微波輔助水熱法合成中孔鎳鈷氧化物於非對稱超級電容器之應用

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研究生：	許湘禹
論文名稱：	微波輔助水熱法合成中孔鎳鈷氧化物於非對稱超級電容器之應用 Microwave-assisted hydrothermal synthesis of mesoporous nickel-cobalt oxides for the application of asymmetric supercapacitors
指導教授：	胡啟章
口試委員:	胡啟章溫惠玲張國興
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2012
畢業學年度：	100
語文別：	中文
論文頁數：	152
中文關鍵詞：	鎳鈷氧化物、超級電容器、微波輔助水熱、中孔、非對稱
相關次數：	點閱：1 下載：0
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此論文中，吾人利用微波輔助水熱法來製備鎳鈷氧化物，其研究內容主要為：
1.藉由前驅物溶液中添加錯合劑、改變氯化鎳/氯化鈷的比例，及微波輔助水熱持溫時間等變因調控，改變鎳鈷氧化物(NiCo2O4)奈米粒子的平均粒徑大小，並找出電容性質最佳之鎳鈷氧化物合成參數，作為後續實驗之固定條件。
2.利用添加非離子型界面活性劑F127合成出具蟲洞結構的鎳鈷氧化物，成功增加材料的比表面積與孔隙度，並提升鎳鈷氧化物的比電容量達480 F g-1。
3.導入工業界研究發展、提升品質時常使用的實驗設計法，找出影響鎳鈷氧化物比電容的主要因素為：界面活性劑濃度、微波反應溫度及熱處理溫度；並在最佳化實驗條件後，使鎳鈷氧化物比電容提升至588 F g-1，其後進一步研究循環伏安活化程序對鎳鈷氧化物材料晶相及孔洞微結構的影響。
4.利用鎳鈷氧化物與石墨烯碳材組裝成非對稱型超級電容器，此非對稱超級電容器在充放電電流密度及電池操作電位窗(cell voltage)為4.15 A g-1及0.2~1.6 V的條件下，比能量及功率密度可達22.34 Wh/kg、1.10 kW/kg，且能量效率高達87%。
材料分析上以X光繞射儀(X-ray Diffraction, XRD)分析鎳鈷氧化物的結晶結構以及結晶強度，掃描式電子顯微鏡(Scanning Electron Microscope, SEM)來觀察其表面型態，比表面積與孔徑分析儀 (Surface Area and Porosity Analyzer, BET) 來觀察其孔洞結構，循環伏安法(Cyclic Voltammetry, CV)、定電流計時電位測定法(Chronopotentiometry, CP)以檢測其電化學性質。

