CN108623185B - Double-layer composite SiO2Preparation method of antireflection film - Google Patents
Double-layer composite SiO2Preparation method of antireflection film Download PDFInfo
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Abstract
本发明公开了一种双层复合SiO2减反射膜的制备方法，将硅源加入至无水乙醇、盐酸和水的混合液中，于室温下搅拌均匀后静置数天，得到酸催化的SiO2溶胶A；将硅源加入至无水乙醇、氨水和水的混合液中，于室温下搅拌均匀后静置数天，得到碱催化的SiO2溶胶B；将SiO2溶胶A和步骤2制得的SiO2溶胶B分别除酸和除氨，得到SiO2溶胶A1和SiO2溶胶B1；将SiO2溶胶A1和SiO2溶胶B按照质量比1∶4进行混合，将SiO2溶胶A和SiO2溶胶B1按照质量比2∶3进行混合，搅拌均匀后静置数天，分别得到复合溶胶S‑20％和S‑40％；在相对湿度环境＜50％的环境下，将经过预处理的基底浸入复合溶胶S‑40％中进行镀膜，将镀膜的基底静置数分钟，再将基底浸入复合溶胶S‑20％中进行镀膜；最后将镀有双层膜的基底置于HMDS气氛中处理即可。
The invention discloses a preparation method of a double-layer composite SiO 2 anti-reflection film. A silicon source is added to a mixed solution of absolute ethanol, hydrochloric acid and water, stirred evenly at room temperature, and then allowed to stand for several days to obtain an acid-catalyzed anti-reflection film. SiO 2 sol A; add the silicon source to the mixed solution of absolute ethanol, ammonia water and water, stir evenly at room temperature and let stand for several days to obtain alkali-catalyzed SiO 2 sol B; combine SiO 2 sol A with step 2 The obtained SiO 2 sol B is deacidified and ammonia removed, respectively, to obtain SiO 2 sol A1 and SiO 2 sol B1; the SiO 2 sol A1 and SiO 2 sol B are mixed according to the mass ratio of 1:4, and the SiO 2 sol A and SiO 2 sol A and B are mixed. The SiO 2 sol B1 is mixed according to the mass ratio of 2:3, stirred evenly and left for several days to obtain the composite sol S-20% and S-40% respectively; under the environment of relative humidity <50%, the pretreatment will be carried out. The substrate was immersed in the composite sol S-40% for coating, the coated substrate was left for several minutes, and then the substrate was immersed in the composite sol S-20% for coating; finally, the substrate coated with the double-layer film was placed in the HMDS atmosphere Just deal with it.
Description
Technical Field
The invention relates to a double-layer composite SiO2A preparation method of an antireflection film belongs to the technical field of optical films.
Background
An antireflection film is a film which is most widely used in modern optics, and utilizes interference of the film to reduce or eliminate reflected light and stray light on an optical surface so as to increase the transmittance of the film. The preparation of the antireflection film by using the sol-gel method has the advantages of simple operation, low cost, suitability for irregular surfaces, large-scale industrial production and the like. SiO prepared by basic catalyst2The antireflection film has the advantages of low refractive index and high transmittance, but has poor mechanical properties and cannot meet the requirements of practical application; SiO prepared by acid catalyst2The antireflection film has excellent mechanical properties and wear resistance, but has poor antireflection effect.
The anti-reflection film is plated on the glass cover plate in the solar cell main part, so that the reflection loss of incident light is reduced, and the actual conversion efficiency is improved. The wavelength range of solar radiation is wide, but most of energy is concentrated in the visible light to near infrared region, but the permeability of silicon in the infrared band is high, and the utilization is low, so the important point for the permeability increase of the solar cell is in the range of 400-800 nm. The antireflection film used at present is basically exposed in the atmospheric environment and needs to withstand the severe environments such as sunlight, rain, high humidity and heat. Therefore, the SiO has high transmittance in the range of 400-800nm and good weather resistance2Development of an antireflection film is necessary.
