溶膠-凝膠法製備有機/無機奈米複合及超疏水材料之研究; Organic/Inorganic Nanocomposite and superhydrophobic Material Synthesized via Sol-Gel Process

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题名:	溶膠-凝膠法製備有機/無機奈米複合及超疏水材料之研究;Organic/Inorganic Nanocomposite and superhydrophobic Material Synthesized via Sol-Gel Process
作者:	翁維祥;Wei-Hsiang Weng
贡献者:	化學工程與材料工程研究所
关键词:	溶膠-凝膠;複合材料;超疏水;薄膜;Superhydrophobic;Composite Material;Sol-Gel;Thin Film
日期:	2005-06-10
上传时间:	2009-09-21 12:22:50 (UTC+8)
出版者:	國立中央大學圖書館
摘要:	本研究利用溶膠-凝膠(Sol-Gel)技術分別應用於製備有機/無機奈米複合材料及超疏水薄膜材料。有機/無機奈米複合材料中包含了環氧樹脂/二氧化矽混成材料與聚甲基丙烯酸甲酯(PMMA)/二氧化矽複合粒子等兩部份；而薄膜材料則分為疏水性薄膜材料與超疏水薄膜材料。環氧樹脂/二氧化矽混成材料中以製備出奈米級混成材料，並提升環氧樹脂之熱穩定性為目的。由結果顯示在一階段合成法中，可在廣範圍的pH條件下製備奈米級混成材料。二階段合成法中，帶有環氧官能基之偶合劑(γ-glycidoxypropyl-methyldiethoxysilane, GPMDES)的添加可使二氧化矽保持於奈米尺寸，並使環氧樹脂與二氧化矽間產生共價鍵結。在相同的二氧化矽添加量下，添加GPMDES之混成材料可得較高的玻璃轉移溫度(Tg)之混成材料，在二氧化矽添加量為10 wt%時，可將環氧樹脂之Tg由80℃提升至113℃。目前製備PMMA/二氧化矽複合粒子之方式中，需採用合成方式將PMMA表面改質成為帶有正電官能基，或是能夠與TEOS進一步反應之官能基進行複合粒子之製備。本研究利用粒徑為300nm之均一粒徑PMMA做為核物質，並在未經由表面改質之條件下達到製備複合粒子之目的。研究中使用帶有胺基之偶合劑(N-β(aminoethyl)-γ-aminopropyltrimethoxysilane, AAPTMS)與四乙氧基矽烷(TEOS)進行包覆。結果顯示當AAPTMS/TEOS(莫耳比)為1/9及PMMA/SiO2(重量比)為1/2之條件下可以得到400nm大小之PMMA/SiO2複合粒子，而殼層之厚度受到系統中之界面活性劑濃度、AATPMS/TEOS及PMMA/SiO2添加之比例影響，而殼層之厚薄會影響複合粒子之熱穩定性。將PMMA粒子移除後可得到中空之二氧化矽粒子，由結果顯示利用階段性升溫之鍛燒方式可得到結構較為完整之中空粒子。疏水性薄膜材料之製備方式中，目前文獻上所使用的方式大多分為兩個步驟，第一步驟利用不同的方式製備具粗糙度之表面，在第二步驟中在粗糙之表面塗佈低表面能材質。而在本研究中將採用簡單之一步驟製備方式，利用塗佈方式分別製備出疏水性及超疏水性薄膜材料。疏水性薄膜材料之製備部份，本研究利用帶有甲基(-CH3)之矽烷化合物(Methyltriethoxysilane, MTES)可在廣泛的條件下製備疏水性薄膜，所得之薄膜硬度為5H且穿透度大於98%。薄膜之平均粗糙度(Ra)隨著反應溫度的提升而變大，但是當反應溫度超過450℃後，薄膜會由於甲基產生熱裂解而由疏水性轉變為親水性。而針對超疏水薄膜材料之製備，由結果顯示，在低表面能矽烷MTES與二氧化矽粉體添加比例為21.8 wt%下，可得到接觸角為156˚但硬度低於HB之薄膜。而薄膜之硬度可經由添加TEOS而提升，當TEOS/MTES (莫耳比)比例為3.42時，硬度可達3H且接觸角可保持於150˚以上。利用田口工程可分析製備高硬度薄膜或高接觸角薄膜之條件選取，並由實驗結果證實利用田口工程分析可有效得到最佳製備條件。薄膜之透明度則可經由調整塗佈條件，如稀釋塗佈液之濃度或提高旋轉塗佈之轉速而獲得提升，當塗佈液稀釋至1/2且轉速為4000rpm條件下可得到接觸角為158˚且穿透度為76.5%之超疏水薄膜。 In this research, sol-gel process was utilized to fabricate organic/inorganic nano-composite material and superhydrophobic film. Organic/Inorganic composite material included two separate parts, one was Epoxy/SiO2 hybrid material and the other one was PMMA/SiO2 composite sphere. The fabrication of superhydrophobic film also discussed with hydrophobic and superhydrophobic film individually. Sol-gel process was utilized to synthesize epoxy-silica hybrid materials in nanoscale in recent years. The purpose of this part is to fabricate hybrid material in nanoscale and improve the thermal property of epoxy resin. From these results, the epoxy and silica could hybrid in nanoscale under extensive pH value of the system in one-step process. On the other hand, the two-step process led to a phase separation phenomenon after mixing epoxy resin and precursor without coupling agent γ-glycidoxypropyl-methyldiethoxysilane (GMPDES). GPMDES was utilized to modify the surface properties of the silica via the sol-gel process. The role of the GPMDES is to provide covalent bonding between the epoxy resin and silica and avoid the aggregation of silica. The GPMDES could avoid the phase separation problem of hybrid