臺灣博碩士論文加值系統

本論文利用化學溶液反應法--油浴法合成氧化鋅奈米顆粒，進行可見光觸媒特性研究。此合成方式不需昂貴真空設備，並且可於5分鐘合成氧化鋅奈米柱，且具備可大量生產且製造成本低之優點，對於商業化之應用極具發展潛力。
使用乙醯丙酮鋅粉末(Zinc acetylacetonate hydrate，(Zn(C5H7O2)2．H2O，純度＞95 %；C5H7O2簡稱AcAc；以下簡稱Zn(AcAc)2)做為提供成長氧化鋅之有機金屬來源並添加變性酒精(Denatured ethanol)與去離子水(DI water)做為溶劑配製前驅物，將此前驅物置於圓底燒杯中，以矽油浴法加熱至200 ℃，並藉由熱還原法將銀離子摻雜入氧化鋅奈米顆粒中。使用油浴法熱裂解合成之氧化鋅奈米柱，為六角柱體之纖鋅礦結構(HCP, Wurzite sturcture)，具自組裝行為方向性附加(Oriented attachment)之成長模式，經由光致發光(PL)與X光光電子能譜儀(XPS)進行檢測，利用此方式合成之氧化鋅為缺陷型光觸媒。在本研究中，發現熱裂解5分鐘合成之氧化鋅奈米柱，具有最高濃度之雙電荷氧空缺，間接產生大量之氫氧根自由基(OH radical)，並經由光觸媒光催化降解甲基橙實驗中，具有最優良之降解效率，且催化效果優於目前市售之商用TiO2 Degussa P25之催化效果。此研究，生產成本低，製程時間短，成長溫度低，適合大量製造，因此在光觸媒與其他氧化鋅相關產業之應用具有極大發展潛力。

In this study, ZnO (Znic oxide) nanorods have been synthesized using chemical solution reaction method, oil bath, which is low cost and short process time (only require five minutes). For commercial application this have development potential. As-synthesized ZnO nanorods have been addressed to characterize the photocatalytic.
Zinc acetylacetonate hydrate (Zn(AcAc)2) was acted as a solute while denatured ethanol and deionized water were used as solvent to prepare the Zn(AcAc)2 precursors. Using Zn(AcAc)2 precursors into the round-bottomed beaker with 200 ℃ silicone oil to synthesize the ZnO nanrods. In addition, we used MOD-Ag as a doping source to synthesize Ag-doped ZnO nanostructures. By thermal decomposition, using oil bath to synthesize the ZnO nanrods, which are wurzite structures with hexagonal cylinder. And ZnO nanorods have Oriented attachment of self-assembly behavior growing mode. By Photoluminescence and X-ray photoelectron spectroscopy analysis, the ZnO nanorods are a kind of deficient photocatalyst. In this study, find out the ZnO nanorods have maximum concentration of double electric oxygen vacancies by thermal decomposition in five minutes. And indirectly caused a lot of hydroxyl radicals. Via photocatalytic degradation methyl orange experiment, it have the most excellent of the degradation efficiency and catalytic effect than commercial TiO2 Degussa P25. In this study, we find out a way which is low production cost, process time is short, the growth temperature is low, suitable for mass production, to synthesize the ZnO nanrods. And have great potential for development in the application of ZnO photocatalyst and other related industries.

第一章 緒論 1
1.1前言 1
1.2研究動機 3
第二章 文獻回顧 4
2.1 氧化鋅簡介 4
2.2 氧化鋅的製備方法 6
2.3氣相沉積法 8
2.3.1氣相-液相-固相(Vapor-liquid-solid, VLS) 8
2.3.2氣相-固相(Vapor-solid, VS) 13
2.4化學溶液反應法 18
2.4.1水熱法 18
2.4.2噴霧熱裂解法 21
2.4.3油浴法 23
2.5光能誘導法 24
2.6乙醯丙酮鋅合成氧化鋅 26
2.6.1化學氣相沉積法 27
2.6.2化學溶液法 29
2.6.3大氣熱裂解 29
2.6.4光能誘導法 32
第三章 實驗方法 33
3.1 實驗方法 33
3.2實驗流程 34
3.2.1.前驅物製備 34
3.2.2油浴法熱裂解成長氧化鋅奈米顆粒 34
3.2.3製備摻雜銀之氧化鋅奈米顆粒 35
3.2.4材料特性分析方法 35
3.2.5實驗流程圖 37
3.3材料特性分析儀器 38
第四章 結果與討論 44
4.1乙醯丙酮鋅DSC-TGA分析與熱裂解機制 44
4.2 油浴法熱裂解合成氧化鋅結構與特性分析 45
4.2.1實驗方法與架構 45
4.2.2 SEM形貌分析 46
4.2.3 XRD晶體結構 49
4.2.4 TEM分析 51
4.3特性分析 57
4.3.1氧化鋅之發光機制 57
4.3.2光致發光(Photoluminescence, PL)分析 58
4.4XPS分析 65
4.5光觸媒催化實驗與分析 69
4.5.1實驗方式與架構 69
4.5.3光催化降解實驗 71
4.5.4氧化鋅光催化分解染料機制 73
4.5.5油浴法氧化鋅光觸媒特性之討論 74
第五章 結論 77
第六章 未來展望 79
參考文獻 82

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