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研究生:蔡孟育
研究生(外文):Meng-Yu Tsai
論文名稱:利用溶膠凝膠法與噴塗技術之玻璃基板表面改質
論文名稱(外文):Surface modification on a glass surface with a combination technique of sol-gel and air brushing processes
指導教授:陳炳煇陳炳煇引用關係
學位類別:碩士
校院名稱:國立臺灣大學
系所名稱:機械工程學研究所
學門:工程學門
學類:機械工程學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:英文
論文頁數:181
中文關鍵詞:超疏水透光玻璃溶膠凝膠法二氧化矽噴塗
外文關鍵詞:superhydrophobictransparentglasssol-gelsilicaair-brushing
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 在日常生活所見到的蓮花葉片,因為其表面具有奈米與微米的複合型結構以及表面的蠟質,故常可見到水珠幾乎呈現球狀在蓮花葉上,水珠流動的過程便能將表面之灰塵給帶走,這樣的超疏水與表面自潔的特性便是著名的蓮花效應。
  藉由此自然界的特性,激起建立類似的仿生結構在玻璃基板上之動機。材料要能表現出超疏水的特性在於降低材料的表面能。方式有二:第一,在表面建立粗糙度,而這些粗糙度會形成許許多多的孔隙並且將空氣困在其中,使得水分子傾向於聚在一起形成小水珠。;第二,在表面塗佈低表面能的材料,亦即降低材料之表面張力。在這兩大方向之下,本研究選用奈米級與微米級之二氧化矽顆粒作為建立表面粗糙度的關鍵材料,並且利用矽烷類化合物(TEOS)做為接合劑,以利顆粒與玻璃表面接合;接著利用適當的噴塗技術與合宜的烘烤溫度將顆粒與接合劑均勻的塗佈和接合在玻璃表面上,如此便能建立出高透光度與具有粗糙度的表面。最後再進行疏水與疏油材料(PFCS)的表面處理,一方面增加其疏水特性使其能表現出超疏水,另一方面也增加表面的耐久性與耐刮性甚至是疏油性,使其能長時間的面對紫外光、高低溫變化以及汙垢之環境。  


This study aims to fabricate the optically transparent superhydrophobic silica based films on glass surface with optimized adhesion and hardness. The hydrophobic performance is determined by two factors i.e. surface roughness and surface energy. To get a superhydrophobic surface, enhancing the roughness of the glass surface and lowering the surface energy are essential. A silane coupling agent, tetraethoxysilane (TEOS), effectively bonds silica particles onto the glass substrate. Desired surface roughness was obtained by adjusting nano silica particles concentration of the precursors prepared by the sol-gel process. 6.38% of nano silica particles concentration was found to be sufficient to create a rough surface, while retaining enough transmittance. Silica suspension was coated onto the glass substrate by the dip-coating and air-brushing methods. Both methods can deposit a uniform, transparent coating on the glass substrate. Diluting the precursor by adding ethanol or a mixture of D.I. water and ethanol at specific volumetric ratio further improved the transmittance and superhydrophobicity efficiency. The coating with optimized adhesion and hardness was obtained by the sol-gel process with the careful control of hydrolysis, condensation reactions, and appropriate baking treatment. To obtain superhydrophobic surface, the baked glass was further treated with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (PFCS), trimethoxyphenylsilane, octadecyltrimethoxysilane, or triethoxy (octyl) silane by immersing, air brushing, or quick dipping method.
The results showed that as the silica particle concentration and the thickness of the coating were increased, the surface roughness was enhanced. Rougher surface displayed a higher superhydrophobicity and lower transmittance. Therefore, the concentration of silica particle, thickness of coatings, and the ratio of ethanol and D.I. water are of great importance to deposit a transparent, superhydrophobic coating on glass. A superhydrophobic (CA= 151.7°) and nearly transparent (T~87%) surface has been successfully made on a glass by the precursor diluted by a solution containing 60 ml D.I. water and 20 ml ethanol, followed by the post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane using the quick-dip method.


