低維金屬氧化物奈米結構之表面修飾在光電與光觸媒特性之研究

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研究生：	潘科穎 Pan, Ko-Ying
論文名稱：	低維金屬氧化物奈米結構之表面修飾在光電與光觸媒特性之研究 Studies on Low-dimensional Metal Oxide Nanostructures and Their Surface Modification on Optoelectric and Photocatalystic Properties
指導教授：	施漢章吳志明
口試委員:	施漢章吳志明莊東漢薛富盛林景崎
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：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	155
中文關鍵詞：	二氧化錫/氧化鋅核殼奈米線、氧化銦及氧化銦錫奈米結構、氧化矽/銀之奈米核殼顆粒、表面電漿子、光觸媒、奈米銀鑲嵌於二氧化矽複合結構、退火、抗菌、陰極激發光譜儀
外文關鍵詞：	core-shell SnO2-ZnO nanowire, Tin-doped indium oxide nanostructure, core-shelled silica-silver nanoparticle, surface plasmon resonance, Photocatalyst, Silver-embedded aluminum/silica nanoparticles, Annealing, Antibacterial, Cathodeluminescence
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本論文之研究中，包含：(一) 二氧化錫/氧化鋅核殼奈米線之合成與光電特性研究，和氧化銦及氧化銦錫奈米結構之合成與其光電特性應用之研究；(二) 二氧化矽/銀之奈米核殼顆粒之合成與其表面電漿子共振引發之光觸媒催化反應研究和奈米銀鑲嵌於二氧化矽複合結構之合成，及其退火與抗菌應用之研究。
在二氧化錫/氧化鋅之核殼奈米線之合成過程中，採用熱蒸鍍法在氧化鋁基板上製造出密集之二氧化錫奈米線。接著以原子層沉積法(atomic layer deposition, ALD)，奈米級氧化鋅附合於二氧化錫奈米線上，以獲得二氧化錫/氧化鋅核殼結構奈米線。材料分析可以確認其成分與結構，電性量測及紫外光分析，顯示本材料具備優秀的紫外光探測能力。
在氧化銦及氧化銦錫奈米結構合成，採用熱蒸鍍法在氧化矽基板上，不同的製程參數，分別沉積出氧化銦奈米棒、奈米塔及氧化銦錫奈米棒。材料分析證明其成分與結構，且更進一步做電性測試及陰極激發光譜儀(Catho- doluminescence, CL) 之分析，發現其可應用於有機發光二極體之元件。
在二氧化矽/銀之奈米核殼顆粒製作過程，先利用Stöber法製作出奈米級二氧化矽球，接著以種子成長法來合成二氧化矽/銀之奈米核殼結構粒子，並用葡萄糖當還原劑來控制奈米銀之幾何形狀。紫外光-可見光吸收光譜特性檢測發現：紅位移現象與特徵吸收峰的寬度皆與銀顆粒尺寸成正比的關係，且當粒子結構外型呈橢圓形時，雙特徵吸收峰的現象，隨即產生。這特殊的表面電漿子共振吸收的現象也與其後之光分解效率試驗相互呼應，共振程度愈高者其效率也愈佳。
在奈米級銀鑲嵌於二氧化矽複合型材料結構之合成、退火及抗菌應用之研究中，先採用溶凝膠法(Sol-gel method)製作二氧化矽奈米顆粒，其後再做退火熱處理。經由化學穩定性及抗菌測試對一系列的產物中，可證明其可有效用於抗菌相關之產業。

