臺灣博碩士論文加值系統

本研究中，我們以PEDGE、DGEBA以及D2000進行交聯合成高分子電解質，也就是P(EO-co-PO)。將製備好的高分子薄膜浸泡於有機電解液中24小時，即可得到膠態高分子電解質(GPE)。將此電解質進行電池組裝測試其性能，並與商業化的隔離膜組裝成有機液相(LE)電池進行性能差異比較並分析我們的膠態高分子電解質優勢。
相對於有機液相電解質，P(EO-co-PO)膠態高分子電解質具備高導離子度(3.82×10-3S cm-1)，容易製備成膜以及較佳的電化學穩定電位窗(5V)。除此之外，P(EO-co-PO)高分子具有較佳的鋰鹽解離能力以及較高的鋰離子遷移數(0.7)。擁有較高的鋰離子遷移數可抑制濃度梯度的產生以及對於電極極化阻力的消除是有益的，可使得電解質-電極界面的穩定性相較於有機液相表現較佳，不只阻力值較小且更容易達到穩定，讓電池在測試時可容忍更快速的充放電且擁有較佳的長效穩定性。
　　電池性能測試方面，我們使用磷酸鋰鐵陰極搭配石墨陽極進行全電池搭配，比較LE與GPE的差異。在低速表現來說，兩者差異其實不大，其值約為125mAh g-1，但當電池放電速度在10C-rate以上時，LE全電池的放電維持率衰減是非常明顯的，相較之下，GPE全電池的放電速度在17C-rate時仍可穩定的進行充放電。除此之外，在長效穩定性測試方面，使用1C-rate進行450圈長效充放電測試，GPE全電池的穩定性直到450圈後尚可維持77%，相較於LE全電池的維持率(44%)來說，表現絕對可以說是非常優秀。
由於石墨陽極在快速充放電的性能表現較差的關係，在本研究中，我們另外發展了水熱法合成二氧化鈦奈米管，二氧化鈦除了有著無毒性、高化學穩定性及價格低廉等優點，藉由奈米管的形成，在快速充放電部分，因為電解液可以深入奈米管中，使得電解液與電極的接觸表面積增加且可減少鋰離子擴散距離，進而減少擴散阻力，使得在進行高速60C-rate充放電時，電池放電量還可以達到70 mAh g-1。

In this study, we used PEDGE, DGEBA and D2000 by cross-linking to synthesis the copolymer –poly(ethylene oxide)-co-poly(propylene oxide) (P(EO-co-PO)). Immersing the polymer film into the organic electrolyte for 24 hours, then we got the gel polymer electrolyte (GPE). Took this GPE film to assemble batteries and test its performance. Compare the difference between GPE and the organic liquid electrolyte battery (LE) , find out the advantages of GPE.
Compare to LE, the proposed GPE has higher ionic conductivity (3.8210-3 S cm-1 at 30 °C) and a wider electrochemical voltage range (5V). Besides, P(EO-co-PO) copolymer equipped better Lithium ion dissociation ability and higher transfer number (0.7). This high GPE transference number decreases electrode polarization caused by anion accumulation and suppresses the concentration gradient to facilitate lithium ion transport. That made the electrolyte-electrode surface of GPE more stable than LE with lower resistance. Therefore, the performance can be better at higher C-rate charge-discharge test and long-term stability.
For battery performance test, we use LiFePO4-cathode and Graphite-anode to assemble the full-cell and compare the difference between GPE and LE. At lower C-rates, the discharge capacity is similar and the value is about 125mAh g-1. When discharge rate is higher than 10 C-rate, the performance decrease dramatically in LE full-cell, while GPE full-cell maintain the capacity even at 17C-rate. For long-term test, we conducted charge-discharge measurement at 1C-rate for 450 cycles. After 450 cycles the capacity retention maintained at ca. 77%. It’s better than the LE full-cell which kept only ca. 44%.
Due to the bad performance at higher C-rates by using Graphite-anode, in this study, we also developed hydrothermal method to synthesis TiO2 nanotube. TiO2 is nontoxic, high chemical stability and low price. Moreover, the nanotube structure can help to catch the electrolyte into the tube, increase the electrolyte-electrode contact surface and decrease the distance of lithium ion diffusion. And then decrease the diffusion resistance, that resulted in a discharge capacity 70 mAh g-1 at 60C-rate.

