本研究使用Hummer’s法改良製備的氧化石墨(Graphite oxide)作為產氧觸媒，產氫觸媒使用摻雜Rh的SrTiO3(簡稱SrTiO3:Rh)以Ru奈米顆粒作為共觸媒。觸媒鑑定部分，以X光繞射光譜儀(XRD)、穿透式電子顯微鏡(TEM)、紫外-可見光光譜儀(UV-vis)、傅立葉轉換紅外光譜儀(FT-IR)、拉曼光譜儀(Raman)與X射線光電子能譜儀(XPS)來分析觸媒之物理、化學特性及表面性質，觸媒催化部分則利用氣相層析儀(GC)測試觸媒產氣活性。並使用產氫觸媒與產氧觸媒結合與[Co(Bpy)3]2+/3+作為氧化還原媒介探討兩步驟光催化全水分解反應(Z-scheme)，將光觸媒於紫外光/可見光的照射下進行光催化水分解，產生氫氣與氧氣。
光催化水分解反應探討分為三個部分，第一部份為氧化石墨在[Co(Bpy)3]2+水溶液中進行產氧反應，其中以0.02克的Hummer’s法改良後氧化石墨(GOc)有最高產氧活性(O2: 3141.38μmole g-1 h-1)；第二部份為Ru/SrTiO3:Rh在[Co(Bpy)3]2+水溶液中進行產氫反應，其中以0.05克有最高產氫活性(H2: 287.87μmole g-1 h-1)；第三部分為將產氫觸媒Ru/SrTiO3:Rh和產氧觸媒GOc以不同比例結合使用於Z-scheme系統中，進行全水分解的產氣反應之研究，其中以0.05克氧化石墨和0.05克Ru/SrTiO3:Rh結合於[Co(Bpy)3]2+水溶液進行光催化全水分解反應有最高產氣活性(H2:505.26、O2:786.11 (μmole g-1 h-1))。

In this study, the graphite oxide(GO) prepared by improved Hummer's method was used as the O2 evolution photocatalyst, and the H2 evolution photocatalyst was Rh doped SrTiO3 (denoted as SrTiO3:Rh) with Ru nanoparticle as cocatalyst. All the catalysts were characterized by X-ray diffraction spectrometer (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-visible Spectrophotometer (UV-vis), Fourier transform infrared spectrometer (FT-IR), Raman spectrometer (Raman) and X-ray photoelectron spectroscopy (XPS) to analyze the physical, chemical and surface properties. The gas-evolution activity of photocatalyst is tested by gas chromatograph (GC). The Z-scheme is a two-photocatalyst system for photocatalytic overall water splitting. It is using H2 evolution catalyst combined with O2 evolution catalyst in [Co(Bpy)3]2+/3+ aqueous solution as redox mediator. The photocatalyst is photocatalyzed by ultraviolet light/visible light to generate H2 and O2.
The activity of the photocatalyst in water splitting reaction is discussed in three parts. First, compare the activity of different grams and preparation of graphite oxide in the oxidation reaction.The highest of photoactivity O2 evolution photocatalyst is 0.02 g of Goc (O2: 3141.38μmole g-1 h-1).The second section is the H2 evolution reaction of Ru/SrTiO3:Rh in [Co(Bpy)3]2+(aq), wherein 0.05g has the highest hydrogen production activity (H2: 287.87μmole g-1 h-1).Last, the combination of Ru/SrTiO3:Rh and graphite oxide in different ratio in the Z-scheme system for the study of the gas evolution reaction. The photocatalytic overall water evolution reaction of 0.05 g of GO and 0.05 g of Ru/SrTiO3:Rh combined with [Co(Bpy)3]2+(aq) has the highest activity (H2:505.26、O2:786.11
(μmole g-1 h-1)).

致謝 I
摘要 III
Abstract V
目錄 VII
圖目錄 XI
表目錄 XV
第一章 研究背景和文獻回顧 1
1.1 前言 1
1.2 研究目的 2
1.3 文獻回顧 3
1.3.1光催化水分解 3
1.3.2 Z-scheme系統 8
1.3.3 共觸媒影響 17
1.3.4 氧化石墨 21
1.3.5 氧化石墨的光催化性質 22
第二章 實驗方法與步驟 23
2.1 實驗藥品與耗材 23
2.2 實驗設備與儀器 24
2.3 光觸媒製備 25
2.3.1 Hummer’s法製備氧化石墨 25
2.3.2 改良後氧化石墨製備 26
2.3.3 微波水熱法製備多孔型STO:Rh 26
2.3.4 STO:Rh添加共觸媒Ru 27
2.3.5 [Co(Bpy)3]SO4製備 27
2.3.6 g-C3N4的製備 27
2.3.7 磷摻雜g-C3N4的製備 28
2.3.8 硫摻雜g-C3N4的製備 28
2.3.9 磷和硫共摻雜g-C3N4的製備 28
2.4 光觸媒性質分析 29
2.4.1 X-Ray繞射儀(X-Ray Diffraction, XRD) 29
2.4.2 紫外-可見光分析儀(UV-visible Spectrophotometer) 31
2.4.3 解析型穿透式電子顯微鏡(Transmission electron microscope,TEM) 32
2.4.4 拉曼光譜儀(Raman spectra) 33
2.4.5 傅立葉轉換紅外線光譜儀(Fourier Transform Infrared Spectrometer , FT-IR) 35
2.4.6 X射線光電子能譜儀(X-Ray Photoelectron Spectroscopy, XPS) 36
2.4.7 氣相層析儀(Gas Chromatography, GC) 37
2.5 GC檢量線製作 39
2.5.1 氫氣檢量線 39
2.5.2 氧氣檢量線 40
2.6 光催化水分解產氣實驗 42
第三章 實驗結果與討論 43
3.1 產氧觸媒氧化石墨鑑定及水解半反應的影響 43
3.1.1 不同製備方法的氧化石墨之X-Ray繞射儀(XRD)分析 43
3.1.2 氧化石墨之解析型穿透式電子顯微鏡(TEM)分析 44
3.1.3 不同製備方法的氧化石墨進行光催化水解半反應 46
3.1.4 不同克數氧化石墨進行光催化水解半反應 48
3.1.5 半反應前後氧化石墨之拉曼光譜儀(Raman)分析 51
3.1.6 半反應前後GOc之傅立葉轉換紅外線光譜儀(FT-IR)分析 52
3.1.7 半反應前後氧化石墨之X射線光電子能譜儀(XPS)分析 53
3.2 產氫觸媒Ru/STO:Rh鑑定及水解半反應的影響 56
3.2.1 X-Ray繞射儀(XRD)分析 56
3.2.2 紫外-可見光(UV-visible)分析 57
3.2.3 解析型穿透式電子顯微鏡(TEM)分析 59
3.2.4 不同克數Ru/STO:Rh進行光催化水解半反應 60
3.2.5 半反應前後Ru/STO:Rh之X射線光電子能譜儀(XPS)分析 62
3.3 Ru/STO:Rh與氧化石墨GOc應用於Z-scheme系統 64
3.3.1 反應溶液對於光催化全水分解效果影響 64
3.3.2 不同克數GOc與Ru/STO:Rh之光催化全水分解效果影響 68
3.4 磷和硫共摻雜的g-C3N4作為一種有效的無金屬光觸媒 69
3.4.1 磷和硫摻雜g-C3N4之X-Ray繞射儀(XRD)分析 69
3.4.2 磷和硫摻雜g-C3N4進行光催化水解反應 70
3.4.3 磷和硫摻雜g-C3N4進行Z-scheme系統光催化全水解反應 72
第四章 結論 77
參考文獻 79

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