臺灣博碩士論文加值系統

本研究的重點工作是以兩種型態的光催化劑用作降解染料為研究方向。首先是製備二氧化鈦摻雜Fe3+的奈米光催化劑粉末，使用四丁基鈦酯(Ti(OC4H9)4)作為原料，以溶膠-凝膠法合成未摻雜TiO2和TiO2摻雜Fe (Fe-TiO2)的奈米光催化劑粉末。藉由XRD、BET、XPS、FTIR和ESR等儀器分析，說明二氧化鈦在不同Fe3+的摻雜濃度條件下，其物理和化學的特徵以及結構型態的變化說明光催化活性。XRD分析結果證明，隨著摻雜Fe3+的濃度增加，其( 1 0 1 )優選成長方向的波峰隨之降低，二氧化鈦的晶粒尺寸隨之降低(18.21~16.94 nm)。0.10 mole% Fe3+-TiO2光催化降解亞甲基藍(MB)的最大速率常數0.716 h-1為最佳。在ESR分析證明Fe3+的摻雜取代了TiO2晶格中的Ti4+ (g=1.997)，並且在相鄰的晶格因為電荷平衡所產生的氧空缺陰離子補償(g=4.252)，說明Fe3+摻雜濃度在0.1 mole%時，陰離子氧空缺達到飽和，摻雜0.5 mole%時，氧空缺濃度失去平衡並形成 的團簇。這意味著過量的Fe3+摻雜到二氧化鈦提高光生電子和電洞的複合，有損光催化活性。XPS分析證明0.1 mole% Fe3+的摻雜其O－H鍵佔O 1s包圍之面積為所有樣品中最大(7.06%)，結果表明，表面羥基濃度明顯影響光催化活性，高表面羥基密度，有助於提高光催化劑的活性。
第二項研究提出了異質結構磁性可回收之可見光光催化降解有機染料溶液。如果研究證實其可行性，它將被應用在有機廢水的處理程序。我們在可磁性回收光催化降解有機染料溶液的研究如下：
(1) 製備核-殼結構可磁性回收催化劑TiO2/Mn-Zn 鐵氧磁體的複合材料粉末。該核的材料Mn-Zn 鐵氧磁體粉末係由酸洗液和廢棄的鹼性電池為原料合成，並使用Titanium isopropoxide (Ti(OC3H7)4)做為原料，以溶膠-凝膠法在鐵氧磁體粉末上包覆TiO2。透過穿透視電子顯微鏡可以清楚觀察，該磁性的Mn-Zn鐵氧磁體奈米粉末被TiO2外殼均勻地包覆，形成核-殼結構TiO2/Mn-Zn 鐵氧磁體可磁性回收催化劑。Mn-Zn鐵氧磁體的是球形或橢圓形的，其粒徑約在20-40奈米的範圍，外殼TiO2的厚度大約2奈米。磁性光催化劑可成功地用於亞甲基藍(MB)染料的降解。
(2) 由於受到光照射TiO2產生光生電子-電洞對，電子或電洞會在TiO2與鐵氧磁體之間的接觸介面發生交互作用反應，導致減少了光生電子和光生電洞遷移到表面，使得光催化活性下降，為了提升磁性回收催化劑的催化活性，我們在TiO2與鐵氧磁體之間加入了SiO2作為阻障層，因此製備異質結構之TiO2/SiO2/Ni-Cu-Zn 鐵氧磁體的複合材料粉末作為可磁性回收催化劑。該複合材料的組成結構是由球形或橢圓形的Ni-Cu-Zn鐵氧磁體奈米粒子作為核，其粒徑約為20-60奈米，緊接著包覆上阻障層SiO2，其厚度為15奈米，最後包覆厚度約1.5奈米的TiO2光催化劑層。在光降解亞甲基藍(MB)的實驗中，相較於TiO2/Ni-Cu-Zn 鐵氧磁體複合材料，含有SiO2阻障層的TiO2/SiO2/Ni-Cu-Zn 鐵氧磁體磁性光催化劑顯示出較高的光催化效率，其一級速率常數(kobs)為0.18427 h-1，以及具有和良好的磁特性，該飽和磁化量(Ms) 為37.45的emu/g，這表明磁性光催化劑可以很容易地被應用外部磁場回收再使用。
(3) 然而，異質結構可磁性回收之光催化劑的最外層仍是TiO2，由於TiO2的光響應波長大約在380-400 nm的範圍，對照太陽光光譜分布圖中，可以發現僅僅只有4-5%可以被用做激發光源使用。故為了提升可見光的被利用率，因此將於可磁性回收之光催化劑的最外層(TiO2)沉積奈米銀顆粒，藉由奈米銀吸收可見光產生表面等離子效應(surface plasmon resonance，LSPR)，電子被激發並傳導到TiO2表面，與表面吸附氧(O2(ads))發生光化學還原反應生成超氧自由基(O2•-)。因此，合成異質結構之AgNPs-TiO2/SiO2/Ni-Cu-Zn 鐵氧磁體的複合材料粉末作為可磁性回收催化劑。在穿透式電子顯微鏡觀察下，可以以清楚的看到奈米銀可粒沉積在TiO2/SiO2/Ni-Cu-Zn 鐵氧磁體的表面上，奈米營的顆粒大小約在18-40奈米。該異質結構複合材料的光催化活性將在光催化降解亞甲基藍(MB)染料的實驗中進行評估。結果表明0.4 wt% AgNPs-TiO2/SiO2/Ni-Cu-Zn 鐵氧磁體在模擬太陽光光源的照射下，對MB的移除率高達87.75%，其中吸附36.10%和降解51.65%。該異質結構複合材料可以容易地透過外加磁場進行分離，在穩定性測試，經過五次循環降解之後該光催化活性逐漸下降，但是可以在500 oC的熱處理之後被活化，對MB的移除率回復到79.85%。

The work focuses on the two kinds of research direction of the dye degradation. First, we synthesized iron-doped TiO2 photocatalysts. The aim of the work is to study the effects of oxygen vacancy and surface hydroxyl group density on the photocatalytic activity of Fe3+-doped TiO2, and to investigate how the titanium dioxide doped with different concentration of the Fe3+ influenced their physical and chemical characterizations. The photocatalysts were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), electron spin resonance (ESR), X-ray photoelectron spectroscope (XPS) and Fourier transform infrared (FTIR) spectroscopy. The results revealed that adsorbed hydroxyl group density significantly influenced in photocatalytic activity, and a small amount of Fe3+ can act as a photo-generated hole and a photo-generated electron trap and inhibit the electron–hole recombination. The 0.10%- Fe3+-TiO2 with the highest surface hydroxyl group density revealed the maximum rate constant of 0.716 and the optimal photocatalytic degradation of methylene blue (MB). As Fe3+ doping levels are larger than 0.10%, the cluster of generated gradually. This implied that an excessive amount of Fe3+ doped into TiO2 is detrimental to the photocatalytic activity due to the formation of clusters and enhances the recombination of photogenerated electrons and holes.
