高折射率ZrO_(2)纳米杂化材料的制备与研究

Preparation and research of high refractive index ZrO_(2) nano-hybrid materials

以4,4’-二羟基二苯硫醚和9,9-二(4-羟苯基)芴,环氧氯丙烷为原料,在碱性条件下缩聚合成一种含S元素含芴结构的环氧树脂基体;通过溶胶-凝胶法,以四正丁醇锆为前驱体,以KH560为偶联剂,在基体上原位合成无机纳米ZrO_(2)粒子,再经过热固化制备出一种具有高折射率的光学纳米杂化材料。通过红外光谱、1H核磁共振、X射线衍射、纳米粒度仪等手段对杂化材料的结构进行表征,并采用紫外分光光度仪、热重分析仪、椭圆偏振光谱仪对其性能进行了表征与测试。结果表明:ZrO_(2)粒子在聚合物基体中合成,并以纳米粒度均匀分散,杂化材料具有很好的光学性能,在可见光范围内普遍保持90%以上的透过率,随着ZrO_(2)含量的增加,杂化树脂折射率呈线性增加,ZrO_(2)含量在19.33%时,折射率达到1.739。

An epoxy resin matrix containing S element and fluorene structure was synthesized by polycondensation of 4,4’-thiodiphenol, 9,9-bis(4-hydroxyphenyl) fluorene and epichlorohydrin under alkaline conditions.Using four n-butanol zirconium as precursor and KH560 as coupling agent, the inorganic nano ZrO_(2)particles were in-situ synthesized on the polymer matrix by sol-gel method, and then an optical nano-hybrid material with high refractive index was further prepared by thermal curing.The structure of the hybrid material was characterized by infrared spectroscopy, ~1H nuclear magnetic resonance, X-ray diffraction, and nanoparticle size analyzer.Its performance was also characterized and tested by ultraviolet spectrophotometer, thermogravimetric analyzer, and Abbe refractometer.The results showed that ZrO_(2)particles were successfully synthesized in the polymer matrix and uniformly dispersed in nanoparticle size.Hybrid material had good optical properties and generally maintained a transmittance of more than 90% in the visible light range.With the increase of ZrO_(2)content, the refractive index of the hybrid resin increased linearly.When ZrO_(2)content was 19.33%,the refractive index reached 1.739.