There are two major parts in this thesis, including Part I: the fabrications, materials characteristics and optoelectronic applications of nanostructures of core-shell SnO2-ZnO, tin-doped indium oxide, and Part II: the syntheses, materials features and optoelectronic applications of nanoparticles of core-shelled silica-silver and silver-embedded aluminum/silica.
In the Part I, as for core-shell SnO2-ZnO nanowires, in advance, tin dioxide nanowires were synthesized by thermal evaporation. Then, depositions of ZnO nanolayer on SnO2 nanowires have been successfully synthesized by atomic layer deposition (ALD). These results demonstrated that the SnO2-ZnO core-shell nanowires have potential application as UV photodetectors with high photon-sensing properties.
In terms of nanostructures of tin-doped indium oxide, indium oxide (In2O3) nanorods, nanotowers and tin-doped (Sn:In=1:100) indium oxide (ITO) nanorods have been successfully fabricated by thermal evaporation, respectively. Judging from cathodeluminescence (CL) spectra of these three nanoproducts, it is clear that tin-doped (Sn:In=1:100) indium oxide (ITO) nanorods cause a blue shift. No doubt that ITO nanorods obtains the most effective performance among these three nanoproducts, and this also means doping elements in original nanomaterials would be the best way to enhance physical properties. Additionally, this study would be beneficial to the applications of In2O3 nanorods, nanotowers and ITO nanorods in optoelectronic nanodevices, especially in organic light-emitting diode (OLED).
In the Part II, as for core-shelled silica-silver nanoparticles, abundant core-shelled silica-silver nanospheres with uniform diameter and morphology were successfully synthesized by Stöber and seed-mediated method, in sequence. Moreover, by the different additions of glucose as the reducing agent, the silver nanoparticles were deposited on silica spheres by redox reaction, and the dimensions of samples were well controlled. The surface plasmon resonance absorption band shifted toward infra-red region and became broader gradually during the dimensions of silver nanoparticles were increased in the growth range. Meanwhile, this intriguing result shows that two absorption characteristics peaks are observed in the spectra while the morphologies of nanoparticles are becoming oval-shaped. The amazing data imply that using core-shelled silica-silver nanospheres efficiently enhances the degradation of the organic pollutants under solar energy, which means the core-shelled silica-silver nanospheres is not only a cost-effective route but an energy-saving way to our planet.
In terms of silver-embedded aluminum/silica nanoparticles, in order to improve the time-consumption issue of the above method, substantial silver-embedded aluminum/silica nanospheres with uniform diameter and morphology were successfully synthesized by a modified sol-gel technique, a one-spot method. The chemical durable examinations and antibacterial tests of each sample were also carried out for the confirmation of usages in practical. As a result of above analyses, the silver-embedded aluminum/silica nanospheres are eligible for fabricating antibacterial utensils.