The second study proposed visible light of the recyclable magnetic photocatalytic degradation of the organic dye solution. If confirmed by studies with its feasibility, it will be applied to organic wastewater treatment program. We are studying for using this magnetic photocatalyst to treat dye wastewater as the following: (1) We prepared the TiO2/Mn-Zn ferrite composite powder for magnetic photocatalyst. The core Mn-Zn ferrite powder was synthesized by using steel pickling liquor and used alkaline batteries as the starting materials. The shell TiO2 nanocrystal was prepared by sol–gel hydrolysis precipitation of titanium isopropoxide (Ti(OC3H7)4) on the Mn-Zn ferrite powder. The thickness of the titania shell was found to be approximately 2 nm. The core of Mn-Zn ferrite is of spherical or elliptical shape and the particle size of the core is in the range of 20-40 nm. The magnetic Mn-Zn ferrite nanopowder is uniformly encapsulated in a titania layer forming the core–shell structure of TiO2/Mn-Zn ferrite powder. The magnetic photocatalyst can be successfully used to treat dye waste waters. (2) The TiO2/SiO2/Ni-Cu-Zn ferrite composite for magnetic photocatalysts with high photocatalytic activity is successfully prepared in this study. The composite are composed of spherical or elliptical Ni-Cu-Zn ferrite nanoparticles about 20-60 nm as magnetic cores, silica as barrier layers with thickness of 15 nm between the magnetic cores and titania shells with thickness approximately 1.5 nm. Photodegradation examination of TiO2/SiO2/Ni-Cu-Zn ferrite composite was carried out in methylene blue (MB) solutions illuminated under a Xe arc lamp with 35 W and color temperature of 6000 K. The results indicated that about 47.1% of MB molecules adsorbed on the TiO2/SiO2/Ni-Cu-Zn ferrite ferrite composite within 30 min mixing due to it higher pore volume of 0.034 cm3/g, and after 6 h Xe lamp irradiation, 83.9% of MB was photodegraded. Compared with the TiO2/Ni-Cu-Zn ferrite composite, the TiO2/SiO2/Ni-Cu-Zn ferrite ferrite composite with silica barrier layer prohibited the photodissolution and enhanced the photocatalytic ability. The magnetic photocatalyst shows high photocatalytic efficiency that the apparent first-order rate constant kobs is 0.18427 h-1, and good magnetic property that the saturation magnetization (Ms) of 37.45 emu/g, suggesting the magnetic photocatalyst can be easily recovered by the application of an external magnetic field. (3) Silver nanoparticles with different weight percentage immobilized on