CN120607370A - PS modified SiO with high radiation resistance, high mechanical property and high antireflection2Method for producing film - Google Patents
PS modified SiO with high radiation resistance, high mechanical property and high antireflection2Method for producing filmInfo
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Abstract
本发明公开了一种紫外吸收剂改性的高抗辐照高力学性能高减反射SiO2薄膜的制备方法。以水杨酸苯酯为致孔剂、硅酸四乙酯和甲基三乙氧基硅烷为前驱体、无水乙醇为溶剂、硝酸为催化剂。先制备好SiO2溶胶，将溶胶涂敷在玻璃上，溶胶经干燥成为凝胶，再经热处理得到多孔纳米薄膜。薄膜在400‑1100nm光谱的透过率(镀膜玻璃的透过率)平均值为92.85％，比玻璃提高了4.35个百分点；薄膜表面硬度达到铅笔法最高级别9H，附着力也达到胶带法最高级别0级。紫外线辐照5000等效太阳时后薄膜的平均透过率为92.15％，仅下降0.7个百分点。本高抗辐照高力学性能高减反射薄膜制备方法工艺简单、适合产业化推广。
The present invention discloses a method for preparing a UV absorber-modified SiO2 film with high radiation resistance, high mechanical properties and high anti-reflection. Phenyl salicylate is used as a porogen, tetraethyl silicate and methyltriethoxysilane are used as precursors, anhydrous ethanol is used as a solvent, and nitric acid is used as a catalyst. A SiO2 sol is first prepared, and the sol is coated on glass. The sol is dried to form a gel, and then heat-treated to obtain a porous nanofilm. The average transmittance of the film in the 400-1100nm spectrum (the transmittance of the coated glass) is 92.85%, which is 4.35 percentage points higher than that of glass; the surface hardness of the film reaches the highest level of 9H by the pencil method, and the adhesion also reaches the highest level of 0 by the tape method. After 5000 equivalent solar hours of ultraviolet irradiation, the average transmittance of the film is 92.15%, which is only a decrease of 0.7 percentage points. This method for preparing a high radiation resistance, high mechanical properties and high anti-reflection film has a simple process and is suitable for industrial promotion.
Description
Technical Field
The invention belongs to the technical field of antireflection film materials, and particularly relates to a preparation method of a Phenyl Salicylate (PS) -modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection.
Background
Solar energy has been an important energy source in the strategy of energy development. The solar energy resource is rich, the energy supply can be continuously obtained, and the solar energy source is clean and pollution-free renewable resource. Solar cells are one of the main means of solar energy utilization, but solar cells generally work outdoors, and solar power stations are mostly located in hills, mountains or deserts, and have severe environments. There is a need for a glass cover plate to protect solar cells from the outside environment. However, the reflection loss of the glass cover plate on the incident light is about 8-9%, and the photoelectric conversion efficiency of the solar cell is seriously reduced.
In order to further improve the light transmittance of the glass cover plate, an antireflection film is generally plated on the surface of the glass cover plate. The antireflection film has a single layer film, a double layer film and a multilayer film. The single-layer film material mainly comprises SiO 2、MgF2, tiO 2 and the like. According to the antireflection principle, a single-layer film with a quarter wavelength thickness can only realize high antireflection for light with a certain wavelength, so that the antireflection spectrum is narrow. While a bilayer multilayer antireflective film can achieve low reflectivity over a wide wavelength range, it can increase the complexity and cost of the coating process [ Solar Energy,2021,217:29-39 ]. The refractive index of the porous film can be adjusted by the porosity of the porous film, so that the porous film can be better matched with the thickness of the film and the refractive index of the substrate, the reflection of incident light is reduced, and the transmittance is increased [ Studies in Surface Science & Catalysis,2003,146:539-542 ]. In addition, in order to cope with a severe working environment, the film is required to have not only a high anti-reflection effect but also higher mechanical properties and irradiation resistance.
