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系統識別號 U0026-0812200914210706
論文名稱(中文) 氯化亞銅與氯化錫在室溫離子液體之電化學研究
論文名稱(英文) Electrochemical Studies of Copper(I) Chloride and Tin(II) Chloride in 1-Ethyl-3-Methylimidazolium Dicyanamide Room Temperature Ionic Liquid
校院名稱 成功大學
系所名稱(中) 化學系碩博士班
系所名稱(英) Department of Chemistry
學年度 96
學期 2
出版年 97
研究生(中文) 梁天猷
研究生(英文) Tin-Iao Leong
電子信箱 l3695101@ccmail.ncku.edu.tw
學號 L3695101
學位類別 碩士
語文別 中文
論文頁數 140頁
口試委員 指導教授-孫亦文
口試委員-楊明長
口試委員-姚學麟
中文關鍵字 電化學  離子液體  電沉積 
英文關鍵字 Ionic Liquid  Electrodeposition  Electrochemistry 
學科別分類
中文摘要 本論文探討,氯化亞銅和氯化錫在空氣與水穩定的室溫離子液體1-Ethyl-3-Methylimidazolium Dicyanamide ( EMI-DCA )內的電化學應用來估量其潛在實用性。
(A) 測量EMI-DCA在溫度範圍297.0 ~ 343.0 K內與溫度相關的密度以及絕對黏度,它們的關係方程式也已被敘述。由於DCA-陰離子的配位基特性,令CuCl、CuCl2和SnCl2都能全部完全溶解於EMI-DCA內。
(B) Cu(I)在EMI-DCA的循環伏安圖與其它兩種離子液體──EMI-Cl-BF4和 EMI-TFSI相較可得,Cu(I)皆可以在這些溶液內被氧化成Cu(II)或被還原為銅金屬。銅沉積在玻璃碳與鎳電極上是牽涉三維逐步成核生長過程。掃描式電子顯微鏡和X光繞射儀的結果都顯示銅鍍層的形態會因施加的沉積電位有關,而且以奈米晶粒組成的緻密銅鍍層可以利用低過電位的定電位電解來得到。
(C) 比較Sn(II)在EMI-DCA和EMI-Cl-BF4的循環伏安圖可知,Sn(II)皆可在這兩離子液體內被還原成錫金屬;而在EMI-DCA內,Sn(II)只能在玻璃碳電極上被氧化成Sn(Ⅳ)。錫在玻璃碳上沉積是牽涉三維逐步與瞬間成核生長過程之間。掃描式電子顯微鏡、X光繞射儀、穿透式電子顯微鏡的結果都顯示錫鍍層的形態和沉積電流密度有關,而以奈米線形成的高表面積錫鍍層可由在定電流密度0.30 ~ 1.21 mA/cm2範圍內得到。
低黏度的EMI-DCA與其對金屬氯化物有高溶解度,令此離子液體在電沉積金屬上更容易。
英文摘要 In this study, the potential utility of the air- and water-stable 1-ethyl-3-methylimidazolium dicyanamide (EMI-DCA) room temperature ionic liquid for electrochemical application was evaluated with copper(I) chloride, copper(II) chloride and tin(II) chloride.
(A) The temperature dependency of the density and absolute viscosity of EMI-DCA were measured over a temperature range from 297 to 343 K, and equations describing the dependencies are presented. Due to the ligand property of the DCA- anion, CuCl, CuCl2 and SnCl2 are soluble in EMI-DCA.
(B) Cyclic voltammograms of Cu(I) in EMI-DCA and other two ionic liquids (EMI-Cl-BF4 & EMI-TFSI) were compared. Cu(I) can be oxidized to Cu(II) or reduced to Cu metal in these solutions. The electrodeposition of Cu on glassy carbon and nickel electrodes involves a three-dimensional progressive nucleation and growth process. Scanning electron microscopy and X-ray diffraction results indicate that the morphology of the copper electrodeposits is dependent on the deposition potential, and compact coatings containing nanocrystalline copper could be obtained by potentiostatic electrolysis at low overpotentials.
(C) Cyclic voltammograms of Sn(II) in EMI-DCA and EMI-Cl-BF4 ionic liquids were compared. Sn(II) can be reduced to Sn metal in these ionic liquids, Sn(II) can only be oxidized to Sn(Ⅳ) on glassy carbon electrode in EMI-DCA. The electrodeposition of Sn on glassy carbon electrode involves between a three-dimensional progressive and instantaneous nucleation and growth process. Scanning electron microscopy, X-ray diffraction and transmission electron microscopy results indicate that the morphology of the tin electrodeposits is dependent on the deposition current density, and high surface area coatings with nanowire could be obtained by applied amperostatic electrolysis over a current density range from 0.30 ~ 1.21 mA/cm2.
The low viscosity of EMI-DCA and the high solubility of metal chlorides in it would facilitate the electrodeposition of metals using this ionic liquid.