Disclosure of Invention
The invention aims to solve the technical problem of providing a double-layer composite SiO2Preparation method of antireflection film and SiO prepared by preparation method2The antireflection film has high transmittance in the visible light range and good weather resistance.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
double-layer composite SiO2The preparation method of the antireflection film comprises the following steps:
step 1, adding a silicon source into a mixed solution of absolute ethyl alcohol, hydrochloric acid and water according to a certain molar ratio, stirring uniformly at room temperature, standing for several days to obtain acid-catalyzed SiO2Sol A; wherein the SiO2The mass percentage concentration of the sol A is 3 percent;
step 3, taking the required amount of SiO prepared in the step 12Removing acid from the sol A to obtain SiO2Sol a 1; taking the required amount of SiO prepared in the step 22Removing ammonia from the sol B to obtain SiO2Sol B1;
step 4, SiO2Sol A1 and SiO2Mixing the sol B according to the mass ratio of 1:4, and mixing SiO2Sol A and SiO2Mixing the sol B1 according to the mass ratio of 2:3, uniformly stirring, standing for several days to respectively obtain composite sol S-20% and composite sol S-40%;
step 5, immersing the pretreated substrate into the composite sol S-40% in the step 4 in an environment with the relative humidity less than 50%, and coating a film on the substrate by adopting a dip-coating method, wherein the coating speed is 80 mm/min; standing the coated substrate for several minutes after pulling, immersing the substrate into the S-20% of the composite sol obtained in the step (4), and coating at a pulling speed of 40 mm/min;
step 6, the substrate plated with the double-layer film in the step 5 is placed in HMDS atmosphere for treatment for a period of time to obtain the required double-layer composite SiO2An antireflection film.
In step 1 and step 2, the silicon source is tetraethoxysilane.
Wherein, in the step 1, the mixing molar ratio of the silicon source, the absolute ethyl alcohol, the hydrochloric acid and the water is 1: 40: 0.04: 4.
Wherein in the step 1, the mass percentage concentration of the hydrochloric acid is 36-38%.
In the step 2, the mixing molar ratio of the silicon source, the absolute ethyl alcohol, the ammonia water and the water is 1: 37.6: 0.17: 3.25.
In the step 2, the mass percentage concentration of the ammonia water is 25-28%.
In the step 5, the substrate is any one of a silicon wafer, a K9 glass substrate, fused quartz or common glass.
In the step 5, the pretreatment of the substrate refers to that the substrate is put into washing liquor to be fully washed, then is fully cleaned by absolute ethyl alcohol and deionized water through ultrasonic waves respectively, and then is dried by nitrogen.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
SiO prepared by the preparation method of the invention2The antireflection film has the advantages of low refractive index and high transmittance, and also has good mechanical property, wear resistance and weather resistance; the average transmittance of the film in a spectral range of 400-800nm is more than 99.4%, and the transmittance of the film does not change after 72 hours of experiments (GB-T2423.3-2006) in a constant humid and hot environment, so that the broadband antireflection film can be used for a long time in complex climatic environments such as high temperature and high humidity and has good weather resistance.
Drawings
FIG. 1 is SiO2In a transmission electron microscope image of the sol A, silicon dioxide in the colloid is in a chain shape;
FIG. 2 is a transmission electron micrograph of the composite sol S-20% in which silica particles are connected to each other;
FIG. 3 is a transmission electron micrograph of the composite sol S-40% showing very close interconnection of silica particles;
FIG. 4 is SiO2The colloidal particles are in a monodisperse state in a transmission electron microscope image of the sol B;
FIG. 5 is a scanning electron micrograph of the composite sol S-20%, wherein the particles are connected with each other and have a plurality of pores;
FIG. 6 is a scanning electron microscope image of S-40% composite sol, with tightly bonded particles and rich pores;
FIG. 7 shows a double-layer composite SiO prepared by the present invention2In a scanning electron microscope image of the front surface of the antireflection film, particles of an upper layer film are connected with each other, and a large number of pores are formed among the particles;
FIG. 8 shows a double-layer composite SiO prepared by the present invention2The scanning electron microscope image of the cross section of the antireflection film shows that the upper layer film is 115nm and the lower layer film is 104 nm;
FIG. 9 is a refractive index curve of composite sol S-20% with a refractive index of 1.180;
FIG. 10 is a refractive index profile of the composite sol S-40% with a refractive index of 1.364;
FIG. 11 shows a double-layer composite SiO prepared by the present invention2The transmittance curve of the antireflection film and the transmittance curves after the HMDS treatment and the damp-heat experiment show that the transmittance is slightly reduced after the HMDS treatment, but the humidity resistance is greatly improved;
FIG. 12 shows a double-layer composite SiO prepared by the present invention2The transmittance curves of the antireflection film and a K9 substrate show that the average transmittance of the antireflection film in a visible light region reaches over 99.40 percent.