Table of Content
Acknowledgement III
Abstract IV
Nomenclature VI
List of Tables X
List of Figures XVI
CHAPTER1. INTRODUCTION 1
1.1. Motivation 1
1.2. Literature review 2
1.2.1. Lotus-effect 2
1.2.2. Self-cleaning effect based on superhydrophobic property 3
1.2.3. Biomimetic technology for superhydrophobic surfaces 3
1.2.4. Approaches used to fabricate a superhydrophobic surface. 5
1.3. Aims and missions 13
CHAPTER2. THEORY 26
2.1. Principle of sol-gel process 26
2.2. Silane coupling agent 31
2.3. Coating methods 34
2.3.1. Spin coating 34
2.3.2. Dip coating 35
2.3.3. Air brushing 36
2.3.4. Advantages and disadvantages of different coating methods 39
2.4. Surface energy 40
2.5. Wetting 41
2.6. Contact angle 42
2.7. Young’s equation 42
2.7.1. Wenzel''s model 44
2.7.2. Cassie–Baxter model 44
2.8. Hydrophilic, hydrophobic, superhydrophilic, and superhydrophobic surfaces 45
2.9. Contact angle hysteresis and Tilt angle 46
CHAPTER3. EXPERIMENTS 52
3.1. Experimental chemistry materials, reagents and equipments 52
3.2. Functional silane structures 55
3.3. Fabrication of silica particles based superhydrophobic films on glass substrate 57
3.4. Fabrication of nano silica particles based superhydrophobic films by different coating methods 58
3.4.1. Fabrication of nano silica particles based superhydrophobic films by dipping approach 59
3.4.2. Fabrication of nano silica particles based superhydrophobic films by air-brushing approach 60
3.5. Fabrication of nano silica particles based superhydrophobic films with mixture of silanes in precursor by air-brushing approach 61
3.5.1. Fabrication of nano silica particles based superhydrophobic films with precursor containing TEOS and isobutyltriethoxysilane by air-brushing approach 62
3.6. Fabrication of nano silica particles based superhydrophobic films with precursor diluted via ethanol at various molar ratios by air-brushing approach 63
3.7. Fabrication of nano silica particles based superhydrophobic films with precursor diluted via ethanol and D.I. water at various volumetric ratio by air-brushing approach 64
3.8. Methods for performing air-brushing process 65
3.9. Measuring Principles of Testing Instruments 66
3.9.1. Contact angle system 67
3.9.2. Ultraviolet-visible spectrophotometer (UV/Vis) 68
3.9.3. Scanning Electron Microscope (SEM) 69
3.9.4. Alpha-step 500 Surface Profiler 71
3.9.5. Hardness test 71
3.9.6. Energy-dispersive X-ray spectroscopy 72
CHAPTER4. RESULTS AND DISCUSSION 85
4.1. Silica based superhydrophobic films by dipping approach 85
4.2. Nano silica particles based superhydrophobic films by air-brushing approach 90
4.3. Roughness of superhydrophobic films enhanced by silica suspension containing TEOS and isobutyltriethoxysilane 122
4.4. Nano silica particles based superhydrophobic films by air-brushing approach with precursor diluted at various ethanol molar ratio 124
4.5. Nano silica particles based superhydrophobic films by air-brushing approach with precursor diluted using the mixture of ethanol and D.I. water at various volumetric ratio 162
4.6. An index for the amount of nano silica particles on a coated surface 174
CHAPTER5. CONCLUSION AND PROSPECT 175
REFERENCES 179
List of Tables
Table 2.1 Characteristics of Various Organic Substituents on Silanes 33
Table 2.2 Non-Organoreactive Alkoxysilanes 33
Table 2.3 The advantages and disadvantages of different coating methods 39
Table 2.4 Definition of hydrophobic surface and hydrophilic surface [41]. 47
Table 3.1 The surface energy of different functional group [42] 74
Table 4.1 Sample outlook with different dipping position 86
Table 4.2 Hyrdrophobic surface fabricated with various weight of micro silica particles. 87
Table 4.3 Hyrdrophobic fabricated surface with various weight of nano silica particles. 88
Table 4.4 Different kind of hydrophobic silane treatment for rough surface through dip-coating method 89
Table 4.5 Different kind hydrophobic silanes treatment for rough surface through dip-coating method 90
Table 4.6 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with trimethoxyphenylsilane (5%). 98
Table 4.7 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with trimethoxyphenylsilane (5%). 98
Table 4.8 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with octadecyltrimethoxysilane (1%). 99
Table 4.9 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with octadecyltrimethoxysilane (1%). 99
Table 4.10 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with triethoxy (octyl) silane (5%). 100
Table 4.11 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with triethoxy (octyl) silane (5%). 100