總 目 錄

中文摘要 I
英文摘要 III
誌 謝 V
本文目錄 V
表目錄 VIII
圖目錄 VIII

本 文 目 錄

第一章 緒論 1
1-1 前言 1
1-2 鋰電池與鋰離子二次電池發展 4
1-3 研究動機與目的 6

第二章 理論說明與文獻回顧 8
2-1 鋰離子電池 8
2-1.1 裝置構造 8
2-1.2 工作原理 8
2-2 電解質 10
2-2.1 液態有機電解質 10
2-2.2 固態高分子電解質 12
2-2.3 膠態高分子電解質 17
2-2.4 微孔型高分子電解質 18
2-2.5 無機固態電解質 20
2-3 電極材料 22
2-3.1 正極材料 22
2-3.2 負極材料 24
2-4 目前全球鋰離子電池材料發展現況及比較 27

第三章 實驗方法與儀器原理介紹 30
3-1 實驗藥品 30
3-2 實驗儀器設備 31
3-3 膠態高分子電解質製備 33
3-4 鈕扣型電池組裝 35
3-5 實驗分析儀器與裝置分析儀器原理簡介 36
3-5.1 穿透式電子顯微鏡 36
3-5.2 物理吸附分析 38
3-5.3 X光繞射分析 40
3-5.4 傅立葉轉換紅外線光譜 42
3-5.5 拉曼光譜分析 44
3-6 電化學測試 46
3-6.1 離子傳導度 46
3-6.2 線性掃描伏安法 46
3-6.3 電解質-電極界面阻力測試 46
3-6.4 鋰離子遷移數 46
3-7 LiFePO4電池性能測試 47
3-7.1 LiFePO4正極之極片製作 47
3-7.2 LiFePO4半電池 47
3-7.3 Graphite/LiFePO4全電池 48
3-8 TiO2半電池測試 48
3-8.1 水熱法合成二氧化鈦奈米管 48
3-8.2 電極製備 48
3-8.3 TiO2半電池 49
3-9 實驗流程 50

第四章 結果與討論 51
4-1 膠態電解質與液態電解質物理化學鑑定 51
4-1.1 FTIR分析 51
4-1.2 Raman分析 52
4-2 離子傳導度 56
4-3 穩定電位窗測試 60
4-4 離子在界面及電解質內之傳輸行為 61
4-4.1 電解質-電極界面阻力測試 61
4-4.2 鋰離子遷移數 64
4-5 LiFePO4半電池性能測試 67
4-6 Graphite/LiFePO4全電池性能測試 70
4-6.1 全電池界面阻力測試 70
4-6.2 充放電性能測試 73
4-6.3 Ragone plots 76
4-6.4 長效穩定性測試 77
4-6.5 文獻比較 78
4-7 TiO2半電池性能測試 79
4-7.1 TEM及XRD分析 79
4-7.2 充放電性能測試 81
4-7.3 長效穩定性測試 83

第五章 結論與建議 84

參考文獻 85

表 目 錄

表2- 1 鋰離子電池中常用有機溶劑的特性 11
表2- 2 常見的正極材料比較 22
表2- 3 常見的負極材料比較 25

圖 目 錄

第一章 緒論
圖1- 1 未來電池的六大需求目標 3
圖1- 2 鋰離子電池與其它電池能量密度比較圖 3

第二章 理論說明與文獻回顧
圖2- 1 鋰離子電池電池裝置圖 9
圖2- 2 鋰離子電池工作原理示意圖 9
圖2- 3 常見正極材料的電位窗-放電量比較及未來趨勢 23
圖2- 4 常用碳材示意圖 25
圖2- 5 常見負極材料的電位窗-放電量比較及未來趨勢 26

第三章 實驗方法與儀器原理介紹
圖3- 1 高分子P(EO-co-PO)之製備流程圖 34
圖3- 2 鈕扣型電池組裝示意圖 35
圖3- 3 基本穿透式電子顯微鏡之結構圖 37
圖3- 4 物理吸附分析儀 39
圖3- 5 X光對原子散射圖 41
圖3- 6 X光對晶體繞射圖 41
圖3- 7 不同化學鍵吸收紅外光的光譜區域 43
圖3- 8 光散射三種途徑之簡易示意圖 45
圖3- 9 高溫高壓反應器 49
圖3- 10 實驗流程圖 50

第四章 結果與討論
圖4- 1 GPE及LE的FTIR吸收光譜圖 51
圖4- 2 GPE及LE的Raman光譜圖 55
圖4- 3離子導電度對溫度的變化關係 59
圖4- 4電化學穩定性 60
圖4- 5界面阻力測試的Nyquist阻抗分析圖 63
圖4- 6 (a)直流電極化後得到的電流-時間圖
(b) GPE及(c) LE極化前後的Nyquist阻抗分析圖 66
圖4- 7 LiFePO4半電池充放電圖 69
圖4- 8 LiFePO4半電池的電位差-放電電流圖 69
圖4- 9 Graphite/LiFePO4全電池的Nyquist阻抗分析圖 72
圖4- 10 Graphite/LiFePO4全電池的充放電圖 75
圖4- 11 LiFePO4/Graphite全電池之Ragone plot 76
圖4- 12 Graphite/LiFePO4全電池長效充放電圖 77
圖4- 13 TiO2的TEM圖 80
圖4- 14 TiO2的XRD圖 80
圖4- 15 TiO2半電池的充放電圖 82
圖4- 16 TiO2半電池長效充放電圖 83

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