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
The invention relates to a double-layer composite SiO2The preparation method of the antireflection film specifically comprises the following steps:
step 1, mixing tetraethoxysilane, absolute ethyl alcohol, hydrochloric acid and water according to the molar ratio of 1: 40: 0.04: 4, stirring for 10 hours at room temperature, standing for 7 days to obtain acid-catalyzed SiO2Sol A; wherein, SiO2Quality of Sol AThe percentage concentration of the amount is 3 percent; in the reaction system, hydrochloric acid is used as an acid catalyst, ethyl orthosilicate is used as a silicon source, and absolute ethyl alcohol is used as a solvent;
step 3, taking the required amount of SiO prepared in the step 12Removing acid from the sol A by adopting a condensation reflux method to obtain SiO2Sol a 1; taking the required amount of SiO prepared in the step 22Removing ammonia from the sol B by adopting a condensation reflux method to obtain SiO2Sol B1;
step 4, SiO2Sol A1 and SiO2Mixing the sol B according to the mass ratio of 1:4, and mixing SiO2Sol A and SiO2Mixing the sol B1 according to the mass ratio of 2:3, uniformly stirring and standing for several days to respectively obtain composite sol S-20% and composite sol S-40%; the composite sol is formed by mixing acid glue and alkali glue;
step 5, immersing the pretreated substrate into the composite sol S-40% in the step 4 in an environment with the relative humidity less than 50%, and coating a film on the substrate by adopting a dip-coating method, wherein the coating speed is 80 mm/min; standing the coated substrate for 5 minutes after pulling, then soaking the substrate into the S-20% of the composite sol obtained in the step (4), and coating at a pulling speed of 40 mm/min; the pretreatment of the substrate means that deionized water and an electronic industry cleaning agent are firstly used for cleaning the surface of the glass until no dirt is left on the surface of the glass; secondly, the glass which is washed by water is put into absolute ethyl alcohol and deionized water, and the double-layer composite SiO of the invention can be obtained after ultrasonic cleaning for 30min respectively2An antireflection film.
Placing the substrate plated with the double-layer film in the step 5 in an HMDS (hexamethyldisilazane) atmosphere for treating for 24 hours to obtain the HMDS-treated double-layer composite SiO2An antireflection film.
The method of the inventionIn the step 1, tetraethoxysilane is used as a precursor, and a linear polycondensate with low porosity is formed under the action of an acid catalyst; step 2, using ethyl orthosilicate as a precursor, and obtaining dispersed SiO under the action of an alkali catalyst2Sol particles.
The transmission electron microscope image of the composite colloid shows obvious difference compared with the two acidic or alkaline colloids. In the S-20%, the ammonia water from colloid B can continue to act as a catalyst in the composite colloid solution, and the chain from the acidic colloid and the particles from the basic colloid undergo a polymerization reaction. The particles are supported by chains, so that the film has a plurality of micropores, thereby having a large porosity, and the refractive index of the film is further reduced to 1.180. As can be seen from the transmission electron microscope image 3, the composite colloid S-40% colloidal particles have a three-dimensional network structure. After the colloid A and the colloid B1 are mixed, under the action of an acid catalyst, the nano chain and the residual methoxyl on the surface of the nano particle are subjected to hydrolysis reaction. The alkaline particles are doped so that the refractive index of the alkaline particles is lower than that of the pure acid gel. The films prepared from S-20% and S-40% colloids have high porosity, but the mechanical properties of the films are greatly improved because the particles are connected by chain-shaped tissues. And after the compact and porous structure is subjected to hydrophobic treatment, a plurality of hydrophobic groups are distributed on the surface of the compact and porous structure, so that the weather resistance of the compact and porous structure in a severe environment is ensured.
