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溶胶-凝胶方法制备ZrO2及聚合物掺杂ZrO2单层光学增反射膜

梁丽萍 徐 耀 张 磊 吴 东 孙予罕 李志宏 吴忠华

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溶胶-凝胶方法制备ZrO2及聚合物掺杂ZrO2单层光学增反射膜

梁丽萍, 徐 耀, 张 磊, 吴 东, 孙予罕, 李志宏, 吴忠华

Sol-gel processing of ZrO2 and polymer doped-ZrO2 monolayer reflective films with high laser damage threshold

Liang Li-Ping, Xu Yao, Zhang Lei, Wu Dong, Sun Yu-Han, Li Zhi-Hong, Wu Zhong-Hua
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  • 以丙醇锆(Zr(OPr)4)为原料,乙酸(HAc)为络合剂,聚乙二醇(PEG200)和聚乙烯吡咯烷酮(PVP)为大分子添加剂,在乙醇体系中成功合成了ZrO2及聚合物掺杂ZrO2溶胶.用旋涂法在K9玻璃基片上制备单层光学增反射膜.借助小角X射线散射和激光动态光散射技术研究胶体的微结构.采用傅里叶变换红外光谱、差示扫描量热分析、X射线衍射分析、原子力显微镜、紫外/可见/近红外透射光谱以及椭偏仪对薄膜的结构和光学性能进行表征.用输出波长为1064
    A series of ZrO2 and polymer doped-ZrO2 sols have been synthesized by the controlled hydrolysis of zirconium n-propoxide. Acetic acid was used as the chelating agent. Poly(ethylene glycol)(PEG) 200 and polyvinylpyrrolidone(PVP) were introduced to produce the hybrid sols. ZrO2 and the polymer doped-ZrO2 optical thin films were then prepared by spin-coating the stable sols on K9 glass substrates. Effects of various synthetic parameters were studied, on the sol stability, the microstructure of colloidal system, the structural and optical properties of the films, as well as the laser damage resistance. In our reaction systems, both hydrolysis and chelation coexist. The preference for any of the two reactions strongly depends on the system composition and ultimately determines the stability and microstructure of the colloidal system. Besides, the addition of a proper amount of PEG200 and PVP, which probably acts as the competitive ligands, particle surface protective polymers and structure directive agents, can modify the hydrolysis-condensation process, thus producing more stable, uniform sols with mass fractal structure (fm=2.33—2.46) and average particle diameter of 19.1—23.7nm. Benefiting from the precursor sol structure, the polymer doped-films exhibit excellent surface planarity and uniform inner structure, which endows the films with good optical property and excellent laser damage resistance. For instance, the hybrid film with 10% PEG200 and 15% PVP (mass fractions) showed a high laser damage threshold of 24.5J/cm2 (for 1ns pulse duration) and a reflectivity increase of about 2% than that of the substrate at wavelength of about 1000nm.
    • 基金项目: 国家自然科学基金重点项目(批准号:20133040)资助的课题.
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  • 文章访问数:  7748
  • PDF下载量:  1264
  • 被引次数: 0
出版历程
  • 收稿日期:  2005-08-11
  • 修回日期:  2006-04-07
  • 刊出日期:  2006-04-05

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