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研究生:邱則明
研究生(外文):Tse-Ming Chiu
論文名稱:石墨烯承載金屬/金屬氧化物複合材料於鋰離子電池陽極之應用
論文名稱(外文):Synthesis of Graphene Supported MOx/C Nanocomposite as an Anode Material for Lithium ion Nattery
指導教授:黃炳照黃炳照引用關係蕭敬業
指導教授(外文):Bing-Joe HwangChing-Yeh Shiau
口試委員:黃炳照蕭敬業
口試日期:2012-07-25
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:化學工程系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2012
畢業學年度:100
語文別:中文
論文頁數:218
中文關鍵詞:石墨烯金屬氧化物鋰離子二次電池陽極
外文關鍵詞:graphenemetal oxidelithium ion secondary batteryanode
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本研究發展以Top-down之合成策略,直接以微米級金屬為前驅物,佐以葡萄糖與氧化石墨烯分散液,成功以水熱法製作出奈米級Graphene@MOx/C (M=Sn、Mn)複合材料。石墨烯材料的導入提升了碳多醣(Carbonaceous polysaccharide,CPS)複合材料之導電度,更可以藉此改善合金材料之循環壽命與質傳阻抗。Graphene@SnO2/C 複合材料在200次循環後達到427mAh/g之電容量。於錳金屬應用之方面,吾人利用相同的水熱操作條件,合成出具8至10 nm晶粒大小Graphene@MnCO3/C 複合材料。於400oC熱處理後成功將其轉變為具電化學活性之Graphene@Mn3O4/C複合材料。在鋰離子二次電池之應用上具有438mAh/g之電容量,首圈庫倫效率約達到50%,成功將葡萄糖氧化法延展至第二金屬系統。
In this work Graphene @ MOx/C (M=Sn、Mn) composite was synthesized through a top-down strategy. In the synthesis procedure, micro-sized metal powder, glucose and 1wt% graphene oxide suspension was directly employed as the precursor. Under hydrothermal reaction conditions, micro-sized metal powders were broken down in to nano-sized, highly dispersed particles. The participation of graphene in this composite increase the electronic conductivity of carbonaceous polysaccharide based hybrid materials and is proven to be beneficial to the capacity retention and also the diffusion resistance. More than 427 mAh/g of reversible capacity is achieved with Graphene @ SnO2/C composite-based half cell at a current density of 200mA/g up to the 200th cycle.
A manganese-based graphene @ MnCO3/C synthesized following the same procedure was also performed. In this case, micro-sized manganese metal was transformed into 8-10 nm sized Manganese carbonate. After 400oC heat treatment, a new kind of electrochemically active compound grapheme @ Mn3O4/C was formed. Cycling under the current density of 200 mA/g a capacity of 438mAh/g was reached up to the 30th cycle.
摘要 I
Abstract II
誌謝 III
目錄 IV
圖目錄 VII
表目錄 XIII
第1章 緒論 1
1.1. 前言 1
1.2. 鋰離子電池的演進與發展 2
1.3. 鋰離子二次電池之組成與機制 5
1.4. 鋰離子二次電池之各元件介紹 7
1.4.1. 正極 (陰極) 7
1.4.2. 負極 (陽極) 13
1.4.3. 電解液 16
1.4.4. 隔離膜與固態電解質 20
1.5. 負極材料發展的趨勢 24
1.5.1. 鋰金屬 25
1.5.2. 碳材 26
1.5.3. 合金材料 30
1.5.4. 過渡金屬氧化物 35
1.6. 負極材料的展望 37
第2章 文獻回顧 40
2.1. 錫複合材料 40
2.1.1. 錫合金類 40
2.1.2. 碳錫復合材料 42
2.2. 氧化錳複合材料 49
2.3. 石墨烯 50
2.3.1. 石墨烯之特點 50
2.3.2. 石墨烯合成 52
2.4. 石墨烯複合材料 54
2.5. 研究動機與目的 58
第3章 實驗 60
3.1. 儀器設備 60
3.2. 實驗藥品 62
3.3. 實驗步驟 63
3.3.1. 氧化石墨烯合成 63
3.3.2. 陽極材料合成 64
3.3.3. 陽極極片之製備 67
3.3.4. 鈕扣型電池組裝 67
3.4. 材料鑑定與分析 69
3.4.1. XRD粉末繞射分析 69
3.4.2. 掃描式電子顯微鏡表面形態分析(SEM) 70
3.4.3. X光能量色散圖譜分析(EDS) 70
3.4.4. 穿透式電子顯微鏡(TEM) 71
3.4.5. TGA分析 71
3.5. 材料電化學特性測試 72
3.5.1. 電化學效能測試 72
3.5.2. 循環伏安分析 72
3.5.3. 交流阻抗分析 72
第4章 結果與討論 75
4.1. 氧化石墨烯的添加 75
4.1.1. Graphene @ SnO2/C XRD分析 76
4.1.2. Graphene @ SnO2/C SEM分析 79
4.1.3. Graphene @ SnO2/C TEM分析 82
4.1.4. Graphene @ SnO2/C TGA分析 84
4.1.5. 電化學分析 86
4.2. 不同還原程度和成Graphene@SnOx/C材料分析 92
4.2.1. Graphene @ SnOx/C XRD分析 93
4.2.2. Graphene @ SnOx/C SEM分析 96
4.2.3. Graphene @ SnOx/C TEM分析 102
4.2.4. Graphene @ SnOx/C TGA分析 107
4.2.5. 電化學分析 109
4.3. 錫金屬/石墨烯含量之提升 120
4.3.1. Graphene @ Sn/C XRD分析 120
4.3.2. Graphene @ Sn/C SEM分析 124
4.3.3. Graphene @ Sn/C TEM分析 129
4.3.4. Graphene @ Sn/C TGA分析 132
4.3.5. 電化學分析 134
4.4. 銅沉積改質Graphene @SnxCu1-x/C材料分析 137
4.4.1. Graphene @SnxCu1-x/C XRD分析 138
4.4.2. Graphene @SnxCu1-x/C SEM分析 141
4.4.3. Graphene @SnxCu1-x/C TEM分析 150
4.4.4. Graphene @SnxCu1-x/C STEM分析 155
4.4.5. Graphene @SnxCu1-x/C TGA分析 159
4.4.6. 電化學分析 161
4.5. Graphene @ Mn3O4/C 複合材料 170
4.5.1. Graphene @ Mn3O4/C XRD分析 170
4.5.2. Graphene @ Mn3O4/C SEM分析 174
4.5.3. Graphene @ Mn3O4/C TGA分析 177
4.5.4. 電化學分析 178
4.6. 綜合討論 180
第5章 結論 186
未來展望 188
參考文獻 189
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