以環氧樹酯合成具不同特性混摻型固 (膠) 態高分子電解質之結構鑑定及電化學研究

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張佑如(Yu-Ju Chang) 查詢紙本館藏

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論文名稱

以環氧樹酯合成具不同特性混摻型固 (膠) 態高分子電解質之結構鑑定及電化學研究

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摘要(中)

本論文分為兩部分，第一部分為利用兩種不同特性之高分子材料 (M-2070及ED2003) 分別與具環氧基團之材料聚合，依據不同重量比混摻，並改變其氧鋰比，合成出混摻型有機無機固態高分子電解質。接著探討鋰鹽濃度對於高分子電解質的性質影響及鋰離子與高分子鏈段的作用情形：利用熱重分析儀 (TGA) 觀察其熱穩定性；以X-ray粉末繞射儀 (Powder X-Ray Diffractometer) 與微差掃描熱卡計 (DSC) 研究高分子鏈段結晶情形；以掃描式電子顯微鏡 (SEM) 分析其表面形態；以傅立葉紅外線吸收光譜儀 (FTIR) 對其結構作鑑定並分析鋰鹽解離程度；以交流阻抗分析儀 (AC Impedance) 測量離子導電度與電化學穩定性；以固態核磁共振光譜儀 (SSNMR) 之13C CP MAS及29Si CP MAS進行結構鑑定，並利用1H-13C 2D WISE與7Li NMR譜寬量測了解鋰離子與高分子鏈段運動性之間的動力學分析研究。比較FTIR、DSC與核磁共振方法其量測結果與離子導電度之趨勢相符，當鋰鹽濃度於此固態電解質達一定程度時，可得到一最佳鋰離子傳遞速率，具有較佳導電度，此固態高分子電解質於30 C下量測其離子導電度可達1.01 × 10-4 S cm-1。
第二部分為將第一部分所合成固態電解質吸附不同種類之液態電解液形成膠態電解質，期望藉由有機溶劑使鋰離子有較佳的傳導效果，以提升離子導電度。接著以澎潤比測試探討膠態電解質吸附各類電解液之吸附情形；以交流阻抗分析儀 (AC Impedance) 測量離子導電度與電化學穩定性，得知此膠態高分子電解質吸附1M LiPF6 in EC/DEC (1:1, v/v) 於30 C下其離子導電度可達到2.04 × 10-2 S cm-1，並可承受約4.2 V之氧化分解電壓；最終將膠態電解質與市售之隔離膜同時吸附1M LiPF6 in EC/DEC (1:1, v/v) 分別組成硬幣型鋰離子電池，探討兩者之電性表現，結果顯示本實驗所合成之膠態電解質具有較佳的充放電循環壽命。

摘要(英)

A new organic-inorganic hybrid electrolyte was synthesized by blending two organic-inorganic hybrid precursors. Two precursors based on reactions of (Ⅰ) triblock co-polymer poly(propylene glycol)-block-poly(ethylene glycol)-block-poly(propylene glycol) bis(2-aminopropyl ether) (ED2003) with poly(ethylene glycol) diglycidyl ether (PEGDGE) and followed by co-condensation with (3-Isocyanatopropyl)triethoxysilane (ICPTES), and (Ⅱ) oligo(oxyalkylene)-amines (M-2070) with poly(ethylene glycol) diglycidyl ether (PEGDGE) via condensation. The hybrid electrolytes were obtained by varying the weight percentages of two precursors and LiClO4 salt.
The structure and electrochemical properties of the polymer electrolytes were characterized by different of techniques including thermogravi-metric analyzer (TGA), Powder X-Ray Diffractometer, differential scanning calorimetry (DSC), scanning electron spectroscopy (SEM), Fourier transform infrared spectroscopy (FTIR), 13C cross-polarization magic-angle spinning (CPMAS), AC impedance and charge–discharge measurement. The hybrid polymer electrolyte was measured the ionic conductivity value of 1.01 × 10−4 S cm−1 at 30 °C. Multinuclear NMR techniques were used to provide a microscopic view for the specific interaction between the polymer chains and Li+ cations. The results of 2D 1H-13C wide-line separation (WISE) and 7Li static line NMR width measurements found that the mobility of the 7Li cations are strongly related to a dynamic environment created by the polymer chains motion in the amorphous phase.
After swelling in different liquid electrolyte solvents, the gel polymer electrolytes were prepared. The swelling ratio and the ionic conductivity of the gel electrolytes were measured with liquid electrolyte solutions, the gel polymer electrolytes immersed in 1M LiPF6 in EC/DEC (1:1, v/v) represents the highest ionic conductivity as 2.04 × 10-2 S cm-1 at 30 °C. This gel electroltyte also had good electrochemical stability up to 4.2 V. Finally, the gel electrolyte compared with commercial separator PP membrane immersed in 1M LiPF6 in EC/DEC (1:1, v/v) applied for charge–discharge measurement of lithium ion batteries. Hence, it can be concluded that this new hybrid polymer system is suitable for use as a gel polymer electrolyte in rechargeable lithium batteries.