Table 4.12 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 101
Table 4.13 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 101
Table 4.14 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:8:4 (TEOS:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 102
Table 4.15 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with trimethoxyphenylsilane (5%). 102
Table 4.16 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with trimethoxyphenylsilane (5%). 103
Table 4.17 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with octadecyltrimethoxysilane (1%). 103
Table 4.18 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with octadecyltrimethoxysilane (1%). 104
Table 4.19 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with triethoxy (octyl) silane (5%). 104
Table 4.20 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with triethoxy (octyl) silane (5%). 105
Table 4.21 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 105
Table 4.22 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 106
Table 4.23 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:1:8:8 (TEOS:isobutyltriethoxysilane:Etoh:D.I. water) molar ratio and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 106
Table 4.24 Surface roughness of the precursor at 1:8:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. 116
Table 4.25 Surface roughness of the precursor at 1:1:8:8 molar ratio (TEOS: isobutyltriethoxysilaneethanol:D.I. water) and various coating parameters. 116
Table 4.26 Transmittance of the modified glasses with precursor with 1:8:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. 119
Table 4.27 Transmittance of the modified glasses with precursor with 1:1:8:8 molar ratio (TEOS: isobutyltriethoxysilaneethanol:D.I. water) and various coating parameters. 120
Table 4.28 Surface hardness of the precursor at 1:8:4 molar ratio (TEOS:ethanol:D.I.water) and various coating parameters. 121
Table 4.29 Surface hardness of the precursor at 1:1:8:8 molar ratio 121
Table 4.30 Oleophobicity evaluation of the modified surface with precursor with 1:1:8:8 molar ratio (TEOS: isobutyltriethoxysilaneethanol:D.I. water) and various coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%); Test oil: sunflower oil 121
Table 4.31 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:8:4, 1:16:4, 1:24:4, and 1:32:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 131
Table 4.32 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:40:4, 1:80:4, 1:120:4, and 1:160:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 132
Table 4.33 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:24:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment at trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 133
Table 4.34 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:32:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 134
Table 4.35 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:40:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 135
Table 4.36 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:80:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 136
Table 4.37 Contact angles of hydrophobic surface fabricated by preparing precursor diluted at 1:120:4 (TEOS:Etoh:D.I. water) molar ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%). 137
Table 4.38 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:80:4 (TEOS:Etoh:D.I. water) molar ratio, various coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by air-brushing method. 138
Table 4.39 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:80:4 (TEOS:Etoh:D.I. water) molar ratio, various coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by quick-dip by hand. 139
Table 4.40 Contact angles of hydrophobic surface fabricated by preparing precursor at 1:80:4 (TEOS:Etoh:D.I. water) molar ratio, various coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by quick-dip by dip-coater. 140
Table 4.41 Contact angles and transmittance of hydrophobic surface fabricated by preparing precursor at 1:120:4 and 1:160:4 (TEOS:Etoh:D.I. water) molar ratio, various coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by quick-dip by dip-coater. 141
Table 4.42 Transmittance of the modified glasses with precursor diluted at 1:8:4, 1:16:4, 1:24:4, 1:32:4, 1:40:4, 1:80:4, 1:120:4, and 1:160:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. 142
Table 4.43 Transmittance of the modified glasses with precursor diluted at 1:24:4 and 1:32:4 ratio (TEOS:ethanol:D.I. water) and various coating parameters. 143
Table 4.44 Transmittance of the modified glasses with precursor at 1:80:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. 144
