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研究生： 蘇修卉
Su, Hsiu-Hui
論文名稱： 製備銀摻雜二氧化鈦奈米管於光催化降解染料薔薇紅之研究
Fabrication of Ag-doped TiO2 nanotubes for photocatalytic degradation of rhodamine B
指導教授： 黃守仁
Whang, Thou-Jen
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： 2021
畢業學年度： 109
語文別： 中文
論文頁數： 80
中文關鍵詞： 陽極氧化法 、二氧化鈦奈米管 、脈衝電流沉積法 、銀摻雜 、光催化降解 、薔薇紅
外文關鍵詞： anodic oxidation method, titanium dioxide nanotubes, pulse current deposition, silver doping, photocatalytic degradation, rhodamine B
相關次數： 點閱：172  下載：0 
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    • 利用陽極氧化法以氟化銨(Ammonium fluoride, NH4F)、乙二醇(Ethylene glycol, EG)及去離子水作為電解液，在鈦(Titanium, Ti)基板上製備二氧化鈦奈米管。再將製備好之二氧化鈦奈米管利用脈衝電流沉積法(Pulse current deposition, PCD)以硝酸銀(Silver nitrate, AgNO3)及去離子水作為電解液，在二氧化鈦奈米管上修飾銀作為欲光催化降解染料薔薇紅(Rhodamine B, Rh B)之材料。
    本實驗中，先透過改變氟化銨濃度、陽極氧化電壓、陽極氧化時間及退火溫度找到最佳光催化降解效率之二氧化鈦奈米管。再利用改變硝酸銀濃度、脈衝電流及脈衝循環次數，找到最有效增強光催化降解率之銀條件。配合掃描式電子顯微鏡(Scanning Electron Microscope, SEM)分析樣品表面形貌、X光繞射儀(X-Ray Diffraction, XRD)鑑定樣品之晶型、能量色散X射線譜(Energy-dispersive X-ray spectroscopy, EDS)進行元素分析，最終以UV-LED光照射於材料上並放在欲降解之染料中，以光纖光譜儀追蹤薔薇紅之吸收度以計算其濃度及降解率。
    實驗的結果發現當氟化銨濃度為0.2 wt%、陽極氧化電壓為50 V、陽極氧化時間為1.5 hr及退火溫度為550℃，有最完整二氧化鈦奈米管之形貌及針對染料薔薇紅濃度為10-5 M時有最高之降解率41.5 %。而銀摻雜則在硝酸銀濃度為2000 ppm、脈衝電流為-15 mA及脈衝循環次數為3 次時能使降解率提升最多(+10.0 %)有最佳的修飾效果。

    In this work, we used ammonium fluoride, ethylene glycol and deionized water as electrolytes to prepare titanium dioxide nanotubes on a titanium substrate by anodic oxidation method. Then the prepared titanium dioxide nanotubes were modified with silver by pulse current deposition (PCD) with silver nitrate and deionized water as the electrolyte. The prepared material was used for the degradation of rhodamine B dye.
    First, we found the titanium dioxide nanotubes with the best photocatalytic degradation efficiency by changing the concentration of ammonium fluoride, anodizing voltage, anodizing time and annealing temperature. Second, we changed the concentration of silver nitrate, pulse current and pulse cycle times to find the most effective condition for enhancing the photocatalytic degradation rate. Cooperated with scanning electron microscope to analyze the surface morphology of the sample, X-ray diffraction to identify the crystal form of the sample, energy-dispersive X-ray spectroscopy for elemental analysis, and finally UV-LED light was irradiated on the material and the absorbance of rhodamine B dye was tracked with a fiber optic spectrometer to calculate its concentration and degradation rate. The results of the experiment found that when the ammonium fluoride concentration was 0.2 wt%, the anodizing voltage was 50 V, the anodizing time was 1.5 hr, and the annealing temperature was 550°C, the morphology of the titanium dioxide nanotube was the most complete and the highest degradation rate was 41.5%. And the silver doping was really increasing the degradation rate by the most 10.0% when the concentration of silver nitrate was 2000 ppm, the pulse current was -15 mA and the number of pulse cycles was 3 times.

    摘要 I 致謝 XVIII 目錄 XIX 圖目錄 XXIII 表目錄 XXVI 第一章 緒論 1 1-1 前言 1 1-2 二氧化鈦簡介 2 1-3 二氧化鈦製備方法 4 1-3-1 水熱法 4 1-3-2 化學氣相沉積法 4 1-3-3 溶膠-凝膠合成法 4 1-3-4 陽極氧化法 5 1-4 二氧化鈦改質 6 1-4-1 金屬摻雜 6 1-4-2 非金屬摻雜 6 1-4-3 半導體複合改質 7 1-5 薔薇紅簡介 8 1-6 研究動機 9 第二章 實驗原理 10 2-1 陽極氧化法 10 2-1-1 製備二氧化鈦奈米管之發展 10 2-1-2 製備二氧化鈦奈米管之電解液 10 2-1-3 二氧化鈦奈米管成長機制 11 2-2 脈衝電流沉積法 13 2-3 退火 14 2-4光催化降解原理及機制 15 2-4-1 二氧化鈦光催化降解過程 15 2-4-2 銀摻雜之二氧化鈦光催化降解過程 16 2-4-3 薔薇紅光催化降解機制 19 第三章 實驗內容 21 3-1 實驗流程 21 3-2 實驗儀器 22 3-3 實驗藥品與金屬基板 23 3-4 實驗步驟與實驗裝置 24 3-4-1 鈦片前處理 24 3-4-2 電解液配置 24 3-4-3 製備二氧化鈦奈米管 24 3-4-4 電沉積銀 26 3-4-5 性質分析 27 第四章 結果與討論 32 4-1 氟化銨濃度對二氧化鈦奈米管之影響 32 4-1-1 表面形貌分析 32 4-1-2 晶型鑑定結果 34 4-1-3 元素分析 35 4-1-4 光催化效能分析 36 4-1-5 製備二氧化鈦奈米管之氟化銨濃度選擇 39 4-2退火溫度對二氧化鈦奈米管之影響 40 4-2-1 表面形貌分析 40 4-2-2 晶型鑑定結果 41 4-2-3 光催化效能分析 42 4-2-4 製備二氧化鈦奈米管之退火溫度選擇 44 4-3 陽極氧化電位對二氧化鈦奈米管之影響 45 4-3-1 表面形貌分析 45 4-3-2 晶型鑑定結果 46 4-3-3 光催化效能分析 47 4-3-4 製備二氧化鈦奈米管之陽極氧化電位選擇 49 4-4 陽極氧化時間對二氧化鈦奈米管之影響 50 4-4-1 表面形貌分析 50 4-4-2 晶型鑑定結果 53 4-4-3 光催化效能分析 54 4-4-4 製備二氧化鈦奈米管之陽極氧化時間選擇 55 4-5 銀摻雜對二氧化鈦奈米管之影響 56 4-5-1 不同脈衝電流下摻雜銀 56 4-5-2 不同硝酸銀濃度下摻雜銀 61 4-5-3 不同脈衝循環次數下摻雜銀 64 4-6 所製備材料與其他文獻比較之結果 68 第五章 結論 70 參考文獻 72 附錄 79

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