SR-494/GMA/VTMS/ZnO有機/無機奈米複合材料合成與性質之研究

Synthesis and Properties of SR-494/GMA/VTMS/ZnO Organic/Inorganic Nanocomposites

本研究是利用溶膠-凝膠法製備具耐熱性佳、高透光性、UV 遮蔽性及符合抗靜電 範圍之 SR-494/GMA/VTMS/ZnO 奈米複合材料。首先將 VTMS 經 pH 2~3 酸性水溶 液水解得到矽醇中間物，再添加無機金屬微粒 ZnO 能經由有機化改質反應順利共價 鍵結至有機基材上，接若將此 VTMS/ZnO 複合物中活性-OH 官能基與環氧樹脂 GMA 行開環反應，合成 GMA/VTMS/ZnO 複合物，最後加入有機壓克力單體 SR-494 與 GMA/VTMS/ZnO 複合物中的活性烯基進行多次紫外光自由基光聚合反應產生理想 程度的網狀共價鍵結結構，以提升材料的耐熱性質、UV 光遮蔽性、抗靜電性及機械 性質，合成理想光電高科技產業使用之奈米複合材料。合成時，使用 FT-IR 光譜儀來 確定其最佳反應條件與最佳組成用量；並利用 TGA 之熱性質測試、抗靜電測試、 UV-Vis 穿透度測試、硬度及附著力等測試對其耐熱性質、透明性、紫外光遮蔽性、 導電性及機械物性等性質進行分析。實驗結果顯示這些複合材料其耐熱性 Td 值最高 可達 421.42℃，較純環氧樹脂的 Td 值高約 76.71℃且在可見光區光穿透度達 85%以 上並有良好 UV 光遮蔽之效果；材料之表面電阻值符合抗靜電範圍(106～1012Ω/sq)； 硬度可達 8H 與 4B 的附著力；最後奈米光學薄膜經掃描式電子顯微鏡(SEM)檢測結 果在 ZnO微粒占整體含量 3.85 微粒均勻分佈且平均粒徑小於 100nm符合奈米材料的 範圍。

This research is to synthesis SR-494/GMA/VTMS/ZnO nanocomposite materials with good high heat resistance, good transparence in visible, UV-shielding and anti-static properties by sol-gel reaction. Firstly, the VTMS was performed the silanol intermediates by hydrolysis in pH2~3 acid solution. The inorganic fillers of powder ZnO could be successfully coupled and crosslinked to SR-494/GMA organic matrices with these silanols of VTMS coupling agents. The remained active-OH functional groups of the VTMS/ZnO complexes graft polymerized with active epoxide group of GMA to get GMA/VTMS/ZnO composites by ring-opening polycondensation Therefore, the GMA/VTMS/ZnO complexes would be successfully prepared. Finally, in order to improve the thermal resistant, UV-shielding, good anti-static and mechanical properties, the SR-494 acrylate monomers and the GMA/VTMS/ZnO composites were chain polymerized by free radical polymerization to form a perfectly cross-linking structure of orgaic/inorganic nanocomposites. The chemical bonding formation and the best weight contents of reaction components were identified by FT-IR spectra. The thermal resistance, optical transmittance, surface resistane, and hardness of these nanocomposites were measured by TGA, UV-Vis, super megohmeter and hardness tester respectively. Experimental results showed that these nanocomposites had the best Td value was 421.42℃ which was 76.71℃higher than that of pure GMA epoxy resin respectively and 85% transmittancein visible region and UV-shielding properties. The surface resistances (Rs) of SR-494/GMA/VTMS/ZnO hybrid thin films conformed to anti-electrostatic range (106 ～1012Ω/sq). The hardness and adhesion of the UV-curing hybrid coatings were as high as 8H and 4B by hardness and cross-cut test. The morphology structures of the hybrid thin films were estimated by SEM. These results showed that the optical thin films were evenly distributed with inorganic colloidal particles and the average particlesize of these nanocomposites less than100nmthat ZnO particles account for 3.85% of the total content.