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以丙醇锆(ZrPr)为锆源,二乙醇胺(DEA)为络合剂,原位引入聚乙烯吡咯烷酮(PVP),在乙醇体系中成功地合成了PVP掺杂-ZrO2溶胶.采用旋涂法在K9玻璃基片上制备了PVP-ZrO2单层杂化薄膜.用不同掺杂量的PVP-ZrO2高折射率膜层与相同的SiO2低折射率膜层交替沉积四分之一波堆高反射膜.借助小角X射线散射研究胶体微结构,用红外光谱、原子力显微镜、紫外/可见/近红外透射光谱、椭圆偏振仪以及1064nm的强激光辐照实验对薄膜的结构、光学和抗激光损伤性能进行表征.研究发现,体系组成的适当配置可以在溶胶稳定的前提下实现ZrPr的充分水解,赋予薄膜良好的结构、光学和抗激光损伤性能.杂化体系中,DEA与ZrPr之间强的配合作用大大降低了ZrO2颗粒表面羟基的活性,使得PVP大分子只是以微弱的氢键与颗粒的表面羟基作用而均匀分散于ZrO2颗粒的周围,对颗粒的形成和生长无显著影响.因而在实验研究范围内,随PVP含量的增大,PVP-ZrO2杂化膜层的折射率和激光损伤阈值均无显著变化.但是,薄膜中均匀分布的PVP柔性链可以有效促进膜层应力松弛,显著削弱不同膜层之间的应力不匹配程度、大大方便多层光学薄膜的制备.当高折射率膜层中PVP的质量分数达到15%—20%时,膜层之间良好的应力匹配使得多层高反射膜的沉积周期数可达到10以上.沉积10个周期的多层反射膜,在中心波长1064nm处透射率约为1·6%—2·1%,接近全反射特征,其激光损伤阈值为16·4—18·2J/cm2(脉冲宽度为1ns).
In this paper, polyvinylpyrrolidone (PVP) was synthesized in situ by using zirconium propoxide (ZrPr) as zirconium source and diethanolamine (DEA) as complexing agent, and PVP doped -ZrO2 sol was successfully synthesized in ethanol system. PVP-ZrO2 single-layer hybrid thin films were prepared on K9 glass substrates.A quarter-wave stack of high-reflectivity films with different doping levels of PVP-ZrO2 high-index films and the same SiO2 low- The structure, optical and anti-laser damage properties of the films were studied by means of small-angle X-ray scattering using infrared spectroscopy, atomic force microscopy, ultraviolet / visible / near infrared transmission spectroscopy, ellipsometer and intense laser irradiation at 1064 nm The results show that proper arrangement of the system components can fully hydrolyze ZrPr under the condition of sol stability and provide good structural, optical and anti-laser damage properties of the films.In the hybrid system, the strong coordination between DEA and ZrPr Greatly reducing the hydroxyl activity on the surface of the ZrO2 particles, making the PVP macromolecules uniformly disperse around the ZrO2 particles with a weak hydrogen bond and the surface hydroxyl groups of the particles, and have no significant effect on the particle formation and growth. However, with the increase of PVP content, there is no significant change in the refractive index and laser damage threshold of PVP-ZrO2 hybrid film in the range of experimental study.However, the uniform distribution of PVP flexible chains in the film can effectively promote the stress relaxation , Significantly weakened the stress mismatch between different layers and greatly facilitated the preparation of multilayer optical thin films.When the mass fraction of PVP in the high refractive index layer reaches 15% -20%, good stress matching between the layers So that the number of multi-layer high-reflective film deposition cycle can reach more than 10. Deposited 10-cycle multilayer reflective film, the center wavelength of 1064nm transmittance of about 1.6% -2.1%, close to the total reflection characteristics of its The laser damage threshold is 16.4-18.2 J / cm2 (pulse width is 1 ns).