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四方相纳米ZrO_(2)的制备、改性及其在水性聚氨酯复合薄膜中的应用

Preparation,modification of tetragonal nano zirconia and its application in waterborne polyurethane composite film
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摘要 为实现室温下稳定的四方相ZrO_(2)和可调折射率透明复合材料的制备,以八水合氧氯化锆为原料,通过水热/微波焙烧法制备了四方相纳米ZrO_(2),经γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH570)改性获得了ZrO_(2)@KH570,将其与水性聚氨酯(WPU)复合制得了透明薄膜(WPU-ZrO_(2)@KH570薄膜)。采用XRD、Raman、TEM、SEM、纳米激光粒度分析仪(LS)和FTIR对四方相纳米ZrO_(2)和ZrO_(2)@KH570进行了表征。通过FTIR、SEM-EDS、原子力显微镜观察了ZrO_(2)@KH570与WPU的相容性。通过SEM-EDS、紫外-可见-近红外分光光度计和光谱椭偏仪考察了ZrO_(2)@KH570添加量对复合薄膜光学性能的影响。结果表明,成功制备了四方相纳米ZrO_(2),其平均粒径17.3 nm;KH570改性提高了ZrO_(2)@KH570的分散性;当WPU用量为8.0 g时,随着ZrO_(2)@KH570添加量(0.3~1.5 g)的增加,复合薄膜的透光率从99.74%降至93.80%,折射率从1.8359线性提升至2.3281(R2=0.969)。当ZrO_(2)@KH570添加量为0.9 g时,复合薄膜的透光率为98.07%,折射率为2.1457,实现了高透光率与高折射率的协同调控。 To achieve the preparation of tetragonal ZrO_(2)and transparent composites with adjustable refractive index at room temperature,tetragonal nano ZrO_(2)was prepared from zirconium oxychloride octahydrate by hydrothermal/microwave calcination method,and then modified withγ-methylacryloyloxylpropyltrimethoxysilane(KH570)to synthesize ZrO_(2)@KH570,which was further compounded with waterborne polyurethane(WPU)to obtain transparent film(WPU-ZrO_(2)@KH570).The tetragonal nano ZrO_(2)and ZrO_(2)@KH570 were characterized by XRD,Raman,TEM,SEM-EDS,nano laser particle size analyzer(LS)and FTIR.The compatibility between ZrO_(2)@KH570 and WPU was analyzed by FTIR,SEM-EDS,AFM.The effect of ZrO_(2)@KH570 addition amount on the optical properties of the composite films was investigated by SEM-EDS,UV-Vis-near-infrared spectrophotometer and spectral ellipsometer.The results showed that tetragonal nano ZrO_(2)was successfully prepared,with an average particle size of 17.3 nm.KH570 modification improved the dispersibility of ZrO_(2)@KH570.When 8.0 g WPU was added,the transmittance of composite films decreased from 99.74%to 93.80%,while the refractive index increased linearly from 1.8359 to 2.3281(R2=0.969)with the increase in ZrO_(2)@KH570 addition amount(0.3~1.5 g).When 0.9 g ZrO_(2)@KH570 was added,the composite film exhibited a transmittance of 98.07%and a refractive index of 2.1457,achieving a synergistic control of high transmittance and high refractive index.
作者 林洁玲 吕维忠 LIN Jieling;LYU Weizhong(College of Chemistry and Environmental Engineering,Shenzhen University,Shenzhen 518060,Guangdong,China)
出处 《精细化工》 北大核心 2026年第3期547-554,共8页 Fine Chemicals
基金 深圳大学专项项目-概念验证项目(纵KJ20250379)。
关键词 纳米二氧化锆 水热/微波法 四方相 高折射率 透明薄膜 功能材料 nano zirconium dioxide hydrothermal/microwave method tetragonal phase high-refractive index transparent films functional materials
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