臺灣博碩士論文加值系統

本研究以水熱法製備釩酸銀(Ag3VO4)，前驅物為硝酸銀及正釩酸鈉，合成條件銀釩比保持3:1，過程中加入硝酸鉍Bi(NO3)3‧5H2O進行改質，Bi2O3/Ag3VO4莫爾比分別為0.25、0.5、0.75及1，分別命名為B/A=0.25、B/A=0.5、B/A=0.75及B/A=1，並以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，接著改變染料pH值及添加不同劑量之觸媒進行光催化實驗，並進行太陽光實驗測試，探討不同變因之影響。
Ag3VO4改質前後均以X−光繞射儀(X-ray diffraction, XRD)鑑定其結晶相、掃描式電子顯微鏡(Scanning electron microscope, SEM)與穿透式電子顯微鏡(Transmission electron microscope, TEM)觀察改質前後表面形貌之改變、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、光激螢光分光光譜儀(Photoluminescence, PL)鑑定電子電洞重組率、傅立葉轉換紅外光譜(Fourier transform infrared spectroscopy, FTIR)進行觸媒官能基鑑定分析，以界達電位(Zeta potential)測定表面電性分析，以電子能譜儀(X-ray photoelectron spectrometer, XPS)進行觸媒之元素組成鑑定與化學鍵結分析，最後以感應式耦合電漿原子發射光譜(Inductively coupled plasma-optical emission spectrometry, ICP-OES)進行金屬溶出實驗。
以XRD鑑定改質前後之結晶相發現，改質後觸媒在三氧化二鉍的特徵峰位置，隨著改質比例的提升，特徵峰隨之明顯，以PL分析發現，改質後觸媒電子電洞對的再結合率有效降低，有助於光催化反應的進行，以ICP-OES測定金屬溶出，發現Ag3VO4在反應後會有大量Ag溶出，導致回收率不佳。
本研究以400W之氙燈進行光催化實驗，紫外-可見光實驗中發現，改質前Ag3VO4之RR2在紫外-可見光下的去除率為90.5%，可見光下去除率僅62.7%，由擬一階反應方程式計算，反應常數分別為0.014及0.0098 min-1，改質過後，在紫外-可見光下以B/A=0.75為最佳化配比，去除率提升至97.6%，反應常數為0.115 min-1，大幅提升紫外-可見光下的反應速率，在可見光照射下以B/A=1為最佳化配比，去除率達92.2%，反應常數為0.039 min-1，在反應速率及效率皆有明顯提升，且發現經改質後之觸媒，回收率隨改質比例提高而上升，在B/A=1的配比下可達60%，利用酸性和鹼性環境進行實驗比對，發現B/A=0.75在酸性環境下的去除效率比鹼性環境提升了20%，並進行太陽光實驗，改質後之觸媒在太陽光激發下具有良好活性，且隨改質比例提升，反應速率越快。

This study synthesized Ag3VO4 via the hydrothermal method. Silver nitrate (AgNO3), sodium vanadate (Na3VO4) and bismuth nitrate (Bi(NO3)3) were used as the precursors of Ag, V and Bi, respectively. The molar ratio of AgNO3/Na3VO4 was 3 for all experiments. This study synthesized Bi2O3/Ag3VO4 (B/A) using the molar ratio of Bi2O3/Ag3VO4 0.25, 0.5, 0.75 and 1. The photocatalytic activity of the Bi2O3/Ag3VO4 was determined by the photodegradation of C.I. Reactive Red 2 (RR2). The prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-Vis spectroscopy (UV-Vis), photoluminescence (PL), zeta potential meter, Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy and inductively coupled plasma optical emission spectrometry (ICP-OES).The intensity of characteristic peak of Bi2O3 increased with the Bi coupling ratio increasing. The PL spectra showed that doping Bi2O3 effectively decreased the recombination of photogenerated electrons and holes in Ag3VO4. The ICP-OES results showed that Ag3VO4 almost dissolved completely after the photodegradation. After 60 min reaction, the RR2 removal efficiency of Ag3VO4 under ultraviolent (UV) and visible light were 90.5% and 62.7%, respectively; moreover, that of B/A=1 was 97.6% and 92.2%, respectively., The RR2 degradation rate constants of Ag3VO4 and B/A=1 under UV irradiation were 0.014 min-1 and 0.115 min-1, respectively, additionally, those of under visible light irradiation were 0.0098 min-1 and 0.039 min-1, respectively. The photocatalytic activity and recovery rate of Ag3VO4 was promoted by coupling with Bi2O3.

目錄
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 4
2-1. 高級氧化處理 4
2-1.1 光催化氧化反應(Photocatalysis) 4
2-2. 釩酸銀(Ag3VO4)特性及製備方法 8
2-3. 三氧化二鉍(Bi2O3)特性 11
2-4. 釩酸銀(Ag3VO4)摻雜改質 11
2-4.1 金屬改質 11
2-4.2 非金屬改質 12
2-4.3 金屬氧化物改質 13
第三章 實驗方法 15
3-1. 研究架構 15
3-2. 藥品及儀器 16
3-3. 實驗流程與變因 17
3-4. 物性分析 19
3-4.1 X光繞射分析儀 19
3-4.2 掃描式電子顯微鏡 19
3-4.3 傅立葉轉換紅外光譜 19
3-4.4 可見光紫外光分光光譜儀 20
3-4.5 X射線光電子能譜 21
3-4.6 螢光分光光譜儀 21
3-4.7 穿透式電子顯微鏡 21
3-4.8 感應耦合電漿原子發射光譜儀 22
3-4.9 界達電位 22
3-5. 光催化活性實驗 23
3-5.1 直接光解實驗 25
3-5.2 吸附實驗 25
3-5.3 紫外-可見光降解實驗 25
3-5.4 可見光降解實驗 26
3-5.5 太陽光降解實驗 26
3-5.6 pH效應 27
3-5.7 再利用實驗 28
3-5.8 自由基捕捉實驗 28
3-5.9 反應動力學模擬 29
3-5.10 金屬溶出實驗 29
第四章 結果與討論 30
4-1. 改質前後樣品圖 30
4-2. 表面特性分析 30
4-2.1 晶相比較分析 30
4-2.2 表面型態觀察分析 34
4-2.3 原子結構觀察分析 38
4-2.4 官能基鑑定分析 39
4-2.5 吸收波長及能隙值鑑定分析 42
4-2.6 螢光光譜測定分析 43
4-2.7 元素組成分析 44
4-2.8 金屬溶出測定分析 54
4-2.9 表面電性分析 55
4-3. 光催化反應探討 56
4-3.1 直接光解效率 56
4-3.2 吸附效率 57
4-3.2 紫外-可見光及可見光降解效率 58
4-3.3 太陽光降解效率 63
4-3.4 pH效應影響探討 64
4-3.5 再利用性探討 65
4-3.6 自由基測定分析 67
4-3.7 一階動力學模擬 68
第五章 結論與建議 71
5-1. 結論 71
5-2. 建議 72
參考文獻 73

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