摘要…………………………………………………………………II
Abstract………………………………………………………………III
圖目錄…………………………………………………………………XI
表目錄………………………………………………………………XVI
第一章 緒論……………………………………………………………1
1-1 電化學原理…………………………………………………………1
1-1-1 電化學反應系統…………………………………………………1
1-1-2 影響電化學系統之因素…………………………………………2
1-2 電極材料……………………………………………………………3
1-3 金屬氧化物電極種類以及製備的方法……………………………4
1-4 複合氧化物……………………………………………………8
1-4-1 複合氧化物簡介………………………………………………8
1-4-2 鎳鈷氧化物……………………………………………………10
1-5 製備鎳鈷氧化物…………………………………………………11
1-5-1 微波輔助水熱法………………………………………………11
1-6 超級電容器……………………………………………………16
1-6-1 超級電容器的分類……………………………………………18
1-6-2 超級電容器之電容量測………………………………………19
1-6-3 影響超級電容器特性的因素…………………………………23
1-7 鎳、鈷氧化物於超級電容器之應用簡介………………………25
第二章 實驗方法、步驟與儀器簡介…………………………………30
2-1藥品與儀器………………………………………………………30
2-1-1藥品……………………………………………………………30
2-1-2儀器…………………………………………………………31
2-2 實驗規劃…………………………………………………………32
2-2-1 鎳鈷氧化物的製備……………………………………………33
2-3 石墨基材的製備與前處理…………………………………33
2-4 電極的製備………………………………………………………34
2-5 電化學分析實驗…………………………………………………34
2-5-1線性伏安掃描(L inear Sweep Voltammetry, LSV)……………35
2-5-2循環伏安掃描(Cyclic Voltammetry, CV)………………………36
2-5-3計時電位測定法(Chronopotentiometry, CP)[3]………………37
2-5-4阻抗頻譜分析(Electrochemical Impedance Spectroscopy EIS)………………………………………………………………………………………………………………………………………………………38
2-5-4-1阻抗頻譜分析原理………………………………………38
2-5-4-2電化學阻抗頻譜理論………………………………………40
2-6材料分析儀器與原理簡介………………………………………42
2-6-1 X光繞射分析(X-ray Diffraction Analysis, XRD)……………………42
2-6-2 掃描式電子顯微鏡(Scanning Electron Microscope, SEM)……44
2-6-3 穿透式電子顯微鏡(Transmission Electron Microscopy, TEM) ……………………………………………………………………………………………………………………………………………………45
2-6-4 比表面積與孔徑分析儀 (Surface Area and Porosity Analyzer)……………………………………………………………47
2-6-5 熱重分析儀(Thermogravimetry Analyzer, TGA)…………………………51
第三章 錯合劑濃度、反應時間及鎳鈷前驅物比例對於微波合成鎳鈷氧化物材料的電化學行為影響……………………………………53
3-1研究動機與本章摘要……………………………………………53
3-2 實驗方法………………………………………………………53
3-3 醋酸根濃度的效應………………………………………………54
3-3-1 醋酸根濃度對鎳鈷氧化物結晶大小之影響…………………54
3-3-2 醋酸根濃度對比表面積與孔徑之影響………………………55
3-3-3醋酸根濃度對鎳鈷氧化物表面型態之影響…………………………………………58
3-3-4 醋酸根濃度對鎳鈷氧化物循環伏安圖譜之影響………………………………………………59
3-4微波反應持溫時間的影響……………………………………… 61
3-4-1 微波反應持溫時間對鎳鈷氧化物結晶大小之影響…………61
3-4-2 微波反應時間對比表面積與孔徑之影響……………………63
3-4-3 微波反應時間對鎳鈷氧化物循環伏安圖譜之影響…………65
3-5 改變氯化鎳/氯化鈷前驅物比例之效應….……………………67
3-5-1 氯化鎳/氯化鈷前驅物比例對鎳鈷氧化物結晶大小之影響………………………68
3-5-2 氯化鎳/氯化鈷前驅物比例對鎳鈷氧化物循環伏安圖譜之影響……………………………………………………………………………………………………………………………………………………69
3-6結果與討論……………………………………………………71
第四章 界面活性劑對合成中孔鎳鈷氧化物的影響……………………………………………72
4-1    研究動機與本章摘要……………………………………………72
4-2    實驗方法……………………………………………72
4-3界面活性劑對微波合成鎳鈷氧化物之影響……………………………………………73
4-3-1 不同種類及濃度之界面活性劑對鎳鈷氧化物結晶特性之影響…………………75
4-3-2 不同種類及濃度之界面活性劑對鎳鈷氧化物比表面積與孔徑大小分佈之影響……………………………………………76
4-3-3 不同種類及濃度之界面活性劑對鎳鈷氧化物循環伏安圖譜的影響…………79
4-3-4不同種類及濃度之界面活性劑對鎳鈷氧化物表面形態的影響……………………81
4-4熱處理對添加界面活性劑合成之鎳鈷氧化物的影響……………………………………83
4-4-1熱處理溫度對添加界面活性劑合成之鎳鈷氧化物結晶的影響…………………83
4-4-2熱處理溫度對添加界面活性劑合成之鎳鈷氧化物循環伏安圖譜的影響………86
4-4-3添加界面活性劑合成之鎳鈷氧化物之熱重損失分析…………………89
4-4-4熱處理溫度對添加不同界面活性劑合成之鎳鈷氧化物比表面積與孔徑大小分佈的影響………………………………………………………………………………………………………………………………………90
4-4-5熱處理溫度對添加不同界面活性劑所合成鎳鈷氧化物的孔洞形態影響………93
4-5結果與討論……………………………………………94
第五章 運用實驗設計法最佳化鎳鈷氧化物之比電容並探討循環伏安活化程序對鎳鈷氧化物的比電容及孔洞特性影響……………………………95
5-1 研究動機與本章摘要……………………………95
5-2實驗設計法簡述……………………………95
5-2-1部分因素實驗設計法……………………………96
5-3影響鎳鈷氧化物比電容值之部分因素設計……………………………98
5-3-1研究方法及因素選擇…………………………………………………………98
5-3-2實驗設計法之結果與分析…………………………………………………………100
5-3-3陡升實驗(steepest ascent)…………………………………………………………105
5-3-3-1陡升實驗之X光繞射圖譜…………………………………………………………106
5-3-3-2陡升實驗之循環伏安圖譜…………………………………………………………107
5-3-3-3陡升實驗之鎳鈷氧化物表面形貌…………………………………………………………108
5-3-3-4陡升實驗之比表面積與孔徑分析…………………………………………………………109
5-4循環伏安活化程序對鎳鈷氧化物的影響…………………………………………………………112
5-4-1活化類型介紹…………………………………………………………………………………………………………112
5-4-2 活化程序對鎳鈷氧化物之電化學特性影響……………………………………………114
5-4-3循環伏安活化程序對鎳鈷氧化物結晶性之影響……………………………117
5-4-4活化程序對鎳鈷氧化物表面之影響…………………………………………………………118
5-4-5活化程序對鎳鈷氧化物的孔洞形態影響……………………………119
5-5結晶指標及比表面積大小對鎳鈷氧化物比電容之影響……………………………120
5-6結果與討論……………………………………………………………………………………………………………………122
第六章 鎳鈷氧化物與石墨烯碳材之非對稱超級電容器組裝………………………124
6-1前言………………………124
6-2電極組裝概念………………………………………………………………………………………………124
6-2-1基本觀念………………………………………………………………………………………………124
6-2-2對稱組裝概念………………………………………………………………………………………………125
6-2-3非對稱組裝概念[69]………………………………………………………………………126
6-3鎳鈷氧化物與石墨烯之非對稱組裝………………………………………………130
6-4不同操作電位窗對非對稱超電容的影響……………………………………………………………132
6-4-1不同操作電位窗下非對稱超電容的充放電曲線………………………132
6-4-2不同操作電位窗對兩電極的充放電影響………………………134
6-4-3不同操作電位窗對鎳鈷氧化物-石墨烯之非對稱超電容的能量效率影響    ………………………………………………………………………………………………………………………………………………136
6-4-4鎳鈷氧化物-石墨烯之非對稱超電容的比能量、功率密度………………………137
6-4-5電化學阻抗頻譜分析…………………………………………………………………139
6-5現行二次電池與鎳鈷氧化物/石墨烯碳材之非對稱超電容的特性比較……………………………………………………………………141
6-6結果與討論……………………………………………………………………………142
第七章 未來展望……………………………………………………………………143
參考文獻………………………………………………………………………………144




                                

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