The double-layer broadband antireflection film prepared by the invention has excellent mechanical property and wear resistance, and has the advantages of high hardness, high transmittance and good weather resistance; the bottom layer is a reticular silicon dioxide structure with large refractive index and high strength, and the upper layer is a reticular silicon dioxide film with smaller refractive index; the double-layer antireflection film has high transmittance, strong wear resistance, strong adhesive force and good hydrophobicity, and water molecules can not enter pores of the film. The double-layer broadband antireflection film simultaneously has the advantages of long antireflection bandwidth, high average transmittance and peak transmittance, stable mechanical property, resistance to damp and heat environments, simple and low preparation process, suitability for large-area film coating and the like, and meets the requirement of industrial production. The double-layer film can increase the transmission of the broadband and meet the requirement on mechanical performance.
The average transmittance of the antireflection film in the spectral range of 400-800nm is more than 99.40%, which is increased by more than 7% compared with that of original glass without a coating, and the difference of the average transmittance of the samples is only 0.1% with 5 samples prepared under the same implementation conditions. The color of the prepared interference film on the glass surface can be light blue, orange yellow and blue purple according to different film thicknesses, so that the solar light transmittance and the energy utilization rate of a solar thermal collector, a photovoltaic module and the like are effectively improved.
The transmittance of the antireflection film provided by the invention is not changed after 72 hours of experiments (GB-T2423.3-2006) in a constant damp and hot environment. The pencil hardness is more than 3H, and the plating layer does not fall off in the scratching method adhesion test (5B level). The broadband antireflection film can be used for a long time in complex climatic environments such as high temperature, high humidity and the like, and has good weather resistance. The antireflection film product prepared by the invention has the characteristics of no corrosion pretreatment on the substrate, low manufacturing cost, simple process, scratch resistance and good weather resistance, and is suitable for industrial production and application.
The invention adopts an acid-base composite method, uses base catalysis and removes acid catalyst to prepare the low-refraction upper layer film with excellent mechanical property, solves the problem that the low-refraction upper layer film with good mechanical property is difficult to prepare in the preparation of the current double-layer film, and simultaneously optimizes the thickness of the film layer by controlling the pulling speed, thereby providing a new idea for the preparation of the double-layer antireflection film.
Claims (8)
1. Double-layer composite SiO2The preparation method of the antireflection film is characterized by comprising the following steps of:
step 1, adding a silicon source into a mixed solution of absolute ethyl alcohol, hydrochloric acid and water according to a certain molar ratio, stirring uniformly at room temperature, standing for several days to obtain acid-catalyzed SiO2Sol A; wherein the SiO2 The mass percentage concentration of the sol A is 3 percent;
step 2, adding a silicon source into a mixed solution of absolute ethyl alcohol, ammonia water and water according to a certain molar ratio, stirring uniformly at room temperature, standing for several days to obtain base-catalyzed SiO2Sol B;wherein the SiO2 The mass percentage concentration of the sol B is 3 percent;
step 3, taking the required amount of SiO prepared in the step 12Removing acid from the sol A to obtain SiO2Sol a 1; taking the required amount of SiO prepared in the step 22Removing ammonia from the sol B to obtain SiO2Sol B1;
step 4, SiO2Sol A1 and SiO2Mixing the sol B according to the mass ratio of 1:4, and mixing SiO2Sol A and SiO2Mixing the sol B1 according to the mass ratio of 2:3, uniformly stirring, standing for several days to respectively obtain composite sol S-20% and composite sol S-40%;
step 5, immersing the pretreated substrate into the composite sol S-40% in the step 4 in an environment with the relative humidity less than 50%, and coating a film on the substrate by adopting a dip-coating method, wherein the coating speed is 80 mm/min; standing the coated substrate for several minutes after pulling, immersing the substrate into the S-20% of the composite sol obtained in the step (4), and coating at a pulling speed of 40 mm/min;
step 6, the substrate plated with the double-layer film in the step 5 is placed in HMDS atmosphere for treatment for a period of time to obtain the required double-layer composite SiO2An antireflection film; in S-20%, ammonia water from colloid B can continue to act as a catalyst in the composite colloid solution, chain-like substances from the acidic colloid and particles from the basic colloid undergo a polymerization reaction, and the particles are supported by chains, so that the film has a plurality of micropores, thereby having a large porosity, and further reducing the refractive index to 1.180.
