有機金屬骨架衍生之氮摻雜碳修飾硫化錳硫化鋅複合材及硫化銅硫化鎳複合材作為鋰(鈉)離子電池負極材料之應用

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論文名稱

有機金屬骨架衍生之氮摻雜碳修飾硫化錳硫化鋅複合材及硫化銅硫化鎳複合材作為鋰(鈉)離子電池負極材料之應用

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至系統瀏覽論文 (2028-6-30以後開放)

摘要(中)

本論文分為兩部分，第一部分將硝酸錳作為金屬離子前驅物，1,3,5-苯三甲
酸作為有機配位基，加入添加劑聚乙烯吡咯烷酮，製備成有機金屬骨架前驅物
MnBTC，並探討最佳鍛燒硫化溫度，接著將硝酸錳和硝酸鋅作為金屬離子前驅
物，製備成雙金屬有機金屬骨架前驅物 Mn/ZnBTC，並經過 700 ℃鍛燒硫化得
到氮摻雜碳修飾硫化錳硫化鋅複合材(Mn,Zn)S/N-C，應用於鋰、鈉離子電池負極
材料，其中(Mn,Zn)S/N-C (1-1)具有最好的電化學表現，組裝鋰離子電池半電池
在電流密度 0.1 A/g 下循環 100 圈有 1003 mAh/g 的比容量，組裝成鈉離子電池
半電池在電流密度 0.05 A/g 下循環 100 圈有 288.6 mAh/g 的比容量，和正極材料
磷酸鐵鋰組成全電池的實際應用在 0.1 C 下充放電 100 圈有 40.6 mAh/g 的可逆
比容量且庫倫效率高達 95.7 %。
第二部分以第一部分的有機配位基為基礎，金屬離子前驅物使用硝酸銅和
硝酸鎳合成有機金屬骨架前驅物 Cu/NiBTC，經過 500 ℃鍛燒硫化後得到硫化銅
硫化鎳複合材，不同鎳加量的複合材作為鋰離子電池負極材料進行循環穩定性
測試可以發現複合材有鎳的情況下，相比於硫化銅複合材，雙金屬的複合材的比
容量、維持率和鋰離子擴散係數會提升，在半電池充放電測試中 Cu1.96S/Ni3S2-50
具有最好的循環穩定性，電流密度 1 A/g 下循環 250 圈有 167 mAh/g 的比容量，
而 0.1 A/g 下循環 100 圈有 385.5 mAh/g 的比容量。

摘要(英)

Metal organic framework (MOFs) have been considered to be the ideal
precursor for metal oxides, metal sulfides, metal selenides or carbon materials which
can be used for anode of lithium and sodium ion batteries. In this work, use the metal
organic framework based on manganese ion, and get manganese sulfide MnS by
sulfurization, the best sulfurization temperature is 700 ℃. After finding the best
sulfurization temperatue, then synthesis manganese and zinc bimetallic metal organic
framework Mn/ZnBTC be the precursor and get the manganese and zinc sulfides
decorated with nitrogen-doped carbon by sulfurization named (Mn,Zn)S/N-C. Then
find the ratio of manganese and zinc which has the best electrochemical performance
for anode material. Finally, (Mn,Zn)S/N-C(1-1) exhibits the most great
electrochemical performance in half-cell lithium ion batteries, it shows specific
capacity of 1003 mAh/g after 100 cycles at a current density 0.1 A/g. And in half-cell
sodium ion battery, it demonstrates a specific capacitance of 266.8 mAh/g after 100
cycles at a current density of 0.05 A/g. In a full-cell configuration with lithium iron
phosphate, it exhibits a reversible capacity of 40.5 mAh/g and a coulombic efficiency
of approximately 95% after 100 cycles at 0.1 C.
The second part is based on the same ligand from the first part. Copper nitrate
and nickel nitrate are used as metal ion precursors to replace the manganese and zinc
ions and synthesize organic metal framework precursors Cu/NiBTC. After
sulfurization, copper sulfide and nickel sulfide composite materials are obtained. Then
test the relation of electrochemical performance and nickel amount. It is observed that
composites with nickel content, specific capacity of those composites can higher than
copper sulfide. Among them, Cu1.96S/Ni3S2-50 exhibits the best cyclic stability, with a
specific capacity of 385.5 mAh/g after 100 cycles at a current density 0.1 A/g. And
also exhibits the highest lithium ion diffusion coefficient.

關鍵字(中)

★ 有機金屬骨架
★ 鋰離子電池
★ 過渡金屬硫化物

關鍵字(英)

