以Mn3O4及有機金屬骨架衍生CoS2修飾南瓜衍生碳材作為鋰(鈉)離子電池負極材料之應用

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林昀築(Yun-Chu Lin) 查詢紙本館藏

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論文名稱

以Mn3O4及有機金屬骨架衍生CoS2修飾南瓜衍生碳材作為鋰(鈉)離子電池負極材料之應用

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至系統瀏覽論文 (2029-6-30以後開放)

摘要(中)

本論文分為兩部分，第一部分研究南瓜衍生碳材的碳化過程、KOH活化劑含量和活化鍛燒溫度，旨在找出最佳條件以得到南瓜衍生活化碳材PAC-4-6。隨後，利用含浸法將過渡金屬氧化物Mn3O4修飾於PAC-4-6，合成出Mn3O4@PAC-4-6複合材料，並探討其作為鋰（鈉）離子電池負極材料的應用。經XPS與TEM mapping分析顯示，PAC-4-6具有微量的氮、硫和氧元素，達到異原子自摻雜的效果。實驗結果顯示，Mn3O4(30)@PAC-4-6具有最佳的電化學表現，在鋰離子電池系統中以電流密度0.1 A/g進行充放電循環測試，經過70圈後能達到879.8 mAh/g優異電容量，另外在鈉離子系統中以電流密度0.05 A/g進行充放電循環測試，經過200圈後，電容量穩定保持在180.1 mAh/g，顯示此材料具有良好的電性表現。
第二部分的研究中，以ZIF-67作為前驅物，經H2/Ar混合氣體鍛燒處理後，Co2+被還原成Co奈米粒子，得到Co@C，再與親水性PAC-4-6混合進行硫化反應，最終合成出二硫化鈷修飾生質碳材CoS2@PAC-4-6，並應用於鋰離子電池的負極材料。添加PAC-4-6生質碳材不僅提升材料的導電性，且有效緩解了CoS2在循環過程中體積膨脹問題。在鋰離子電池系統中以電流密度0.1 A/g進行充放電循環測試，經過240圈後，達到710.3 mAh/g。這表明材料具有良好的循環穩定性。

摘要(英)

This thesis is divided into two parts. The first part investigates the carbonization process of pumpkin-derived carbon material, KOH activator content, and the activation calcination temperature, aiming to identify the optimal conditions to obtain the pumpkin-derived activated carbon material PAC-4-6. Mn3O4 is incorporated into PAC-4-6 using an impregnation method, synthesizing Mn3O4@PAC-4-6 composite material, which is evaluated as an anode material for lithium and sodium ion batteries. XPS and TEM mapping analyses show that PAC-4-6 contains trace amounts of nitrogen, sulfur, and oxygen, indicating heteroatom self-doping. Experimental results demonstrate that Mn3O4(30)@PAC-4-6 exhibits excellent electrochemical performance, achieving a capacity of 879.8 mAh/g after 70 cycles at 0.1 A/g in lithium-ion batteries, and maintaining a stable capacity of 180.1 mAh/g after 200 cycles at 0.05 A/g in sodium-ion batteries.
The second part uses ZIF-67 as a precursor, which is calcined in a H2/Ar mixed gas to reduce Co2+ to Co nanoparticles, forming Co@C. This is mixed with hydrophilic PAC-4-6 and subjected to a sulfidation reaction to synthesize CoS2@PAC-4-6, applied as an anode material for lithium-ion batteries. Adding PAC-4-6 enhances conductivity and mitigates volume expansion of CoS2 during cycling. The lithium-ion battery achieves a specific capacity of 710.3 mAh/g after 240 cycles at 0.1 A/g, indicating excellent cycling stability.

關鍵字(中)

★ 生質碳材
★ 有機金屬骨架材料
★ 鋰(鈉)離子電池
★ 過渡金屬材料

關鍵字(英)

