Preparation and Properties of HDDA/GMA/MSMA/ZrO2 Organic/Inorganic Nanocomposites

• Main Authors: LIN, NIAN-DE, 林念德
• Other Authors: CHEN, JUNG-HUI
• Format: Others
• Language: zh-TW
• Published: 2018
• Online Access: http://ndltd.ncl.edu.tw/handle/328tyq

碩士 === 國立高雄師範大學 === 化學系 === 106 === The main object of this research is to develop HDDA/GMA/MSMA/ZrO2 organic/inorganic nanocomposites with good heat resistance, high hardness and adhesion, good transparence in visible, UV-shielding and anti-static properties by sol-gel reaction. HDDA (1,6-hexanediol diacrylate), GMA (glycidyl methacrylate), MSMA (3-(trimethoxysilyl)propyl methacrylate), ZrO2 (zirconium oxide), TAIC (triallyl isocyanurate) and PMDA (pyromellitic dianhydride) were used as organic acrylate monomer, epoxy resin, silane coupling agent, inorganic filler, cross-linking reagent and curing agent respectively. First, the coupling agent MSMA formed its reactive silanol intermediate by acid hydrolysis for 45 min in pH=2 ~ 3 acid solution. Second, after into the acidic solution of ZrO2, we get the MSMA/ZrO2 complexes by active Si-OH groups of these silanols and Zr-OH bonding covalently in order to modify zirconium oxide surface, and then after adding epoxy resin GMA, the remained active Si-OH functional groups graft polymerized with active epoxide group of GMA to get GMA/MSMA/ZrO2 composites by ring-opening polycondensation. Finally, TAIC, PMDA, HDDA and the GMA/MSMA/ZrO2 complexes were covalently bonded by UV-activated free radical polymerization to obtain a cross-linking structure of HDDA/GMA/MSMA/ZrO2 nanocomposite after mixing and stir dispersion. During every steps, the best time and weight content of reaction components were identified through FT-IR spectra. The thermal resistance properties, Tg point of these composites and the visible transmittance, UV-shielding, anti-electrostatic properties, hardnesses and adhesions of these optical membranes were measured by TGA, DSC, UV-Vis , super megohmeter, pencil hardness tester and adhesion tester respectively. The experimental results showed that the best Td value of these composites is 409.42 °C which was 60.03 °C higher than pure epoxy resin GMA and the glass transition temperature was not detected in 55 ~ 200 °C. The composites had 90 % transmittance in visible region and UV-shielding properties. Moreover, the surface resistances (Rs) of hybrid thin films below 5.55 % of ZrO2 content conformed to anti-electrostatic range (106~ 1012Ω/sq). Finally, the morphology structures , particle size and circumstances of dispersion of different ZrO2 fractions were estimated by SEM. The results showed that the composites below 5.55 % of ZrO2 content were a uniformity dispersion and conformed to the nanocomposites structure in 1.0 % of ZrO2 content. Notably, the hardness and adhesion of the UV-curing hybrid coatings were as high as 9H and 4B by hardness and cross-cut test compared with the HDDA and GMA polymer coatings.