臺灣博碩士論文加值系統

本研究以水熱法合成釩酸銀(Ag3VO4)及鎢酸鉍(Bi2WO6)，並透過液-液一步驟及固-液二步驟複合Ag3VO4及Bi2WO6，複合後觸媒稱為AB系觸媒，以液-液一步驟合成過程中Ag3VO4/Bi2WO6莫耳比為1, 0.5, 0.33, 0.25及2，分別命名為AB-1, AB-2, AB-3, AB-4及AB-5，以固-液二步驟合成過程中，將水熱法觸媒粉末Ag3VO4與水熱法Bi2WO6前驅液以莫耳比1:1合成觸媒命名為AB-6；將水熱法觸媒粉末Bi2WO6與水熱法Ag3VO4前驅液以莫耳比1:1合成觸媒命名為AB-7；將水熱法觸媒粉末Bi2WO6與水熱法Ag3VO4前驅液以莫耳比3:1合成觸媒命名為AB-8，以C.I. Reactive Red 2 (RR2)為目標污染物進行光催化降解實驗，找出最佳配比，並進行表面分析、pH效應實驗、活性物種捕捉實驗、重複再使用實驗及太陽光實驗。
Ag3VO4及Bi2WO6複合前後皆以X-光繞射儀(X-Ray Diffraction, XRD)鑑定其晶相、掃描式電子顯微鏡(Scanning Electron Microscope, SEM)及穿透式電子顯微鏡(Transmission Electron Microscope, TEM)觀察複合前後表面之形貌、比表面積分析儀(Brunauer-Emmett-Teller, BET)分析其比表面積及孔洞大小、螢光分光光譜儀(Photoluminescence, PL)鑑定電子電洞對再結合率、界達電位儀(Zeta-Potential)測定觸媒表面電位、紫外-可見光光譜儀(UV-Vis Spectrophotometer)分析臨界吸收波長並計算觸媒能隙值及電子能譜儀(X-Ray Photoelectron Spectrometer, XPS)進行觸媒之元素組成鑑定與化學鍵結分析。
以BET分析比表面積發現，複合後觸媒除了AB-6及AB-7，其餘觸媒比表面積皆有提升之趨勢。透過PL分析得知，複合後觸媒之電子電洞再結合率與複合前相比皆有下降趨勢。以紫外-可見光光譜儀分析各觸媒之臨界吸收波長，發現複合後觸媒之吸收臨界波長皆落在可見光區段。XPS分析結果得知Ag-O及Bi-O鍵比例符合本研究複合觸媒所使用之配比。ICP-OES分析金屬溶出得知複合後大幅降低Ag流失，且可提升觸媒結構之穩定性。
複合前之Ag3VO4在可見光系統下反應60分鐘，其RR2去除效率僅有24%，複合後最佳觸媒AB-3在可見光系統下反應60分鐘，RR2去除效率高達93%，複合後在可見光系統下之去除效率明顯提升。經活性物種捕捉實驗後得知AB-3觸媒主要反應物種為電洞，複合後之電子電洞再結合率明顯被抑制，因而提高了光催化效率。

Silver vanadate (Ag3VO4) and bismuth tungstate (Bi2WO6) were prepared by a hydrothermal method. Ag3VO4/Bi2WO6 hybrid photocatalyst was prepared by the hydrothermal method and permeation liquid-liquid one-step process with Ag3VO4/Bi2WO6 with a molar ratio of 0.33, denoted as AB-3. C.I. Reactive Red 2 (RR2) was the target compound. The surface characteristics and photocatalytic activities of the prepared photocatalysts were determined and compared. The surface properties of the photocatalysts were characterized by X-ray diffraction (XRD), Brunauer Emmett Teller analysis (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-Vis spectroscopy (UV-Vis), photoluminescence analysis (PL), inductively coupled plasma optical emission spectrometry (ICP-OES), zeta potential analysis and X-ray photoelectron spectroscopy (XPS).
The specific surface area increased from 0.056 m2/g for Ag3VO4 to 36.68 m2/g for AB-3. The recombination rate of electron and holes decreased after the synthesis of AB-3. The ICP-OES results reveal that AB-3 under UV light irradiation, the Ag dissolution ratio after three instances of photocatalysis was 18.89%. After 60 minutes of irradiation by visible light, the RR2 removal efficiency of Ag3VO4 was 24%, and the RR2 removal percentage of AB-3 was 93%. The experimental results concerning the trapping of active oxidation species indicate that the photogenerated holes (h+) played an important role in the AB-3 system.

