快速合成不同形態奈米氧化鎢結構與其光學特性之研究

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研究生：	謝雲從 Hsieh, Yun-Tsung
論文名稱：	快速合成不同形態奈米氧化鎢結構與其光學特性之研究 Controllable Morphologies and Optical Properties with Rapid and Efficient Synthesis of Tungsten Oxide Nanobundles
指導教授：	施漢章 Shih, Han C.
口試委員:	杜正恭丁志明呂福興林景崎
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2011
畢業學年度：	99
語文別：	英文
論文頁數：	162
中文關鍵詞：	奈米氧化鎢、微波電漿輔助化學氣相沈積、熱化學氣相沈積、不同形態、快速
外文關鍵詞：	tungsten oxide nanomaterials, microwave plasma-enhanced chemical vapor deposition, CVD, controllable morphology
相關次數：	點閱：2 下載：0
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本研究中，利用了微波電漿輔助化學氣相沈積系統(Microwave Plasma-Enhanced Chemical Vapor Deposition, MPECVD)，以無觸媒的方式，在極短時間內，於矽基板上生長不同形態的氧化鎢 (W18O49 => WO2.72) 奈米材料，成長過程中，不同的反應時間下：1.5、 3 和 4 分鐘，分別生長了WO2.72 的奈米線、奈米棒及奈米片，晶體結構與化學組成經分析得知，這些不同形態WO2.72 奈米材料皆為單晶，且成長方向皆為[010]，奈米線為15–30 奈米、奈米棒為40–60奈米、奈米片為30奈米，亦即隨著反應時間的增加，WO2.72奈米材料長與寬的尺寸也隨之增加。另外，陰極激發光（Cathodoluminescence, CL）光譜得知，WO2.72奈米線由於量子尺寸效應，造成了紅移現象，也因為大量缺陷或氧空缺的緣故，WO2.72奈米線發出紅橙光。研究結果顯示，由於具優勢的極短生長時間，讓MPECVD成為一種高效率，並可隨意地控制生長不同形態之WO2.72奈米材料的方法。
相較於MPECVD，熱化學氣相沈積系統（Thermal Chemical Vapor Deposition, TCVD)，為一種廣泛並有效控制基板溫度的生長方式，我們利用TCVD以無觸媒的方式，生長不同形態的氧化鎢(WO3) 奈米材料，[002]為主要成長方向，此外，生成的WO3奈米材料與其光學性質，和生長過程中矽基板溫度的分佈有直接的關係，由於氧空缺的緣故，使得WO3奈米線相較於一般的WO3材料在可見光吸收光譜中有紅移現象，WO3奈米材料的能階也與晶體結構和量子尺寸效應相對應，在TCVD的成長環境下，氧氣流量和矽基板溫度決定了WO3奈米材料的良率與形態。研究結果顯示，在適當的生長環境參數下，TCVD系統為一種簡單、普遍、易控制並可大量生產不同形態WO3奈米材料的生長方式。

Contents
Abstract………………………………………………………………… I
Acknowledgement............................................V
Contents…………………………………………………………………VI
Table Captions………………………………………………………… X
Figure Captions……………………………………………………… XI
Chapter 1 Introduction ………………………………………………1
1.1 An Overview of Nanotechnology…………………………………1
1.2 Physics of Nanomaterials……………………………………… 4
  1.2-1 Surface Effects………………………………………………5
  1.2-2 Quantum Confinement Effect……………………………… 7
  1.2-3 Quantum Tunneling Effect…………………………………10
1.3 Preparation and Growth Mechanism of Nanomaterials…… 13
  1.3-1 Thermal Chemical Vapor Deposition (TCVD)……………13
  1.3-2 Plasma - Enhanced Chemical Vapor Deposition
        (PECVD)……………………………………………………… 14
  1.3-3 Sol -Gel Process……………………………………………14
  1.3-4 Reverse Microemulsion…………………………………… 15
  1.3-5 Electroplating Process……………………………………15
1.4 The Potential Disadvantages of Nanotechnology………… 16
1.5 Thesis Organization overview…………………………………19
References………………………………………………………………21
Chapter 2 Introduction to Tungsten-based Nanomaterials……27
2.1 Structure Properties of Tungsten Oxides………………… 27
2.2 Growth Mechanism of Tungsten Oxide Nanomaterials………34
  2.2-1 Vapor-Liquid-Solid (VLS) Mechanism……………………35
  2.2-2 Vapor-Solid (VS) Mechanism………………………………36
2.3 Preparation of WOx Nanomaterials……………………………38
  2.3-1 Chemical Vapor Deposition (CVD)……………………… 38
  2.3-2 Physical Vapor Deposition (PVD)……………………… 39
  2.3-3 Sol -Gel Process……………………………………………40
  2.3-4 Electroplating Method……………………………………41
2.4 Application of Tungsten-based Nanomaterials…………… 42
  2.4-1 Application as Gas Sensors………………………………42
  2.4-2 Application as Field Emitters………………………… 45
2.5 Motivations……………………………………………………… 46
References………………………………………………………………50
