矽烷基偶合劑表面修飾策略以提高聚偏乙烯-六氟丙烯/聚碳酸亞丙酯高分子系統與鋰鑭鋯鋁氧化物無機粉末界面兼容性之鋰金屬電池應用

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劉品榮(Pin-Rong Liu) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

矽烷基偶合劑表面修飾策略以提高聚偏乙烯-六氟丙烯/聚碳酸亞丙酯高分子系統與鋰鑭鋯鋁氧化物無機粉末界面兼容性之鋰金屬電池應用
(Silane coupling agent surface modification strategies to enhance the interfacial compatibility between PVDF-HFP/PPC polymer systems and LLZAO garnet-type inorganic powders for Lithium metal battery applications)

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至系統瀏覽論文 (2027-8-20以後開放)

摘要(中)

複合型固態電解質同時具備有機高分子的高機械性能和無機陶瓷粉末的高熱穩定性，因此是應用於鋰金屬電池的理想選擇。然而，複合型固態電解質存在一個嚴重問題，由於有機/無機界面不相容，無機粉末難以均勻分散在有機高分子中，導致團聚現象，從而阻礙鋰離子的傳輸，降低鋰金屬電池的電性能。
在這種情況下，矽烷基偶合劑的加入是一個很好的解決方案。通過矽烷基的親水端與無機粉末(LLZAO)上的-OH鍵結合，以及親油端含氮元素官能基的孤對電子與高分子進行路易斯酸鹼反應，可以改善有機/無機界面。
本實驗選擇了三種含氮官能基的矽烷基偶合劑，分別是3-異氰酸丙基三乙氧基矽烷(IPTS)、3-氨丙基三乙氧基矽烷(KH550)以及3-(2-咪唑啉-1-基)丙基三乙氧基矽烷(ITES)進行比較。
經過3-異氰酸丙基三乙氧基矽烷(IPTS)偶合劑修飾後的複合型固態電解質具有穩定的鋰離子傳輸通道，並展現出較高的離子導電率（在室溫下為8.4 x 10-4 S/cm）。此外，由於無機粉末與有機高分子的界面得到改善，固態電解質本身的拉伸強度達到0.79 MPa。經由組裝NCM811|CSEs|Li固態電池的測試，該電池在室溫充放電速率1.5C下，放電比容量高達125.85 mAh/g，且在0.5C充放電150圈的長循環測試中，比容量保持率高達98.72%。
這種經矽烷偶合劑修飾的複合型固態電解質將會為新一代的全固態鋰金屬電池拓展一條全新的道路。

摘要(英)

Composite solid electrolytes (CSEs) possess the high mechanical properties of organic polymers and the high thermal stability of inorganic ceramic powders, making them an ideal choice for use in lithium metal batterie s. However, CSEs face a significant challenge: the incompatibility of organic/inorganic interfaces results in inorganic powders not dispersing uniformly within the organic polymer, leading to agglomeration.This agglomeration obstructs the transport of lithium ions and decreases the electrochemical performance of lithium metal batteries.
In this context, the addition of silane coupling agents presents a promising solution. By forming bonds between the hydrophilic end of the silane and the
-OH groups on the inorganic powder (LLZAO), and through Lewis acid-base reactions between the lone pairs of electrons on the nitrogen-containing functional groups of the hydrophobic end and the polymer, the organic/inorganic interface can be improved.
This study selected three nitrogen-containing silane coupling agents for comparison: 3-Isocyanatopropyltriethoxysilane (IPTS), 3-Aminopropyltriethoxy -silane (KH550), and 3-(2-Imidazolin-1-yl)propyltriethoxysilane ( ITES).
The composite solid electrolyte modified with 3-Isocyanatopropyltriethoxysilane (IPTS) exhibited stable lithium-ion transport channels and a high ionic conductivity of 8.4 x 10-4 S/cm at room temperature. Furthermore, due to the improved interface between the inorganic powder and the organic polymer, the solid electrolyte itself demonstrated a tensile strength of 0.79 MPa, which is better than the tensile strength of the unmodified powder, 0.46 MPa. Testing the NCM811|CSEs|Li solid-state battery configuration revealed a high discharge specific capacity of 125.85 mAh/g at a 1.5C charge-discharge rate at room temperature, with a capacity retention rate of 98.72% after 150 cycles at 0.5C.
This novel design of CSEs with silane coupling agent modification paves the way for a new generation of all-solid-state lithium metal batteries.