Table 4.45 Transmittance of the modified glasses at precursor diluted at 1:40:4 and 1:120:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. 145
Table 4.46 Hardness of the modified glasses with precursor diluted at 1:8:4, 1:16:4, 1:24:4, 1:32:4, 1:40:4, 1:80:4, 1:120:4, and 1:160:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. The baking period was 4 h. 146
Table 4.47 Hardness of the modified glasses with precursor diluted at 1:24:4 and 1:32:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. The baking period was 4 h. 147
Table 4.48 Hardness of the modified glasses with precursor diluted at 1:40:4 and 1:120:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. The baking period was 4 h. 148
Table 4.49 Hardness of the modified glasses with precursor at1:80:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. The baking period was 4 h. 149
Table 4.50 Hardness of the modified glasses with precursor at 1:120:4 and 1:160:4 molar ratio (TEOS:ethanol:D.I. water) and various coating parameters. The baking period was 6 h. 150
Table 4.51 Contact angle measurement of hydrophobic surface fabricated by preparing precursor diluted by ethanol and D.I. water with various volume ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by quick-dip by dip-coater. 165
Table 4.52 Contact angle measurement of hydrophobic surface fabricated by preparing precursor diluted by ethanol and D.I. water with various volume ratio, coating parameters and post treatment with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) by quick-dip by dip-coater. 166
Table 4.53 Hardness of the modified glasses with precursor diluted by ethanol and D.I. water at various volume ratio and coating parameters 172
Table 4.54 Transmittance of the modified glasses with precursor diluted by ethanol and D.I. water at various volume ratio and coating parameters 173
Table 4.55 Silica particle concentrations correspond to the indexes with various suspensions of volumes (unit:g/cm^2) (area of coated surface:19.3548 cm^2) 174


List of Figures
Fig. 1.1 Water droplets on lotus leaf surface can roll freely. [1] 14
Fig. 1.2 Water droplets on micro/nano-scale on the leaf surface [3] 15
Fig. 1.3 SEM image of the surface of lotus leaves is found to be covered by micro and nano bumps [3]. 15
Fig. 1.4 Water carries dust particles away much more efficiently on a superhydrophobic surface (right) than on a hydrophobic surface (left) [4]. 16
Fig. 1.5 Images of the non-wetting leg of a water strider. (a) water strider walking on water (b) scanning electron microscope images of the water strider’s leg on micro scale (c) water strider’s leg on nano scale [5]. 17
Fig. 1.6 SEM images of (a) lotus leaf-like PDMS surface by nanocasting [10], and (b) PS-PDMS surface cast from a 5 mg/ml solution in dimethylformamide (DMF) in humid air [11]. 18
Fig. 1.7 (a) AFM image of the PET surfaces coated with TMS layer after the oxygen plasma treatment [13] ; (b) SEM image of the aluminum surfaces etched with a Beck’s dislocation etchant for 15 s at room temperature and the shape of a water droplet on the surface after fluoroalkylsilane coating [14]. 19
Fig. 1.8 SEM image of the nanopillars after hydrophobization the base diameter of the pillars is about 120nm [15]. 20
Fig. 1.9 SEM images of (a) the ultra water-repellent thin film prepared under TMMOS partial pressure of 50 Pa, with a water contact angle greater than 150°, and ( b) the water-repellent thin film prepared under a TMMOS partial pressure of 18 Pa, with a water contact angle of about 110° [16]. 21
Fig. 1.10 SEM images of the superhydrophobic surfaces made by electrochemical reaction. The copper surface after electrochemical reaction with sulfur gas [18]. 22
Fig. 1.11 SEM images of (PAH/PAA) films after a single acid treatment (A) and after a combined acid treatment (B) (C) SEM image of the fully treated structure with silica nanoparticles. (D) Water droplet on this superhydrophobic surface. [24]. 23
Fig. 1.12 SEM images (60u) of the size-reduced polystyrene beads and the water contact angle measurement on the corresponding modified surfaces (insets). The diameters of polystyrene beads and water contact angles on these surfaces were measured to be (a) 400 nm, 135°, (b) 360 nm, 144°, (c) 330 nm, 152° and (d) 190 nm, 168°. Bar: 1 μm [25]. 24
Fig. 1.13 Shape of water droplet on the (a) HMDZ modified, (b) TMCS modified silica films. [26] 25
Fig. 2.1 Silica particles and glass display the hydroxyl group while such materials meet deionized water. 29
Fig. 2.2 The hydrolysis reaction of tetraethyl orthosilicate (TEOS) 29