★ Metal Organic Framework
★ Lithium Ion Battery
★ Transition Metal Sulfide

論文目次

目錄
第一章緒論 ................................................................................................................. 1
1-1 鋰離子電池 ......................................................................................................... 1
1-1-1 鋰離子電池簡介 ......................................................................................... 1
1-1-2 鋰離子電池正極材料 ................................................................................. 2
1-1-3 鋰離子電池負極材料 ................................................................................. 4
1-2 鈉離子電池 ......................................................................................................... 6
1-2-1 鈉離子電池簡介 ......................................................................................... 6
1-2-2 鈉離子電池正極材料 ................................................................................. 8
1-2-3 鈉離子電池負極材料 ............................................................................... 10
1-3 固態電解質界面 ............................................................................................... 12
1-3-1 固態電解質界面的形成 ........................................................................... 12
1-3-2 固態電解質界面的組成 ........................................................................... 13
1-4 過渡金屬硫化物 ............................................................................................... 13
1-4-1 過渡金屬硫化物製備方式 ....................................................................... 14
1-4-2 在鋰、鈉離子電池負極的應用 ............................................................... 17
1-4-3 雙金屬過渡金屬硫化物複合材應用於負極材料 ................................... 21
1-5 有機金屬骨架 ................................................................................................... 23
1-5-1 有機金屬骨架形成 ................................................................................... 23
1-5-2 有機金屬骨架結構控制 ........................................................................... 26
1-5-3 有機金屬骨架衍生物應用於負極材料 ................................................... 30
1-6 研究動機 ........................................................................................................... 38
第二章實驗步驟與儀器 ........................................................................................... 39
2-1 實驗藥品 ........................................................................................................... 39
2-2 實驗步驟 ........................................................................................................... 40
2-2-1 錳鋅有機金屬骨架合成(Mn/Zn-BTC) .................................................... 41
2-2-2 製備有機金屬骨架衍生之複合材(Mn,Zn)S/N-C ................................... 41
2-2-3 有機金屬骨架合成(Cu/Ni-BTC) .............................................................. 42
2-2-4 製備有機金屬骨架衍生之複合材 Cu1.96S/Ni3S2 ..................................... 43
2-3 電極製備及電化學測試方法 ........................................................................... 44
2-3-1 負極極片製作 ........................................................................................... 44
2-3-2 正極極片製作 ........................................................................................... 44
2-3-3 硬幣型 2032 型電池組裝 ......................................................................... 44
2-3-4 定(變)電流充放電循環穩定性測試 ....................................................... 45
2-3-5 循環伏安法(CV) ....................................................................................... 46
2-3-6 電化學阻抗分析(EIS) ............................................................................... 46
2-4 實驗鑑定儀器 ................................................................................................... 47
2-5 材料鑑定儀器之原理 ....................................................................................... 48
2-5-1 X 射線粉末繞射(XRD) ............................................................................. 48
2-5-2 掃描式電子顯微鏡(SEM) ........................................................................ 49
2-5-3 穿透式電子顯微鏡(TEM) ........................................................................ 50
2-5-4 熱重分析儀(TGA) ..................................................................................... 50
2-5-5 感應耦合電漿質譜儀(ICP-MS) ............................................................... 51
2-5-6 X 射線光電子能譜儀(XPS) ...................................................................... 52
2-5-7 電化學阻抗譜(EIS) ................................................................................... 56
2-5-8 循環伏安法(CV) ....................................................................................... 57
第三章結果與討論 ................................................................................................... 60
3-1 材料鑑定 ........................................................................................................... 60
3-1-1 大角度 X 光繞射分析(PXRD) ................................................................. 60
3-1-2 掃描式電子顯微鏡(SEM)形貌鑑定 ........................................................ 62
3-1-3 穿透式電子顯微鏡(TEM)結果分析 ........................................................ 69
3-1-4 氮氣吸脫附結果分析(BET) ..................................................................... 79
3-1-5 熱重分析(TGA) ......................................................................................... 86
3-1-6 感應電漿耦合質譜(ICP-MS)分析及元素分析(EA) ............................... 89
3-1-7 X 光電子能譜(XPS)分析 .......................................................................... 90
3-2 材料於鋰離子電池半電池之電化學測試 ...................................................... 96
3-2-1 循環伏安曲線及充放電曲線之分析 ....................................................... 96
3-2-2 循環穩定性及倍率性測試 ....................................................................... 99
3-2-3 交流阻抗分析 ......................................................................................... 105
3-2-4 電容貢獻度計算 ..................................................................................... 108
3-3 材料於鈉離子電池的電化學表現................................................................. 112
3-3-1 循環伏安曲線及充放電曲線之分析 ..................................................... 112
3-3-2 循環穩定性及倍率性測試 ..................................................................... 113
3-3-3 交流阻抗分析 ......................................................................................... 115
3-3-4 電容貢獻度計算 ..................................................................................... 116
3-4 實際應用及相關文獻比較 ............................................................................. 120
第四章結果與討論 ................................................................................................. 123
4-1 材料鑑定 ......................................................................................................... 123
4-1-1 大角度 X 光繞射分析(PXRD) ............................................................... 123
4-1-2 掃描式電子顯微鏡(SEM)結果分析 ...................................................... 124
4-1-3 穿透式電子顯微鏡(TEM)結果分析 ...................................................... 128
4-1-4 氮氣吸脫附結果分析(BET) ................................................................... 135
4-1-5 熱重分析(TGA) ....................................................................................... 139
4-1-6 感應電漿耦合質譜(ICP-MS)分析 ......................................................... 140
4-1-7 X 光電子能譜(XPS)分析 ........................................................................ 140
4-2 材料於鋰離子電池半電池之電化學測試 .................................................... 144
4-2-1 循環伏安曲線及充放電曲線之分析 ..................................................... 144
4-2-2 循環穩定性及倍率性測試 ..................................................................... 146
4-2-3 交流阻抗分析 ......................................................................................... 149
第五章結論 ............................................................................................................. 152
第六章參考文獻 ..................................................................................................... 154

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13562

指導教授

高憲明(Hsien-Ming Kao)

審核日期

2023-7-19

推文