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研究生：	鄧名傑 Deng, Ming-Jay
論文名稱：	在1-乙基-3 -甲基-咪唑氰胺離子液體中以電化學法製備多孔鎳電極並應用於製作氧化鈷擬電容器電極 Electrochemical preparation of porous Ni electrodes from 1-ethyl-3-methylimidazolium-dicyanamide ionic liquid and its application for Co oxides pseudocapacitor
指導教授：	孫亦文 Sun, I-Wen
學位類別：	博士 Doctor
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2010
畢業學年度：	98
語文別：	中文
論文頁數：	99
中文關鍵詞：	EMI-DCA離子液體、鎳銅合金、多孔性鎳、氧化鈷、擬電容器
外文關鍵詞：	EMI-DCA, Ni-Cu alloys, porous Ni, Co oxide, pseudocapacitor
相關次數：	點閱：78 下載：2
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本論文探討室溫離子液體1-Ethyl-3-Methylimidazolium Dicyanamide (EMI-DCA)的物理性質(密度與溫度以及絕對黏度與溫度的關係)並評估其在電化學的潛在應用性。由於DCA-陰離子本身所具備的配位基特性，使得很多過渡金屬離子都能溶解於EMI-DCA內。這也使EMI-DCA在電沉積金屬的進行更容易。在此我們也藉由電流滴定實驗來幫助了解Ni(II)與DCA-陰離子的配位關係為[Ni(DCA)4]2-。
Cu(I)與Ni(II)在EMI-DCA的電化學也在此論文中研究，由結果得知銅與鎳的還原電位在EMI-DCA當中是非常接近的，這樣的結果是有利於共沉積Ni-Cu合金薄膜特別是在沒有添加劑的情況下。而利用定電位方法沉積出來的Ni-Cu合金薄膜其成分組成也被探討。由結果得知Ni-Cu合金薄膜的成分不僅與還原電位有關係同時也受到EMI-DCA溶液中Cu(I)與Ni(II)的濃度比例影響。在EMI-DCA溶液中利用電化學選擇性溶解Ni-Cu合金薄膜的方法製備多孔性鎳電極，這是由於合金薄膜上較活潑的銅被溶解，剩下的是較為不活潑的鎳金屬而呈現多孔狀結構。隨後利用此多孔性鎳電極作為基材，在醋酸鈷溶液中陽極沉積氧化鈷並分析其表面形貌與成分。並將製備好的多孔性鎳電極應用於氧化鈷擬電容器電極上，以循環伏安法測試其電容性質與電化學可逆性。在掃描速率10 mV/s時比電容值為1356 F/g，比電容值相較於平面電容器高出6倍左右，且經過500次的循環伏安法連續掃瞄後比電容值仍可維持90 %以上。

In this study, the 1-ethyl-3-methyl -imidazolium dicyanamide (EMI-DCA) ionic liquid for electrochemical application was evaluated with transition metal ion. The temperature dependency of the density and absolute viscosity of EMI-DCA were measured. Due to the ligand property of the DCA- anion, CuCl and NiCl2 are soluble in EMI-DCA. Amperometric titration experiments suggest that Ni(II) reacted with DCA- anions forming [Ni(DCA)4]2- complex anion, which could be reduced to metal via a single-step electron transfer process. Cyclic voltammograms of Ni(II), Cu(I), and Ni(II) + Cu(I), respectively, in EMI-DCA were recorded on the glassy carbon electrode. The thermodynamic deposition potentials of Ni and Cu are very close to each other and favorable for the electrodeposition of Ni-Cu alloys. The Ni-Cu alloys were electrodeposited using bulk controlled-potential electrolysis experiments. Energy-dispersive spectroscopy (EDS) data indicates that the composition of the Ni-Cu alloys not only depends on the deposition potential, but also on the Cu(I) and Ni(II) concentrations in the ionic liquid. The preparation of porous Ni films by electrochemical deposition of Ni-Cu alloy followed by the selective anodic etching of the active component (Cu) from the alloy was studied in the EMI-DCA ionic liquid containing Cu(I) and Ni(II) at room temperature. Afterwards, anodic deposition was carried out to disperse Co oxide onto the porous Ni substrate. As a result, a novel oxide electrode with a high-porosity structure was fabricated by the totally electrochemical procedure, which is very simple and efficient. Pseudocapacitive performance of this Co oxide electrode was evaluated by cyclic voltammetry in 1 M KOH solution. The data indicated that specific capacitance of the Co oxide was as high as 1356 F/g, which was 6-fold over that of flat Co oxide. Capacitance retained ratio after 500 charge–discharge cycles of the Mn oxide was also significantly improved from 75 % to 93 % due to the use of the porous substrate.

