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Method for preparing high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating

A technology of anti-reflection and anti-reflection, composite coating, applied in the direction of coating, can solve the problems of anti-reflection and anti-reflection performance easily affected by moisture, the coating is not resistant to humidity and heat strength, affecting the anti-reflection effect of the coating, etc. Achieve the effect of excellent anti-reflection and anti-reflection performance, good durability and superior performance

Active Publication Date: 2017-09-08
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, a series of hydrophilic or hydrophobic anti-reflection and anti-reflection coatings have been prepared by using sol-gel technology, but the coating is not resistant to heat and humidity or has weak strength, which limits the wide application of anti-reflection and anti-reflection coatings, such as Prevo et al. (J.Mater.Chem, 2007,8,791-799) prepared a superhydrophobic silica coating based on the sol-gel method and modified with fluorosilane
Niu Yanyan et al. (China Sol-Gel Symposium and International Forum Conference Guidelines and Abstracts Collection, 2014) added an appropriate amount of hexamethyldisilazane (HMDS) to the basic catalyzed silica sol to obtain HMDS Modified sol, and prepared a super-hydrophobic anti-reflective coating, but the strength of the coating prepared by these two methods still needs to be further strengthened, and the preparation process also needs to be further simplified
In addition, Yao Lanfang et al. (TFC'03 National Thin Film Technology Symposium, 2003) and Zhang Zhihui et al. (Applied Chemistry, 2013, 7, 794-800) prepared acid-catalyzed silica sol by acid-catalyzed ethyl orthosilicate method and prepared Coating, the coating that this method prepares has more than 6H pencil hardness, overcomes the defect of coating strength aspect, but it has stronger hygroscopicity, has a strong impact on the anti-reflection effect of coating; People such as Xu Ligang (J.Mater. Chem.C, 2013, 1, 4655–4662) prepared an anti-reflection and anti-reflection wear-resistant silica film by using an alkaline catalytic one-step deposition method, but the coating also has weak moisture resistance, which affects the coating’s durability. Anti-reflection effect
In order to obtain an anti-reflection and anti-reflection coating with both moisture resistance and high strength, Yan Wang et al. (SolarEnergy Materials and Solar Cells, 2014, 130, 71–82) added Phosphoric acid is used as a cross-linking agent to prepare a high-strength anti-reflection and anti-reflection coating, but the anti-reflection and anti-reflection performance of the coating is easily affected by moisture, and it is easy to be corroded by water vapor during use, thus affecting the long-term effect of the coating. sex

Method used

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  • Method for preparing high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating
  • Method for preparing high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating
  • Method for preparing high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) Mix ethyl orthosilicate, methyltrimethoxysilane, water and ethanol according to the molar ratio of 0.5~0.6:0.5~0.4:3~7:30~50 to obtain a mixed solution, add acid catalyst hydrochloric acid to adjust and mix The pH value of the solution is 1 to 3, then add 2 to 4 wt% of the surfactant cetyltrimethylammonium bromide and 1.5 to 3.5 wt% phosphoric acid in the total amount of the mixed solution, and stir at room temperature for 12 hours to obtain carbon Silicon oxyphosphorus composite sol solution.

[0033] 2) Coating the carbon-silicon-oxygen-phosphorus composite sol solution prepared in step 1) on a common glass substrate to prepare a coating. The coating method is spin coating, pulling, spray coating or roll coating.

[0034]3) Keep the coating prepared in step 2) at 200-400 degrees Celsius for 20-1000 minutes, then anneal at 600-750 degrees Celsius for 1-5 minutes, and then in a mixture of water and ethanol with a volume ratio of 2:1 A high-strength heat-resistant, ...

Embodiment 2

[0040] Same as Example 1, except that ethyl orthosilicate, methyltrimethoxysilane, water, and ethanol are mixed evenly in a molar ratio of 0.2-0.4:0.8-0.6:3-7:30-50.

[0041] 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 image 3 Shown at midline 1. image 3 The middle line 1 is the transmission spectrum of the prepared sample. The maximum light transmittance of the coated substrate is 98.7%, 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.

[0042] Humidity and heat resistance test: place the high-strength dampness and heat resistance antireflection and antireflection carbon silicon oxygen phosphorus composite coating prepared in this embodiment in saturated water vapor at 100 degrees Celsius for 12 hours, and measure th...

Embodiment 3

[0049] Same as Example 1, except that 1 wt% of surfactant cetyltrimethylammonium bromide was added at the end. The coating still has anti-reflection and anti-reflection, high strength, and heat and humidity resistance properties similar to those of Example 1.

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Abstract

The invention discloses a method for preparing a high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating. The method comprises the following steps: uniformly mixing silicate ester, silane, water and ethyl alcohol at the molar ratio of x:(1-x):(3-7):(30-50) to obtain a mixed solution, adding an acid catalyst to adjust the pH value of the mixed solution to be 1-3, then adding a surfactant and phosphoric acid, and performing stirring at the room temperature to obtain a carbon silicon oxygen phosphorus composite sol solution, wherein x is larger than or equal to 0.2 and smaller than 0.7; coating a glass substrate with the prepared sol solution to prepare a coating; and performing heat treatment on the coating, and after that, performing ultrasonic cleaning to remove a redundant cross-linking agent to obtain a final product, namely the high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating. The prepared high-strength heat-and-humidity resistant anti-reflection carbon silicon oxygen phosphorus composite coating has excellent anti-reflection performance, is resistant to heat and humidity, and is high in strength. Meanwhile, the one-step sol preparation and coating depositing method has the advantages of simple and quick preparation process, low cost, superior performance, good durability, wide application range 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 a high-strength heat-and-humidity anti-reflection and anti-reflection carbon-silicon-oxygen-phosphorus composite coating. Background technique [0002] Anti-reflection and anti-reflection coating refers to a film on the surface of optical materials that can reduce light reflectivity and increase light transmittance. It is widely used in architectural glass, display screens, solar cells, optical devices, building materials, transportation and other fields. Wide application value. According to the Fresnel principle, the reflection of light at the interface comes from the difference in refractive index between the substrate and the air. If a coating with a proper refractive index is coated between the optical substrate and the air interface, the reflectivity of the optical material can be increased. Corresponding decline. To pre...

Claims

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Application Information

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IPC IPC(8): C09D1/00C09D7/12
CPCC09D1/00
Inventor 贺军辉李彤
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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