 傅立葉紅外線光譜分析（FT-IR）…………………….…105 4-2-4 X光繞射結構分析（XRD）……………………….……108 4-2-5 X光射線光電子光譜分析（XPS）……………………..110 4-2-6 13C固態核磁共振儀分析（solid-state NMR）…………..114 4-2-7 微分掃瞄熱卡計分析（DSC）……………………………117 4-2-8 X光繞射光譜在高分子電解質之分析（XRD）………..120 4-2-9 傅立葉紅外線光譜在高分子電解質之分析（FT-IR）…122 4-2-10 X光射線光電子光譜在高分子電解質分析（XPS）…128 4-2-11 交流阻抗儀在高分子電解質之分析（AC-Impedance）..132 4-3 不同製備條件對複合高分子電解質之影響與探討………….…139 4-3-1 微分掃瞄熱卡計分析（DSC）……………………………140 4-3-2 交流阻抗儀之分析（AC-Impedance）………………..…146 4-4 三相複合高分子電解質……………………………………...…..152 4-4-1 微分掃瞄熱卡計分析（DSC）……………………………153 4-4-2 交流阻抗儀在高分子電解質之分析（AC-Impedance）.....159 4-5 第四章參考文獻…………………………………………...……..164 第五章 結論與未來展望………………………………………..167

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