A kind of anti-pollution vacuum anti-reflection film and preparation method thereof

An anti-reflection film and anti-pollution technology, which is applied in the direction of instruments, optical components, coatings, etc., can solve the problems of poor weather resistance and poor transmission performance, and achieve high anti-pollution ability, improved weather resistance, and reduced free energy.

Active Publication Date: 2019-12-17
LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide an anti-pollution vacuum anti-reflection film and its preparation method to solve the existing problems of poor weather resistance and poor transmission performance

Method used

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  • A kind of anti-pollution vacuum anti-reflection film and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of the anti-pollution vacuum anti-reflection film of this embodiment includes the following steps:

[0027] (1) In an environment with a temperature of 3°C and a relative humidity of 50%, tetraethyl orthosilicate, nitric acid, and butanol are mixed in a mass ratio of 2:0.5:20 and fully stirred, and hydrolyzed and polycondensed to obtain unmodified SiO 2 Sol A of porous particles;

[0028] (2) Add 2,2,3,3,4,4,5,5,6,6,7,7-perfluoro-1,8-octanediol to sol A to make it react with orthosilicate tetra The mass ratio of ethyl ester is 5%, stirred at room temperature for 5h, and then aged at 30°C for 12 days to obtain the modified SiO 2 Sol B of porous particles;

[0029] (3) By ultrasonic-assisted method (ultrasonic frequency 18kHz, ultrasonic power 500W, ultrasonic time 10min), 0.25g of hexafluoro-2-methylisopropyl acrylate polymer was completely dissolved in 200mL of acetone with a mass ratio of 1:1 And in the mixed solution of sec-butanol, obtain t...

Embodiment 2

[0033] The preparation method of the anti-pollution vacuum anti-reflection film of this embodiment includes the following steps:

[0034] (1) In an environment with a temperature of 4°C and a relative humidity of 40%, tetraethyl orthosilicate, hydrochloric acid, and ethanol are mixed according to a mass ratio of 3.5:1:30 and fully stirred, and hydrolyzed and polycondensed to obtain an unmodified SiO 2 Sol A of porous particles;

[0035] (2) Add 2,2,3,3,4,4,5,5,6,6,7,7-perfluoro-1,8-octanediol to sol A to make it react with orthosilicate tetra The mass ratio of ethyl ester was 6%, stirred at room temperature for 6h, and then aged at 25°C for 14 days to obtain the modified SiO 2 Sol B of porous particles;

[0036] (3) By ultrasonic-assisted method (ultrasonic frequency 18kHz, ultrasonic power 500W, ultrasonic time 10min), 0.5g of hexafluoro-2-methylisopropyl acrylate polymer was completely dissolved in 260mL of acetone with a mass ratio of 1:1.5 And in the mixed solution of s...

Embodiment 3

[0040] The preparation method of the anti-pollution vacuum anti-reflection film of this embodiment includes the following steps:

[0041](1) In an environment where the temperature is 5°C and the relative humidity is lower than 30%, tetraethyl orthosilicate, ammonium chloride, and acetone are mixed according to the mass ratio of 5:1.5:40 and fully stirred, and hydrolyzed and polycondensed to obtain Modified SiO 2 Sol A of porous particles;

[0042] (2) Add 2,2,3,3,4,4,5,5,6,6,7,7-perfluoro-1,8-octanediol to sol A to make it react with orthosilicate tetra The mass ratio of ethyl ester is 7%, stirred at room temperature for 7h, and then aged at 20°C for 16 days to obtain the modified SiO 2 Sol B of porous particles;

[0043] (3) By ultrasonic-assisted method (ultrasonic frequency 18kHz, ultrasonic power 500W, ultrasonic time 10min), 0.75g of hexafluoro-2-methylisopropyl acrylate polymer was completely dissolved in 320mL of acetone with a mass ratio of 1:1.5 And in the mixed ...

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Abstract

The invention discloses an anti-pollution vacuum anti-reflection coating and a preparation method thereof, and belongs to the technical field of the optical material. The preparation method comprisesthe following steps: adding a modifying agent 2,2,3,3,4,4,5,5,6,6,7,7-perfluoro-1,8-capryl glycol after accomplishing sol synthesis, performing fluorination modification on a generated silicon dioxidesurface, wherein the modifying gent is the perfluoro-substituted glycol; and adopting hexafluoro-2-methyl isopropyl acrylate polymer as a filler at the same time, thereby guaranteeing that the anti-reflection coating has high performance in a vacuum device. The vacuum anti-reflection coating prepared through the invention is low in surface free energy, the grease or moisture is hard to adsorb onthe surface, and the anti-reflection coating has high transmissivity of 99% at the ultraviolet band of 3-51nm; the high-energy output of frequency-tripled laser in a strong laser device can be realized, and the transmissivity basically maintains unchanged after the anti-pollution vacuum anti-reflection coating is placed for several days in a vacuum environment containing an organic pollution source.

Description

technical field [0001] The invention relates to the technical field of optical thin film materials, in particular to an anti-pollution vacuum anti-reflection film and a preparation method thereof. Background technique [0002] The sol-gel chemical coating method is widely used in the thin film preparation of components in high-power lasers due to its advantages of simple preparation process, low cost, good uniformity of large-area film formation, and high resistance to laser damage threshold. High-power lasers, especially ultraviolet lasers, must be operated in a vacuum device to ensure that their beam quality and transmission energy are not affected, but substances that increase sealing properties such as vacuum esters used in vacuum devices are also more volatile and adhere to the surface of the component, resulting in its Performance degradation or even complete failure. Therefore, making the film layer have a weather resistance function in the vacuum device can improve ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09D1/00C09D7/65C03C17/00G02B1/113
CPCG02B1/04G02B1/11G02B1/111
Inventor 张清华邓雪然杨伟雷向阳马红菊王震惠浩浩王梓龙张剑锋张帅
Owner LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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