光聚合複合型固態電解質應用於鋰離子電池之研究

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游勝宇(Sheng-Yu You) 查詢紙本館藏

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光聚合複合型固態電解質應用於鋰離子電池之研究

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至系統瀏覽論文 (2028-7-1以後開放)

摘要(中)

傳統鋰電池通常使用液體電解質作為傳導介質，並使用多孔隔離膜來區分正極和負極。然而，這種傳統方法在製作隔離膜時需要耗費大量時間並回收相關溶劑，而且液體電解質的高易燃性引發安全疑慮。因此，本研究採用光聚合方法，能夠快速製造出無需溶劑且不需要大量電解液的固態電解質，作為製造固態鋰電池的基礎。首先，從高分子的角度來看，導電需要具有長鏈分子的擺動來進行傳導，但同時不能受結晶區的影響。因此，我們使用PEGDA和MA進行共聚合，與PEO結合形成無結晶網狀交聯型高分子，提供離子傳導的功能。為了進一步提高導電性，我們添加了SCN和LiTFSI，它們之間的晶體轉換機制可以增加導電度。實驗結果顯示，在0.5C和1C的條件下，添加30%的SCN時，具有高電容量分別為148.5 mAh/g和111.7 mAh/g，並在長時間循環中保持90%以上的電容保持率。然而，由於SCN本身不是高強度分子，添加過多會降低電解質隔膜的強度。為了解決這個問題，我們添加了LAGP形成複合電解質，結合了高分子、無機陶瓷材料和添加劑三種導電途徑。然而，在電池元件中，LAGP本身的特性會與鋰金屬發生還原反應。為避免這個負面影響，我們首先鋪平LAGP混合物，然後倒入高分子液體進行光聚合，以獲得LAGP聚集在同一側（陰極端）的複合薄膜。在進一步的實驗中，添加5%的LAGP和30%的SCN表現出良好的電性，分別在0.5C和1C條件下具有154.9 mAh/g和110.1 mAh/g的高電容量。此外，材料的強度接近未添加SCN時的數值。綜上所述，本研究成功地製備了具有快速、環保、強度、安全和電性等五個關鍵指標的複合電解質，該材料展現出優異的固態鋰電池性能。

摘要(英)

Traditional lithium batteries typically require liquid electrolytes as a conducting medium using porous membranes to separate the positive and negative electrodes. However, this conventional method not only involves significant time and solvent recovery efforts during the production of the membrane but also raises safety concerns due to the high flammability of liquid electrolytes. Therefore, in this study, we adopted a solvent-free and electrolyte-minimized approach using photopolymerization to rapidly produce a solid-state electrolyte.
From a polymer perspective, conductivity in the solid-state electrolyte requires long-chain polymer segments for ion transport while remaining unaffected by crystalline regions. To achieve this, we utilized a co-polymerization of PEGDA and MA, combined with PEO, to form a networked crosslinked polymer matrix that provides ion conductivity and electron insulation. To further enhance the conductivity, we introduced additives such as SCN and LiTFSI, which undergo a crystalline-to-conductive transition mechanism. Experimental results demonstrated high capacity values of 148.5 mAh/g and 111.7 mAh/g at 0.5C and 1C rates, respectively, with the addition of 30% SCN. Moreover, the electrolyte maintained a capacity retention of over 90% even after numerous charge-discharge cycles. However, due to SCN′s lower molecular strength, excessive amounts led to a decline in the mechanical properties of the electrolyte membrane. To address this issue, we incorporated LAGP to form a composite electrolyte, comprising polymer, inorganic ceramic material, and additives, thereby creating three pathways for conductivity.
Nevertheless, LAGP itself undergoes reduction when it comes into contact with lithium metal. To mitigate this effect, we first applied a uniform LAGP slurry and subsequently poured the polymer liquid for photopolymerization, resulting in a composite thin film with LAGP aggregating on one side (cathode side). In further experiments, the addition of 5% LAGP and 30% SCN exhibited excellent electrochemical performance, with high capacities of 154.9 mAh/g (at 0.5C) and 110.1 mAh/g (at 1C). Additionally, the strength of the material approached values comparable to those before the addition of SCN. This study successfully developed a composite electrolyte that fulfills five key criteria: rapid production, environmental friendliness, mechanical strength, safety, and electrochemical performance for solid state lithium battery.