TiO2/SiO2/Ni-Cu-Zn ferrite nanoparticles were successfully prepared via coprecipitation and sol-gel hydrolysis precipitation method. The synthesized product was characterized using various techniques. Room temperature magnetic hysteresis curves shows that as synthesized 0.4wt% Ag immobilized TiO2/SiO2/Ni-Cu-Zn ferrite display superparamagnetic behavior with saturation magnetization of 39.93 emu g-1. XPS characterization confirmed the presence of Ag nanoparticles on the surface of magnetic semiconductor photocatalyst. Surface morphology was analyzed using TEM, which shows a non-uniform shaped core-shell structure with an average particle size of 18-40 nm of Ag nanoparticles deposited on the surface. The effect of immobilization of Ag nanoparticles on structural, optical and photocatalytic properties of TiO2/SiO2/Ni-Cu-Zn ferrite was investigated by X-ray diffraction (XRD), UV-Visible spectrophotometer, Photoluminescence (PL) spectroscopy and electrochemical measurements. Photocatalytic dye degradation of Ag-TiO2/SiO2/Ni-Cu-Zn ferrite composite was carried out in methylene blue (MB) solutions. The results indicated 87.75% of MB was photodegraded under Xe lamp irradiation for 0.4 wt% of Ag immobilized TiO2/SiO2/Ni-Cu-Zn ferrite. Moreover, it can be easily separated and recycled without significant loss of photocatalytic activity after being used five times. Therefore, compared to the conventional photocatalysts, this magnetic core–shell photocatalyst is green, cheap and more suitable for large scale applications.

Acknowledgement I
Chinese Abstract III
Abstract V
Table of the contents VII
List of Tables XI
List of Figures XIII
List of publications in Ph. D program XIX
Chapter 1 Introduction and Literature review 1
1.1 Foreword 3
1.2 Research of motivation and objective 6
1.3 Literature review 7
1.3.1 Effects of surface hydroxyl group density on the photocatalytic activity of Fe3+-doped TiO2 7
1.3.2 Immobilization of visible light driven magnetic recyclable photocatalysts based on ferrite 8
1.3.2.1 Characterizations of TiO2/Mn-Zn ferrite powders for magnetic photocatalyst prepared from used alkaline batteries and waste steel pickling liquor 9
1.3.2.2 Characterizations and role of silica layer of TiO2/SiO2/Ni-Cu-Zn ferrite powders for magnetic photocatalyst 9
1.3.2.3 Magnetic recyclable photocatalysts of Ag-TiO2/SiO2/Ni-Cu-Zn ferrite and their photocatalytic activity 10
1.4 Architecture of the experimental 11

Chapter 2 Basic theory 13
2.1 Characterization and principle of titanium dioxide photocatalytic 15
2.1.1 Characterization of titanium dioxide photocatalytic 15
2.1.2 Photocatalytic principle of titanium dioxide 17
2.2 The mechanism of degradation and decolorization for the methylene blue 23
2.3 Principle and application of electron spin resonance for the photocatalyst 27
2.3.1 Principle of electron spin resonance for the photocatalyst 27
2.3.2 Application of electron spin resonance for the photocatalyst 29
2.4 Superparamagnetic properties of ferrite magnets 31
