臺灣博碩士論文加值系統

本研究利用水熱法在 pH 7 下合成觸媒合成釩酸鉍(BiVO4)、釩酸銀(Ag3VO4)及三氧化二
鉍(Bi2O3 Hydrothermal, BOH)，另以溶劑熱法合成三氧化二鉍(Bi2O3 Solvothermal, BOS)，將
BOH 及 BOS 燒結條件為 200℃, 12hr 稱為 BOH-1 及 BOS-1；燒結條件為 120℃, 6hr 稱為
BOH-2 及 BOS-2，將水熱法合成 BiVO4 前驅液與水熱法合成 Ag3VO4 前驅液以莫耳比 1:1 透
過液-液一步驟合成觸媒 BA-1，將水熱法合成 BiVO4 前驅液與水熱法合成 Ag3VO4 前驅液以
莫耳比 1:2 及 2:1 透過液-液一步驟合成觸媒 BA-2 及 BA-3，將水熱法合成觸媒粉末 BiVO4 與
水熱法合成 Ag3VO4 前驅液以莫耳比 1:1 透過固-液二步驟合成觸媒 BA-4，將水熱法合成觸媒
粉末 Ag3VO4 與水熱法合成 BiVO4 前驅液以莫耳比 1:1 透過固-液二步驟合成觸媒 BA-5，將水
熱法合成 Bi2O3 前驅液、水熱法合成 BiVO4 前驅液與水熱法合成 Ag3VO4 前驅液以莫耳比
1:1:1 透過液-液-液一步驟合成 BBA-1，將觸媒 BOH-1 及 BOS-1 分別與 BA-1 前驅液透過固-
液二步驟合成 BBA-2 及 BBA-3，將觸媒 BA-1 與 BOH-1, BOS-1, BOH-2 及 BOS-2 前驅液透
過固-液二步驟合成 BBA-4 至 BBA-7，以反應紅二(C.I. Reactive Red 2, RR2)為目標污染物進
行光催化降解實驗，找出最佳化觸媒並進行表面物性分析、重複使用性實驗、活性物種捕捉
實驗及太陽光實驗。
BiVO4, Ag3VO4 合成為觸媒 BA 系，Bi2O3, BiVO4 及 Ag3VO4 合成為觸媒 BBA 系，合成前
後以 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)觀察改質前後
表面形貌、比表面積分析儀(Brunauer-Emmett-Teller, BET)分析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
觸媒表面電位及分散穩定性、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、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。
光催化反應 60 分鐘後 Ag3VO4 之紫外光光催化效率達 97%，觸媒 BA-1 及 BBA-1 紫外光
光催化效率為 92%及 99%；Ag3VO4 之可見光光催化效率僅 10%，觸媒 BA-1 及 BBA-1 可見
光光催化效率分別為 82%及 97%。活性物種捕捉實驗發現，BA-1,BBA-1 及 BBA-7 之主要反
應物種為電洞。觸媒 BA-1, BBA-1 及 BBA-7 可有效抑制電子電洞的再結合，進而提升觸媒對
污染物的降解效率。
將 BA-1, BBA-1 及 BBA-7 進行 ICP-OES 實驗，BA-1, BBA-1 及 BBA-7 之 Ag 總溶出率
分別為 9.33%, 36.2%及 16.6%，推測 BA-1 最能穩定 Ag3VO4 結構。將紫外光光催化反應後之
觸媒 BA-1, BBA-1 及 BBA-7 進行表面特性分析，反應後觸媒之 XRD 特徵峰訊號值以 BA-1
下降幅度最小；SEM 及 TEM 分析結果發現，Ag3VO4 於光催化實驗後有結構崩壞之現象，僅
BA-1 之形貌存在 Ag3VO4 最多且最完整；BET 分析反應後觸媒之比表面積變化發現，BA-1
之比表面積由 4.21 m2g-1 升至 6.95 m2g-1; BBA-1 比表面積由 10.22 m2g-1 升至 12.43 m2g-1; BBA-
7 比表面積由 11.34 m2g-1 升至 11.69 m2g-1。
觸媒 BA-1, BBA-1 及 BBA-7 對目標污染物進行可見光光催化降解實驗，效率以 BBA-7
為最佳可達 97%；重複使用實驗以觸媒 BA-1 為最佳，重複三次光催化實驗效率尚未衰退。