Chapter 3 Experimental Procedures……………………………… 64
3.1 Synthesis of Tungsten Oxide Nanomaterials……………… 64
  3.1-1 MPECVD…………………………………………………………64
  3.1-2 TCVD……………………………………………………………66
3.2 Characterization and Analysis……………………………… 69
  3.2-1 Field Emission Scanning Electron Microscope (FESEM)
        …………………………………………………………………69
  3.2-2 X-ray Diffraction (XRD)………………………………… 70
  3.2-3 High-resolution Transmission Electron Microscopy
      (HRTEM)………………………………………………………… 71
  3.2-4 Raman Spectroscopy…………………………………………72
  3.2-5 Cathodoluminescence (CL) Spectrometry……………… 73
  3.2-6 Ultraviolet UV-Visible……………………………………74
Chapter 4 Rapid Formation and Characterizations of Tungsten Oxide Nanobundles by MPECVD……………………………………… 76
4.1 Introduction………………………………………………………76
4.2 Experimental Procedures……………………………………… 79
4.3 SEM Analysis of Synthesized WO2.72…………………………80
4.4 XRD Analysis of Synthesized WO2.72…………………………82
4.5 TEM Analysis of Synthesized WO2.72…………………………87
  4.5-1 TEM Image of Synthesized WO2.72 Nanorods……………87
  4.5-2 TEM Image of Synthesized WO2.72 Nanoslabs………… 91
4.6 Raman Spectroscopy Analysis of Synthesized WO2.72…… 93
  4.6-1 Raman Spectra of Synthesized WO2.72 Nanorods………93
  4.6-2 Raman Spectra Analysis of Synthesized WO2.72
      Nanoslabs……………………………………………………… 95
4.7 Analysis of the Growth Mechanism……………………………96
4.8 Role of O2 in MPECVD Growth…………………………………104
4.9 CL Analysis of WO2.72 ……………………………………… 106
4.10 Summary………………………………………………………… 108
References…………………………………………………………… 109
Chapter 5 Growth and Optical Properties of Tungsten Oxide by Thermal CVD……………………………………………………… 115
5.1 Introduction…………………………………………………… 115
5.2 Experimental Procedures………………………………………119
5.3 SEM Analysis of Synthesized WO3……………………………120
5.4 XRD Analysis of Synthesized WO3......................121
5.5 TEM Analysis of Synthesized WO3……………………………125
5.6 Raman Spectroscopy Analysis of Synthesized WO3……… 128
5.7 Analysis of Growth Mechanism……………………………… 130
5.8 Role of O2 in TCVD Growth……………………………………133
5.9 Role of Substrate Temperature in TCVD Growth………… 135
5.10 UV-visible Spectra of Synthesized WO3………………… 138
5.11 CL Analysis of the Synthesized WO3………………………140
5.12 Summary………………………………………………………… 144
References…………………………………………………………… 146
Chapter 6 Concusions and Future Words…………………………155
6.1 Conclusions………………………………………………………155
6.2 Suggestions for Future Work…………………………………157
Publish List………………………………………………………… 159
Vita…………………………………………………………………… 162

Table Captions
Table 1-1 Summary of WO3 polymorphs…………………………… 31
Table 4-1 Characteristic Raman frequencies of tungsten
oxides……………………………………………………………………95
Table 4-2 Summary of reaction times v.s. morphology………100
Table 4-3 Summary of O2 flow rate v.s. morphology by MPECVD………………………………………………………………… 106
Table 5-1 Characteristic Raman frequencies of tungsten oxides………………………………………………………………… 129
Table 5-2 Summary of O2 flow rate v.s. morphology by TCVD…………………………………………………………………… 134
Table 5-3 Summary of Substrate Temperatures v.s. morphology…………………………………………………………… 138

Figure Captions
Figure 1-1 The scale of nanoworld……………………………… 3
Figure 1-2 The percentage of surface atoms / total atoms… 7
