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研究生: 毛薇婷
Mao, Wei-Ting
論文名稱: 在離子液體中電沉積鐵和鐵-鈷
Electrodeposition of Iron and Iron-Cobalt from Ionic Liquids
指導教授: 孫亦文
Sun, I-Wen
學位類別: 碩士
Master
系所名稱: 理學院 - 化學系
Department of Chemistry
論文出版年: 2015
畢業學年度: 103
語文別: 中文
論文頁數: 99
中文關鍵詞: 離子液體電沉積鐵-鈷奈米線
外文關鍵詞: ionic liquids, electrodeposition, iron-cobalt, iron, nanowire
相關次數: 點閱:99下載:24
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  • 論文中探討添加氯化亞鐵(Iron(II) chloride)於氯化鈷-1-乙基-3-甲基咪唑(cobalt chloride-1-ethyl-3-methylimidazolium chloride,CoCl2-EMIC)離子液體中的電化學行為,利用定電位沉積所得的鐵-鈷會依沉積電位、氯化亞鐵添加的濃度以及電鍍時的溫度不同而產生不同形貌,如顆粒狀或奈米線狀結構等,並且也會影響鍍層中鐵-鈷的比例。可藉由調控電沉積電位與電鍍時所使用的基材來得到垂直於基材表面的鐵-鈷金屬奈米線。電沉積所得之鐵-鈷樣品以掃描式電子顯微鏡(SEM)觀察鍍層表面形貌、以能量分散光譜儀(EDS)分析鍍層成分,並且以X 射線繞射儀(XRD)以及穿透式電子顯微鏡(TEM)探討晶形結構。
    利用沉積所得之鐵-鈷進行電溶測試,發現具高表面積的線狀結構其電容效果較形貌為顆粒狀電容來的高,並發現添加FeCl2 於CoCl2-EMIC 溶液中電沉積所得到的鐵-鈷奈米線其電容較鈷奈米線高。
    另外論文中亦進行氯化亞鐵-1- 乙基-3- 甲基咪唑(Iron(II) chloride-1-ethyl-3-methylimidazolium chloride,FeCl2-EMIC)離子液體中電沉積鐵的探討,並利用循環伏安法觀察不同比例的FeCl2-EMIC 之電化學行為,而於EMIC 系統中,改變電沉積電位、溫度以及利用EMI-BF4 稀釋FeCl2-EMIC,皆會影響鍍層的形貌,並將電沉積所得之樣品分別以掃描式電子顯微鏡(SEM)、能量分散光譜儀(EDS)、X 射線繞射儀(XRD)以及穿透式電子顯微鏡(TEM)進行鑑定及結構分析。

    In this study,the electrochemical behaviors of iron (Fe(II)) and cobalt (Co(II)) were studied in 40-60mol% cobalt chloride-1-ethyl-3-methylimidazolium chloride(CoCl2-EMIC)ionic liquid containing various concentration of FeCl2. Various morphologies of Fe-Co deposits can be obtained by adjusting the deposition parameters such as deposition potential,Fe(II) concentration and temperature. The morphologies and the composition of Fe-Co deposits were examined by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS),X-ray diffraction (XRD) and transmission electron microscopy (TEM). Direct template-free electrodeposition of aligned Fe-Co nanowires was achieved on a tungsten substrate in a quiescent Lewis acidic CoCl2-EMIC ionic liquid containing FeCl2 by applying an extremely large overpotential. The investigations of cyclic votammetry and constant current charge/discharge measurements on the capacitive behavior of nanowires reveal the wire deposited electrode are suitable or the supercapacitors applications.
    Moreover, the electrochemical behaviors of iron (Fe(II)) was studied in iron chloride-1-ethyl-3-methylimidazolium chloride (FeCl2-EMIC) ionic liquid on glassy carbon electrode. The speciation and coordination of iron-chloride-based ionic liquids with various mole percentages of FeCl2 were investigated using electrospray ionization mass spectrometry (ESI-MS). The electrodeposition of iron was investigated in 40-60mol% FeCl2-EMIC ionic liquid . Fe deposits were characterized by scanning electron microscopy (SEM),X-ray diffraction (XRD) and transmission electron microscopy (TEM).

    摘要 I Abstract II 誌謝 III 目錄 IV 圖目錄 VI 表目錄 XVI 第一章 緒論 1 1-1 離子液體(Ionic liquid) 1 1-2 鐵的性質與文獻回顧 4 1-3 電沉積法制備鐵和鈷之文獻回顧 5 1-4 氧化鐵、氫氧化鈷電極運用於電容之相關文獻的回顧 6 1-5 奈米線文獻回顧 8 1-5-1 陽極氧化鋁模板輔助沉積法(anodic aluminum oxide template-assisted method)製備奈米線 8 1-5-2 無模板製備奈米線 10 1-6 研究動機與目的 13 第二章 實驗原理 14 2-1 電化學原理 14 2-2 循環伏安法(cyclic Votammetry,CV) 15 2-3 電流時間法 16 2-4 電化學成核原理 17 2-4-1 成核動力學 18 2-4-2 二維空間核成長 (Growth of monolayers) 20 2-4-3 三維空間核成長 (Growth of three-dimention centers)21 2-5 電容行為探討 26 第三章 實驗藥品與儀器 27 3-1 實驗藥品 27 3-2 電沉積基材及作為電極用之金屬 29 3-3 離子液體製備 30 3-4 實驗儀器與裝置 31 第四章結果與討論 35 4-1 Fe(II)及Co(II)在FeCl2-CoCl2-EMIC 熔鹽中的行為 35 4-1-1 FeCl2 在CoCl2-EMIC 熔鹽中的電化學行為 35 4-1-2 Fe(II)在CoCl2-EMIC 熔鹽不同條件電沉積的結果 (無攪拌)41 4-1-3 EDS 與TEM 分析 58 4-2 探討鐵鈷合金奈米線結構之電容行為 64 4-3 Fe(II)在FeCl2-EMIC 熔鹽中的電化學行為71 4-3-1Fe(II)在FeCl2-EMIC 熔鹽中的配位型態 71 4-3-2Fe(II)在FeCl2-EMIC 熔鹽中的電化學行為 72 4-3-3 Fe(II)在FeCl2-EMIC 熔鹽中還原成Fe(0)的成核反應 76 4-3-4 Fe(II)在40-60mol% FeCl2-EMIC 熔鹽不同條件電沉積的結 79 4-3-5 EDS、XRD 與TEM 分析87 第五章結論 89 參考文獻 91 Extended Abstrac 95

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