關鍵字：釩酸鉍、釩酸銀、三氧化二鉍、光觸媒、光催化

BiVO4/Ag3VO4 coupled-photocataltst was prepared by hydrothermal method permeation liquidliquid one-step process with BiVO4/Ag3VO4 molar ratio of 1 and was denoted as BA-1.
BiVO4/Ag3VO4/Bi2O3 coupled-photocataltst was generated by hydrothermal method permeation
liquid-liquid-liquid one-step process with BiVO4/Ag3VO4/Bi2O3 molar ratio of 1/1/1 and was
denoted as BBA-1. Adding BA-1 to Bi2O3 precursor solution with BiVO4/Ag3VO4/Bi2O3 molar ratio
of 1/1/1 by sovolthermal method, the generated coupled-photocataltst was noted as BBA-7. C.I.
Reactive Red 2 (RR2) was selected as the target compound. The surface characteristics and
photocatalytic activities of prepared photocatalysts were determined and compared in this study. The
surface properties of photocatalysts were characterized by X-ray diffraction (XRD), brunauer
Emmett teller (BET), scanning electron microscopy (SEM), transmission electron microscopy
(TEM), UV-Vis spectroscopy (UV-Vis), photoluminescence (PL), inductively coupled plasma optical
emission spectrometry (ICP-OES), zeta potential meter and X-ray photoelectron spectroscopy (XPS).
After 60 minutes of UV irradiation, the RR2 removal efficiency of Ag3VO4 was 97%, the RR2
removal percentage of BA-1 and BBA-1 was 92% and 99%, respectively; after 60 minutes of visible
light irradiation, the RR2 removal efficiency of Ag3VO4 was 10%, the RR2 removal percentage of
BA-1 and BBA-1 were 82% and 97%, respectively. The experimental results of active oxidation
species trapping revealed that hydroxyl radicals could be ignored in BA-1, BBA-1 and BBA-7
system, conversely, the photogenerated hole (h+) played a major role and photoinduced electrons
played a minor role in the BA-1, BBA-1 and BBA-7 system. The ICP-OES results showed that BA-
1, BBA-1 and BBA-7 under UV light irradiation showed the Ag dissolution ratio after three times
photocatalysis was 9.33%, 36.2% and 16.6%. The used BA-1, BBA-1 and BBA-7 were characterized
by SEM and found the structure of the used Ag3VO4 collapsed. According to the SEM and TEM
observation, the used BA-1 showed that Ag3VO4 was remain immobilized on the surface of BiVO4
and the structure was not destroyed. After three times photocatalysis, the specific surface area of BA-
1 increased from 4.21 m2/g to 6.95 m2/g; BBA-1 increased from 10.22 m2/g to 12.43 m2/g and BBA-
7 increased from 11.34 m2/g to 11.69 m2/g.