The sol-gel method has the advantages that the microstructure of the film can be changed by adding a pore-forming agent to influence the porosity of the film, and the sol-gel method is commonly used for preparing porous silica films and has excellent anti-reflection performance [ MATERIALS LETTERS,2016,184:305-307 ]. However, the mechanical properties and the irradiation resistance of the sol-gel porous membrane are still in need of improvement. Generally, the higher the porosity of the film, the lower the refractive index, the better the antireflection performance, but the lower the mechanical properties, in particular the hardness, and the poorer the irradiation resistance.
Chinese patent CN 105399340A discloses a super-hydrophobic high-transmission SiO 2 antireflection film and a preparation method thereof, wherein trimethylchlorosilane is added into sol, and the prepared film has higher transmittance and hydrophobicity, the peak transmittance is improved by 5.56 percent, but the irradiation resistance and mechanical property of the antireflection film are not related. Chinese patent CN 108545753A discloses a network-shaped SiO 2 coated sol, a preparation method and application thereof, wherein the network-shaped SiO 2 coated sol is prepared by copolycondensation of three kinds of organic silicon of tetramethyl orthosilicate, methyltriethoxysilane and trimethylmethoxysilane, the average light transmittance of the obtained antireflection film after calcining at 450 ℃ is more than 97% in visible light (400-800 nm), the contact angle is 165 °, and the average light transmittance of the antireflection film after irradiating for 1000 hours in 150W ultraviolet is reduced by not more than 0.5%, but the hardness and adhesion of the antireflection film are not involved. Chinese patent CN 109052981A discloses a preparation method of a high-hardness super wear-resistant anti-reflection film, which uses a uniform and stable sol containing needle whisker structure, i.e. Al-wisker/SiO 2 sol prepared by cohydrolysis of alumina sol and organosilane. The anti-reflection film is prepared by using a lifting dipping method. The sol lifting-dipping method is used for plating a double-sided antireflection film on the surface of glass, and the glass is calcined at 200-250 ℃ to obtain the glass with the average light transmittance of over 96 percent at 400-800nm and the contact angle of 125 degrees, wherein the pencil hardness of the antireflection film is only 5H, and the ultraviolet resistance and the adhesive force are not tested. Chinese patent CN 109502987A discloses a method for preparing high hardness antireflection film based on hollow silica, using tetraethyl silicate as raw material, polyacrylic acid as template, 2-isopropoxyethanol and methanol as solvent, ammonia water as catalyst, preparing central control SiO 2 coated sol by template method, plating coating on common glass by dip-pull method, calcining at 550 ℃ to obtain antireflection film. The average transmittance of the film in the wave band of 400-800 nm is improved by 6 percentage points, the film hardness reaches 4H, and the irradiation resistance and the adhesive force are not characterized. Chinese patent CN 111320396A discloses a preparation method of anti-radiation silicon oxide anti-reflection film, in which an emulsifier polytetrafluoroethylene and nano-scale powder lead chloride are added into the solution, the preparation method is simple to operate, the process is simplified, the effective space radiation protection of the prepared silicon oxide anti-reflection film can be precisely controlled, the hardness is high and controllable, but the effect of irradiation and hardness adhesion is not represented. Chinese patent CN 115872629A discloses a high-performance mesoporous antireflection nano film and a preparation method thereof, wherein polyethylene glycol monomethyl ether substances are adopted as pore-forming agents in the sol-gel process. The obtained film is attached to the surface of the photovoltaic glass, the transmittance of 380-1100nm can be improved by 4-6 percentage points, the pencil hardness is more than 9H, the adhesive force reaches more than 0 level, but the characterization of the irradiation resistance of the film is not involved.