關鍵字(中)

★ 固態電解質
★ 鋰電池

關鍵字(英)

★ solid polymer electrolyte
★ lithium ion battery

論文目次

第一章前言 1
1-1. 鋰二次電池簡介 1
1-2. 文獻回顧 4
1-2-1. 鋰離子電池 4
1-2-2. 高分子電解質 6
1-2-3. 固態高分子電解質 9
1-2-4. 膠態高分子電解質 15
1-3. 鋰離子鹽類 21
第二章研究規劃 26
2-1. 研究動機 26
2-1-1. 具環氧樹脂之高分子 26
2-1-2. 有機矽高分子 29
2-2. 研究方向 30
2-3. 研究架構 31
第三章實驗部分與原理 32
3-1. 實驗藥品 32
3-2. 儀器設備 34
3-3. 高分子電解質膜製備 35
3-3-1. 固態高分子電解質製備 35
3-3-2. 膠態高分子電解質製備 38
3-3-3. 硬幣型 2032 型電池組裝 39
3-4. 儀器分析原理 40
3-4-1. 熱重量分析儀 (Thermo Gravimetric Analyzer, TGA) 40
3-4-2. X-射線粉末繞射 (Powder X-Ray Diffractometer, XRD) 40
3-4-3. 微差掃描熱卡計 (Differential Scanning Calorimeter, DSC) 41
3-4-4. 傅立葉紅外線吸收光譜儀 (FTIR) 42
3-4-5. 交流阻抗分析儀 (AC-impedance) 42
3-4-6. 掃描式電子顯微鏡 (Scanning Electron Microscopy, SEM) 43
3-4-7. 固態核磁共振 (Solid State NMR) 43
3-4-8. 線性掃描電位測試 48
3-4-9. 電池性能測試 49
第四章結果與討論 50
4-1. 固態高分子電解質 MP-EDPI-X-Y 50
4-1-1. 混摻型高分子主體之離子導電度 51
4-1-2. 熱重量分析 54
4-1-3. X-ray粉末繞射圖譜分析 56
4-1-4. 微差式掃描熱卡計分析 58
4-1-5. 紅外線吸收光譜之鑑定分析 61
4-1-6. 掃描式電子顯微鏡之表面分析 66
4-1-7. 交流阻抗儀之離子導電度測試 69
4-1-8. 固態核磁共振光譜儀分析 74
4-1-9. 線性掃描伏安法 92
4-2. 膠態高分子電解質 MP-EDPI-60- 94
4-2-1. 電解質吸附之澎潤比測試 95
4-2-2. 交流阻抗儀之離子導電度測試 98
4-2-3. 線性掃描伏安法 101
4-2-4. 電池性能測試 102
第五章結論 108
參考文獻 110
附錄 - 以規則有序中孔洞碳材改質金屬氧化物之鋰電池陽極材料 121
第六章前言 121
第七章文獻回顧 122
7-1. 中孔洞碳材 (Mesoporous carbon materials) 122
7-1-1. 奈米模鑄法 (Nanocasting) 124
7-1-2. 以奈米模鑄法合成規則有序之中孔洞碳材文獻回顧 126
7-2. 陽極材料 132
7-2-1. Fe3O4陽極之文獻回顧 132
7-2-2. Co3O4陽極之文獻回顧 133
第八章實驗方法 135
8-1. 藥品 135
8-2. 奈米模鑄法合成三維孔道結構 (Ia3 ̅d) 中孔洞碳材 136
8-2-1. 三維立方體Ia3 ̅d中孔洞矽材模板KIT-6合成 136
8-2-2. 三維立方體 Ia3 ̅d 中孔洞碳材 CMK-8合成 137
8-3. 含浸法合成Fe3O4@CMK8陽極複合物 137
8-4. 含浸法合成Co3O4@CMK8陽極複合物 137
8-5. 材料電化學性能測試 138
8-5-1. 陽極極片製作(Co3O4@CMK8及Fe3O4@CMK8) 138
8-5-2. 硬幣型電池組裝 138
8-5-3. 電池性能測試之變電流充放電循環測試 138
8-6. 實驗鑑定儀器 139
8-7. 鑑定儀器之原理 139
8-7-1. 同步輻射光束線 139
8-7-2. 氮氣等溫吸脫附曲線、表面積與孔洞特性鑑定 140
第九章結果與討論 143
9-1. 低角度XRD結果分析 143
9-2. 氮氣等溫吸附/脫附結果分析 144
9-3. 不同電流密度充放電測試 146
參考文獻 148

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指導教授

高憲明(Hsien-Ming Kao)

審核日期

2016-7-26

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