臺灣博碩士論文加值系統

近年來，半導體觸媒的異相光催化反應在環境污染防治的研究上相當廣泛，其中奈米二氧化鈦因具有高活性、化學穩定性、無毒性及容易取得之優點，故應用性極具潛力，為了增加二氧化鈦的表面積，本研究乃使用水熱法來製備高比面積二氧化鈦奈米管(TNs)及多元空間花形二氧化鈦奈米結構(HFTNs)，具有不需繁複的設備及步驟即可得到大量的產物之優點，並且摻雜金屬以增加其可見光光催化能力，因此，本實驗之主要目的在於對TNs及HFTNs之水熱法合成條件及結構特性分析進行討論，並參雜金屬W至TNs及HFTNs中，以強化其光觸媒催化之性質；並探討TNs及HFTNs對6種不同特性染料廢水，測試其光催化之效能及求得反應動力參數。另外，亦深入瞭解HFTNs之特殊空間光反射精細結構，對提升光催化特性之影響。
實驗中二氧化鈦奈米管是以水熱法在10 M NaOH的濃度，150oC，24 h之條件下製備，並經酸洗過程製備TNs，接著以場發掃描式電子顯微鏡(FE-SEM)及穿透式電子顯微鏡(TEM)觀察其特性。結果顯示TNs的長度與直徑，分別分佈在400~1000和10~15 nm中。X射線光電子能譜(XPS)數據指出，TNs含有O和TiIV種元素，指出TNs樣品為高純度TiIV (93.95%)為主。所製備之TNs具有約292 m2/g的高比表面積，以及總孔洞體積1.026 cm3/g。為了改善TNs的光觸媒性質，不同含量的鎢(W) (5、10、15及20 wt%)以含浸法(Impregnation Method)負載在TNs奈米材料表面及結構中。增加W的含量，Ti 2p3/2分配給Ti4+的鍵結能將由459.36 eV增加到459.63 eV。XPS指出Ti 2p的鍵結能移動到較高能，顯示由於W參雜，造成TiO2的單位晶格的收縮。這些觀察表示W原子對TiO2晶格中Ti之取代作用。此外，分配給W的鍵結能亦增加，表示WO3單位晶格之收縮，乃由於WO3晶體中Ti之取代所導致。
二氧化鈦奈米管對6種染料溶液中的光分解效率程度之依序為：Methylene Blue (MB) > Basic Violet 3 (BV3) > Basic Violet 10 (BV10) > Acid Blue 9 (AB9) > Acid Orange 7 (AO7)> Acid Red 1 (AR1)。此外，負載金屬的W可以提升光觸媒效率，但染料降解的效率亦會隨著TNs上所負載的W含量增加而下降，其中以5 wt %之效率最佳，這指都顯示W金屬負載之TNs確實明顯促進光觸媒降解染料之效率。另外，本研究亦利用一個簡單的Langmuir-Hinshelwood model來計算ln(C0/Ca)對時間的關係，以描述其與廢水的2次反應；甲基藍之光催化反應參數k1 = 0.0068 min-1 及 k2 = 0.0001 min-1。W-loaded TNs的對6種染料溶液，其光降解效率依序為：MB (98.3%) > BV3 (72.58%) > BV10 (49.77%) > AB9 (14.95%) > AO7 (2.12%) > AR1 (0.54%)。其中亦發現由5 wt% W參雜之TNs在先前吸附程序階段後，其光觸媒效率(4.58-11.99%)，增加程度高於TNs (1.74-2.94%)。
本論文亦成功地開發以水熱法製備多元空間花形二氧化鈦奈米結構(Hierarchical Flower-like TiO2 Nanostructures, HFTNs)，作為不同光催化觸媒之比較。由於其特殊結構能顯著地增進鹼性染料在水溶液中之吸附能力和光觸媒性能。實驗中利用FE-SEM、HR-TEM、BET、XRD、XPS、SSNMR、EPR及XENAS/EXAFS貴重儀器可以瞭解HFTNs之結晶性、表面形態和精細結構特性。HFTNs的光降解效率對6種染料溶液中，在180 min後其染料光降解效率亦被研究及討論。HFTNs在先期吸附階段後，HFTNs光觸媒效率增加6.91-19.26%，較TNs (1.74-2.94%)以及W參雜之TNs (4.58-11.99%)要高出許多，顯示HFTNs光觸媒之光解效率較TNs為佳，乃因為其較多之{001}面比率之片狀特殊空間光反射結構及反應活性表面，讓光容易集中且不易被散射減弱其光強度，因而提升HFTNs光觸媒之染料光解效率。

Recently, titanium dioxide has been recognized as an excellent photocatalyst material applied on many field especially for environmental science or engineering. Titanium dioxide nanotubes (TNs) with high specific surface area have been studied due to its excellent catalytic activities, long-term stability, nontoxicity, and low cost. Therefore, the main objectives of the present study were the preparation of TNs and hierarchical flower-like TiO2 nanostructures (HFTNs) in large quantities by hydrothermal routes, and the characterization the photocatalytic properties, fine structures of TNs, HFTNs, and metallic doped TNs/HFTNs to understand the removal efficiencies of dye pollutants in wastewaters by using TNs/HFTNs.
