臺灣博碩士論文加值系統

本研究是以陽極處理搭配脈衝製程，以純鈦為陽極、鉑為陰極在純鈦基板上製備出排列規則有序的二氧化鈦奈米管陣列，可經由溫度、時間、電壓、脈衝頻率及電解液的種類等參數的控制製備欲得到的奈米管結構。此奈米管具有較大的比表面積及較高的表面活性。
以乙二醇添加0.5wt％氟化銨及0~5wt％去離子水均勻混合作為電解液，並於持溫10℃、反應時間3小時下作20V、30V、40V、50V、60V的電壓變化做為實驗參數，藉此得到二氧化鈦奈米管，再進行奈米管的特性分析，包含表面形貌、管長、管徑量測及電化學交流阻抗分析。
以此方法可製備垂直基板的奈米管，且奈米管的管長控制在0.7μm到12μm的範圍之內，而奈米管的管徑可控制在30nm到150nm的範圍之中。當有水的添加時，可降低電解液的黏性，有助於離子在電解液中的擴散，可改善覆蓋的氧化層並且降低了化學溶解的現象發生率。

In this research, the order titanium dioxide nanotube arrays be preparing by anodizing with pulse process, titanium as anode and platinum as cathode. It could get nanotubes that we need in controlling many parameter, like temperature、time、voltage、pulse frequency and electrolytes. The nanotubes were more surface area and higher surface active.
The titanium dioxide nanotube can be gain at 10℃ and 3hours by changing voltage about (20V、30V、40V、50V、60V) as experiment parameter with electrolyte of mixed of 0.5wt％ ammonium fluoride (NH4F)＋0~2wt％ Deionized water (H2O)＋ethylene glycol (EG). Then, the morphology、diameter、length、Electrochemical Impedance Spectroscopy analysis of titanium dioxide nanotube were investigated. Effects of micro-morphologies on the composition of the electrolytes and applied potentials were elucidated by using scanning electron microscope (SEM, JEOL 6500). Electrochemical impedance spectroscopy (EIS) analyses were monitored to the electrochemical properties of nanotubes with models of equivalent circuit demonstrated.
By applying each of different voltages, the titanium dioxide nanotube were grown vertically on the surfaces of titanium specimens where their length could be controlled from 30nm to 150nm with diameters of 0.7μm to 12μm. Increasing proportions of deionized water added in EG solution, the descended viscosity of solution would enhance its ion diffusion and reduce chemical dissolution to a stable oxide layer.

中文摘要 .................................................................................................... i
英文摘要 .................................................................................................... ii
誌謝 ........................................................................................................... iv
目錄 ........................................................................................................... v
表目錄 ....................................................................................................... viii
圖目錄 ....................................................................................................... ix
第一章 緒論 ............................................................................................ 1
1.1前言 ............................................................................................ 1
1.2研究目的與動機 ........................................................................ 1
第二章 理論與文獻回顧 ......................................................................... 3
2.1二氧化鈦 .................................................................................... 3
2.2光觸媒 ........................................................................................ 4
2.3二氧化鈦奈米管製備方法 ......................................................... 5
2.3.1 模版製造法 .................................................................... 6
2.3.2 溶膠凝膠法 .................................................................... 7
2.3.3 水熱法 ............................................................................ 8
2.3.4 自組裝法 ........................................................................ 9
2.3.5 陽極處理法 .................................................................... 10
2.4二氧化鈦奈米管形成機制 ......................................................... 11
2.4.1 阻障層 ............................................................................ 12
2.4.2 多孔層 ............................................................................ 12
2.4.3 奈米管 ............................................................................ 13
2.4.4 化學溶解 ........................................................................ 14
2.4.5 電流密度-時間曲線........................................................ 15
2.5脈衝製程 .................................................................................... 16
2.5.1 電流模式介紹 ................................................................ 16
2.5.2 脈衝模式與逆脈衝模式 ................................................. 17
2.6交流阻抗法 ................................................................................ 19
2.6.1 基本電子元件與阻抗特性 ............................................. 20
2.6.1.1 電阻之特性...................................................... 20
2.6.1.2 電容之特性...................................................... 20
2.6.2 Warburg Impedance ........................................................ 21
2.6.3 Nyquist plot .................................................................... 22
2.6.3.1 溶液電阻 ......................................................... 23
2.6.3.2 電荷轉移電阻 .................................................. 23
2.6.3.3 電雙層電容...................................................... 23
2.6.3.4 電荷擴散轉移阻抗 .......................................... 24
2.6.3.5 總阻抗 ............................................................. 24
2.6.4 Bode Phase Angle Plot .................................................... 28
2.6.5 Bode Magnitude Plot ....................................................... 30
2.6.5.1 電雙層電容...................................................... 30
2.6.5.2 電荷擴散轉移阻抗 .......................................... 30
第三章 實驗方法與設備 ......................................................................... 32
3.1實驗藥品與設備 ........................................................................ 32
3.1.1 實驗藥品 ........................................................................ 32
3.1.2 實驗設備 ........................................................................ 33
3.2實驗步驟 .................................................................................... 34
3.2.1 詴片前處理 .................................................................... 36
3.2.2 脈衝陽極法 .................................................................... 37
3.2.3 電化學交流阻抗 ............................................................. 38
第四章 結果與討論 ................................................................................ 39
4.1二氧化鈦奈米管分析 ................................................................. 39
4.1.1 顯微結構分析 ................................................................ 39
4.1.2 電流密度-時間曲線........................................................ 59
4.1.3 陽極脈衝處理與陽極處理之比較 .................................. 61
4.2 水添加量對奈米管之影響 ........................................................ 63
4.2.1 顯微結構分析 ................................................................ 63
4.2.2 交流阻抗分析 ................................................................ 68
第五章 結論 ............................................................................................ 75
參考文獻 .................................................................................................... 76

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