研究一種新的絕緣膜沉積技術－液相沉積法生長二氧化鈦膜，並探討此技術對於製程二氧化鈦光催化劑，氣體感測器和電致變色元件上的應用。針對不同可能的應用，發展最適合的製程參數，並討論其薄膜特性。
首先，我們研究以液相沉積法生長二氧化鈦膜的生長參數，和二氧化鈦膜的材料特性。並且研究熱處理對於二氧化鈦膜特性和研究熱處理溫度對於不同應用的影響。在研究中發現，二氧化鈦膜的結晶特性和薄膜致密性能夠被熱處理改善。在 經過400 ℃的熱處理後，二氧化鈦銳鈦礦結構能夠被獲得。然而以液相沉積法生長的二氧化鈦膜由銳鈦礦結構轉為金紅石結構的轉相溫度為900 ℃。經過氧氣的熱處理後，以液相沉積法生長的二氧化鈦膜的折射率可以達到2.46，而其介電常數可以達到17。在以液相沉積法生長二氧化鈦膜在砷化鎵基板的實驗中，我們發現生長溶液會蝕刻砷化鎵基板。造成薄膜中會含有砷和鎵元素。在經過400 ℃的熱處理後可改善其電壓-電容特性，但是漏電流也會增加。
我們也用液相沉積法成長二氧化鈦膜製成電致變色膜，並探討其電致變色的能力。利用液相沉積法在透明導電玻璃基板上生長二氧化鈦膜，其過程簡單、成本低廉、而且成長溫度低 (40 ℃)，值得進一步研究。利用掃描式電子顯微鏡 (SEM)、拉曼光譜(Raman Spectroscopy)、紫外光可見光譜，探討薄膜的特性，並由實驗結果顯示具最大穿透率變化量為45 %。
為求擴大液相沉積法二氧化鈦膜的應用範圍和價值，我們也研究液相沉積法二氧化鈦膜摻雜鈮(Nb)和貴重金屬金和鉑（Au、Pt）的製程方法，並探討經過摻雜後的薄膜特性。最後我們探討以液相沉積法生長的二氧化鈦膜其光催化特性和對氧氣的感測特性，並且和經過摻雜的薄膜比較。實驗結果顯示，以液相沉積法生長的二氧化鈦膜摻雜鈮之後其光催化特性為未摻雜的四倍，並且對氧氣的感測性上，也有最大的靈敏度和最短的反應時間。

Liquid Phase Deposited (LPD) TiO2 film technology and the characterization of films were described in detail in this thesis. The LPD-TiO2 film can be utilized in electrochromic, photocatalyst and gas sensor devices. The optimum parameters for deposition of LPD-TiO2 were studied.
First of all, we study the deposition properties and deposition parameter of LPD-TiO2 film. The effect of heating treatment on LPD-TiO2 film was investigated in this thesis. The as-deposited LPD-TiO2 film is amorphous and the TiO2 anatase phase can be obtained by annealing at 400 ℃. The rutile phase can be observed at the annealing temperature of 900 ℃. After annealing, the crystalling characteristic of LPD-TiO2 film can be improved and its refractive index can reach 2.46 annealed in O2 ambience. Its dielectric constant can be as high as 17 at annealing temperature of 700 ℃ in O2 ambience.
LPD-TiO2 film can deposit on GaAs substrate successfully. The GaAs was etched by the treatment solution during deposition. Therefore, Ga and As are contained in the LPD film. The C-V characterization can be improved at annealing 400 ℃. But the leakage current increases with higher annealing temperature.
The electrochromic (EC) phenomena of TiO2 have been first reported by Inoue et al., where the films are prepared by hydrolysis of titanium tetraoxide. The film shows cathodic coloration and turns dark blue. The LPD-TiO2 film was deposited at 40 ℃ with (NH4)2TiF6 in the process of 0.1 M and 0.2 M boric acid. The films were transparent in the visible range and can be colored in a 1M LiClO4 + propylene carbonate solution. The deposition rate can be controlled quite well at 43 nm/hours. The 270 nm thickness LPD-TiO2 film gives the best electrochromic characteristic.
In order to further strength the feasibility and enlarge the application of LPD-TiO2 film. The characterizations of Nb, Au and Pt doped LPD-TiO2 film were investigated. The concentrations of Nb and Au in the film can be controlled by adjusting the concentrations of Nb and Au source solution added into the treatment solution, respectively. The Nb, Au and Pt species in the LPD-TiO2 film are Nb2O5, metallic Au and Pt(OH)x, respectively. The crystallite size of metal-doped LPD-TiO2 film is smaller than that of pure LPD-TiO2 film.
The photocalytic activities of undoped and Nb-doped LPD-TiO2 film were investigated. The photocatalytic activity of Nb-doped LPD-TiO2 film is about four times higher than that of pure LPD-TiO2 film.
The gas sensing properties of undoped and Nb, Au and Pt-doped LPD-TiO2 films were investigated for oxygen detection sensitivity. Experimental results show that the Nb-doped LPD-TiO2 film displays the highest in oxygen detection, and the Nb-doped LPD-TiO2 film has also a shorter response time.