Titanium dioxide nanotubes prepared by hydrothermal method at 150oC for 24 h, 10M NaOH solution, and with acid-wash were characterized using FE-SEM, and TEM techniques. The results showed that the lengths and diameters of nanotubes were ranged of 400~1000 and 10~15 nm, respectively. The XPS data indicated that TNs consist of Ti contributed mainly from TiIV and O, it indicated that TNs sample obtained high purity (93.35%) of TiIV. The prepared TNs exhibit high specific surface areas of ca. 292 m2/g and total pore volumes of 1.026 cm3/g. In order to improve the photocatalytic efficiency of TNs, different amount of W (5, 10, 15, and 20 wt%) with impregnation method were loaded in TNs. The Ti 2p3/2 binding energies assigned to Ti4+ increased from 459.36 to 459.63 eV with the increasing W contents. The XPS indicated binding energies of Ti2p shifted to the higher energies, indicating the contraction of the unit cells of TiO2 due to the W doping into their frameworks. These observations suggest the substitution of W for Ti in TiO2 lattice. Furthermore, the binding energies assigned to W4f also increased, suggesting the contraction of WO3 unit cells caused by the substitution of Ti in WO3 crystals.
The photodegradative efficiency order of TNs on six kinds of dyes solutions was Methylene Blue (MB) > Basic Violet 3 (BV3) > Basic Violet 10 (BV10) > Acid Blue 9 (AB9) > Acid Orange 7 (AO7)> Acid Red 1 (AR1). Moreover, loading W metal with promoting the photocatalytic efficiency was found, but the efficiency of dye remediation decreased with increasing of W-loaded percentages on TNs. It indicated that W-loaded TNs indeed influenced the photocatalytic efficiencies significantly. In addition, a simple Langmuir-Hinshelwood model was used and calculated by the relationship of ln(C0/Ca) versus time to describe the second-order reactions with the wastewaters. Methylene blue photodecomposion rates were highest with k1 of 0.0068 min-1 and k2 of 0.0001 min-1. The photodegradative efficiency of W-loaded TNs on six kinds of dyes solutions was MB (98.3%) > BV3 (72.58%) > BV10 (49.77%) > AB9 (14.95%) > AO7 (2.12%) > AR1 (0.54%) in series. It was found that the photocatalytic efficiency increase of 5 wt% W-doped TNs (4.58-11.99%) after the previous adsorption process was higher than that of TNs (1.74-2.94%).
In addition, a hydrothermal route for the preparation of HFTNs has been successfully developed that markedly enhance the adsorption and visible light photocatalytic capabilities of basic dyes in aqueous solution. Their crystallinity, surface morphology, and fine structures were investigated by FE-SEM, HR-TEM, BET, XRD, XPS, SSNMR, EPR, and XENAS/EXAFS. Order of the photodegradative efficiencies for six kinds of dyes solutions after 180 min onto HFTNs was also investigated. The photocatalytic efficiency increases of HFTNs (6.91-19.26%) after previous adsorption process was higher than the efficiencies of TNs (1.74-2.94%) and W-doped TNs (4.58-11.99%), respectively because the {001} facets of TiO2 nanosheets enhanced photocatalytic activity is seen on comparing it with TiO2 nanoparticles. The two-dimensional (2D) nanosheets with exposed {001} facets can more easily enhance the adsorption of dye pollutant molecules due to its highly reactive surface, which would lead to the enhancement of photocatalytic activity.