Figure 1-3 Density of states for bulk, quasi-2D, quasi-1D, and zero-dimensional system…………………………………………9
Figure 1-4 (a) The passage of a particle through a barrier in the traditional world, and (b) the passage of a particle through a barrier in the quantum world……………………… 12
Figure 2-1 Orbitals of tungsten………………………………… 28
Figure 2-2 WO3 showing a yellow to bright green color…… 28
Figure 2-3 (a) Unit cell for perovskite lattice, and (b) Structure of crystalline WO3………………………………………30
Figure 2-4 W-O Phase diagrams (condensed system, 0.1 MPa)……………………………………………………………………………31
Figure 2-5 Schematic band structures of WO3. Tungsten and oxygen orbitals are indicated, using standard notation, as well as the location of the Fermi level (εF). The indicated numbers of electrons (e-) can be accommodated in the bands. Filled states are shaded…………………………… 34
Figure 2-6 Schematic illustration of vapor-liquid-solid nanowire growth mechanism including three stages……………36
Figure 2-7 The schematic illustration of vapor-solid mechanism by fabrication tungsten oxide nanomaterials by MPECVD……………………………………………………………………37
Figure 3-1 Schematic representation of the MPECVD system…65
Figure 3-2 MPECVD facility…………………………………………66
Figure 3-3 Schematic representation of the thermal CVD system……………………………………………………………………68
Figure 3-4 Thermal CVD facility………………………………… 68
Figure 3-5 FE-SEM JEOL JSM6500F………………………………… 69
Figure 3-6 Shimadzu x-ray diffractometer XRD-6000………… 70
Figure 3-7 High-Resolution Transmission Electron Microscopy (HRTEM)………………………………………………………………… 71
Figure 3-8 Raman spectrometer ((LabRAM; Dilor)………………73
Figure 3-9 JEOL-JSM-7001F………………………………………… 74
Figrue 3-10 UV-visible (Hitachi, U3010)……………………… 75
Figure 4-1 Procedure for synthesis of WO2.72 with controllable morphologies………………………………………… 79
Figure 4-2 SEM images of nanobundles grown under different reaction times. (a)–(c): Morphologies of nanobundles obtained under reaction times of 1.5, 3, and 4 min…………81
Figure 4-3 SEM images of the WO2.72 nanoslabs at different magnifications…………………………………………………………82
Figure 4-4 XRD spectrum of the nanobundles fabricated at 1.5, 3, and 4 min…………………………………………………… 84
Figure 4-5 JCPDS Card No. 36-0101……………………………… 85
Figure 4-6 XRD spectra of sample from: (a) the top and (b) the bottom nanoslabs…………………………………………………87
Figure 4-7 (a) Transmission electron microscopy (TEM), (b) high-resolution TEM (HRTEM) images of the nanowires. Inset shows the corresponding selected-area diffraction (SAD) pattern, (c) typical energy-dispersive x-ray spectroscopy (EDS) of the nanowires showing the presence of only W and O with an atomic ratio W:O =1:2.72. Peaks due to C and Cu are a result of TEM copper grids, and (d) corresponding EDS elemental line profile………………………………………………89
Figure 4-8 (a) and (b): Typical EDS of the nanobundles fabricated under reaction times of 3 min and 4 min, respectively. The nanobundles comprise only W and O Peaks due to C and Cu originate from the TEM copper grids……… 90
Figure 4-9 (a) TEM image and (b) HRTEM image of the  nanowslab. Inset shows the SAD pattern of the nanoslab……92