Xin et al [ Solar Energy 2012,86 (11): 3345-3352 ] modified base catalyzed sols with acid catalyzed polysiloxanes. Although the visible light transmittance of the alkali catalytic sol film is as high as 97.81%. However, the film remained between 0.22% and 2.70% in transmittance decay after 90 days of outdoor exposure, without mechanical property characterization and long-term irradiation performance cause anxiety. Wang et al [ Rsc Advances.2016,6 (30): 25191-25197 ] prepared upper and lower mesoporous SiO 2 films on borosilicate glass by solvent evaporation self-assembly method by using polyether F127 and cetyltrimethylammonium bromide as templates, the transmittance of the film is improved by 5.7% in the solar spectrum range of 300-2400 nm, and the pencil hardness is 6H, and the adhesive force and the irradiation resistance are not characterized. Guo et al [ Solar ENERGY MATERIALS AND Solar Cells,2017,170:143-148 ] prepared a silicon dioxide anti-reflection film with a closed surface from tetraethyl orthosilicate, the film has a light transmittance as high as 97.1%, but the surface structure has a pencil hardness of 5H, the nano indentation hardness is about 2.0GPa, the hardness is improved, and the irradiation resistance of the film is not known. Chi et al [ Results in Physics.2020,18:103315 ] prepared a silica antireflection film by sol-gel method, and the peak transmittance was as high as 99.8% under ammonia treatment, but the pencil hardness was only 4H, and the irradiation resistance of the film was not known yet. Wang et al [ Applied nanoscience.2021, 11:875-885 ] prepared hybrid silica sol coatings by a simple and cost-effective two-step sol-gel process with base catalyzed silica sol aging time and impregnation rate optimized, light transmittance improved by about 6.35% and hardness of 4H compared to bare glass substrates, without characterizing adhesion and irradiation resistance. Dong et al [ REACTIVE AND Functional Polymers,2022,171:105176 ] prepared porous anti-reflection films by sol-gel method using polyethylene glycol monomethyl ether (mPEG) as a porogen. When the amount of mPEG is 0.6g, the average transmittance of the film in the wavelength range of 380-1100 nm is highest, and the film is 4.2 percent higher than that of the glass substrate. The film adhesion reaches 0 level, the hardness is more than 9H, but the irradiation resistance is not characterized.
In summary, the preparation process of the SiO 2 film is simple, and the refractive index can be changed by adjusting the porosity. On the basis of meeting high optical performance, the anti-reflection film has high radiation resistance and high mechanical performance, and can meet the requirement of continuous and efficient operation of the solar cell under a field severe environment.
Disclosure of Invention
The invention aims to provide a preparation method of a PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection, which overcomes the defects of the prior art. The anti-reflection film prepared by the method has high transmittance, high radiation resistance and high mechanical property. The average value of the transmittance (the transmittance of coated glass) in the wavelength range of 400-1100nm is increased by 4.35 percent, which reaches 92.85 percent, and the spectral peak value of the transmittance appears at the wavelength of about 550nm, which is as high as 96.3 percent. The film has high hardness, reaches the highest level 9H of a pencil method, has high adhesive force, and reaches the highest level 0 of an adhesive tape method. And after 5000 equivalent sun is irradiated by ultraviolet rays (ESHs), the average transmittance of the film is 92.15 percent, and the average transmittance is reduced by 0.7 percent. Meanwhile, the adhesive has pencil hardness of 8H and adhesive force of 1 grade by an adhesive tape method. The preparation method of the technical scheme of the invention has the advantages of simple process, low cost, suitability for large-area film coating, good stability and easy industrialized popularization.
In order to achieve the above purpose, the invention adopts the following technical scheme:
A preparation method of a PS modified high-radiation-resistance high-mechanical-property high-antireflection SiO 2 film is characterized in that the antireflection film is prepared from tetraethyl silicate, methyltriethoxysilane, nitric acid, water and PS by adopting a sol-gel method, wherein the mass ratio of a pore-forming agent to sol is 1:10-1:200, and the volume ratio of the tetraethyl silicate, the methyltriethoxysilane, absolute ethyl alcohol, deionized water and concentrated nitric acid is 1:0.1-6.0:10.3:0.1-1.0. According to the invention, PS is used as a pore-forming agent to prepare the anti-reflection film, and the transmittance, the anti-irradiation performance, the surface hardness and the adhesive force of the anti-reflection film are adjusted by adjusting the content of PS.
