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Water-proof broad band high anti-reflection film and its preparation method

An anti-reflection film and waterproof technology, applied in optical components, instruments, optics, etc., can solve the problems of non-waterproof, complicated preparation process, restrictions, etc., and achieve good waterproof performance

Inactive Publication Date: 2007-10-31
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But SiO 2 The hydroxyl group on the pore surface of the anti-reflection film is an active physical adsorption center, which is very easy to absorb water vapor in the environment, and does not have hydrophobic properties. The microporous silica film adsorbed by water vapor may continue to undergo condensation reactions and lead to the collapse of the pore structure. As a result, it affects the separation effect of the gas, limits its application in the water vapor environment, and becomes the bottleneck of industrial application. Due to the influence of moisture in the air, its service life is also short. my country's sol-gel silica waterproof anti-reflection The research work of the membrane has made a lot of technological progress, but it is still unable to realize the waterproof performance while realizing multi-window anti-reflection, which greatly limits its application.
[0003] As early as 1992, Floch and Belleville applied a layer of fluorine-containing material on the outside of the anti-reflection coating to increase the hydrophobicity of the coating. The raw materials of this method are expensive and the preparation process is relatively complicated.
At present, SiO is also prepared by sol-gel method in my country. 2 After the film, the surface is modified to obtain hydrophobic properties, but the film prepared by this method does not have the performance of multi-window anti-reflection; there are also inventions using polymethyl methacrylate or polystyrene and SiO 2 The sol is mixed and then coated to achieve multi-window anti-reflection performance, but it is not waterproof

Method used

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preparation example Construction

[0011] The preparation operation steps of the present invention are as follows:

[0012] 1. Measure tetraethyl orthosilicate, absolute ethanol, PEG400 (or PEG200), ammonia water (or ammonium bicarbonate) according to the above mass percentage, and mix them;

[0013] 2. Stir the mixed solution at 25-35°C for 3-6 hours;

[0014] 3. Reflux, the reflux temperature is 50-65°C, and the reflux time is 6-9 hours to obtain SiO 2 Sol;

[0015] 4. SiO 2 The sol is aged for 7-10 days, and then the PS or PMMA and SiO 2 The sol is mixed evenly;

[0016] 5. Spin coating to form a film, the spin coating speed is 1000-4000rpm / s;

[0017] 6. Surface modification. After the surface is dried, the plated film is immersed in n-hexane solution containing about 8-15% trimethylchlorosilane for 12-16 hours, and then immersed in ethanol for 12-48 hours to age.

[0018] 7. Heat-treat the film layer at 150-300°C for 5-9 hours to obtain the required waterproof anti-reflection film.

Embodiment 1

[0020] The composition of the waterproof anti-reflection film is represented by mass percentage: tetraethyl orthosilicate 7.0%, ammonia water 2.0%, dehydrated alcohol 62.5%, polyethylene glycol (400) 28.5%, adding PS with a molecular weight of about 5000, PS accounts for 0.07% of the mass of silica sol, mix the raw materials (except PS) and stir at 30°C for 3 hours, reflux to keep the pH value of the solution at about 8.5, and mix the PS dissolved in ether with the sol after aging the sol for 7 days. The film is formed by spin coating method, the speed is 1100rpm / s, spin coating for 1min, after the surface is dried, the coated film is immersed in a 10% n-hexane solution containing trimethylchlorosilane, soaked for 14 hours, and then immersed in ethanol for aging for 28 hours. Take it out and dry it naturally, and finally heat-treat at 150°C for 5 hours to get the desired PS-SiO 2 film. The contact angle of the film is 105.4°, and the light transmittance at 351nm, 527nm and 10...

Embodiment 2

[0022] The composition of the waterproof anti-reflection film is represented by mass percentage: tetraethyl orthosilicate 7.6%, ammonia water 1.2%, dehydrated alcohol 68.0%, polyethylene glycol (400) 23.2%, adding PS with a molecular weight of about 10000, PS accounts for 0.05% of the quality of silica sol, mix the raw materials (except PS) and stir at 35°C for 4 hours, reflux to keep the pH value of the solution at about 8.5, and mix the PS dissolved in ether with the sol after aging the sol for 10 days. The film is formed by spin coating, the speed is 2000rpm / s, spin coating for 1min, after the surface is dried, the coated film is immersed in a n-hexane solution containing 12% trimethylchlorosilane, soaked for 15 hours, and then immersed in ethanol for 30 hours to age. Take it out and dry it naturally, and finally heat-treat at 200°C for 8 hours to obtain the desired PS-SiO 2 film. The contact angle of the film is 105.4°, and the light transmittance at 351nm, 527nm and 1054...

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Abstract

A method for preparing wideband and high anti-reflection film of waterproof type includes forming SiO2 collosol by utilizing sol-get means, adding PS or PMMA then plating film with spiral coating, surface-modifying by trimethyl chlorosilane and n-hexane to obtain wideband and high anti-reflection film of waterproof type.

Description

technical field [0001] The invention belongs to the technical field of optical thin film materials, specifically a new type of SiO 2 Waterproof broadband high anti-reflection film and preparation method thereof. technical background [0002] Inertial confinement fusion (ICF) uses high-power pulsed laser as the research method, and SiO prepared by sol-gel method 2 Anti-reflection coatings have excellent characteristics such as high damage threshold and low refractive index, and have attractive application prospects in the field of high-power lasers. But SiO 2 The hydroxyl group on the pore surface of the anti-reflection film is an active physical adsorption center, which is very easy to absorb water vapor in the environment, and does not have hydrophobic properties. The microporous silica film adsorbed by water vapor may continue to undergo condensation reactions and lead to the collapse of the pore structure. As a result, it affects the separation effect of the gas, limits...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G02B1/10G02B1/111
Inventor 彭波杨雨婷蒋蕾郭睿倩
Owner FUDAN UNIV