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姓名 李坤穆(Kun-Mu Li)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 溶膠-凝膠法製備超疏水性薄膜材料
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摘要(中) 本研究利用溶膠-凝膠法(sol-gel process)來製備超疏水薄膜材料。分別探討前置物法(precursor)與同時聚合法(in-situ)兩種反應系統對所製備之薄膜材料之影響。 在前置物系統中,將個別種類矽烷、乙醇及水在酸性環境下進行水解-縮合反應後再加入二氧化矽粉體進行混合,以旋轉塗佈方式(spin-coating)塗佈於玻璃基材上,在不同反應溫度及反應時間下進行反應並藉由改變TEOS/矽烷比例來探討表面性質之變化。 在同時聚合系統中,利用乙醇將個別粒徑之SiO2粉體分散後,藉由改變TEOS/矽烷比例與改變矽烷種類、加水在酸性環境下進行水解-縮合反應,以旋轉塗佈方式(spin-coating)塗佈於玻璃基材上,並在不同溫度下進行反應來探討薄膜表面性質之變化。 將實驗所得之薄膜材料進行接觸角(Contact Angle)、掃瞄式電子顯微鏡(SEM)、原子力顯微鏡(AFM)、紫外光/可見光分光光譜儀(UV)等儀器分析,來探討薄膜材料表面之接觸角變化及表面結構與接觸角、硬度、透明度之關係。 由實驗結果得知,以前置物法所製備之超疏水薄膜材料,其接觸角可達158°,藉由TEOS的加入可提升薄膜硬度至3H。但以前置物法製備薄膜材料需兩步驟完成,進而考慮一步驟反應,即所謂同時聚合法。而以同時聚合法所製備之超疏水薄膜材料方面,在以親水性之SiO2-B粉體之反應系統,反應後其接觸角可高達160°,最佳硬度可達6H。最佳配方之接觸角為158°,硬度3H。 透明度方面,利用導入平均為252.1 nm SiO2粉體(SiO2-B)並改變反應液濃度及塗佈轉速,可得接觸角158°,平均穿透度76.5%之高透明度超疏水性薄膜材料。3
關鍵字(中) ★ 溶膠凝膠法
★ 超疏水
★ 接觸角
關鍵字(英) ★ contact angle
★ super hydrophobic
★ sol-gel
論文目次 目錄……………………………………………….Ⅰ
流程圖索引……………………………………….Ⅲ
圖索引…………………………………………….Ⅳ
表索引…………………………………………….Ⅵ
第一章 前言…………………………………………1
1-1 超疏水原理及其機制……………………………2
1-2 超疏水現象數學模式……………………………3
1-3 表面粗糙度製備方式……………………………7
1-4 溶膠凝膠法介紹…………………………………10
1-4-1 pH值對溶膠凝膠法的影響……………………15
1-4-2水含量的多寡對溶膠-凝膠法的影響…………16
1-4-3溶劑的比例對溶膠-凝膠法的影響……………16
1-5 實驗目的…………………………………………20
第二章 實驗……………………………………….…21
2-1 實驗藥品……………………………………..…22
2-2 實驗儀器………………………………………..24
2-3 超疏水性薄膜材料製備…………………………25
2-3-1 前置物製備………………………………..…25
2-3-2 前置物法製備超疏水薄膜材料………………25
2-3-3 同時聚合法製備超疏水薄膜材料…………..28
2-4 超疏水薄膜材料之物性測試……………………30
2-4-1 接觸角測量……………………………….….30
2-4-2 硬度測試………………………………………30
2-4-3 穿透度測試……………………………………30
2-4-4 SEM進行表面微結構分析…………………….30
2-4-5 AFM進行表面微結構分析…………………….31
第三章 結果與討論………………………………….32
3-1 前置物法之製備實驗參數探討…………………33
3-1-1 矽烷種類與TEOS對接觸角之影響………....33
3-1-2 前置物於不同pH值反應對接觸角之影響……34
3-1-3 系統中溶劑含量對接觸角之影響…………..36
3-1-4 系統中水含量對接觸角之影響……………..36
3-1-5不同反應時間與反應溫度對接觸角之影響….39
3-1-6前置物中含不同量之SiO2粉體對接觸角之影響47
3-1-7添加SiO2粉體於不同溫度反應對接觸角與硬度之影響….47
3-1-8 TEOS/KBE-13不同比例對接觸角與硬度之影響..52
3-2同時聚合法之製備實驗參數探討……………………56
3-2-1利用田口品質工程(L9)研究最佳接觸角與硬度配方 (1)….56
3-2-2疏水官能基密度與粗糙度對接觸角及硬度比較…66
3-2-3利用田口品質工程(L9)研究最佳接觸角與硬度配方(2)…68
3-2-4 透明度探討…………………………………….77
3-2-4-1反應液濃度對接觸角及透明度之影響…….77
3-2-4-2轉速對接觸角及透明度之影響…………….77
第四章 結論…………………………………………84
參考文獻……………………………………………..86
IIList of Schemes
Scheme2-1 The process of preparing precursor…26
Scheme 2-2 The sol-gel process of preparing superhydrophobic materials by precursor method...27
Scheme. 2-3 The sol-gel process of preparing superhydrophobic materials by in-situ method…29
IIIList of Figures
Fig.1-1 Micromorphological characteristics of lotus leaf surfaces………4
Fig.1-2 The pristine leaves of the lotus plant have inspired studies into the superhydrophobic mechanism of self-cleaning…………..…..4
Fig.1-3 “Self-cleaning effect” of the roughness of surface………………5
Fig.1-4 The relationship of colors andhydrophobic of the butterfly with the surface texture………5
Fig.1-5 Wetting of solid surfaces according to Young’s equation……8
Fig.1-6 (a)Wenzel’s theory (b)Cassie’s theory………………………8
Fig.1-7 The relationship of Roughness and Contact Angle……………8
Fig.1-8 The hydrolysis and condensation of silane……………………..12
Fig.1-9 The sol-gel process……………………..13
Fig. 1-10 Polymerization behavior of aqueous silica…………………...17
Fig. 1-11 Effects of pH in aqueous silica sol-gel system……………….18
Fig. 1-12 Models of silica growth………………………………………19
Fig. 2-1 The structural formula of Silanes………………………………23
Fig. 3-1 TEOS、EtOH、H2O ternary-phase diagram…………………..38