materials and enhance the thermal stability of the materials through this process. At the same time, the Glass transfer temperature(Tg) of the materials also increased proportionally to the content of silica from 80℃ to 113℃. In the recent research on fabrication method of composite sphere, the core sphere should be modified the surface property by polymerization method first. In this part, the PMMA/SiO2 composite sphere was synthesized by sol-gel process with the mono-disperse PMMA sphere (300nm) without any surface modify successfully. In this research, the coupling agent with amine group, N-β(aminoethyl)-γ-aminopropyltrimethoxysilane (AAPTMS), was utilized with TEOS to synthesize PMMA/SiO2 composite sphere. From the result, when the mole ratio between AAPTMS/TEOS was 1/9 and the ratio between PMMA and silica was 1/2, the diameter of the composite sphere will be 400nm. The thickness of the silica shell structure influenced with the concentration of surfactant in the system, the ratio of AAPTMS/TEOS and PMMA/Silica in this study. The thickness of the silica shell structure also influenced the thermal stability of the composite sphere. The silica hollow sphere was obtained by removing PMMA sphere by calcinations. In the research field of superhydrophobic film, the fabricate process should be divided into two steps. First one is the fabrication of roughness of the surface and the second part is coating the low surface energy material. In this research, we expect to fabricate superhydrophobic film by one step. The film with hydrophobic property could be synthesized with methyltriethoxysilane (MTES) by sol-gel process. The film could fabricate with extensive conditions and exist hydrophobic property. From the results, the hardness of the film could achieve 5H and the transparency of the film was 98%. The average roughness (Ra) increased by raising the reaction temperature. The film will be hydrophilic when the reaction temperature higher than 450℃ due to the decompose of methyl group of the film surface. The film with superhydrophobic property could be synthesized by MTES and silica powder. From the results, the contact angle higher than 150° when the ratio of SiO2/MTES = 21.8 wt%. Hardness of the film could achieve 3H by adjusting TEOS/MTES mole ratio = 3.42 and contact angle still maintain above 150°. Taguchi Quality Method was used to find the optimum operation conditions in this study. Two of Taguchi Quality Methods were used in this research to find the optimum production conditions for four different fabricate conditions of high contact angle and hardness of superhydrophobic film respectively. In order to fabricate superhydrophobic film of high transparency, the study also explored into the effect of rotation rate of the spin coater and concentration of the coating solution. When the coating solution was diluted to 1/2 and the spin rate at 4000rpm, the film produced possessed continuous roughness layer, the transparency under visible light was 76.5% and contact angle of 158°.
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