Acknowledgment
中文摘要 I
Abstract III
Contents VI
Figure Captions VIII

Chapter 1 Introduction 1
1.1 TiO2: An Introduction 1
1.2 Preparations of TiO2 2
1.3 Motivation 3
1.4 Thesis Organization 6

Chapter 2 Experiment 7
2.1 Deposition Procedures 7
2.1.1 Si Wafer Cleaning Procedures 7
2.1.2 GaAs Wafer Cleaning Procedures 8
2.1.3 Glass Substrates Cleaning Procedures 8
2.2 Preparation of Deposition Solution 9
2.2.1 Preparation of (NH4)2TiF6 Solution 9
2.2.2 Preparation of Boric Acid Solution 10
2.3 Film Growth 10
2.4 Equipments 10
2.5 Basic Mechanism 11
2.6 Characterization 12
2.6.1 Physical and Chemical Properties 12
2.6.2 Electrical Properties 12

Chapter 3 As-Deposited LPD-TiO2 Film 17
3.1 Introduction 17
3.2 Growth Parameters 17
3.2.1 Concentration of Boric Acid 17
3.2.2 Deposition Time and H2O Addition 19
3.2.3 Structure Determination of LPD-TiO2 Film 20
3.3 Chemical Reaction and Growth Mechanism for LPD-TiO2 20
3.4 Electrical Characteristics 23

Chapter 4 Annealing of LPD-TiO2 Film 39
4.1 Introduction 39
4.2 Experiment 39
4.3 Structures Analysis of Post-annealed LPD-TiO2 Films 39
4.3.1 X-ray Diffraction Studies 39
4.3.2 Crystalline Size 40
4.3.3 Raman Spectrum 41
4.4 Physical and Chemical Analyses of Post-annealed LPD-TiO2 Films 42
4.5 Electrical Characteristics 45

Chapter 5 LPD-TiO2 Deposited on GaAs 62
5.1 Introduction 62
5.2 Experiment 62
5.3 Growth Characterization 63
5.4 Thermal Treatment Effects 65
5.4.1 XPS Analysis 65
5.4.2 Electrical Characteristics 66
5.5 Summary 68

Chapter 6 Electrochromic Property of the LPD-TiO2 Film 77
6.1 Introduction 77
6.2 Experiment 77
6.3 Electrochromic Reaction 78
6.4 Deposition of LPD-TiO2 Film on ITO-coated Glass 80
6.5 Optical Properties 80
6.6 Summary 82

Chapter 7 Doping of LPD-TiO2 Film 97
7.1 Introduction 97
7.2 Nb-doped LPD-TiO2 Film 98
7.2.1 Preparation of deposition solution 98
7.2.2 Properties of Nb-doped LPD-TiO2 Film 98
7.3 Au- and Pt-doped LPD-TiO2 Film 100
7.3.1 Preparation of Deposition Solution 100
7.3.2 Properties of Au-doped LPD-TiO2 film 101
7.3.3 Properties of Pt-doped LPD-TiO2 film 102
7.4 Summary 103

Chapter 8 Photocatalytic and Gas Sensing Properties of LPD-TiO2 Film 118
8.1 Photocatalytic Properties 118
8.1.1 Introduction 118
8.1.2 Mechanisms of TiO2 Photocatalysis 118
8.1.3 Experiment 120
8.1.4 Results and Discussion 121
8.2 Gas Sensing Properties 123
8.2.1 Introduction 123
8.2.2 Mechanism of the Gas Sensor 123
8.2.3 Experiment 123
8.2.4 Results and Discussion 124
8.3 Summary 126

Chapter 9 Conclusion and Future Works 135
9.1 Conclusions 135
9.2 Future Works 137

Reference 139

Publication List 157

Autobiography 162

Chapter 1
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Chapter 2
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Chapter 3
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[5.16] M. Taniguchi, T. Murakawa, and Y. Kajitani, “A novel passivation technique of GaAs power MESFETs”, Appl. Surf. Sci., vol. 56-58, pp. 827-831, 1992.

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Chapter 6
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[6.4] B. Reichman and A. J. Bard, J. Electrochem. Soc., vol. 127, pp. 697, 1980.

Chapter 7
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[7.6] Rajnish K. Sharma, and M. C. Bhatnagar, “Improvement of the oxygen gas sensitivity in doped TiO2 thick films”, Sens. Actuators B, vol. 56, pp. 215-219, 1999.

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Chapter 8
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[8.3] M. R. Hoffmann, S. T. Martin, W. Choi, and D. W. Bahnemann, “ Environmental Applications of Semiconductor Photocatalysis”, Chem. Rev., vol. 95, pp. 69-96, 1995.

[8.4] M. S. Jeon, T. K. Lee, D. H. Kim, H. Joo, and H. T. Kim, “ The enhancement of redox reaction with mixed oxide catalysts by the sol-gel process”, Sol. Energy Mater. Sol. Cells, vol. 57, pp. 217-227, 1999.

[8.5] M. Li, Y. Chen “ An investigation of response time of TiO2 thin film oxygen sensors”, Sens. Actuators B, vol. 32, pp. 83-85, 1996.

[8.6] Y. Yamada, Y. Seno, Y. Masuoka, T. Nakamura, and K. Yamashita, “ NO2 sensing characteristics of Nb doped TiO2 thin films and their electronic properties”, Sens. Actuators B, vol. 66, pp. 164-166, 2000.

[8.7] T. Iwanaga, T. Hyodo, Y. Shimizu, and M. Egashira, “H2 sensing properties and mechanism of anodically oxidized TiO2 film contacted with Pd electrode”, Sens. and Actuators B, vol. 93, pp. 519-525, 2003.

[8.8] K. Galatsis, Y.X. Li, W. Wlodarsky, E. Comini, G. Sberveglieri, C.
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[8.9] R. K. Sharma, M. C. Bhatnagar, G. L. Sharma, “ Mechanism in Nb doped titania oxygen gas sensor”, Sens. Actuators B, vol. 46, pp. 194-201, 1998.