CN-117924979-B - Linear high polysilane reinforced wear-resistant anti-reflection coating and preparation method thereof

Abstract

The invention belongs to the technical field of coatings, and particularly relates to a linear high polysilane reinforced wear-resistant anti-reflection coating and a preparation method thereof. Tetraethyl orthosilicate and methyltriethoxysilane/methyltrimethoxysilane are used as co-precursors, an alkaline network-shaped silica sol is synthesized by adopting a sol-gel method under an alkaline condition, poly (methyl hydrosiloxane) is used as a silicon source, linear high polysilicone sol is synthesized under the action of a catalyst, then the two silica sols are mixed, aged and deaminated to obtain neutral mixed sol, a double-sided anti-reflection coating is plated on the surface of high borosilicate glass by utilizing a dipping-pulling method, and finally the wear-resistant anti-reflection coating is obtained by calcining for 2 hours in a muffle furnace at 550 ℃. The prepared anti-reflection coating has high transmittance and good wear resistance, avoids the use of acid in the preparation process, prevents corrosion to production equipment and environmental pollution, and is environment-friendly in production operation.

Inventors

• CHEN RUOYU
• HU LIANG
• JIA QIAN
• LIU XIAOHUA

Assignees

• 常州大学

Dates

Publication Date

20260505

Application Date

20240110

Claims (5)

1. 1. The preparation method of the linear high polysilane reinforced wear-resistant anti-reflection coating is characterized by comprising the following steps of: (1) Absolute ethyl alcohol EtOH is used as a solvent, ammonia water NH 4 OH is used as a catalyst, tetraethyl orthosilicate TEOS and methyltriethoxysilane MTES/methyltrimethoxysilane MTMS are used as silicon sources, and an alkaline network silica sol is prepared by a sol-gel method; Taking absolute ethyl alcohol EtOH as a solvent, karstedt as a catalyst, taking poly (methyl hydrogen siloxane) PMHS as a silicon source, and adopting a sol-gel method to prepare linear high polysilica sol; (2) Weighing alkaline network silica sol and linear high-polymer silica sol, mixing, aging, removing ammonia, and preparing stable and uniform mixed sol; (3) And (3) plating the mixed sol obtained in the step (2) on a glass substrate by adopting a dipping-pulling method, and then placing the glass substrate into a muffle furnace for calcination to obtain the wear-resistant anti-reflection coating.
2. 2. The abrasion-resistant antireflection coating according to claim 1, wherein in the step (1), the alkaline network-like silica sol is prepared by vigorously stirring for 12 hours in an oil bath at 60 ℃.
3. 3. The abrasion-resistant anti-reflection coating according to claim 1, wherein in the step (1), the linear high-silica sol is prepared by stirring for 5min at 25 ℃ and performing water bath ultrasonic treatment for 30 min.
4. 4. The wear-resistant anti-reflection coating according to claim 1, wherein in the step (2), the mass ratio of SiO 2 in the alkaline network silica sol to PMHS used in the linear high-silica sol is 1:1-1:5.
5. 5. The wear-resistant anti-reflection coating according to claim 1, wherein in the step (3), the dipping and pulling speed of the mixed sol is 600-1000 μm/s, the dipping time is 360s, the dipping is 2 times, the residence time is 120s, and the mixed sol is calcined in a muffle furnace at 550 ℃ for 2h.

Description

Linear high polysilane reinforced wear-resistant anti-reflection coating and preparation method thereof Technical Field The invention belongs to the technical field of coatings, and particularly relates to a linear high polysilane reinforced wear-resistant anti-reflection coating and a preparation method thereof. Background Mechanical stability is critical to the anti-reflective coating during manufacturing, installation, maintenance and cleaning. In general, base-catalyzed silica coatings exhibit excellent transmittance, but since silica particles are randomly stacked with only point contact force, they are susceptible to mechanical scratches, making them easy to remove. On the other hand, acid catalyzed silica antireflective coatings consist of linear chains that are strongly crosslinked by chemical bonds, providing strong adhesion on the substrate. However, the linear chain structure results in low porosity, resulting in high refractive index and poor transmittance. Thus, neither base-catalyzed nor acid-catalyzed coatings provide excellent transmittance and high attrition resistance at the same time. The traditional solution is to combine the advantages of base-catalyzed and acid-catalyzed antireflective coatings, providing good transmittance and mechanical stability. Rubing Xi et al dip-coat a mixed suspension of acid-catalyzed silica sol and hydrophobic silica nanoparticles, the prepared coating had high mechanical stability (3H pencil scratch test), an average transmittance increase of 4.0% in the wavelength range of 400-800 nm, but the pH in the acid catalysis process was 1-2. CN 108455872B discloses a preparation method of a scratch-resistant hydrophobic anti-reflection coating, the hybrid sol is formed by cross-linking and hybridization of hydrophobic modified hollow sphere silica nano particles and hydrophilic inorganic nano binders, the transmittance curve of the prepared hydrophobic anti-reflection coating is basically unchanged after 1000 times of reciprocating washing tests, but the pH value is 0.1-5 in the preparation process. Chen Jinglei preparing acid-catalyzed silica sol and alkali-catalyzed silica sol by a sol-gel method, mixing the acid-catalyzed silica sol and the alkali-catalyzed silica sol in a volume ratio of 1:5, wherein the highest transmittance of the antireflection coating prepared by a dipping and pulling method in a visible light region is about 99%, after the glass is coated with the film by repeatedly rubbing a cotton ball soaked with alcohol for 100 times, the transmittance is only slightly reduced (< 1%), and the pH of the acid gel is 2-3; In addition FANGTING CHI et al, through an ammonia treatment process to increase the mechanical durability of the silica coating, synthesized two different sized silica nanoparticles for the purpose of obtaining a nanocoating, which were then deposited on a glass substrate. By placing 50mL of ammonia water in a 5L sealed glass container to create an ammonia atmosphere, the hardness of the coating increases with increasing ammonia treatment time, the average transmittance of the coating remains substantially unchanged after ammonia treatment by the 2H pencil hardness test, but a large amount of ammonia water is required during ammonia treatment, which is also easily detrimental to the environment. In order to enhance the mechanical stability of the anti-reflective coating, the conventional approach is to use an acid-catalyzed linear silica sol as binder mixed with an alkali gel. However, a large amount of acid substances such as hydrochloric acid are needed in the acid catalysis process, so that production equipment can be corroded in industrial production, and great environmental risks are brought. Therefore, it is very desirable and challenging to develop a method to produce a robust anti-reflective coating under neutral conditions. Disclosure of Invention In order to solve the technical problems pointed out in the background art, the invention provides a linear high polysilane reinforced wear-resistant anti-reflection coating and a preparation method thereof, wherein an alkaline network-shaped silica sol is prepared by a sol-gel method, poly (methyl hydrogen siloxane) is used as a silicon source, linear high polysilane sol is synthesized under the action of a catalyst, the alkaline network-shaped silica sol and the linear high polysilane sol are mixed according to the mass ratio of SiO 2 in alkali gel to PMHS used by the linear high polysilane sol, the linear high polysilane sol and the network-shaped silica sol are aged, the linear high polysilane sol and the network-shaped silica sol are combined, crosslinked and filled in the middle of silicon dioxide network-shaped nano particles, then a double-layer coating is plated on two sides of glass at the same time by adopting a dipping-pulling method, and the wear-resistant anti-reflection coating is obtained after calcination in a muffle furnace. The preparation method mainly comprises th