2. The double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 1 and the step 2, the silicon source is tetraethoxysilane.
3. The double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 1, the mixing molar ratio of the silicon source, the absolute ethyl alcohol, the hydrochloric acid and the water is 1: 40: 0.04: 4.
4. the double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 1, the mass percentage concentration of the hydrochloric acid is 36-38%.
5. The double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 2, the mixing molar ratio of the silicon source, the absolute ethyl alcohol, the ammonia water and the water is 1: 37.6: 0.17: 3.25.
6. the double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 2, the mass percentage concentration of the ammonia water is 25-28%.
7. The double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 5, the substrate is any one of a silicon wafer, a K9 glass substrate, fused quartz or common glass.
8. The double-layer composite SiO of claim 12The preparation method of the antireflection film is characterized by comprising the following steps: in the step 5, the pretreatment of the substrate refers to that the substrate is put into washing liquor to be fully washed, then is fully cleaned by absolute ethyl alcohol and deionized water through ultrasonic waves respectively, and then is dried by nitrogen.
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| CN109439031A (en) * | 2018-10-16 | 2019-03-08 | 江苏四季森林纳米科技有限公司 | Self-cleaning Essence, preparation method, self-cleaning coat, application and structural body |
| CN109665720B (en) * | 2018-12-21 | 2022-05-03 | 中国工程物理研究院激光聚变研究中心 | SiO with ultralow refractive index2Preparation method of antireflection film |
| CN109467317A (en) * | 2019-01-04 | 2019-03-15 | 中国工程物理研究院激光聚变研究中心 | A kind of surface layer has the antireflecting silicon dioxide film and preparation method thereof of meso-hole structure with hole sealing structure internal layer |
| CN110408070B (en) * | 2019-07-31 | 2022-03-01 | 中国工程物理研究院激光聚变研究中心 | High-threshold-value scratch-resistant high-transmittance fundamental-frequency laser film and preparation method thereof |
| CN114105488A (en) * | 2020-08-26 | 2022-03-01 | 上海西源新能源技术有限公司 | Neutral color double-layer anti-reflection coating, glass with the coating and preparation method thereof |
| CN113462206B (en) * | 2021-07-07 | 2022-10-28 | 凯盛晶华玻璃有限公司 | Photovoltaic glass antireflection film coating composition and preparation method thereof |
| CN113683311A (en) * | 2021-07-13 | 2021-11-23 | 凯盛晶华玻璃有限公司 | Photovoltaic glass with antireflection film |
| CN113387596A (en) * | 2021-08-02 | 2021-09-14 | 凯盛晶华玻璃有限公司 | Wear-resistant super-hydrophobic photovoltaic glass and preparation method thereof |
| CN114089455B (en) * | 2021-12-03 | 2022-10-28 | 天津大学 | Preparation method of near-ultraviolet region distributed Bragg reflector |
| CN115555235B (en) * | 2022-10-28 | 2023-07-18 | 西南科技大学 | A kind of preparation method of silicon dioxide anti-reflection film |
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| CN103408229A (en) * | 2013-07-31 | 2013-11-27 | 同济大学 | Method for preparing silica broadband antireflection film by adjusting porosity |
| CN105776883A (en) * | 2014-12-24 | 2016-07-20 | 北京有色金属研究总院 | Method for preparing antireflection coating by silica particles film-formation |
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