Figure 4-10 EDS spectra of the sample from: (a) the top nanoslabs, and (b) the bottom nanoslabs……………………… 93
Figure 4-11 Raman spectra of the as-prepared WO2.72 nanowires……………………………………………………………… 94
Figure 4-12 Raman spectra of the as-prepared nanoslabs from: (a) the top nanoslabs, and (b) the bottom nanoslabs 96
Figure 4-13 SEM image of the nanobundles grown under different reaction times: (a) 2 min, and (b) 3.5 min…… 100
Figure 4-14 (a) Cross-sectional SEM image of WO2.72 nanowires grown on the base layer. The inset shows a magnified image depicting the bottom of nanowire growth,
and (b) WO2.72 nanowires in regions where only a base layer exists………………………………………………………………… 102
Figure 4-15 Schematic illustration of the growth mechanism of the metal oxide nanostructures from bulk material upon exposure to highly dissociated oxygen plasma. Four main stages of nanostructure growth are shown: (a) nucleation, (b) nanowire growth, (c) nanorod growth, and (d) nanoslab growth………………………………………………………………… 103
Figure 4-16 SEM image of the WO2.72 nanowires grown at different O2 flow rates: (a) 0 sccm (b) 25 sccm (c) 100 sccm, and (d) 175 sccm…………………………………………… 105
Figure 4-17 Cathodoluminescence (CL) spectra of the as-prepared WO2.72 nanowires…………………………………………107
Figure 5-1 Procedure for synthesis of WO3 with controllable morphologies………………………………………………………… 119
Figure 5-2 SEM images of tungsten oxide nanobundles formed at different substrate temperatures: (a) 250–350°C, (b) 450–550°C, and (c) 550–650°C………………………………… 121
Figure 5-3 XRD spectra of the nanobundles fabricated at substrate temperatures of 250–350°C, 450–550°C, and 650–750°C……………………………………………………………………123
Figure 5-4 JCPDS Card No. 43-1035………………………………124
Figure 5-5 (a) TEM and (b) high-resolution TEM (HRTEM) images of a nanowire. Inset shows the corresponding selected-area diffraction (SAD) pattern, and (c) TEM and (d) HRTEM images of a nanorod……………………………………126
Figure 5-6 (a) Energy-dispersive x-ray spectroscopy (EDS) elemental line profile of nanowire shown in Figure 5-5a (b) and (c) EDS spectra for nanobundles fabricated at
substrate temperatures of 250–350°C and 450–550°C, respectively. Nanobundles contain only W and O atoms. Peaks due to C and Cu signals can be attributed to copper TEM grids……………………………………………………………………127
Figure 5-7 Raman spectrum of the as-prepared WO3 nanowires………………………………………………………………129
Figure 5-8 SEM image of the WO3 nanowires grown at various O2 flow rates: (a) 0 sccm (b) 0.5 sccm, and (c) 2 sccm…134
Figure 5-9 SEM images of WO3 nanorods grown with different silicon substrates at different temperatures: (a) 400–500°C (b) 600-700°C, and (c) left region is silicon
substrate for temperatures of 500–600°C, and right region is silicon substrate for temperatures of 600–700°C………137
Figure 5-10 UV-visible spectrum of the as-prepared WO3 nanowires; the inset shows the corresponding (αE)2-E curve……………………………………………………………………140
Figure 5-11 Cathodoluminescence (CL) spectrum of the as-prepared WO3 nanowires…………………………………………… 142
Figure 5-12 CL spectra of the as-prepared WO3 nanorods… 144

                                

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