關鍵字(中)

★ 高分子
★ 光聚合
★ 電解質
★ 陶瓷材料
★ 電容量
★ 長圈數循環

關鍵字(英)

論文目次

摘要 i
Abstract iii
誌謝 v
目錄 vi
圖目錄 xii
表目錄 xix
第一章緒論 1
1-1 前言 1
1-2 鋰電池固態電解質的研究困境 3
第二章文獻回顧 5
2-1 鋰離子電池工作原理以及簡介 5
2-2 液態電解質及SEI層分析 7
2-3 有機高分子膠體電解質 10
2-3-1 高分子類電解質傳導機制 10
2-3-2 高分子類電解質實際應用例子 13
2-4 交聯聚合型高分子電解質 20
2-4-1 交聯聚合型高分子反應機制 20
2-4-2 熱聚合交聯型電解質 23
2-4-3 光聚合交聯型電解質 25
2-5 無機物類電解質 31
2-5-1 無機物類電解質簡介及導電原理 31
2-5-2 氧化物類無機電解質 35
2-5-3 硫化物類無機電解質 42
2-6 複合型固態電解質 47
2-6-1 高分子複合氧化物 47
2-6-2 高分子複合硫化物 51
2-6-3 氧化物複合硫化物 52
2-7 電解質添加劑 53
2-7-1 有機分子添加劑 53
2-7-2 無機分子添加劑 56
2-8 研究動機與設計 58
第三章實驗手法 60
3-1 實驗藥品 60
3-2 實驗器材與儀器 62
3-3 實驗步驟 63
3-3-1 正極極片之製備 63
3-3-2 膠體電解質之製備 64
3-3-3 複合電解質之製備 64
3-3-4 組裝半電池 65
3-4 實驗儀器分析及原理 67
3-4-1 超高真空冷場發射掃描式電子顯微鏡(SEM) 67
3-4-2 超高解析穿透式電子顯微鏡(TEM) 67
3-4-3 X光繞射儀(XRD) 68
3-4-4 X射線光電子能譜儀(XPS) 68
3-4-5 熱重分析儀(TGA) 69
3-4-6 示差熱掃描分析儀(DSC) 69
3-4-7 傅立葉轉換紅外光譜(FTIR) 70
3-4-8 複合薄膜機械強度測試 70
3-5 鋰電池效能及電化學特性分析 71
3-5-1 離子傳導度(Ionic Conductivity) 71
3-5-2 電池充放電測試 71
3-5-3 交流阻抗分析儀(AC Impedance) 72
3-5-4 循環伏安法分析(CV) 74
第四章結果討論 75
4-1 膠體電解質導電度分析 76
4-1-1 小分子材料選擇 76
4-1-2 小分子比例選擇 80
4-2 膠體電解質聚合反應程度 82
4-3 膠體電解質熱穩定性分析 85
4-3-1 熱重TGA分析 85
4-3-2 熱差DSC分析 86
4-4 膠體電解質張力性質分析 87
4-5 膠體電解質電池電性分析 88
4-5-1 不同SCN比例變速率充放電 88
4-5-2 不同SCN比例長圈數循環 91
4-5-3 不同SCN比例介面電阻分析 96
4-5-4 不同SCN比例循環伏安法分析 98
4-5-5 不同SCN比例電極極化分析 100
4-6 複合電解質製程分析 102
4-6-1 LAGP品質分析 102
4-6-2 LAGP摻雜方法解析 104
4-6-3 XPS分析LAGP還原反應 106
4-7 複合電解質導電度分析 108
4-8 複合電解質內部結構分析 110
4-8-1 電解質XRD晶體分析 110
4-8-2 電解質SEM表面影像分析 111
4-9 複合電解質熱穩定性分析 113
4-10 複合電解質張力性質分析 114
4-11 複合電解質電池電性分析 115
4-11-1 不同LAGP比例介面電阻分析 115
4-11-2 不同LAGP比例變速率充放電 117
4-11-3 不同LAGP比例長圈數循環 120
4-11-4 不同LAGP比例電極極化分析 124
4-12 LATP複合電解質分析 126
4-12-2 不同LATP比例介面電阻分析 127
4-12-3 不同LATP比例變速率充放電 128
第五章結論與未來展望 130
參考文獻 134

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指導教授

諸柏仁

審核日期

2023-7-25

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