Keywords: BiVO4; Ag3VO4; Bi2O3; photocatalyst; photodegradation

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..................................................................................................................................3
2-1 高級氧化處理法 ........................................................................................................................3
2-1.1 光催化(Photocatalysis) .......................................................................................................3
2-1.2 光化學法(Photochemical Method) .....................................................................................4
2-2 偶氮染料 ....................................................................................................................................5
2-3 釩酸鉍(BiVO4)特性及合成方法...............................................................................................9
2-3.1 BiVO4 金屬氧化物改質.....................................................................................................16
2-4 釩酸銀(Ag3VO4)特性及合成方法 ..........................................................................................26
2-4.1 Ag3VO4 金屬氧化物改質 ..................................................................................................30
2-5 三氧化二鉍(Bi2O3)材料特性 ..................................................................................................35
第三章 實驗方法................................................................................................................................40
3-1 研究架構 ..................................................................................................................................40
3-2 藥品及儀器 ..............................................................................................................................41
3-3 觸媒命名及合成流程 ..............................................................................................................43
3-3.1 觸媒之命名 .......................................................................................................................43
3-3.2 觸媒合成流程 ...................................................................................................................45
3-3.2.1 水熱法合成 BiVO4 ....................................................................................................45
3-3.2.2 水熱法合成 Ag3VO4..................................................................................................46
3-3.2.3 水熱法合成 Bi2O3......................................................................................................47
3-3.2.4 溶劑熱法合成 Bi2O3..................................................................................................48
3-3.2.5 BA-1 之合成 ...............................................................................................................49
3-3.2.6 BA-2 之合成 ...............................................................................................................50
3-3.2.7 BA-3 之合成 ...............................................................................................................50
VIII
3-3.2.8 BA-4 之合成 ...............................................................................................................51
3-3.2.9 BA-5 之合成 ...............................................................................................................51
3-3.2.10 BBA-1 之合成...........................................................................................................52
3-3.2.11 BBA-2 之合成...........................................................................................................52
3-3.2.12 BBA-3 之合成...........................................................................................................53
3-3.2.13 BBA-4 之合成...........................................................................................................53
3-3.2.14 BBA-5 之合成...........................................................................................................54
3-3.2.15 BBA-6 之合成...........................................................................................................54
3-3.2.16 BBA-7 之合成...........................................................................................................55
3-4 物性分析 ..................................................................................................................................58
3-4.1 紫外-可見光光譜儀(Ultraviolet-Visible Spectroscopy, UV-Vis).....................................58
3-4.2 X 光繞射分析儀(X-Ray Diffraction, XRD)......................................................................59
3-4.3 X 射線光電子能譜(X-Ray Photoelectron Spectroscopy, XPS) ........................................59
3-4.4 掃描式電子顯微鏡(Scanning Electron Microscope, SEM) .............................................59
3-4.5 穿透式電子顯微鏡(Transmission Electron Microscope, TEM) ......................................60
3-4.6 光激螢光分光光譜儀(Photoluminescence, PL)...............................................................60
3-4.7 比表面積分析儀(Brunauer-Emmett-Teller, BET)............................................................60
3-4.8 感應耦合電漿發射光譜儀(Inductively Coupled Plasma Optical Emission Spectrometry,
ICP-OES) .....................................................................................................................................62
3-4.9 粒徑分析儀(Particle Size Analyzer).................................................................................62
3-4.10 界達電位儀(Zeta Potential) ............................................................................................63
3-5 光催化活性實驗 ......................................................................................................................63
3-5.1 直接光解實驗 ...................................................................................................................65
3-5.2 吸附實驗 ...........................................................................................................................65
3-5.3 紫外光降解實驗 ...............................................................................................................66
3-5.4 可見光降解實驗 ...............................................................................................................66
3-5.5 pH 效應實驗 ......................................................................................................................66
3-5.6 活性物種捕捉實驗 ...........................................................................................................67
3-5.7 重複使用性實驗 ...............................................................................................................67
3-5.8 金屬溶出實驗 ...................................................................................................................68
3-5.9 太陽光降解實驗 ...............................................................................................................68
3-5.10 反應動力學模擬 .............................................................................................................68
第四章 結果與討論............................................................................................................................69
4-1 觸媒粉末樣品說明 ..................................................................................................................69
4-2 表面特性分析 ..........................................................................................................................70
4-2.1 晶相分析 ...........................................................................................................................70
4-2.2 掃描式電子顯微鏡分析 ...................................................................................................82
4-2.3 穿透式電子顯微鏡分析 ..................................................................................................100
IX
4-2.4 比表面積分析 .................................................................................................................105
4-2.5 電子-電洞對再結合率比較............................................................................................107
4-2.6 表面電性分析 .................................................................................................................109
4-2.7 觸媒光譜吸收範圍及能隙值鑑定 .................................................................................110
4-2.8 元素組成及鍵結分析 .....................................................................................................113
4-3 光催化活性實驗結果 ............................................................................................................123
4-3.1 直接光解 .........................................................................................................................123
4-3.2 Ag3VO4 光催化實驗結果 ................................................................................................124
4-3.3 Bi2O3 光催化實驗結果 ....................................................................................................125
4-3.4 BiVO4 光催化實驗結果...................................................................................................127
4-3.5 Ag3VO4, BiVO4 及 BA-1 之光催化實驗結果.................................................................127
4-3.6 BA-1, BA-2 及 BA-3 之光催化實驗結果.......................................................................128
4-3.7 BA-1, BA-4 及 BA-5 之光催化實驗結果.......................................................................129
4-3.8 BA-1 及 BBA-1 之光催化實驗結果...............................................................................130
4-3.9 BBA-1, BBA-2, BBA-3, BBA-4 及 BBA-5 之光催化實驗結果 ...................................131
4-3.10 BBA-1, BBA-6 及 BBA-7 之光催化實驗結果.............................................................133
4-3.7 pH 效應 ............................................................................................................................137
4-3.8 重覆使用性實驗 .............................................................................................................138
4-3.9 金屬溶出分析 .................................................................................................................141
4-3.10 活性物種捕捉實驗 .......................................................................................................143
4-3.11 觸媒光催化反應動力學模擬 .......................................................................................146
4-3.12 太陽光實驗 ...................................................................................................................151
4-4 光觸媒催化反應機制 ............................................................................................................154
4-5 光催化反應實驗後之表面分析 ............................................................................................157
4-5.1 晶相分析 .........................................................................................................................157
4-5.2 掃描式電子顯微鏡分析 .................................................................................................160
4-5.3 穿透式電子顯微鏡分析 ..................................................................................................165
4-5.4 比表面積分析 .................................................................................................................172
第五章 結論與建議..........................................................................................................................174
5-1 結論 ........................................................................................................................................174
5-2 建議 ........................................................................................................................................175
參考文獻............................................................................................................................................176

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