Abstract     I
Acknowledge    IV
Contents    V
List of Tables    IX
Figure Captions    X
Chapter 1 Introduction    1
1.1 SnO2-ZnO core-shell nanowires    1
1.2 Thermally evaporated tin-doped indium oxide nanostructures    2
1.3 Core-shelled silica-silver nanospheres    4
1.4 Silver-embedded aluminum/silica nanoparticles    6
1.5 Motivation    8
Chapter 2 Literature Review    10
2.1 Brief description of nanomaterials and nanotechnology    10
2.2 Physics of Nanomaterials    14
2.2.1 Surface effects    16
2.2.2 Quantum confinement effects    18
2.2.3 Quantum tunneling effects    21
2.3 Brief description of tin oxide, zinc oxide and indium oxide nanostructures    24
2.3.1 Crystal structure and physical characteristics of tin oxide    24
2.3.2 Crystal structure and physical characteristics of zinc oxide    25
2.3.3 Crystal structure and physical characteristics of indium oxide    26
2.4 Preparation and growth mechanism of tin oxide, zinc oxide and indium oxide nanostructures    27
2.4.1 Thermal chemical vapor deposition (TCVD)    28
2.4.2 Plasma-enhance chemical vapor deposition (PECVD)    29
2.4.3 Hydrothermal technique    30
2.4.4 Growth mechanisms of one dimensional nanostructures    32
2.4.4.1 Vapor-liquid-solid (VLS) mechanism    32
2.4.4.2 Vapor-solid (VS) mechanism    34
2.4.4.3 Solution-liquid-solid (SLS) mechanism    34
2.5 Brief description of silicon oxide and silver    37
2.5.1 Crystal and physical characteristics of silicon oxide    37
2.5.2 Crystal and physical characteristics of silver    38
2.6 Preparation of core-shelled nanoparticles    40
2.6.1 Brief description of core-shell nanoparticles    40
2.6.2 Synthesis of silica nanospheres by Stöber method    42
2.6.3 Deposition of silver nanoparticles on silica nanoparticles by seed-growth method    43
2.6.4 Surface plasmon resonance of metal nanoparticles    45
2.6.5 Dipolar coupling model of two-particle system    46
2.6.6 Optical properties of core-shell nanoparticles    51
Chapter 3 Experimental    53
3.1 Fabrication process of SnO2-ZnO core-shell and tin-doped indium oxide nanostructures    53
3.1.1 Fabrication of SnO2-ZnO core-shell nanowires    53
3.1.2 Fabrication of tin-doped indium oxide nanostructures    54
3.2 Synthesis process of core-shelled silica-silver and silver-embedded  
  aluminum/silica nanoparticles    55
3.2.1 Synthesis process of core-shelled silica-silver nanoparticle    55
3.2.2 Synthesis process of silver-embedded aluminum/silica nanoparticles    57
3.3 The facilities for characterization and analysis    59
3.3.1 Field emission scanning electron microscopy (FESEM)    59
3.3.2 X-ray diffraction (XRD)    60
3.3.3 High-resolution transmission electron microscopy (HRTEM)    61
3.3.4 Energy dispersion spectrometer (EDS)    62
3.3.5 X-ray photoelectron spectrum (XPS)    62
3.3.6 Raman spectroscopy    63
3.3.7 Cathodoluminescence (CL)    64
Chapter 4 Results and Discussion    65
4.1 Analyses and examinations of SnO2-ZnO core-shell nanowires    65
4.1.1 The facilities for analyses and examinations of SnO2-ZnO core-shell nanowires    65
4.1.2 XRD analysis and SEM images of SnO2-ZnO core-shell nanowires    65
4.1.3 HRTEM images of SnO2-ZnO core-shell nanowires    68
4.1.4 XPS analysis of SnO2-ZnO core-shell nanowires    71
4.1.5 Optoelectronic properties of SnO2-ZnO core-shell nanowires    73
4.2 Analyses and examinations of nanostructures of tin-doped indium oxide    77
4.2.1 The facilities of analyses and examinations for nanostructures of tin-doped indium oxide    77
4.2.2 SEM images and XRD analysis of nanostructures of tin-doped indium oxide    78
4.2.3 TEM and HRTEM images of nanostructures of tin-doped indium oxide    81
4.2.4 XPS analysis of nanostructures of tin-doped indium oxide    87
4.2.5 Optoelectronic properties of nanostructures of tin-doped indium oxide    93
4.3 Analyses and examinations of core-shelled silica-silver nanoparticles    98
4.3.1 The instruments of analyses and examinations for core-shelled silica-silver nanoparticles    98
4.3.2 Structure and morphology of core-shelled silica-silver nanoparticles    99
4.3.3 XRD pattern and HRTEM image of SiO2@Ag nanospheres    101
4.3.4 XPS analysis of SiO2@Ag nanospheres    103
4.3.5 UV-visible spectrum of SiO2@Ag nanospheres    106
4.3.6 Photocatalytic degradation of SiO2@Ag nanospheres    109
4.4 Analysis and examinations of silver-embedded aluminum/silica nanoparticles       111
4.4.1 The instruments of analyses and examinations for silver-embedded aluminum/silica nanoparticles    111
4.4.2 Morphology of silver-embedded aluminum/silica nanospheres    113
4.4.3 XPS analysis of silver-embedded aluminum/silica nanospheres    118
4.4.4 UV-visible spectrum of silver-embedded on aluminum/silica nanospheres       124
4.4.5 Chemical durable analysis of silver-embedded aluminum/silica nanospheres     126
4.4.6 Antibacterial analysis of silver-embedded aluminum/silica nanospheres
    129
Chapter 5 Conclusions    132
References    134
Publication list    154











List of Tables

Table 4.1 Synthesis conditions and morphology characteristics of In2O3 and ITO nanostructures    82
Table 4.2 Atomic of In2O3 nanorods, nanotowers and ITO nanorods by XPS    88
Table 4.3 The XPS results of Ag0 and Ag+ by deconvolution of Ag(3d5/2) curve
.    120
Table 4.4 The results of antibacterial examinations.    131



