Table of Contents
摘 要 I
ABSTRACT I
Acknowledgement III
Table of Contents V
List of Figures X
List of Tables XVII
Chapter 1 Introduction 1
1.1 Background 1
1.2 Research Scope of the Dissertation 3
Chapter 2 Literature Review 6
2.1 Titanium Dioxide and Titania Nanotubes 6
2.1.1 Titanium dioxide 6
2.1.2 Titania nanotubes 8
2.2 Fabrication of TNs 10
2.2.1 Hydrothermal methods 11
2.2.2 Template-assisted synthesis 14
2.2.3 Anodic oxidation process 15
2.3 Properties of Titanium Dioxide Powders and TNs 18
2.3.1 Crystal structure 18
2.3.2 Reactivity 20
2.3.3 Surface hydroxyl groups and surface charges 24
2.3.4 Electrical properties 25
2.3.5 Optical properties 27
2.4 Modification of TNs 31
2.4.1 Doping 32
2.4.2 Annealing 37
2.4.3 Filling and decoration 40
2.4.4 Monolayers 43
2.4.5 Conversion of tubes (titanates, semimetallic phase) 46
2.5 Applications of TNs 48
2.5.1 Photocatalysis under visible light 48
2.5.1.1 What is the photocatalyst? 48
2.4.1.2 Photocatalysis under visible light 49
2.5.1.3 Water purification 54
2.5.1.4 Water splitting to produce hydrogen 55
2.5.1.5 Chemical sensors 57
2.5.1.6 Anti-bacterial and cancer treatment 58
2.5.2 Dark photocatalysis 59
2.5.3 Solar cells 59
2.5.4 Drug delivery and the release of other payloads 63
2.5.5 Other applications and aspects 65
2.6 Hierarchical Flower-like TiO2Nanostructures with {001}Facets Active 67
Chapter 3 Experimental Methodology 72
3.1 Synthesis of TNs and W-doped TNs 72
3.1.1 Titania nanotubes 72
3.1.2 Preparation of W-doped TNs 76
3.2 Synthesis of Hierarchical Flower-like TiO2Nanostructures 76
3.3 Adsorption and Photocatalysis of Different Dyes on TNs, W-doped TNs and Hierarchical Flower-like TiO2 Nanostructures 78
3.4 X-Ray Powder Diffraction 80
3.5 Field-Emission Scanning Electron Microscopy (FE-SEM) 81
3.6 Low-Magnification Transmission Electron Microscope (TEM) and High-Resolution Transmission Electron Microscope (HR-TEM) 83
3.7 Thermo Gravimetric Analysis/Differential Thermal Analysis (TGA/DTA) 86
3.8 Nitrogen Adsorption Isotherm (ASAP) 88
3.9 X-ray Photoelectron Spectroscopy (XPS) 93
3.10 Solid-State Nuclear Magnetic Resonance (SSNMR) 96
3.11 Electron Paramagnetic Resonance 100
3.12 X-ray Absorption Spectroscopy (XANES and EXAFS) 104
3.10.1 Fundamentals of XANES and EXAFS 104
3.10.2 Experiments of EXAFS and XANES 105
Chapter 4 Results and Discussion 107
4.1 Characterization of Titania Nanotubes 107
4.1.1 FE-SEM and HR-TEM analysis for the identification of TNs structure 107
4.1.2 X-Ray diffraction for the identification of TNs structure 113
4.1.3 Nitrogen adsorption for the identification of TNs structure 115
4.1.4 Synchrotron radiation analysis for the identification of TNs structure 118
4.1.5 X-ray photoelectron spectrum analysis for the identification of TNs structure 123
4.1.5.1 High resolution spectra of the Ti 2p region 124
4.1.5.2 High resolution spectra of the O 1s region 128
4.1.6 Fourier transform infrared spectroscopy analysis for the identification of TNs structure 130
4.2 Tungsten Doped Titania Nanotubes 131
4.2.1 FE-SEM and HR-TEM analysis for the identification of W-doped TNs structure 131
4.2.2 X-Ray diffraction for the identification of W-doped TNs structure 134
4.2.3 Nitrogen adsorption for the identification of W-doped TNs structure 135
4.2.4 X-ray photoelectron spectrum analysis for the identification of W-doped TNs structure 139
4.2.5 Synchrotron radiation analysis for the identification of W-doped TNs structure 146
4.2.6 UV-vis diffuse reflectance spectra analysis for the identification of W-doped TNs structure 153
4.2.7 Fourier transform infrared spectroscopy analysis for the identification of W-doped TNs structure 155
4.2.8 Solid-state nuclear magnetic resonance analysis for the identification of TNs and W-doped TNs structure 156
4.3Absorption and Photocatalysis Six Dyes by TNs and W-doped TNs 158
4.3.1 Analysis of adsorption and photocatalysis kinetics 158
4.3.2 Analysis of adsorption and photocatalysis mechanisms 173
4.4 Characterization of Hierarchical Flower-like TiO2Nanostructures 185
4.4.1 FE-SEM and HR-TEM analysis for the identification of hierarchical flower-like TiO2 nanostructures 185
4.4.2 X-Ray diffraction for the identification of hierarchical flower-like TiO2 nanostructures 189
4.4.3 X-ray photoelectron spectrum analysis for the identification of hierarchical flower-like TiO2 nanostructures 190
4.4.4 Nitrogen adsorption for the identification of hierarchical flower-like TiO2 nanostructures 194
4.5 Adsorption and Photocatalysis Six Dyes by Hierarchical Flower-like TiO2 Nanostructures 197
4.5.1 Photocatalysis six dye by hierarchical flower-like TiO2 nanostructures under different concentration 197
4.5.2 Comparison photocatalysis between TNs, HFTNs, P25 and P25-HF 206
Chapter 5 Conclusions 208
5.1 Conclusions 208
5.2 Future works 212
References 213

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