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A kind of preparation method of anti-reflection and anti-reflection coating with high-strength humidity and heat resistance

A technology of anti-reflection and anti-reflection, heat and humidity resistance, applied in optical components, optics, instruments, etc., can solve the problems of stability affecting the anti-reflection performance of coatings, complex preparation process, small preparation area, etc., to achieve low cost, durable Good performance, simple and fast preparation process

Active Publication Date: 2018-05-08
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Physical methods include physical vapor deposition, plasma etching, sputtering and other methods. At present, targets such as zirconia and magnesium fluoride are mainly used to coat substrates, and anti-reflection and anti-reflection coatings with high hardness can be obtained. For example, Fu Xiaoyong et al. (patent CN 1752275A) have invented a kind of preparation method that prepares wide-spectrum anti-reflection film on K9 glass, and this method obtains broad-spectrum anti-reflection and anti-reflection coating by physical vapor deposition zirconia under certain conditions, but prepares in It is carried out under vacuum conditions, and steps such as melting the target material limit the preparation of large-area coatings; Seungmuk Ji et al. (Nanoscale, 2012, 4, 4603-4610) used CF4 or oxygen plasma etching to prepare a maximum light transmittance of up to 99% anti-reflection and anti-reflection coating with moth-eye structure, but the complex preparation process and small preparation area of ​​this method limit its application
Chemical methods include chemical deposition, chemical etching, sol-gel method and other ways to prepare coatings. For example, the applicant (Langmuir, 2013, 29, 3089-3096) obtained the highest light transmittance by chemically etching glass sheets with fluorosilicic acid The rate can reach 99.0% of the sample, but the hydrophilic mesoporous pores of this sample are easy to absorb water, which will affect the stability of the anti-reflection performance of the coating. -Gel technology, controlled acid / acid two-step method by HCl, hydrolyzed ethyl orthosilicate to prepare sol solution, and then modified with methyltriethoxysilane to prepare a composite low refractive index nanoporous dioxide Silicon film, this film has hydrophobic properties, which can avoid the problem of hygroscopicity of the coating, but the two-step preparation process is complicated, and the light transmission properties of the film need to be further studied

Method used

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  • A kind of preparation method of anti-reflection and anti-reflection coating with high-strength humidity and heat resistance
  • A kind of preparation method of anti-reflection and anti-reflection coating with high-strength humidity and heat resistance
  • A kind of preparation method of anti-reflection and anti-reflection coating with high-strength humidity and heat resistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Mix methyl orthosilicate, methyltrimethoxysilane, water, and ethanol in a molar ratio of 0.5-0.6:0.5-0.4:3-7:30-50 to obtain a mixed solution, and then add hydrochloric acid to adjust the solution pH = 1-3, finally add 2.5wt% surfactant cetyltrimethylammonium bromide to the total amount of the mixed solution, and stir at room temperature for 12-72 hours to obtain a homogeneously mixed composite silica sol solution.

[0036] (2) The homogeneously mixed composite silica sol solution prepared in step (1) is used to prepare a coating on a common glass substrate by a pulling coating method.

[0037] (3) annealing the coating obtained in step (2) in a muffle furnace at 600 degrees centigrade for 1-100 minutes to obtain an anti-reflection and anti-reflection coating with high strength and moisture resistance.

[0038] (4) Carry out light transmittance, heat and humidity resistance, hardness and adhesion tests on the anti-reflection and anti-reflection coating with high str...

Embodiment 2

[0045] Same as Example 1, except that ethyl orthosilicate, methyltriethoxysilane, water, and ethanol are mixed evenly in a molar ratio of 0.2-0.3:0.8-0.7:3-7:30-50.

[0046] Light transmittance test: test the transmittance spectrum of the substrate with the above-mentioned coating with an ultraviolet-visible spectrometer, and the results are as follows Figure 5 Shown at midline 1. Figure 5 The middle line 1 is the transmission spectrum of the prepared sample. The maximum light transmittance of the coated substrate is 99.2%, and the average light transmittance in the wavelength range of 400-800nm ​​is 97.2%, which shows that the coating has excellent anti-reflection and anti-reflection effects.

[0047] Moisture and heat resistance test: the high-strength anti-reflection and antireflection coating with high strength and humidity and heat resistance prepared in this embodiment was placed in saturated water vapor at 100 degrees Celsius for 12 hours, and the light transmittance...

Embodiment 3

[0050] Same as Example 1, except that methyl orthosilicate, methyltrimethoxysilane, water, and ethanol are mixed according to the molar ratio of 0.7-0.8:0.3-0.2:3-7:30-50.

[0051] Light transmittance test: test the transmittance spectrum of the substrate with the above-mentioned coating with an ultraviolet-visible spectrometer, and the results are as follows Figure 6 Shown at midline 1. Figure 6 The middle line 1 is the transmission spectrum of the prepared sample. The maximum light transmittance of the coated substrate is 98.9%, and the average light transmittance in the wavelength range of 400-800nm ​​is 97.1%, which shows that the coating has excellent anti-reflection and anti-reflection effects.

[0052] Damp heat resistance test: place the prepared high-strength damp heat resistant anti-reflection and anti-reflection coating in saturated water vapor at 100 degrees Celsius for 12 hours, and measure the change of light transmittance of the coated substrate. The results ...

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Abstract

The invention discloses a preparation method of a damp and heat-resistant anti-reflection coating with high strength. The preparation method comprises the following steps of uniformly mixing silicate ester, silane, water and ethyl alcohol according to the molar ratio of x:(1 to x):(3 to 7):(30 to 50), so as to obtain mixing solution; adding acid catalyst, and adjusting the pH (potential of hydrogen) value of the mixing solution to 1 to 3; adding surfactant, and stirring at room temperature, so as to obtain composite silicon dioxide sol solution, wherein x is greater than or equal to 0.2 and is smaller than or equal to 0.8; coating the prepared composite silicon dioxide sol solution onto a glass substrate, and preparing a coating; annealing the prepared coating, so as to obtain a finished product, namely the damp and heat-resistant anti-reflection coating with high strength. The prepared coating has the advantages that the anti-reflection property is excellent, the heat and damp-resistant property is realized, and the strength is high. The method for preparing the composite silicon dioxide sol solution by a one-step type has the advantages that the preparation technology is simple and rapid, the cost is low, the property is excellent, the durability is good, the application range is wide, and the like.

Description

technical field [0001] The invention relates to the technical field of material preparation. More specifically, it relates to a method for preparing an anti-reflection and anti-reflection coating with high strength and heat and humidity resistance. Background technique [0002] Anti-reflection and anti-reflection coating refers to a film on the surface of a light-transmitting substrate that can increase light transmission and reduce light reflection, thereby increasing the light transmittance of optical components. At present, the light transmittance of ordinary optical glass in the visible light range is about 90.4%. If a layer of anti-reflection and anti-reflection coating is coated on the surface of the substrate, it can not only eliminate the reflected light of the optical glass, but also increase the light transmittance. It has a wide range of application values ​​in solar cells, optical devices, building materials, transportation and other fields. To prepare anti-ref...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G02B1/111
Inventor 贺军辉李彤
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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