Figure Captions

Figure 2.1 The scale of nanoworld    12
Figure 2.2 Scheme of the nanotechnology    13
Figure 2.3 Classification of Nanomaterials (a) 0D spheres and clusters, (b) 1D nanofibers, wires, and rods, (c) 2D films, plates, and networks, (d) 3D nanomaterials
    15
Figure 2.4 The percentage of surface atoms / total atoms    16
Figure 2.5 The schematic illustration of photocatalyst TiO2    18
Figure 2.6 Density of states in a bulk materials, a quantum well (2-D nanomaterial), a quantum wire (1-D nanomaterial), and a quantum dot (0-D nanomaterial)    21
Figure 2.7 A particle tunneling through a barrier    23
Figure 2.8 Sketch of the tetragonal rutile structure of tin dioxide includes the blue balls and red balls, which represent the tin and oxygen atoms, respectively    24
Figure 2.9 Wurtzite structure of ZnO    25
Figure 2.10 The unit cell model of In2O3    26
Figure 2.11 Illustration of thermal evaporation furnace working system    29
Figure 2.12 Schematic illustration of PECVD system    30
Figure 2.13 The schematic illustration of the autoclave for hydrothermal technique    31
Figure 2.14 Schematic illustration of this mechanism (a) Growth of a nanowire via VLS mechanism; (b) The binary phase diagram between Au and Ge with an indication of compositional zones responsible for alloying, nucleation and growth    33
Figure 2.15 Growth mechanisms. (A) VLS mechanism: the flux droplet is a metal such as Au, Ag, Pd, Pt, Ni, or Cu, and E1 and E2 are elements of the crystal phase dissolved in the metallic flux droplet. The whiskers on the left and right are early and late in the VLS growth process, respectively. (B) SLS mechanism: the flux droplet is in, and M and E are elements of the III-V semiconductor dissolved in the flux droplet. The crystalline fiber and attached flux droplet are suspended in the reaction solution
    36
Figure 2.16 Illustration of the tetrahedral structure of silica. The blue ball represents a silicon atom; the coffee ball represents an oxygen atom.    37
Figure 2.17 Crystal lattice of metallic silver. The blue balls represent silver atoms    38
Figure 2.18 UV-vis spectrum of silver nanoparticles    39
Figure 2.19 Variety of core shell particles. (a) Surface-modified core particles anchored with shell particles; (b) More shell particles reduced onto core to form a complete shell; (c) Smooth coating of dielectric core with shell; (d) Encapsulation of very small particles with dielectric material; (e) Embedding number of small particles inside a single dielectric particle; (f) Quantum bubble; (g) Multishell particle.    41
Figure 2.20 SEM image of colloidal silica particles    43
Figure 2.21 Fabrication of SiO2-Ag core-shelled nanoparticles by seed-growth. method.    44
Figure 2.22 (a) Normalized extinction spectra of spherical Ag, Au and Cu nanoparticles. (b) Spatial distribution of the SPR-induced enhancement of electric field at the SPR peak wavelength (420 nm), from a FDTD simulation of a 75 nm Ag nanocube    46
Figure 2. 23 The sketch of the dipole-dipole coupling between metallic nanoparticles
    46
Figure 2.24 UV-Vis absorption spectra of different nanosized silver particles    52
Figure 2.25 Variation in SPR band with shell thickness    52
Figure 3.1 FE-SEM JEOL JSM6500F    59
Figure 3.2 Shimadzu X-ray Diffractometer XRD-6000    60
Figure 3.3 High-Resolution Transmission Electron Microscopy    61
Figure 3.4 X-ray Photoelectron Spectrum    63
Figure 3.5 Micro-Raman system    64
Figure 3.6 JEOL-JSM-7001F    64
Figure 4.1 (a) XRD pattern (b) SEM image of SnO2-ZnO core-shell nanowires (ALD:200 cycles)    67
Figure 4.2 (a),(b) Low-magnification TEM, and (c) HRTEM image of a SnO2-ZnO core-shell nanowires (ALD:200 cycles)    70
Figure 4.3 The XPS (a) Zn 2p (b) O 1S spectrum    72