Fig. 3-2 AFM photographs of films prepared at different reaction temperature for 1hr………45
Fig.3-3 TGA curves of KBE-13 precursor reacted at different temperature for 1hr…………………46
Fig. 3-4 The particle size distribution of SiO2 powder………………….48
Fig. 3-5 SEM photograph of superhydrophobic material’s surface texture by adding different amount of SiO2 powder………….50
Fig. 3-6 The characteristic of water drop on the glass by different kinds of precursor……….51
Fig. 3-7 The influence factor of Contact Angle by Taguchi method….61
Fig. 3-8 The influence factor of Hardness by Taguchi method…………63
Fig. 3-9 SEM photograph of No.I2-5 Surface texture.………………...65
Fig. 3-10 SEM photograph of No.I2-3 Surface texture...……………….65
Fig. 3-11 The influence factor of Contact Angle by Taguchi method…..72
Fig. 3-12 The particle size distribution of A-200……………………….74
Fig. 3-13 The influence factor of Hardness by Taguchi method………..75
Fig. 3-14 SEM、AFM photographs and drop type of dilute 1/2………80
Fig. 3-15 SEM photographs of different concentration reactants in system…………….81
Fig. 3-16 The transparent of different concentration of reactants and different spin coating rate…………………………………….82
Fig. 3-17 Photograph of a droplet on superhydrophobic material………83
List of Tables
Table 1-1 Characteristics of precursors………14
Table 3-1 Preparation conditions and characteristics of thin films prepared by different silanes………………………………….35
Table 3-2 Preparation conditions and characteristics of hydrophobic films by different value of pH ……………………………….37
Table 3-3 Preparation conditionsand characteristics of hydrophobic films by different amount of solvent…………………………40
Table 3-4 Preparation condition and characteristics of hydrophobic films by different amount of H2O…………………………….41
Table 3-5 Preparation conditions(a) and characteristics of films by changing reaction time and reaction temperature…………44
Table3-6 Preparation conditionsand characteristics of superhydrophobic materials by adding varies amount of SiO2 powder………….49
Table 3-7 Preparation conditions and characteristics of superhydrophobic materials in different reaction temperature after spin coating..53
Table 3-8 Preparation conditions and characteristics of superhydrophobic materials by different molar ratio of TEOS/Silane…………...55
Table 3-9 L9 experiment dispose of Quality Engineering……………….59
Table 3-10Preparation conditions and characteristics of superhydrophobic materials by Taguchi method…………………………………60
Table 3-11 The Rank of influence factor of Contact Angle…………….62
Table 3-12 The optimum prescription of Contact Angle………………..62
Table 3-13 The Rank of influence factor of Hardness…………………..64
Table 3-14 The optimum prescription of Hardness……………………..64
Table 3-15 The importance of roughness and hydrophobic function group comparison sheet…67
Table3-16 Preparation conditions and characteristics of superhydrophobic materials by Taguchi method…………………………………71
Table 3-17 The Rank of influence factor of Contact Angle…………….73
Table 3-18 The optimum prescription of Contact Angle………………..73
Table 3-19 The Rank of influence factor of Hardness…………………..76
Table 3-20 The optimum prescription of Hardness……………………..76
Table 3-21 Preparation conditions and characteristics of superhydrophobic materials by different concentration of reactants……………79
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指導教授 陳暉(Hui Chen) 審核日期 2004-6-23
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