臺灣博碩士論文加值系統

本研究為了探討對鋰離子電池陰極材料信行改質所造成之影響，使用化學氣相沉積法（CVD）一步驟合成奈米碳管/石墨烯複合材料於泡沫鎳基材表面。為了提升電極材料的電化學性質，依序使用了電漿化學氣相沉積法（RECVD）與電沉積等方式對陰極材料進行改質。電漿化學氣象沉積法為使用氮電漿轟擊碳材以達到氮摻雜改質之目的。接著使用恆電流陰極電沉積將鐵與鎳的氫氧化物披覆於電極材料上，並改變電沉積的電流密度與時間等以尋找最佳之改質參數；再將樣品至於氬氣環境中進行熱處理，使氫氧化物轉變為氧化鐵/氧化鎳混合物，最終製得有/無氮摻雜之奈米碳管/石墨烯/氧化鐵/氧化鎳複合電極材料。之後就由拉曼光譜分析（Raman）與X-射線電子光譜（XPS）檢測樣品之元素與鍵結結構。為了瞭解樣品之電化學性質，將複合電極材料（正極）與鋰箔（負極）組成鋰離子半電池，進行循環充放電、循環伏安法（CV）、倍率性能測試與電化學阻抗測試（EIS），再輔以掃描式電子顯微鏡（SEM）與原子力顯微鏡（AFM），進一步的了解複合電極材料之電化學性質。最終在未氮摻雜、電沉積參數為電流密度1 mA沉積時間450秒下製倍之複合電極材料有較佳之電化學性質，其第2圈與第20圈之放電電容量分別為514.05與523.95 mAh/g。

In this study, in order to investigate the influence of the modification of the cathode material of lithium-ion batteries, a carbon nanotube/graphene composite material was synthesized on the surface of the nickel foam substrate by chemical vapor deposition (CVD) in one step. In order to improve the electrochemical properties of the electrode material, the cathode material was modified by plasma chemical vapor deposition (RECVD) and electrodeposition in sequence. The plasma chemical vapor deposition method uses nitrogen plasma to bombard carbon materials to achieve the purpose of nitrogen doping modification. Then use constant current cathodic electrodeposition to coat iron and nickel hydroxide on the electrode material, and change the current density and time of electrodeposition to find the best modification parameters; then place the sample in an argon atmosphere Heat treatment to convert the hydroxide into a mixture of iron oxide/nickel oxide, and finally obtain a composite electrode material of carbon nanotubes/graphene/iron oxide/nickel oxide with or without nitrogen doping. Afterwards, the elements and bonding structures of the samples were detected by Raman spectroscopy (Raman) and X-ray electron spectroscopy (XPS). In order to understand the electrochemical properties of the samples, the composite electrode material (positive electrode) and lithium foil (negative electrode) were used to form a lithium-ion half-cell, which was subjected to cycle charge and discharge, cyclic voltammetry (CV), rate performance test and electrochemical impedance test (EIS ), supplemented by scanning electron microscopy (SEM) and atomic force microscopy (AFM), to further understand the electrochemical properties of composite electrode materials. Finally, the composite electrode material prepared under the conditions of no nitrogen doping and electrodeposition parameters of current density 1 mA deposition time 450 seconds has better electrochemical properties, and the discharge capacity of the second cycle and the 20th cycle are 514.05 and 523.95 mAh/g respectively.

摘要 i
ABSTRACT ii
目錄 iii
表目錄 v
圖目錄 vi
第一章 緒論 1
1.1 前言 1
1.2研究方向與目標 4
第二章 文獻回顧及理論 6
2.1 鋰二次電池 6
2.2 鋰電池的發展與原理 7
2.3鋰鈷氧化物的簡介 8
2.4奈米碳管的簡介： 9
2.4.1奈米碳管之性質： 10
2.4.2奈米碳管的製備方法： 10
2.5 石墨烯的簡介 14
2.5.1石墨烯的性質 15
2.5.2石墨烯的製備： 16
2.6 氮摻雜碳材介紹 18
2.6.1氮摻雜材料在鋰離子電池的應用 19
2.7電漿化學氣相沉積的介紹 20
2.8金屬氧化物用於鋰離子電池之文獻探討 21
2.8.1金屬氧化物之文獻探討 21
2.8.2氧化鐵、氧化鎳/炭材複合材料作為鋰離子電池電極之文獻回顧 24
2.9 金屬氧化物的製備與文獻 27
2.9.1 氧化鐵、氧化鎳電沉積之文獻探討 28
第三章 實驗 30
3.1實驗流程圖 30
3.2實驗藥品、設備與分析儀器 31
3.2.1實驗藥品 31
3.2.2實驗設備 31
3.2.3 實驗檢測儀器 32
3.3實驗步驟 33
3.3.1 基材前處理 33
3.3.2 CVD 成長奈米碳管/石墨烯複合材料 33
3.3.3 氮電漿改質奈米碳管/石墨烯複合材料 33
3.3.4 氧化鐵/氧化鎳修飾奈米碳管/石墨烯複合材料 34
3.4鋰電池組裝 34
第四章 結果與討論 37
4.1氮摻雜奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料元素分析 37
4.1.1氮摻雜奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料Raman光譜分析 37
4.1.2 氮摻雜奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料XPS分析 40
4.2 有/無氮摻雜奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料電化學分析 41
4.2.1奈米碳管/石墨烯複合材料之電化學分析 41
4.2.2有/無氮摻雜奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之充放電分析 44
4.2.3奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之循環伏安法測試 50
4.2.4奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之倍率性能測試 51
4.2.5奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之交流阻抗測試 52
4.3奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之表面形貌分析 54
4.3.1奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之SEM測試 54
4.3.2奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之AFM測試 60
4.4奈米碳管/石墨烯/氧化鐵/氧化鎳複合材料之全電池測試 64
第五章 結論 66
參考文獻 67

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