Figure 4.4 The I-V curve of SnO2-ZnO core-shell nanowires (ALD: 200cycles) and pure SnO2 nanowires    75
Figure 4.5 Photoresponse curves of (a) pure SnO2 nanowires and (b) SnO2-ZnO core-shell nanowires-based photodetectors    76
Figure 4.6. (a) SEM images of In2O2 nanorods. Inset: Enlarged image. (b) SEM images of In2O3 nanotowers. Inset: Enlarged image. (c) SEM images of ITO nanorods. Inset: Enlarged image.    80
Figure 4.7 XRD patterns of In2O3 nanorods, nanotowers and ITO nanorods.    80
Figure 4.8 (a) Low-magnification TEM image of In2O3 nanorods. (b) HRTEM image of In2O3 nanorods. Lower right inset: SAD pattern. (c) TEM-EDS analysis at spectrum1 ( The tip of In2O3 nanorods).    84
Figure 4.9 (a) Low-magnification TEM image of In2O3 nanortowers. (b) HRTEM image of In2O3 nanotowers. Lower right inset: SAD pattern. (c) Low-magnification TEM image of ITO nanorods. (d) HRTEM image of ITO nanorods. Lower right inset: SAD pattern    86
Figure 4.10 XPS spectra of In2O3 nanorods: (a) O 1s and (b) In 3d spectrum. XPS spectra of In2O3 nanotowers: (c) O 1s and (d) In 3d spectrum. XPS spectra of ITO nanorods: (e) O 1s, (f) In 3d and (g) Sn 3d spectrum    92
Figure 4.11 CL spectra: (a) In2O3 nanotowers, (b) In2O3 nanorods and (c) ITO nanorods. In CL signal of (a) and (b), two peaks concentrated at 599 nm and 641 nm. In CL signal of (c), two peaks concentrated at 566 nm and 628 nm. Two arrows mean the revelation of blue-shift.    96
Figure 4.12 Measured I-V curves of (a) ITO nanorods, (b) In2O3 nanotowers and (c) In2O3 nanorods obtained. Lower middle inset: the schematic picture of measurement system.    97
Figure 4.13 (a) SEM image of silica nanospheres, (b) TEM image of SiO2@Ag NSs (SA0), (c) TEM image of SiO2@Ag NSs with 1-cycle redox reaction(SA1), (d) TEM image of SiO2@Ag NSs with 2-cycle redox reaction(SA2). Upper right sides photos show the individual nanospheres TEM images taken of SA0, SA1 and SA2, respectively.    100
Figure 4.14 XRD pattern for SiO2@Ag NPs.    102
Figure 4.15 HRTEM image of SiO2@Ag NPs    102
Figure 4.16 The XPS of (a) survey scan of Sn2+-sensitized SiO2 nanospheres (b) survey scan of SiO2@Ag NSs (c) Si 2p of SiO2@Ag NSs (d) O 1s of SiO2@Ag NSs (e) Ag 3d of SiO2@Ag NSs (f) Sn 3d of SiO2@Ag NSs.    105
Figure 4.17 UV-visible absorption spectra of three kinds of SiO2@Ag NSs. (SA0, SA1 and SA2)    108
Figure 4.18 C/ C0 versus irradiation time plots for MB photodegradation    110
Figure 4.19 SEM image of silver-embedded silica nanospheres    115
Figure 4.20 The illustration of fabricating silver-embedded on aluminum/silica nanospheres and annealing    116
Figure 4.21 TEM images of (a) as-prepared sample; (b) SAS-250; (c) SAS-400; (d) 
SAS-600; (e) SAS-800; (f) SAS-1000: all scale bars are 100 nm    116
Figure 4.22 Enlarged TEM images of (a) as-prepared sample; (b) SAS-250; (c)  
SAS-400; (d) SAS-600; (e) SAS-800; (f) SAS-1000: all scale bars are 20 nm    117
Figure 4.23 XP spectra of silver-embedded silica nanospheres. (a) Survey scan, (b) Si 2p, (c) O 1s and (d) Al 2p.    121
Figure 4.24 The mechanisms of silver-embedded on aluminum/silica nanospheres at different annealing temperatures    122
Fig. 4.25 XP spectra of Ag 3d3/2 and 3d5/2 in silver-embedded silica nanospheres. (a) As-prepared, (b) SAS-250, (c) SAS-400, (d) SAS-600, (e) SAS-800, (f) SAS-1000
    123
Figure 4.26 UV-visible spectra of silver-embedded silica nanospheres    125
Figure 4.27 Al, Si and Ag ions released rate of silver-embedded silica nanospheres in water.    128
Figure 4.28 Antibacterial examinations for (a) placebo film (100% PE), (b) film of As-prepared sample, (c) film of SAS-400, (d) film of SAS-600, (e) film of SAS-800 and (f) film of SAS-1000.    131

                                

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