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静电自组装SiO2光学薄膜的研究

Studies of SiO2 Optical Thin Films Prepared by Electrostatic Self-Assembly Multilayer Method

【作者】 许丕池;

【导师】 姜德生; 余海湖;

【作者基本信息】 武汉理工大学 , 材料学, 2003, 硕士

【摘要】 光学薄膜是光学元件的重要组成部分,它能改善光学元件及仪器的性能。本文用静电自组装(ESAM)法制备了聚电解质PDDA与SiO2胶体粒子的有机/无机复合光学薄膜以及SiO2光学增透膜,研究在可见光范围内透光性能及抗机械损坏能力等。 本文讨论了ESAM法制备薄膜所用的溶胶与Sol-gel法所用的溶胶在性能上的区别,在HC1或NH·H2O分别单独催化和HC1/NH3·H2O分步催化三种催化条件下制备了SiO2溶胶(以下规定HC1/NH3·H2O分步催化的SiO2溶胶为1#溶胶,相应的薄膜为1#薄膜,NH3·H2O催化的SiO2溶胶为2#溶胶、相应的薄膜为2#薄膜),在通过组装薄膜并用透射电镜(TEM)观察薄膜微观结构以及用721分光光度计测试样品的光透射率,得出了后两种催化方法所制备的溶胶适合于ESAM法镀膜,而第一种溶胶不适于用此法镀膜的结论,用傅立叶红外光谱(FT-IR)研究了溶胶组成;用差热失重分析仪(DTA-TG)对胶体进行了热分析。 用ESAM法制备了聚电解质PDDA与SiO2纳米复合薄膜,研究了薄膜在可见光谱范围内的光学性能以及薄膜的耐机械擦伤强度,发现1#复合薄膜的透光性能较2#的小,但耐机械擦伤强度大,2#反之;研究了溶胶的颗粒度对薄膜光学性能以及耐机械擦伤强度的影响;研究了薄膜的光学性能随薄膜的层数和所用光的波长的变化规律;研究了薄膜的透光率随湿度的变化规律;用FT-IR研究了薄膜的组成;用XPS对光学薄膜进行了表面分析,探讨了SiO2吸附层在聚合物PDDA层的覆盖状况。 用ESAM法制备了SiO2多孔光学增透薄膜,研究了PDDA/SiO2纳米复合薄膜在热处理过程中光学性能随温度的变化规律,发现520℃热处理后一定波长下的光透过率大大增强;用FT-IR研究了热处理后的薄膜的组成,用XPS进行了表面分析,研究了薄膜的耐机械擦伤强度,发现1#薄膜的耐机械擦伤强度较小,甚至小于相应的PDDA/SiO2纳米复合薄膜的耐机械擦伤强度,而2#薄膜的耐机械擦伤强度则大大增强,即使用刀片平刮也只略有损伤。

【Abstract】 Optical films are of importance as parts of optical elements and can be used to improve the performances of optical elements and apparatus. Electrostatic self-assembly multiplayer (ESAM) method has advantages in preparing films and develops fast in recent years. In this work, PDDA/SiOa complex films and SiO2 anti-reflective films were prepared by ESAM method, and their optical properties in the visible light spectrum range and anti-scratching performance were investigated.In this paper, the property difference of SiO2 sols used for preparing thin films by ESAM method or Sol-gel process has been discussed. Three kinds of SiO2 sols were prepared, catalyzed by HCl or NH3 H2O only, or HCl first and then NH3 H2O respectively (please note: in following text, the SiO2 sol catalyzed by HC1 first and then NH3 H2O and its correspondent films will benamed SiO2 sol 1# and film 1 ; the SiO2 sol catalyzed by NH3 H2O only and itscorrespondent films will be named SiO2 sol 2# and film 2#). Through investigating the assembling properties of the sols, observing thin films’ microscopic structure with TEM and testing their transmissivity with 721 spectrophotometer, we find that the first kind of sol is not suitable for preparing ESAM films, but the last two, i.e. sol 1# and sol 2#, are good. Fourier transform infrared spectrum (FT-IR) and DTA-TG heat analysis of the gels were carried out.PDDA/SiO2 complex films were prepared with ESAM method. The optical properties of the films were studied in the visible light spectrum range and their anti-scratching performance were investigated. The effects of the size of the colloidal particles on the optical properties and their anti-scratching performance of the thin films were studied. The optical properties of thin films following the bilayer numbers and the light wavelengths, and the light transmittance of films following the humidity were studied. Composition of the thin films was carried out with FT-IR and surface analysis of the films, e.g. the distribution of SiO2particles on the last PDDA layer, was analyzed with XPS.SiO2 optical anti-reflective thin films with micropores were prepared with ESAM method. The optical properties of PDDA/SiO2 complex films against the changes in temperature in the processof heat treatment were studied.After heat treated at 520 C, the light transmittance at certain wavelengths of the thin improved greatly. The chemical bond structures of the optical thin films was studied with FT-IR, and surface analysis of the thin films was carried out using XPS and their anti-scratching performances were studied. The result indicates that thin film 2# possesses very good anti-scratching performance. Its surface can’t be destroyed obviously even scraped with a blade. However, that of film 1# is smaller, even smaller than that of the corresponding PDDA/SiO2 complex films.

  • 【分类号】TB43
  • 【被引频次】5
  • 【下载频次】397
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