論文目次 表目錄 V
圖目錄 VII

第一章 緒論 1
1-1 室溫離子液體的簡介( Introduction of Room Temperature Ionic Liquids )
1
1-2 室溫離子液體的發展( Development of Room Temperature Ionic Liquids )
9
第二章 銅與錫在離子液體中的文獻回顧 21
2-1 銅( Copper ) 21
2-2 錫( Tin ) 22
第三章 電化學原理與方法 25
3-1 法拉第電解定律( Faraday's Laws of Electrolysis ) 26
3-2 循環伏安法( Cyclic Voltammery ) 26
3-3 電位階升法( Potential Step Chronoamperometry ) 27
3-4 庫倫法( Coulometry ) 29
3-5 電化學成核原理( Principle of Electrocrystallization ) 29
3-5-1 成核動力學 30
3-5-2 二維空間的核成長( 2-D Growth ) 33
3-5-2 三維空間的核成長( 3-D Growth ) 34
3-5-4 其他的成核理論探討 40
第四章 黏度原理及測量 42
第五章 實驗裝置、儀器與藥品 45
5-1 電化學實驗裝置 45
5-1-1 參考電極( Reference Electrode ) 45
5-1-2 輔助電極( Counter Electrode ) 45
5-1-3 工作電極( Working Electrode ) 45
5-2 儀器( Instruments ) 46
5-2-1 手套箱( Glove Box ) 46
5-2-2 定電位/定電流儀( Potentiostat/Galvanostat ) 46
5-2-3 電磁攪拌加熱器( Stirring Hot Plate ) 46
5-2-4 數位式熱偶溫度計( Thermocouple Thermometer ) 46
5-2-5 掃瞄式電子顯微鏡( Scanning Electron Microscope ) 47
5-2-6 X光繞射分析儀( X-Ray Diffraction Meter ) 47
5-2-7 穿透式電子顯微鏡( Transmission Electron Microscopy ) 47
5-2-8 拋光機( Polisher ) 47
5-2-9 密度計( Density Meter ) 47
5-2-10 黏度計( Viscometer ) 47
5-2-11 恆溫水槽( Circulator ) 48
5-3 實驗藥品( Reagents ) 51
5-3-1 氯化1-乙基-3-甲基咪銼( EMIC ) 51
5-3-2 二氰胺鈉( NaDCA ) 52
5-3-3 金屬( Metal ) 52
5-3-4 氯化亞銅( CuCl )和氯化銅( CuCl2 ) 52
5-3-5 氯化錫( SnCl2 ) 53
5-3-6 氫氧化鈉( NaOH ) 53
5-3-7 二次去離子水( Deionized Water ) 53
5-3-8 酸液與鹼液( Acidic Solution and Lye ) 53
5-4 EMI-DCA離子液體的製備與純化 54
第六章 實驗結果與討論 55
6-1 EMI-DCA離子液體 55
6-1-1 物理性質──密度與黏度( Density and Viscosity ) 55
(A) 密度的測量 55
(B) 黏度的測量 56
6-1-2 EMI-DCA離子液體的電位窗 62
6-1-3 EMI-DCA對金屬鹽類的溶解性 64
6-2 CuCl在EMI-DCA內的電化學與電沉積探討 66
6-2-1 CuCl在EMI-DCA內的電化學行為 66
(A) CuCl和CuCl2在EMI-DCA的最大溶解度 66
(B) Cu(I)在不同離子液體內的電化學行為 66
(C) 以電位階升法去推算Cu(I)和Cu(II)的擴散係數 68
(D) 在不同電極上的電化學行為 69
(E) 在不同電極上的成核-生長現象 70
6-2-2以定電位法電沉積銅( Chronoamperometry ) 72
6-3 SnCl2在EMI-DCA內的電化學與電沉積探討 76
6-3-1 SnCl2在EMI-DCA內的電化學行為 76
(A) SnCl2在EMI-DCA的最大溶解度 76
(B) Sn(II)的電化學行為 77
(C) EMI-DCA與EMI-Cl-BF4的比較 79
(D) Sn(II)提供來源的比較 81
(E) 不同折返電位 83
(F) 電極上多圈掃描的循環伏安圖 87
(G) 雙電位階升法 90
(H) 以不同掃描速率去探討Sn(II)/Sn(0) 92
(I) 以電位階升法去推算Sn(II)/Sn(0)擴散係數 94
(J) 在不同電極上的成核-生長現象 97
6-3-2以定電流法來電沉積錫( Chronopotentiometry ) 99
(A) 定電流法電沉積錫 100
(B) 不同沉積電量密度探討錫鍍層成長過程 109
(C) 錫鍍層的EDS、XRD和TEM分析 112
(D) EMI-Cl-BF4內以定電流法電沉積錫 116
6-3-3錫的奈米線鍍層對Benzil Bromide的電化學偵測 121
第七章 結論 ( Conclusion ) 126
第八章 未來研究工作( Future Research Work ) 129
第九章 參考文獻( Reference ) 130
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