論文目次

中文摘要 i
Abstract ii
謝誌 iii
目錄 v
圖目錄 xi
表目錄 xix
第一章緒論 1
1-1 前言 1
1-2 鋰離子電池 2
1-2-1 鋰離子電池正極材料 4
1-2-2 鋰離子電池負極材料 7
1-2-3 鋰離子電池之電解液 12
1-3 鈉離子電池 14
1-4 生質碳材 16
1-5生質碳材性能的改進策略 18
1-5-1 熱裂解法(Pyrolysis) 19
1-5-2 水熱法(Hydrothermal method) 20
1-5-3 活化法(Activation method) 20
1-5-4 模板法(Template method) 24
1-5-5 異原子摻雜(Heteroatoms doping) 25
1-5-6 負載過渡金屬化合物(Loading of transition metal compounds) 27
1-6 有機金屬骨架 29
1-6-1 有機金屬骨架形成 29
1-6-2 類沸石咪唑骨架材料 32
1-6-3 類沸石咪唑骨架材料-67 34
1-6-4 類沸石咪唑骨架材料-67衍生物應用於負極材料 38
1-7 研究動機 42
第二章實驗藥品與儀器原理 43
2-1 實驗藥品 43
2-2 第壹部分之負極材料製備 45
2-2-1 南瓜衍生碳材(Pumpkin-Derived Carbon, PC) 45
2-2-2 利用活化劑氫氧化鉀(KOH)活化南瓜衍生碳材 46
2-3-3 利用含浸法合成Mn3O4@PAC-4-6負極材料 48
2-3 第貳部分之負極材料製備 49
2-3-1 ZIF-67合成 49
2-3-2 製備有機金屬骨架衍生之複合材CoS2@PAC-4-6 49
2-4 電化學測試之材料製備 51
2-4-1 負極極片製作 51
2-4-2 正極極片製作 51
2-4-3 硬幣型2032型電池組裝 52
2-4-4 定(變)電流充放電循環穩定性測試 53
2-4-5 循環伏安法(CV) 54
2-4-6 電化學阻抗分析(EIS) 54
2-5 實驗鑑定儀器 55
2-6 材料鑑定儀器之原理 57
2-6-1 X射線粉末繞射(XRD) 57
2-6-2 拉曼光譜分析儀(Raman Spectroscopy) 58
2-6-3 氮氣等溫吸脫附曲線、表面積與孔洞性質鑑定(BET) 59
2-6-4 熱重分析儀(TGA) 64
2-6-5 掃描式電子顯微鏡(SEM) 64
2-6-6 穿透式電子顯微鏡(TEM) 65
2-6-7 X射線光電子能譜儀(XPS) 66
2-6-8 元素分析儀(EA) 67
2-6-9 感應耦合電漿質譜儀(ICP-MS) 68
2-6-10 電化學阻抗譜(EIS) 69
2-6-11 循環伏安法(Cyclic Voltammetry, CV) 71
第三章結果與討論 72
3-1 材料鑑定 72
3-1-1 大角度X光繞射分析(WXRD) 72
3-1-2 拉曼光譜分析(Raman) 75
3-1-3 氮氣吸脫附結果分析(BET) 78
3-1-4 熱重分析(TGA) 83
3-1-5 元素分析(EA)及感應電漿耦合質譜(ICP-MS)分析 84
3-1-6 X光電子能譜(XPS)分析 85
3-1-7 掃描式電子顯微鏡(SEM)形貌鑑定 88
3-1-8 穿透式電子顯微鏡(TEM)結果分析 94
3-2 材料於鋰離子電池半電池之電化學測試 101
3-2-1 循環伏安法(CV)分析 101
3-2-2 充放電曲線之分析 102
3-2-3 電性分析 104
3-2-4 交流阻抗分析 111
3-2-5 電容貢獻度計算 114
3-2-6 循環後的SEM和TEM圖 117
3-3材料於鈉離子電池半電池之電化學測試 120
3-3-1 循環伏安曲線及充放電曲線之分析 120
3-3-2 電性分析 121
3-3-3 交流阻抗分析 123
3-3-4 電容貢獻度計算 124
3-3-5 全電池分析 128
3-4 相關文獻比較 130
第四章結果與討論 131
4-1 材料鑑定 131
4-1-1 大角度X光繞射圖譜分析(WXRD) 131
4-1-2 拉曼光譜分析(Raman) 132
4-1-3 氮氣吸脫附結果分析(BET) 134
4-1-4 熱重分析(TGA) 137
4-1-5 元素分析(EA)分析 138
4-1-6 X光電子能譜(XPS)分析 139
4-1-7 掃描式電子顯微鏡(SEM)之結果分析 142
4-1-8 穿透式電子顯微鏡(TEM)之結果分析 144
4-2 材料之電化學測試 148
4-2-1 循環伏安法(CV)分析 148
4-2-2 充放電曲線之分析 149
4-2-3 電性分析 150
4-2-4 交流阻抗分析 154
4-2-5 電容貢獻度計算 156
第五章結論 160
參考文獻 162

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指導教授

高憲明(Hsien-Ming Kao)

審核日期

2024-7-11

推文