摘要 I
Abstract III
致謝 V
目錄 VI
表目錄 IX
圖目錄 X
第一章 緒論 1
1-1 研究動機 1
1-2 研究目的及內容 2
第二章 文獻回顧 2
2-1 高級氧化處理法 3
2-1.1 光催化(Photocatalysis) 3
2-2 偶氮染料 4
2-3 釩酸銀(Ag3VO4) 8
2-3.1 Ag3VO4金屬氧化物改質 10
2-4 鎢酸鉍(Bi2WO6) 13
2-4.1 Bi2WO6金屬氧化物改質 15
第三章 實驗方法 18
3-1 研究架構 18
3-2 藥品及儀器 19
3-3 觸媒命名及實驗流程 21
3-3.1 觸媒之命名 21
3-3.2 觸媒合成流程 22
3-4 物性分析 35
3-4.1 紫外-可見光光譜儀(Ultraviolet-Visible Spectroscopy, UV-Vis) 35
3-4.2 X射線光電子能譜(X-Ray Photoelectron Spectroscopy, XPS) 36
3-4.3 X光繞射分析儀(X-Ray Diffraction, XRD) 36
3-4.4 掃描式電子顯微鏡(Scanning Electron Microscope, SEM) 36
3-4.5 穿透式電子顯微鏡(Transmission Electron Microscope, TEM) 37
3-4.6 光激螢光分光光譜儀(Photoluminescence, PL) 37
3-4.7 比表面積分析儀(Brunauer-Emmett-Teller, BET) 37
3-4.8 感應耦合電漿發射光譜儀(Inductively Coupled Plasma Optical Emission Spectrometry, ICP-OES) 39
3-4.9 粒徑分析儀(Particle Size Analyzer) 39
3-4.10 界達電位儀(Zeta Potential) 40
3-5 光催化活性實驗 40
3-5.1 直接光解實驗 42
3-5.2 吸附實驗 42
3-5.3 紫外光降解實驗 43
3-5.4 可見光降解實驗 43
3-5.5 pH效應實驗 43
3-5.6 活性物種捕捉實驗 44
3-5.7 重複使用性實驗 44
3-5.8 金屬溶出實驗 45
3-5.9 太陽光降解實驗 45
3-5.10 反應動力學模擬 45
第四章 結果與討論 47
4-1 觸媒粉末樣品說明 47
4-2 表面特性分析 48
4-2.1 晶相分析 48
4-2.2 掃描式電子顯微鏡分析 54
4-2.3 穿透式電子顯微鏡分析 65
4-2.4 比表面積分析 68
4-2.5 電子電洞對再結合率分析 69
4-2.6 表面電性分析 70
4-2.7 觸媒光譜吸收範圍及能隙值鑑定 71
4-2.8 元素組成及鍵結分析 73
4-3 光催化活性實驗 82
4-3.1 直接光解 83
4-3.2 Ag3VO4光催化實驗結果 83
4-3.3 Bi2WO6光催化實驗結果 84
4-3.4 Ag3VO4, Bi2WO6及AB-1之光催化實驗結果 85
4-3.5 AB-1, AB-2, AB-3及AB-4之光催化實驗結果 86
4-3.6 AB-3及AB-5之光催化實驗結果 87
4-3.7 AB-3, AB-6, AB-7及AB-8之光催化實驗結果 88
4-3.8 AB-3之三重複實驗 90
4-3.9 pH效應實驗 91
4-3.10 重複再使用實驗 93
4-3.11 金屬溶出分析 95
4-3.12 活性物種捕捉實驗 96
4-3.13 觸媒光催化反應動力學模擬 97
4-3.14 太陽光實驗 100
4-4 光觸媒催化反應機制 102
4-5 光催化反應實驗後之表面分析 104
4-5.1 反應後觸媒之晶相分析 104
4-5.2 反應後觸媒之掃描式電子顯微鏡分析 106
4-5.3 反應後觸媒之穿透式電子顯微鏡分析 108
4-5.4 反應後觸媒之比表面積分析 111
第五章 結論與建議 113
5-1 結論 113
5-2 建議 114
參考文獻 115

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