以Ni摻雜Mn3O4修飾管狀有序中孔洞碳材CMK-5於高能鋰離子電池負極材料之應用及複合式有機無機固(膠)態高分子電解質之結構鑑定與電化學特性研究

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曾昱豪(Yu-Hao Zeng) 查詢紙本館藏

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論文名稱

以Ni摻雜Mn3O4修飾管狀有序中孔洞碳材CMK-5於高能鋰離子電池負極材料之應用及複合式有機無機固(膠)態高分子電解質之結構鑑定與電化學特性研究

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至系統瀏覽論文 (2024-6-30以後開放)

摘要(中)

本論文分為兩部分，第一部分主要是利用摻雜Ni的過渡金屬氧化物Mn3O4修飾於管狀有序中孔洞碳材CMK-5，以含浸法合成出Ni摻雜Mn3O4@CMK-5奈米複合材料，並應用於鋰離子電極的負極。Mn3O4的理論電容高達937 mAh/g，其含量豐富且毒性低，但具有過渡金屬氧化物充放電後體積變化大的缺點，利用中孔洞碳材CMK-5的有序孔道能有效抑制其體積膨脹及提升導電度，並摻入Ni作為晶格膨脹的緩衝劑，避免顆粒聚集情況的發生．藉此提升其電性表現，在電流密度100 mA/g下進行電性測試，經過50圈循環後，能得到高達1263 mAh/g的優異電容量表現。
第二部分是複合式有機無機高分子電解質的合成，根據使用需求製成固態和膠態兩種型態，並應用於鋰離子電池的電解質。製備過程是以4,4′-Methylene diphenyl diisocyanate (MDI)作為交聯劑，與Jeffamine ED2003形成線性前驅物，並導入無機矽源GLYMO及MPEOPS進行聚合水解，合成出導電度優異的高分子電解質薄膜，其中固態電解質於30 °C下離子導電度達1.11 × 10-4 S cm-1，膠態電解質於30 °C下則高達1.86 × 10-3 S cm-1，後續組裝成硬幣型電池進行電性測試，顯示本研究之膠態電解質的循環表現優於市售隔離膜。

摘要(英)

Transition metal oxides as anode materials in lithium ion batteries have attracted immense attention in recent years due to their high theoretical capacities as compared with commercial graphite. However, the huge volume change during the charge-discharge process leads to unstable electrochemical performances. In first part, we design a nanocomposite of Ni-doped Mn3O4@CMK-5 to solve the problem. Mn3O4 has high theoretical capacity (937 mAh/g), natural abundance and low toxicity. Ordered mesoporous carbon CMK-5 has nanoscale uniform mesopore, large surface area and good conducting network for both Li ions and electrons. Nickel doping could avoid the drastic volume change and aggregation of nanoparticles. Ni-doped Mn3O4@CMK-5 display a high reversible capacity up to 1263 mAh/g enen after 50 cycles at a current density of 100 mAh/g. The Ni-doped Mn3O4@CMK-5 nanocomposite is expected to be a promising anode material for lithium-ion batteries.
In second part, we design a new hybrid organic-inorganic polymer electrolyte, base on 4,4′-Methylene diphenyl diisocyanate (MDI), Jeffamine ED2003, and silica sources like GLYMO and MPEOPS. The solid polymer electrolyte(SPE) was measured the ion conductivity value of 1.11 × 10-4 S cm-1 at 30 °C. A maximum ion conductivity value of 1.86 × 10-3 S cm-1 is achieved for the gel polymer electrolytes(GPE) immersed in liquid electrolyte solution. And as the gel electrolyte, the test cell shows good cycling performance. The new hybrid polymer system hold promise for application in lithium ion batteries.