關鍵字(中)

★ 鋰金屬半電池
★ 矽烷基偶合劑
★ 複合型固態電解質
★ 鋰鑭鋯鋁氧化物

關鍵字(英)

★ Lithium metal half cell
★ Silane coupling agents
★ Composite solid electrolytes
★ Garnet-type oxide LLZAO

論文目次

摘要 i
Abstract iii
致謝 v
目錄 vii
圖目錄 xi
表目錄 xvii
第一章緒論 1
1-1 前言 1
1-2 研究動機 2
第二章文獻回顧 6
2-1 正極活性物質-LiNi0.8Co0.1Mn0.1O2(NCM811)介紹 6
2-2 高分子固態電解質介紹 7
2-3 複合型固態電解質介紹 17
2-4 無機陶瓷粉末介紹 20
2-5 石榴石型(Garnet type)-鋰鑭鋯鋁氧化物(LLZAO)介紹 23
2-5-1 石榴石型無機陶瓷填料-LLZO介紹: 23
2-5-2 Al參雜LLZO介紹: 26
2-6 偶合劑介紹 29
第三章實驗方法 33
3-1 實驗藥品 33
3-2 實驗設備 34
3-3 實驗步驟 35
3-3-1 高分子固態電解質膜的製備 35
3-3-2 複合型固態電解質膜的製備 35
3-3-3 正極的製備 37
3-3-4 離子液體的製備 38
3-3-5 無機固態粉末修飾 38
3-3-6 鈕扣電池的組裝 39
3-4 材料分析及鑑定 41
3-4-1 粉末X光繞射儀(Powder X-ray diffraction,PXRD) 41
3-4-2 冷場發射掃描式電子顯微鏡(The field-emission scanning electron 41
microscope, FE-SEM) 41
3-4-3 傅立葉轉換紅外光譜(FT-IR) 42
3-4-4 高解析掃描穿透式電子顯微鏡(HR-TEM) 42
3-4-5 機械拉伸強度測試 43
3-5 電化學性質分析及鑑定 43
3-5-1 計時電位法(Chronopotentimetry)量測: 43
3-5-2 循環測試 (Cycling tests): 44
3-5-3 交流阻抗測試 (Electrochemical impedance spectroscopy, EIS): 45
3-6 實驗流程圖 51
第四章結果與討論 52
4-1 修飾無機粉末LLZAO之材料與電性分析 53
4-1-1 XRD分析 53
4-1-2 FT-IR分析 57
4-1-3 定性分析 62
4-1-4 不同電流密度充放電分析 70
4-1-5 交流阻抗之離子導電率 96
4-1-6 HR-TEM分析 103
4-2 水的添加對於修飾無機粉末LLZAO製程差異 105
4-2-1 定性分析 106
4-2-2 不同電流密度充放電分析 108
4-2-3 交流阻抗之離子導電率 111
4-3 各偶合劑最佳修飾時間材料與電性比較 113
4-3-1 SEM分析 114
4-3-2 機械拉伸強度比較 121
4-3-3 鋰離子遷移率(tLi+)比較 124
4-3-4 循環壽命分析 127
第五章結論與未來展望 132
第六章附錄 135
6-1-1 SEM以及定性分析 136
6-1-2 不同電流密度充放電分析 138
6-1-3 交流阻抗之離子導電率 145
6-1-4 鋰離子遷移率(tLi+)比較 147
6-1-5 循環壽命分析 149
參考文獻 153

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指導教授

李岱洲張仍奎(Tai-Chou Lee Jeng-kuei Chang)

審核日期

2024-8-20

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