具有梯度渐变折射率的超疏水减反膜的制备及其性能

doi:10.15541/jim20170575

摘要/Abstract

摘要：

具有梯度折射率的减反膜可以在更宽光谱波段和更大入射光角度实现减反射性能。本研究利用溶胶-凝胶和溶剂热法分别合成实心氧化硅(SiO₂)、空心氧化硅(H-SiO₂)和空心氟化镁(MgF₂)溶胶, 利用浸渍-提拉法在玻璃双面镀制SiO₂/H-SiO₂/MgF₂梯度折射率薄膜。结果表明, 在380~1600 nm波长, 镀膜基片在光垂直入射时透光率高达99.88%, 当光以0°~45°入射时, 平均透光率均高于97.85%, 即使光以75°入射时, 最高透光率仍达95.51%。同时发现, 经十六烷基三甲氧基硅烷(HDTMOS)修饰, 薄膜疏水角达到150.6°, 显示出良好的疏水自清洁效果。

关键词: 梯度折射率, 全方位, 宽带, 疏水, 减反膜

Abstract:

Gradient refractive index antireflection film achieves antireflective performance in wider spectrum band at larger incident of angle. In this study, solid silica nanometer particles (SiO₂) sol and hollow silica nanometer particles (H-SiO₂) sol were synthesized by Sol-Gel method, while hollow rod-shaped magnesium fluoride nanometer particles (MgF₂) sol was prepared by solvothermal method. Then, the SiO₂/H-SiO₂/MgF₂ gradient refractive index antireflection film was successfully coated on double sides of borosilicate glass by dip-coating method. The experimental results show that in the wavelength range of 380~1600 nm, when light is incident vertically, the transmittance of the coated glass reaches 99.88%; when the light is at the incident angle of 0°~45°, with the average transmittance higher than 97.85%. And the light is even at the incident angle of 75°, its maximum transmittance is still as high as 95.51%. After modified by hexadecyl trimethoxysilane (HDTMOS) the contact angle of the coated glass is up to 150.6°, showing good hydrophobic self-cleaning performance.

Key words: gradient refractive index, omnidirectional, broadband, hydrophobic, antireflective film

中图分类号:

TB34

荚桂玉, 李怡雯, 王红宁, 陈若愚. 具有梯度渐变折射率的超疏水减反膜的制备及其性能[J]. 无机材料学报, 2018, 33(9): 1011-1016.

JIA Gui-Yu, LI Yi-Wen, WANG Hong-Ning, CHEN Ruo-Yu. Preparation and Property of Superhydrophobic Antireflective Film with Gradient Refractive Index[J]. Journal of Inorganic Materials, 2018, 33(9): 1011-1016.

图/表 7

图1 (a)SiO2粒子、(b) H-SiO2粒子和(c) MgF2棒高分辨透射电镜照片

Fig. 1 TEM images of (a) solid SiO2 particles, (b) H-SiO2 particles and (c) hollow rod-shaped magnesium fluoride

图2 SiO2/H-SiO2/MgF2薄膜FESEM (a)表面SEM照片和(b)截面

Fig. 2 FESEM (a) surface image, and (b) cross-sectional image of the SiO2/H-SiO2/MgF2 film

表1 SiO2、H-SiO2、MgF2膜层椭偏仪测试结果

Table 1 Ellipsometer test results of SiO2, H-SiO2, MgF2 films

Layer position	Material	Thickness/nm	n¹ ₍_λ_{= 550 nm)}
Layer 1	SiO₂	110	1.36
Layer 2	H-SiO₂	125	1.25
Layer 3	MgF₂	135	1.14

图3 (a)镀SiO2单层膜、SiO2/H-SiO2双层膜、SiO2/H- SiO2/MgF2三层薄膜基片和空白基片在380~1600 nm波段内的透光率曲线图, (b) SiO2/H-SiO2/MgF2镀膜基片在不同光入射角度下的透光率曲线图, (c) SiO2/H-SiO2/MgF2镀膜基片在不同入射角和不同波长下的透光率曲线三维图

Fig. 3 Transmittances of (a) the blank substrate and the coated substrates with SiO2 monolayer, SiO2/H-SiO2 bilayer, and SiO2/H-SiO2/MgF2 three-layer graded refractive index film in the wavelength of 380-1600 nm, (b) the coated substrate with SiO2/H-SiO2/MgF2 film at different angles of incidence, and (c) three-dimensional transmittances of the coated substrate with SiO2/H-SiO2/MgF2 film

图4 (a)光通过三层薄膜进入基底的光路图, (b)不同入射角下膜层界面处的菲涅耳反射系数

Fig. 4 (a) Optical path of the light enters in the substrate through three-layer coating, (b) Fresnel reflection coefficients at the coating interfaces at different angles of incidence

图5 SiO2/H-SiO2/MgF2梯度折射率薄膜在(a) 0°、(b) 30°、(c) 60°和(d) 75°的光入射角度下的理论和实验非偏振和偏振透光率曲线

Fig. 5 Theoretical and experimental and polarization transmittance curves of the SiO2/H-SiO2/MgF2 three-layer graded refractive index film coated substrate at the incident angles of (a) 0°, (b) 30°, (c) 60°, (d) 75°

图6 (a) SiO2/H-SiO2/MgF2梯度折射率薄膜修饰前的水接触角和AFM图, (b) HDTMOS修饰后的水接触角

Fig. 6 (a) Water contact angle and AFM pattern of the SiO2/H-SiO2/MgF2 gradient index film, and (b) water contact angle of the SiO2/H-SiO2/MgF2 film was modificated by HDTMOS

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