2.4.1 The crystal structure of ferrite magnets, characteristics and application 31
2.4.2 Special magnetic properties of nanoparticles of the ferrite magnets 35
2.4.3 Preparation method of ferrite magnets 37
2.5 Theory of the localized surface plasmon resonance (LSPR) 39
Chapter 3 Experimental methods 43
3.1 Characterization of photocatalysts 45
3.2 Photoelectrochemical measurements 47
3.3 Photocatalytic activity 49
3.4 Photocatalytic degradation kinetics 50
Chapter 4 Effects of surface hydroxyl group density on the photocatalytic activity of Fe3+-doped TiO2 51
4.1 Experimental 53
4.1.1 Preparation of TiO2-based photocatalysts 53
4.1.2 Characterization of TiO2 and Fe3+-doped TiO2 photocatalysts 53
4.1.3 Measurement of undoped TiO2 and Fe3+-doped TiO2 photocatalytic activity 54
4.2 Results and discussion 55
4.2.1 Characterization of TiO2-based photocatalysts 55
4.2.2 Oxygen vacancy of the Fe3+-doped TiO2 photocatalysts 59
4.2.3 Surface hydroxyl-groups density of Fe3+-doped TiO2 photocatalysts 62
4.2.4 Photocatalytic activity 66
4.3 Conclusions 73
Chapter 5 Characterizations of TiO2/Mn-Zn ferrite powders for magnetic photocatalyst prepared from used alkaline batteries and waste steel pickling liquor 75
5.1 Experimental procedure 77
5.1.1 Preparation of TiO2/Mn-Zn ferrite nanoparticles 77
5.1.2 Photocatalytic activity 78
5.2 Results and discussion 79
5.2.1 Structural characterization of the TiO2/Mn-Zn ferrite composite 79
5.2.1 Photocatalytic activity 85
5.3 Conclusions 89
Chapter 6 Characterizations and role of silica layer of TiO2/SiO2/Ni-Cu-Zn ferrite powders for magnetic photocatalyst 91
6.1 Experimental procedure 93
6.1.1 Preparation of samples 93
6.1.1.1 Preparation of Ni-Cu-Zn ferrite nanoparticles 93
6.1.1.2 Preparation of TiO2/Ni-Cu-Zn ferrite composite 93
6.1.1.3 Preparation of TiO2/SiO2/Ni-Cu-Zn ferrite composite 94
6.1.2 Characterization of TiO2/Ni-Cu-Zn ferrite and TiO2/SiO2/Ni-Cu-Zn ferrite composite 94
6.1.3 Photocatalytic activity 95
6.2 Results and Discussion 96
6.2.1 Characterization of the TiO2/SiO2/Ni-Cu-Zn ferrite composite 96
6.2.2 Photocatalytic activity 104
6.3 Conclusions 112
Chapter 7 Magnetic recyclable photocatalysts of Ag-TiO2/SiO2/Ni-Cu-Zn ferrite and their photocatalytic activity 113
7.1 Experiment 115
7.1.1 Materials 115
7.1.2 Preparation of Ag-TiO2/SiO2/Ni-Cu-Zn ferrite composite 115
7.1.3 Photocatalyst characterization 116
7.1.4 Photoelectrochemical measurements 117
7.1.5 Photocatalytic activity 117
7.2 Results and discussion 118
7.2.1 Structural characterization of Ag-TiO2/SiO2/Ni-Cu-Zn ferrite magnetic photocatalyst 118
7.2.2 Optical and electrochemical properties of the Ag-TiO2/SiO2/Ni-Cu-Zn ferrite 129
7.2.3 Visible light photocatalytic activity and mechanism for the photodegradation 132
7.2.4 The reusability of the Ag-TiO2/SiO2/Ni-Cu-Zn ferrite composite 137
7.3 Conclusion 140
Chapter 8 Overall Conclusion 141
References 145

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