臺灣博碩士論文加值系統

此研究係利用高壓水熱法(hydrothermal methods)來合成銀釩氧化合物以及銀釩氧化合物複合氧化石墨烯(graphene oxide, GO)，並以可見光作為光源，降解草脫淨(Atrazine)及結晶紫染料(Crystal Violet ,CV) 。本實驗首先以硝酸銀、偏釩酸銨及氧化石墨烯為起始物，分別溶解在去離子水 ( DI water )中攪拌並混合，並利用氨水(NH4OH)調整pH值，之後將該水溶液裝入至23毫升高壓釜並放置烘箱中加熱。最終得到的觸媒樣品以X射線粉末繞射儀(XRD)、場發掃描式電子顯微鏡及能量分散譜儀(FE-SEM-EDS)、場發穿透式電子顯微鏡(FE-TEM)、傅立葉轉換紅外線光譜儀(FT-IR) 、紫外光-可見光漫反射光譜儀(DRS)、比表面積分析儀(BET) 、X射線光電子能譜儀(XPS)等儀器分析鑑定材料的特性。最後，利用不同條件之光觸媒降解Atrazine和CV，並探討銀釩氧化合物及銀釩氧化合物複合GO對於光催化效率的影響。研究結果發現，AgxVyOz之最佳參數條件，不論是用於降解草脫淨或結晶紫染料皆具有良好之效果。並且，複合GO後，不只縮短其降解時間，另一面也提高了光觸媒之穩定性及回收效率。

In this study, a series of the silver vanadium oxide and silver vanadium oxide composite graphene oxide (GO) are prepared using hydrothermal methods, and using the visible light as the light source of degradation of Atrazine and CV. In the experiment, first, AgNO3 、NH4VO3 and commercial GO are used as the starting material, then seperately dissolved in DI water, stirring and mixing, and using NH4OH to adjust the pH value. Then the aqueous solution is placed in a 23ml autoclave and put into an oven, and heated. The ultimate products of photocatalyst are characterized by XRD, FE-SEM-EDS, FE-TEM, FT-IR, DRS, BET, and HR-XPS. Last, using different conditions of photocatalyst to conduct the process of degradation of Atrazine and CV, investigating silver vanadium oxide and silver vanadium oxide/GO for photocatalytic efficiency. In the study, we collect that the best parameter condition of AgxVyOz is effective in the degradation of both Atrazine and Crystal Violet. Moreover, the composite of AgxVyOz and GO not only shortens the duration of degradation, but also increases the stability and the quantity of recycling of photocatalyst.

摘要 Ⅰ
Abstract Ⅱ
目錄 Ⅲ
圖目錄 VI
表目錄 XII
第一章 緒論 1
1.1 研究動機 1
1.2 研究目的 4
第二章 文獻回顧 5
2.1 光觸媒(Photocatalyst) 5
2.2銀釩氧化合物 6
2.3氧化石墨烯(Graphene oxide) 10
2.4草脫淨(Atrazine) 12
2.5結晶紫染料(Crystal Violet) 15
第三章 實驗材料與方法 16
3.1實驗架構 16
3.2 實驗材料 17
3.2.1觸媒合成之材料及儀器藥品 17
3.2.2草脫淨 18
3.2.3結晶紫染料 18
3.3 實驗合成 19
3.3.1銀釩氧化合物的合成(以Ag:V=3:1為例) 19
3.3.2銀釩氧化合物複合GO的合成(以Ag:V=3:1為例) 20
3.4 實驗合成樣品總表 21
3.5樣品材料鑑定及特性分析 23
3.6光催化降解測試 24
3.7實驗儀器設備 26
3.7.1儀器廠牌規格 26
3.7.2儀器條件 27
第四章 結果與討論 29
4.1 AgxVyOz之表面特性分析 29
4.1.1改變AgxVyOz之銀釩莫耳比 30
4.1.1.1 X射線繞射分析儀 30
4.1.1.2 場發式掃描電子顯微鏡(FE-SEM-EDS) 35
4.1.1.3 紫外光/可見光漫反射光譜儀(DRS) 41
4.1.1.4 傅立葉轉換紅外光譜儀(FT-IR) 46
4.1.1.5 X射線光電子能譜儀(XPS) 47
4.1.1.6 場發式穿透電子顯微鏡(TEM) 50
4.1.1.7 比表面積及孔徑測定儀(BET) 52
4.1.1.8 光降解效率分析─透過高效液相層析儀(HPLC) 55
4.1.1.9 光降解效率分析─透過紫外光可見光分光光譜儀 58
4.1.1.10 活性物種測試-草脫淨 61
4.1.1.11 活性物種測試-結晶紫染料 62
4.1.2改變AgxVyOz之合成溫度 63
4.1.2.1 X射線繞射分析儀 63
4.1.2.2 場發式掃描電子顯微鏡(FE-SEM-EDS) 67
4.1.2.3 紫外光/可見光漫反射光譜儀(DRS) 72
4.1.2.4 光降解效率分析─透過高效液相層析儀(HPLC) 77
4.1.2.5 光降解效率分析─透過紫外光可見光分光光譜儀 82
4.1.2.6 光觸媒之穩定性與回收率-草脫淨 89
4.1.2.7 光觸媒之穩定性與回收率-結晶紫染料 91
4.1.3AgxVyOz結論 93
4.2 AgxVyOz/GO之表面特性分析 94
4.2.1改變AgxVyOz/GO之合成溫度 95
4.2.1.1 X射線繞射分析儀 95
4.2.1.2 場發式掃描電子顯微鏡(FE-SEM-EDS) 97
4.2.1.3 紫外光/可見光漫反射光譜儀(DRS) 100
4.2.1.4 傅立葉轉換紅外光譜儀(FT-IR) 102
4.2.2改變AgxVyOz/GO之合成時間 103
4.2.2.1 X射線繞射分析儀 103
4.2.2.2 場發式掃描電子顯微鏡(FE-SEM-EDS) 106
4.2.2.3 紫外光/可見光漫反射光譜儀(DRS) 109
4.2.2.4 光降解效率分析─透過高效液相層析儀(HPLC) 111
4.2.2.5 光降解效率分析─透過紫外光可見光分光光譜儀 113
4.2.3改變AgxVyOz/GO之複合GO的量 116
4.2.3.1 X射線繞射分析儀 116
4.2.3.2 場發式掃描電子顯微鏡(FE-SEM-EDS) 118
4.2.3.3 紫外光/可見光漫反射光譜儀(DRS) 121
4.2.3.4 場發式穿透電子顯微鏡(TEM) 124
4.2.3.5 比表面積及孔徑測定儀(BET) 126
4.2.3.6 光降解效率分析─透過高效液相層析儀(HPLC) 129
4.2.3.7 活性物種測試-草脫淨 134
4.2.3.8 光觸媒之穩定性與回收率-草脫淨 135
4.2.3.9 光降解效率分析─透過紫外光可見光分光光譜儀 137
4.2.3.10 活性物種測試-結晶紫染料 140
4.2.3.11 光觸媒之穩定性與回收率-結晶紫染料 141
4.2.3.12 草脫淨之中間產物分析 144
4.2.3.13 近年來光催化降解草脫淨效果之文獻比較 147
4.2.4AgxVyOz/GO結論 148
第五章 結論與建議 149
5.1 結論 149
5.2 未來方向與建議 151
參考文獻 152

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