關鍵字(中)

★ 中孔洞碳材
★ 四氧化三錳
★ 鋰離子電池
★ 高分子電解質

關鍵字(英)

論文目次

中文摘要 i
Abstract ii
謝誌 iii
目錄 v
圖目錄 ix
表目錄 xv
第一章緒論 1
1-1 前言 1
1-2 蓄電池 2
1-3 鋰離子電池 4
1-4 研究目的 7
第二章文獻回顧 10
2-1 中孔洞碳材 10
2-1-1 奈米模鑄法( Nanocasting )之機制 12
2-1-2 奈米模鑄法合成中孔洞碳材之發展 14
2-2 負極材料 20
2-2-1 碳材 20
2-2-2 非碳材 23
2-2-3 碳材-非碳材複合材料 24
2-2-3-1 鎳摻雜四氧化三錳修飾碳材的負極材料 26
2-3 高分子電解質 31
2-3-1 固態高分子電解質 33
2-3-2 膠態高分子電解質 41
2-3-3 鋰離子鹽類 47
2-3-4 有機矽高分子 52
第三章實驗方法 53
3-1 藥品 53
3-2 負極材料製備 57
3-2-1 二維六角柱狀p6mm中孔洞矽材SBA-15合成 57
3-2-2 二維結構p6mm中孔洞管狀碳材CMK-5合成 57
3-2-3 含浸法合成Mn3O4@CMK-5負極材料 58
3-2-4 含浸法合成Ni摻雜Mn3O4@CMK-5負極材料 58
3-3 高分子電解質製備 59
3-3-1 固態高分子電解質製備 59
3-3-2 膠態高分子電解質製備 61
3-4 材料電化學測試 62
3-4-1 負極極片製作 62
3-4-2 硬幣型電池組裝 62
3-4-3 電池性能測試方法 64
3-4-3-1 定(變)電流充放電循環測試 64
3-4-3-2 循環伏安法(CV) 64
3-4-3-3 電化學阻抗分析(EIS) 64
3-5 實驗鑑定儀器 65
3-6 鑑定儀器之原理 67
3-6-1 同步輻射光束線 67
3-6-2 X射線粉末繞射(XRD) 70
3-6-3 氮氣等溫吸脫附曲線、表面積與孔洞性質鑑定 71
3-6-4 熱重分析儀(TGA) 75
3-6-5 穿透式電子顯微鏡(TEM) 76
3-6-6 掃描式電子顯微鏡(SEM) 78
3-6-7 示差掃描量熱儀(DSC) 79
3-6-8 傅立葉紅外線光譜儀(FTIR) 80
3-6-9 交流阻抗分析儀(AC-Impedance) 82
3-6-10 固態核磁共振儀(SSNMR) 83
3-6-11 線性掃描伏安法(LSV) 88
第四章結果與討論 89
4-1 含浸法合成Ni摻雜Mn3O4@CMK-5負極材料 89
4-1-1 小角度X光繞射圖譜分析 89
4-1-2 大角度X光繞射圖譜分析 91
4-1-3 氮氣吸脫附結果分析 93
4-1-4 熱重分析 96
4-1-5 ICP-MS結果分析 98
4-1-6 SEM結果分析 99
4-1-7 TEM結果分析 102
4-1-8 XPS結果分析 112
4-1-9 拉曼光譜分析 114
4-1-10 電性分析 116
4-1-11 循環伏安法分析 124
4-1-12 交流阻抗分析 127
4-1-13 充放電後的SEM結果分析 132
4-2 固(膠)態高分子電解質EDMGM-X 134
4-2-1 熱重分析 134
4-2-2 示差掃描量熱儀分析 136
4-2-3 紅外線吸收光譜分析 139
4-2-4 SEM表面分析 143
4-2-5 交流阻抗儀之離子導電度分析 147
4-2-6 固態核磁共振光譜儀分析 149
4-2-6-1 13C CP/MAS NMR 150
4-2-6-2 29Si CP/MAS NMR 152
4-2-6-3 7Li 譜寬分析 154
4-2-6-4 7Li & 7Li-{1H} MAS NMR 160
4-2-7 線性掃描伏安法 163
4-2-8 膠態高分子電解質吸附之澎潤比測試 165
4-2-9 膠態高分子電解質之離子導電度測試 168
4-2-10 膠態高分子電解質之線性掃描伏安法分析 171
4-2-11 電池性能測試 172
第五章結論 174
參考文獻 176

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指導教授

高憲明(Hsien-Ming Kao)

審核日期

2019-7-23

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