以Fe3O4修飾管狀有序中孔洞碳材CMK-9及Cu摻雜SnO2中孔洞碳氮材於高能鋰離子電池負極材料之應用

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賴沅鋐(Yuan-Hung Lai) 查詢紙本館藏

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化學學系

論文名稱

以Fe3O4修飾管狀有序中孔洞碳材CMK-9及Cu摻雜SnO2中孔洞碳氮材於高能鋰離子電池負極材料之應用
(Fe3O4 nanoparticles confined in mesoporous carbon CMK-9 and Cu doped SnO2 in mesoporous carbonitride MUFC as efficient nanocomposite anode for lithium ion batteries with improved electrochemical performance)

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摘要(中)

本論文分為兩部分，第一部分為過渡金屬氧化物Fe3O4修飾於管狀有序中孔洞碳材CMK-9，以含浸法合成出Fe3O4@CMK-9奈米複合材料，並應用於鋰離子電極的負極。Fe3O4的理論電容高達925 mAh/g，其自然資源含量豐富且成本低，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-9的有序孔道能有效抑制其體積膨脹及提升導電度，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1117 mAh/g的優異電容量表現。
第二部分為通過奈米模鑄法(Nanocasting)合成出中孔洞碳氮材料（MUFC），利用摻雜Cu的過渡金屬氧化物SnO2中孔洞碳氮材，以含浸法合成出Cu摻雜SnO2@MUFC奈米複合材料，藉由MUFC上不僅可以利用有缺陷的CN位點和氮間隙，可以很均勻分散二氧化錫金屬顆粒，且由於其具有鹼性的含氮位點可有效促進鋰離子的傳遞，並摻入Cu作為晶格膨脹的緩衝劑，必免顆粒聚集的情況發生，藉此提升其電性的表現，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1064 mAh/g的優異電容量表現。

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 tubular nanocomposite of Fe3O4@CMK-9 to solve the problem. A three-dimensional (3-D) hollow-type ordered mesoporous carbon (CMK-9) could not only provide enough space during the Li+ insertion-extraction process, but also increase the electrical conductivity. Ordered mesoporous carbon CMK-9 has nanoscale uniform mesopore, large surface area and good conducting network for both Li ions and electrons. Fe3O4 has high theoretical capacity (925 mAh/g), natural abundance and low in cost. Fe3O4@CMK-9 display a high reversible capacity of 1117 mAh/g after 50 cycles at a current density of 100 mAh/g with an outstanding rate performance. The Fe3O4@CMK-9 nanocomposite is expected to have high specific capacity and good cycling performance.
In second part, we synthesize nitrogen–rich carbon materials with hierarchical porosity were obtained by pyrolyzing melamine-urea- formaldehyde mesoporous carbonitride materials (MUFC). The MUFC nanocomposite can not only use the defective CN sites and nitrogen gaps on the MUFC, but also can disperse tin oxide metal particles very uniformly. And then MUFC has alkaline nitrogen sites, it can effectively promote the transfer of lithium ions. Copper doping SnO2 could avoid the drastic volume change and aggregation of nanoparticles. Cu-doped SnO2@MUFC display a high reversible capacity of 1064 mAh/g after 50 cycles at a current density of 100 mAh/g with an outstanding rate performance.

關鍵字(中)

★ 中孔洞
★ 鋰離子電池
★ 四氧化三鐵
★ 中孔洞碳氮材
★ 二氧化錫
★ 銅摻雜二氧化錫

關鍵字(英)

論文目次

目錄
中文摘要 i
Abstract ii
謝誌 iv
目錄 vi
圖目錄 x
表目錄 xvi
第一章緒論 1
1-1 前言 1
1-2 二次電池 2
1-3 鋰離子電池 4
1-4 研究目的 7
第二章文獻回顧 9
2-1 有序中孔洞碳材 9
2-1-1 奈米模鑄法( Nanocasting )合成機制 12
2-1-2 奈米模鑄法合成中孔洞碳材之發展 14
2-1-3奈米模鑄法合成有序中孔洞碳氮材之發展 20
2-2 負極材料 27
2-2-1 碳材 27
2-2-2 非碳材 31
2-2-3 碳材-非碳材複合材料 32
2-2-3-1 四氧化三鐵修飾碳材的負極材料 34
2-2-3-2 銅摻雜二氧化錫修飾碳氮材的負極材料 36
第三章實驗方法 38
3-1 藥品 38
3-2 奈米模鑄法合成三維孔道結構 (Ia3d)中孔洞碳材 41
3-2-1 三維六角柱狀p6mm中孔洞矽材KIT-6合成 41
3-2-2 三維立方Ia3d中孔洞管狀碳材CMK-9合成 41
3-2-3 含浸法合成Fe3O4@CMK-9負極材料 42
3-3 奈米模鑄法合成中孔洞碳氮材MUFC 42
3-3-1 含浸法合成SnO2@MUFC負極複合材料 43
3-3-2 含浸法合成Cu摻雜SnO2@MUFC負極合材料 44
3-4 材料電化學測試 45
3-4-1 負極極片製作 45
3-4-2 硬幣型電池組裝 45
3-4-3 電池性能測試方法 47
3-4-3-1 定(變)電流充放電循環測試 47
3-4-3-2 循環伏安法(CV) 47
3-4-3-3 電化學阻抗分析(EIS) 47
3-5 實驗鑑定儀器 48
3-6 鑑定儀器之原理 49
3-6-1 同步輻射光束線 49
3-6-2 X射線粉末繞射(XRD) 52
3-6-3 氮氣等溫吸脫附曲線、表面積與孔洞性質鑑定 53
3-6-4 熱重分析儀(TGA) 57
3-6-5 穿透式電子顯微鏡(TEM) 58
3-6-6 掃描式電子顯微鏡(SEM) 60
3-6-7 交流阻抗分析儀(AC-Impedance) 61
3-6-8 循環伏安法(Cyclic Voltammetry, CV) 62
第四章結果與討論 63
4-1 含浸法合成Fe3O4@CMK-9負極材料 63
4-1-1 小角度X光繞射圖譜分析 63
4-1-2 大角度X光繞射圖譜分析 65
4-1-3 氮氣吸脫附結果分析 67
4-1-4 熱重分析 70
4-1-5 ICP-MS結果分析 72
4-1-6 SEM結果分析 73
4-1-7 TEM結果分析 75
4-1-8 XPS結果分析 82
4-1-9 拉曼光譜分析 84
4-1-10 電性分析 86
4-1-11 循環伏安法分析 91
4-1-12 交流阻抗分析 93
4-1-13 充放電後的SEM結果分析 98
4-2 含浸法合成Cu摻雜SnO2@MUFC負極複合材料 100
4-2-1小角度X光繞射圖譜分析(SAXRD) 100
4-2-2 大角度X光繞射圖譜分析 102
4-2-3 氮氣吸脫附結果分析 104
4-2-4 熱重分析 108
4-2-5 ICP-MS及EA元素分析結果 110
4-2-6 SEM結果分析 112
4-2-7 TEM結果分析 115
4-2-8 XPS結果分析 125
4-2-9 拉曼光譜分析 127
4-2-10 電性分析 129
4-2-11 循環伏安法分析 137
4-2-12 交流阻抗分析 140
4-2-13 充放電後的SEM結果分析 145
第五章結論 147
參考文獻 149

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指導教授

高憲明(Hsien-Ming Kao)

審核日期

2020-7-28

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