表目錄---------------------------------------------------------------------------------------------III
圖目錄--------------------------------------------------------------------------------------------IV
第一章 緒論--------------------------------------------------------------------------------------1
1-1 離子液體的介紹-----------------------------------------------------------------------1
1-2室溫離子液體的發展-----------------------------------------------------------------7
1-3奈米孔洞材料介紹-------------------------------------------------------------------16
1-4研究動機-------------------------------------------------------------------------------19
第二章 背景資料與文獻回顧----------------------------------------------------------------20
2-1 去合金化的原理--------------------------------------------------------------------20
2-2 電鍍鎳合金及其去合金化的文獻-----------------------------------------------21
2-3 鈷氧化物電極於超高電容器中的應用-----------------------------------------24
第三章 實驗方法與步驟----------------------------------------------------------------------31
3-1 循環伏安法(Cyclic Voltammery)-----------------------------------------------31
3-2 庫倫法(Coulometry)--------------------------------------------------------------32
3-3 電化學成核原理(Principle of Electrocrystallization)------------------------32
3-3-1 成核動力學------------------------------------------------------------------33
3-3-2 三維空間的核成長(3-D Growth)---------------------------------------36
3-4 黏度原理及測量--------------------------------------------------------------------41
3-5 實驗器材與裝置---------------------------------------------------------------------43
3-5-1 三極式反應槽(Three-Electrode Cell)----------------------------------43
3-5-2 手套箱(Glove Box)-------------------------------------------------------44
3-5-3 定電位/定電流儀(Potentiostat/Galvanostat)--------------------------45
3-5-4 電磁攪拌加熱器(Stirring Hot Plate)-----------------------------------45
3-5-5 掃描式電子顯微鏡(Scanning Electron Microscope)----------------45
3-5-6 化學光譜分析儀(Electron Spectroscopy Chemical Analysis, ESCA) ----------------------------------------------------------------------------------------45
3-5-7 X光繞射分析儀(X-Ray Diffraction Meter)--------------------------45
3-5-8 火焰原子吸收光譜儀(Atomic Absorption Spectrometer, AA)---45
3-5-9 拋光機(Polisher)----------------------------------------------------------46
3-5-10 密度計(Density Meter)---------------------------------------------------46
3-5-11 黏度計(Viscometer)------------------------------------------------------46
3-5-12 恆溫水槽(Circulator)-----------------------------------------------------46
3-5-13 原子力學顯微鏡(Atomic Force Microscopy, AFM)---------------46
3-6藥品(Reagents)----------------------------------------------------------------------48
3-6-1 氯化1-乙基-3-甲基咪唑(EMIC)---------------------------------------48
3-6-2 二氰胺鈉(NaDCA) ------------------------------------------------------ --49
3-6-3 金屬(Metal)----------------------------------------------------------------49
3-6-4 無水氯化亞銅(CuCl)-----------------------------------------------------50
3-6-5 無水氯化鎳(NiCl2)--------------------------------------------------------50
3-6-6 氫氧化鈉(NaOH)---------------------------------------------------------50
3-6-7 醋酸鈷(Co(CH3COOH)2〃4H2O)---------------------------------------50
3-6-8 氫氧化鉀(KOH)-----------------------------------------------------------50
3-6-9 二次去離子水(Deionized Water)---------------------------------------50
3-6-10酸液與鹼液(Acidic Solution and Lye) ------------------------------- --50
3-6-11 EMI-DCA離子液體的製備與純化-------------------------------------50
第四章 實驗結果與討論----------------------------------------------------------------------52
4-1 EMI-DCA離子液體-----------------------------------------------------------------52
4-1-1 物理性質──密度與黏度(Density and Viscosity)--------------------52
(A) 密度的測量--------------------------------------------------------------52
(B) 黏度的測量---------------------------------------------------------------53
4-1-2 EMI-DCA離子液體的電位窗---------------------------------------------56
4-2 NiCl2在EMI-DCA離子液體中的電化學與電沉積探討----------------------58
4-2-1 NiCl2在EMI-DCA離子液體中的電化學行為-------------------------58 4-2-2 Ni(II)與DCA- 陰離子之配位探討----------------------------------------61
4-2-3鎳在電極上的成核-生長機制---------------------------------------------64
4-2-4以定電位法電沉積鎳(Chronoamperometry)---------------------------67
4-3在EMI-DCA內共沉積Ni-Cu薄膜-----------------------------------------------71
4-3-1 CuCl在EMI-DCA內的電化學探討-------------------------------------71
4-3-2 Cu(I)與Ni(II)在EMI-DCA內的電化學探討 ----------------------- --73
4-3-3電沉積Ni-Cu薄膜與表面分析-------------------------------------------74
4-4用電化學方法在EMI-DCA離子液體內製作多孔性鎳電極-----------------77
4-4-1 ITO電極在0.05 M Cu(I) + 0.05 M Ni(II) EMI-DCA中的電沉積研究------------------------------------------------------------------------------------------------------77
4-4-2不同沉積電位之Ni-Cu合金薄膜選擇性溶解後表面形貌及成份關係---------------------------------------------------------------------------80
4-4-3 Ni-Cu合金薄膜階段性選擇性溶解--------------------------------------82
4-5多孔性鎳電極應用於製作氧化鈷擬電容器電極 ---------------------------- --87
4-5-1利用陽極沉積法製備氧化鈷電極與表面形貌研究 ---------------- --87
4-5-2多孔性化鈷電極與平板性氧化鈷電極之擬電容行為研究 ------- --89
第五章 結論 ---------------------------------------------------------------------------------- --93
第六章 參考文獻 ---------------------------------------------------------------------------- --94
                                    

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