Fig. 2.3 The unreacted TEOS react with the silica present to form a strong siloxane bonds, thus bonding with both the silica and glass surface particles. 29
Fig. 2.4 The hydrolyzed TEOS react with the silica present to form a strong siloxane bonds, thus bonding with both the silica and glass surface particles. 30
Fig. 2.5 The format of TEOS couple with silica particles and glass substrates. 30
Fig. 2.6 Miscibility diagram of water, ethanol and TEOS [33] 31
Fig. 2.7 Illustration of Young’s equation on a flat idea surface 48
Fig. 2.8 Schematic drawing of (a) Wenzel’s state, the water droplet was assumed to penetrate into the structure. (b) Cassie-Baxter state, the water droplet was assumed to suspend on the structure. 49
Fig. 2.9 Schematic drawing of the method for measuring contact angles: 50
Fig. 2.10 Illustration of advancing angle (θa) and receding angle (θr) on a tilted surface 51
Fig. 3.1 High temperture furnace 54
Fig. 3.2 Dip-coater 54
Fig. 3.3 Air-brush gun and air compressor 54
Fig. 3.4 Large-sized glass container 55
Fig. 3.5 Scheme of the experimental procedure 75
Fig. 3.6 The procedure of silica based superhydrophobic films by dip-coating with a tilt angle equals to 30°. 76
Fig. 3.7 The procedure of silica based superhydrophobic films by dip-coating with a tilt angle equals to 90°. 77
Fig. 3.8 The procedure of nano silica based superhydrophobic films by air-brushing. 78
Fig. 3.9 The procedure of nano silica based superhydrophobic films with precursor containing TEOS and isobutyltriethoxysilane by air-brushing. 79
Fig. 3.10 The procedure of nano silica based superhydrophobic films with precursor diluted via ethanol at various molar ratios by air-brushing. 80
Fig. 3.11 The procedure of nano silica based superhydrophobic films with precursor diluted via ethanol and D.I. water at various volumetric ratios by air-brushing. 81
Fig. 3.12 Contact angle meter, VCA-2500 82
Fig. 3.13 Ultraviolet-visible spectrophotometer (UV/Vis): HR4000CG 83
Fig. 3.14 The principle drawing of ultraviolet-visible spectrophotometer (UV/Vis). 83
Fig. 3.15 Scanning electron microscope (SEM) LEO 1530 84
Fig. 3.16 A schematic drawing of principle of scanning electron microscope (SEM) [43]. 84
Fig. 4.1 SEM micrographs of modified glass surface with particle concentration was 2.00% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 107
Fig. 4.2 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 107
Fig. 4.3 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 108
Fig. 4.4 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 108
Fig. 4.5 SEM micrographs of modified glass surface with particle concentration was 6.97% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 109
Fig. 4.6 SEM micrographs of modified glass surface with particle concentration was 8.14% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 109
Fig. 4.7 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 110
Fig. 4.8 SEM micrographs of modified glass surface with particle concentration was 6.97% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 110
Fig. 4.9 SEM micrographs of modified glass surface with particle concentration was 8.14% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:ethanol:D.I. water = 1:8:4) 111
Fig. 4.10 SEM micrographs of modified glass surface with particle concentration was 2.00% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 111
Fig. 4.11 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 112
Fig. 4.12 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 112
Fig. 4.13 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 113
Fig. 4.14 SEM micrographs of modified glass surface with particle concentration was 6.97% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 113
Fig. 4.15 SEM micrographs of modified glass surface with particle concentration was 8.14% and volume of coatings was 2 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 114
Fig. 4.16 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 114
Fig. 4.17 SEM micrographs of modified glass surface with particle concentration was 6.97% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 115
Fig. 4.18 SEM micrographs of modified glass surface with particle concentration was 8.14% and volume of coatings was 3 ml at different magnifications: (A) 1000X (B) 250X (TEOS:isobutyltriethoxysilane:ethanol:D.I. water = 1:1:8:8) 115
Fig. 4.19 Sample outlook of the precursor with 1:8:4 molar ratio 117
Fig. 4.20 Sample outlook of the precursor at 1:1:8:8 molar ratio (TEOS: isobutyltriethoxysilaneethanol:D.I. water) and various coating parameters. 118
