BEA/DGEBA/MSMA/TiO_2耐熱有機／無機奈米複合材料合成及其性質之研究

Synthesis and Properties of Thermal Resistant BEA/DGEBA/MSMA/TiO_2 Organic/Inorganic Nanocomposites

陳榮輝(Jung-hui Chen) ； 賴翊瑞(Yi-jui Lai) ； 趙芳鈺(Fang-yu Chao) ； 林念德(Nian-de Lin) ； 呂郁賢(Yu-shen Lu) ； 陳俊宇(Jyun-yu Chen) ； 鄧聖霖(Sheng-lin Deng) ； 謝孟杰(Meng-chieh Heish)

《高雄師大學報：自然科學與科技類》 44期 (2018/06) Pp. 1-17

摘要

本研究目的是利用溶膠—凝膠法來合成具優異耐熱性之BEA/DGEBA/MSMA/TiO_2 有機／無機奈米複合材料。於實驗中先將MSMA 矽氧烷耦合劑在酸性環境下pH2~3 水解形成矽醇(silanol)中間物，以利進行經前處理之TiO_2 無機金屬微粒與矽醇中間物的有機化改質反應，使其能順利共價鍵結至有機基材上形成MSMA/TiO_2 複合物。接著將MSMA/TiO_2 複合物中活性羥基與Epoxy 環氧樹脂預聚物以進行熱縮開環聚合反應形成DGEBA/MSMA/TiO_2 複合物，最後加入有機壓克力BEA 單體與DGEBA/MSMA/TiO_2 複合物上的活性烯基進行自由基光聚合反應使有機／無機複合材料上之聚合物鏈具備理想之網狀共價鍵結，以利於提升複合材料之耐熱性和機械抗性，製備理想符合光電高科技產業應用之奈米複合材料。合成過程中以FT-IR 傅立葉轉換光譜儀來確定反應最佳條件以及最佳組成配方用量比、利用熱重分析儀TGA 進行耐熱測試、利用UV-Vis 光譜儀來觀測材料在紫外光區和可見光區之透光性測試、最後對進行附著力、鉛筆硬度等機械物理性質測試且分析。結果顯示耐熱性熱裂解溫度Td 值最高可達465.2℃，相較於純DGEBA 環氧樹脂與DGEBA/MSMA/TiO_2 複合物最多提升約182.4℃與54.2℃，在可見光區透光性可達到85%以上並UV 光區也有遮蔽效果，最後奈米光學薄膜藉由掃描式電子顯微鏡(SEM)檢測，確認無機粉體微粒均勻分佈，且平均粒徑為15~40nm 符合奈米材料範圍。

關鍵字

環氧樹脂 ； 壓克力單體 ； 奈米複合材料 ； 耐熱性 ； 二氧化鈦

並列摘要

The principal objective in this research is to develope BEA/DGEBA/MSMA/TiO_2 organic/inorganic nanocomposites materials with high thermal resistance, UV-shielding and high transmittance properties. The MSMA (Methacryloxypropyl-trimethoxysilane) coupling agent was treated the silanol intermediates by acid hydrolysis for 45min in pH 2~3 tetrahydrofuran solution. These silanol intermediates have some active Si-OH functional groups that could form covalent bond between organic matrix and inorganic titanium oxide colloids. Afterward, the MSMA-modified titanium oxoclusters graft polymerized with epoxide groups of DGEBA (Diglycidyl ether of bisphenol A) resins monomer to form DGEBA/MSMA/TiO_2 complexes by the epoxide ring-opening polycondensation mechanism. After mixing BEA acrylate monomer, the final compound BEA (Bisphenol A ethoxylate diacrylate)/DGEBA/MSMA/TiO_2 nanocomposites were synthesized by free radical photopolymerization. The BEA/DGEBA/MSMA/TiO_2 organic/ inorganic nanocomposites will enhance the thermal resistant, optical properties. The chemical covalent bonding formation and the best weight contents of reaction components were identified by FT-IR spectra. The thermal resistance, hardness and optical transmittance of these nanocomposites were measured by TGA, pencil hardness tester and UV-Vis respectively. Experimental results showed that these nanocomposites have 85% transmittance in the visible regions and UV-shielding properties. The best Td value is 465.2℃ which is 182.4℃ and 54.2℃ higher than those of pure DGEBA resin and DGEBA/MSMA/TiO_2 hybrid material respectively. The morphology structures of the hybrid thin films are estimates by SEM that show inorganic colloids particles and the average particle size of these nanocomposites is about 15~40nm.

並列關鍵字

Epoxy ； Acrylic monomer ； Nanocomposites ； Thermal Resistance ； TiO_2