A preparation method of a PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The preparation of the raw materials comprises the steps of preparing the anti-reflection film raw materials, wherein the mass ratio of the pore-forming agent to the sol is 1:10-1:200, and the volume ratio of the tetraethyl silicate, the methyltriethoxysilane, the absolute ethyl alcohol, the deionized water and the concentrated nitric acid is 1:0.1-6.0, 10:0.3 and 0.1-1.0.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated nitric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring for 0.1-25 h at a rotating speed of 1-3000 r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask, carrying out water bath at 25-100 ℃ for 0.1-25 h, and aging for 0.1-10 days to obtain the required sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into a baking oven at 25-200 ℃ for drying for 1-5 hours, then moving into a muffle furnace, and annealing for 0.1-25 hours at 200-600 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
The invention adds organic PS to improve the transmittance, the radiation resistance, the surface hardness and the adhesive force of the acid catalysis SiO 2 film. The space configuration of PS makes the molecule easily form hydrogen bond, under the action of the hydrogen bond in the molecule, the two groups of phenol group and carboxylic ester deviate slightly, and the extinction coefficient is reduced, so that the refractive index is reduced, and the antireflection performance is more excellent. And the hydroxyl on PS molecules can attract more SiO 2 particles to be gathered together to generate condensation reaction, so that more Si-O-Si cross-linked network structures are formed, and the surface hardness and the adhesive force of the SiO 2 film are further improved. And because PS rearranges under the action of light to form 2-hydroxy benzophenone. The 2-hydroxy benzophenone absorbs energy under the irradiation of ultraviolet rays, and the carbonyl and the hydroxyl in the molecule can generate intramolecular hydrogen bonds to form a chelate ring. The absorbed energy is released through heat release, the molecular heat vibration is aggravated, the intramolecular hydrogen bond is destroyed, the chelate ring is opened, and the ultraviolet light energy is converted into heat energy to be released, so that the irradiation resistance of the film is improved. The SiO 2 film with high radiation resistance, high mechanical property and high antireflection is prepared by adopting a sol-gel method, the operation is simple, the cost is low, the preparation method belongs to a safe and effective SiO 2 antireflection film preparation method, and the preparation cost can be reduced while the film quality is ensured.
Drawings
FIG. 1 is a graph showing the transmittance of the ultra-white glass coated with the anti-reflective film and the transmittance of the ultra-white glass without the anti-reflective film in comparison with the transmittance after 5000ESHs ultraviolet irradiation, and shows that the film has good anti-reflection effect, maintains higher transmittance after 5000ESHs irradiation, and still has good anti-reflective performance.
Fig. 2 is a graph of the variation of average transmittance with irradiation time and a linear fitting curve thereof during uv irradiation of 5000ESHs of the ultra-white glass coated with an antireflection film according to the present invention.
FIG. 3 is a Scanning Electron Microscope (SEM) image of the surface of the SiO 2 film with high anti-radiation and high mechanical properties, prepared by the invention, after and before 5000ESHs ultraviolet irradiation, after adhesive force testing by the tape method, and the adhesive force of the film is tested according to the standard GB/T6379-2006. It can be seen that the scratch edge is not obviously dropped off after the adhesive tape is torn before irradiation, the adhesive force is above 0 level, the scratch edge is slightly dropped off after irradiation, and the adhesive force is still above 1 level.
FIG. 4 is a Scanning Electron Microscope (SEM) diagram of the surface of a high-irradiation-resistance high-mechanical-property high-antireflection SiO 2 film with the hardness of 5000ESHs before and after ultraviolet irradiation, wherein the surface hardness of the film is tested according to the standard GB/T33049-2016, the pencils used in the diagram are 9H and 8H, no pencil scratch is left before irradiation, the film hardness reaches 9H, a slight scratch is left after irradiation, no scratch is left on an 8H pencil, and the hardness is more than 8H.
Detailed Description
A PS modified SiO 2 film with high radiation resistance and high mechanical property and high antireflection performance and a preparation method thereof are provided, wherein the mass ratio of pore-foaming agent to sol in the SiO 2 antireflection film is 1:10-1:200, and the volume ratio of tetraethyl silicate, methyltriethoxysilane, absolute ethyl alcohol, deionized water and concentrated nitric acid is 1:0.1-6.0:10:0.3:0.1-1.0, and the film is prepared by a sol-gel method.
A PS modified SiO 2 film with high ultraviolet resistance, high mechanical property and high antireflection performance and a preparation method thereof comprise the following steps:
The SiO 2 antireflection film is prepared from absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, concentrated nitric acid, deionized water and PS by adopting a sol-gel method.