Fig. 4.21 EDS spectrum of the thin film from TEOS: isobutyltriethoxysilane:ethanol:D.I. water=1:1:8:8 and water repelling material coating with trichloro (1h, 1h, 2h, 2-perfluorooctyl) silane (1%) 123
Fig. 4.22 SEM micrographs of modified glass surface at particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:24:4) 151
Fig. 4.23 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:24:4) 151
Fig. 4.24 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:32:4) 152
Fig. 4.25 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:32:4) 152
Fig. 4.26 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:40:4) 153
Fig. 4.27 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:40:4) 153
Fig. 4.28 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 154
Fig. 4.29 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 154
Fig. 4.30 SEM micrographs of modified glass surface with particle concentration was 3.29% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:120:4) 155
Fig. 4.31 SEM micrographs of modified glass surface with particle concentration was 4.55% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:120:4) 155
Fig. 4.32 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 1 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 156
Fig. 4.33 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 156
Fig. 4.34 SEM micrographs of modified glass surface with particle concentration was 5.78% and volume of coatings was 3 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 157
Fig. 4.35 SEM micrographs of modified glass surface with particle concentration was 6.38% and volume of coatings was 1 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 157
Fig. 4.36 SEM micrographs of modified glass surface with particle concentration was 6.38% and volume of coatings was 2 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 158
Fig. 4.37 SEM micrographs of modified glass surface with particle concentration was 6.38% and volume of coatings was 3 ml at different magnifications: (A) 250X (B) 1000X (TEOS:ethanol:D.I. water = 1:80:4) 158
Fig. 4.38 Contact angle versus molar ratio of ethanol at low silica particles concentration and low volume of coatings. 159
Fig. 4.39 Transmittance versus molar ratio of ethanol at low silica particles concentration and low volume of coatings. 159
Fig. 4.40 Contact angle versus molar ratio of ethanol at low silica particles concentration and medium volume of coatings. 160
Fig. 4.41 Transmittance versus molar ratio of ethanol at low silica particles concentration and medium volume of coatings. 160
Fig. 4.42 Contact angle versus molar ratio of ethanol at low silica particles concentration and high volume of coatings. 161
Fig. 4.43 Transmittance versus molar ratio of ethanol at low silica particles concentration and high volume of coatings. 161
Fig. 4.44 SEM micrographs of modified glasses with precursor diluted by 80 ml D.I. water at different magnifications: (A) 250X (B) 1000X 167
Fig. 4.45 SEM micrographs of modified glasses with precursor diluted by ethanol 20 ml and D.I. water 60 ml and the volume of suspension was 1 ml at different magnifications: (A) 250X (B) 1000X 168
Fig. 4.46 SEM micrographs of modified glasses with precursor diluted by ethanol 20 ml and D.I. water 60 ml and the volume of suspension was 2 ml at different magnifications: (A) 250X (B) 1000X 168
Fig. 4.47 SEM micrographs of modified glasses with precursor diluted by ethanol 40 ml and D.I. water 40 ml and the volume of suspension was 1 ml at different magnifications: (A) 250X (B) 1000X 169
Fig. 4.48 SEM micrographs of modified glasses with precursor diluted by ethanol 40 ml and D.I. water 40 ml and the volume of suspension was 2 ml at different magnifications: (A) 250X (B) 1000X 169
Fig. 4.49 SEM micrographs of modified glasses with precursor diluted by ethanol 60 ml and D.I. water 20 ml and the volume of suspension was 1 ml at different magnifications: (A) 250X (B) 1000X 170
Fig. 4.50 SEM micrographs of modified glasses with precursor diluted by ethanol 60 ml and D.I. water 20 ml and the volume of suspension was 2 ml at different magnifications: (A) 250X (B) 1000X 170
Fig. 4.51 SEM micrographs of modified glasses with precursor diluted by ethanol 80 ml and the volume of suspension was 1 ml at different magnifications: (A) 250X (B) 1000X 171
Fig. 4.52 SEM micrographs of modified glasses with precursor diluted by ethanol 80 ml and the volume of suspension was 2 ml at different magnifications: (A) 250X (B) 1000X 171
Fig. 5.1 Optically transparent superhydrophobic glass 178




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