The invention is described in further detail below with reference to examples:
embodiment one:
In order to compare the modification effect of PS, firstly, an acid-catalyzed SiO 2 film without PS is prepared, and the preparation method comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, and the volume ratio of the components is 10:1:1:0.3:0.3.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the acid-catalyzed sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the antireflection SiO 2 film.
Embodiment two:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:110.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Embodiment III:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:90.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Embodiment four:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Fifth embodiment:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:2:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Example six:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:3:0.3:0.5, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 2h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Embodiment seven:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.1, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Example eight:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.6, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Example nine:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 2 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Example ten:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 4 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then transferring the glass substrate into a muffle furnace, and annealing for 1h at 400 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
Example eleven:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then moving into a muffle furnace, and annealing for 2h at 300 ℃ to obtain the PS modified high-radiation-resistance high-mechanical-property high-antireflection SiO 2 film.
Embodiment twelve:
The preparation method of the PS modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance comprises the following steps:
(1) The raw materials are absolute ethyl alcohol, tetraethyl silicate, methyltriethoxysilane, deionized water and concentrated nitric acid, wherein the volume ratio of the components is 10:1:1:0.3:0.3, and the mass ratio of PS to sol is 1:70.
(2) The preparation of the sol, namely accurately measuring according to the stoichiometric ratio of a target product, pouring concentrated hydrochloric acid, water and absolute ethyl alcohol into a pre-cleaned beaker, placing the beaker on a magnetic stirrer, stirring the beaker for 2 hours at a rotating speed of 1500r/min, adding tetraethyl silicate, methyltriethoxysilane and PS into the solution while stirring, transferring the solution into a conical flask at 60 ℃, carrying out water bath for 2 hours, cooling to room temperature, and aging for 3 days to obtain the modified acid catalytic sol.
(3) And (3) preparing the antireflection film, namely plating a film layer on clean glass, putting the plated glass substrate into an oven at 80 ℃ for drying for 1h, then moving into a muffle furnace, and annealing for 0.5h at 500 ℃ to obtain the PS modified SiO 2 film with high radiation resistance and high mechanical property.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (4)
1. A preparation method of an ultraviolet absorbent Phenyl Salicylate (PS) modified SiO 2 film with high radiation resistance, high mechanical property and high antireflection performance is characterized in that PS is used as a pore-forming agent, tetraethyl silicate (TEOS) and Methyltriethoxysilane (MTES) are used as precursors, concentrated nitric acid is used as a catalyst, absolute ethyl alcohol, TEOS, MTES, deionized water, nitric acid and PS are sequentially added into a pre-cleaned beaker, magnetic stirring is carried out at room temperature for a period of time, water bath reflux is carried out, cooling is carried out to room temperature, aging is carried out to obtain a required sol, the sol is coated on glass, the sol is dried into gel, and then organic matters in the gel are volatilized to form nano holes, thus finally the porous nano film is formed.
2. The preparation method of the PS-modified high-radiation-resistance high-mechanical-property high-antireflection SiO 2 film is characterized in that the mass ratio of a pore-forming agent to sol is 1:10-1:200, and the volume ratio of tetraethyl silicate, methyltriethoxysilane, absolute ethyl alcohol, deionized water and concentrated nitric acid is 1: (0.1-6.0) to 10:0.3: (0.1-1.0).
3. The preparation method of the PS-modified high-radiation-resistance high-mechanical-property high-antireflection SiO 2 film is characterized by sequentially adding tetraethyl silicate, methyltriethoxysilane, absolute ethyl alcohol, deionized water, concentrated nitric acid and PS into a pre-cleaned beaker according to the proportion of claim 2, stirring at the speed of 1-3000r/min for 0.1-25 h at room temperature, transferring into a conical flask, bathing in a water bath at 25-100 ℃ for 0.1-25 h, and aging for 0.1-10 days to obtain the required sol.
4. The preparation method of the PS-modified high-radiation-resistance high-mechanical-property high-antireflection SiO 2 film is characterized by coating sol on glass, drying at 25-200 ℃ for 1-5 h and then heat-treating at 200-600 ℃ for 0.1-25 h.
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