Mesoporous silica microsphere solution and anti-reflection composite coating liquid
By using ethyl cellulose and hexadecyltrimethylammonium bromide as dual template agents to prepare mesoporous silica microsphere solutions, combined with silane coupling agents and acrylic resins, the problems of low transmittance and poor coating stability of photovoltaic glass were solved, and an antireflective coating with high transmittance and good adhesion was achieved, which is suitable for the industrial production of photovoltaic glass.
Patent Information
- Application Number
- CN202510808501.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2025-11-07
AI Technical Summary
Existing photovoltaic glass has low transmittance, and traditional antireflective coatings have defects in film uniformity, adhesion and long-term stability. Furthermore, the particle size distribution, porosity and film thickness are difficult to control precisely, resulting in unsatisfactory optical performance, especially poor performance consistency over a wide spectral range.
Ethyl cellulose and hexadecyltrimethylammonium bromide were used as dual template agents to prepare a mesoporous silica microsphere solution, forming a hierarchical pore structure. Combined with silane coupling agent and acrylic resin, an antireflection composite coating solution was prepared, and a uniform and strongly adherent coating was formed on photovoltaic glass by spraying or roller coating.
It significantly improves the optical transmittance of photovoltaic glass, enhances the adhesion and weather resistance of the coating, reduces production costs, and is suitable for large-scale industrial applications.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of photovoltaic glass coating, and particularly relates to a mesoporous silica microsphere solution and an antireflection composite coating solution. BACKGROUND
[0002] At present, the solar photovoltaic industry is facing huge development opportunities. Crystalline silicon cells account for the mainstream of photovoltaic power generation, and photovoltaic glass as a solar cell cover material is one of the important component materials. Photovoltaic cells are priced according to power generation, and the level of photoelectric conversion efficiency is directly related to the price, so the power generation efficiency of solar cells has always been one of the focuses of the industry.
[0003] Under the current technical conditions, it is difficult to simply increase the power of the cell through the improvement of the processing and packaging technology of the silicon wafer, and the increase of the transmittance of the photovoltaic glass can increase the photoelectric conversion energy and improve the power generation efficiency, which is the focus and important development direction of the industry at present. Developing an antireflection super-white embossed glass with high transmittance in the response spectrum range of solar cells can improve the power generation efficiency of solar cells to the same extent, which has very good economic prospects. The popularization and application of the antireflection solution for solar photovoltaic use has a positive effect on the improvement of the efficiency of solar cells, the reduction of the cost, the improvement of the competitiveness of solar cell power generation, and the shortening of the cost recovery period of grid-connected power generation. SUMMARY
[0004] The purpose of the present application is to provide a mesoporous silica microsphere solution and an antireflection composite coating solution.
[0005] The conventional glass or optical material has low transmittance at the air-glass interface, resulting in light energy loss and affecting the light transmission efficiency and display effect of the optical device. The existing antireflection coating has defects in film uniformity, adhesion and long-term stability, and is easy to fail due to environmental influences (such as humidity, temperature change, etc.). In the existing antireflection solution material, the particle size distribution, porosity and film thickness are difficult to accurately control, resulting in unsatisfactory optical performance, especially poor performance consistency in a wide spectral range. Some traditional coating preparation methods require expensive equipment and high-precision control, which limits the widespread application in industrialization.
[0006] In order to achieve the above purpose, the first aspect of the present application provides a mesoporous silica microsphere solution, wherein the preparation raw materials of the solution include: a silicon source, a double template agent, an alkaline catalyst, an organic solvent and water.
[0007] The double template agent includes ethyl cellulose and cetyltrimethylammonium bromide.
[0008] The present application adopts ethyl cellulose and cetyltrimethylammonium bromide as double templates to prepare a mesoporous silica microsphere solution, wherein the cetyltrimethylammonium bromide provides a surfactant template effect to form a regular mesoporous structure; the ethyl cellulose acts as a pore-forming agent to further regulate the pore size and pore distribution, and can enhance the stability of the mesoporous structure. The synergistic effect of the double templates helps to precisely control the pore structure in the micro and meso scales, and improve the specific surface area and pore volume of the mesoporous silica.
[0009] The second aspect of the present application provides an anti-reflection composite coating solution, wherein the preparation raw materials of the anti-reflection composite coating solution comprise the mesoporous silica microsphere solution of the first aspect, a silane coupling agent, an acrylic resin, an organic solvent and water.
[0010] The third aspect of the present application provides an anti-reflection coating prepared from the anti-reflection composite coating solution of the second aspect.
[0011] The fourth aspect of the present application provides the application of the anti-reflection coating of the third aspect in photovoltaic glass.
[0012] Through the above technical solution, the present application has the following beneficial technical effects:
[0013] (1) The present application forms a gradient refractive index structure by utilizing the low refractive index and controllable pore size design of the hollow silica microspheres, maximally reduces the light reflection loss, and improves the optical transmittance of the film layer.
[0014] (2) The anti-reflection coating prepared by introducing specific double templates can be uniform, has strong adhesion and can resist complex environments (such as humidity, ultraviolet light and temperature change).
[0015] (3) The present application is based on cheap and environmentally friendly raw materials (such as ethyl cellulose and common silicon sources), combined with a simple and easy-to-control preparation process, reduces the production cost, and is suitable for large-scale industrial application. BRIEF DESCRIPTION OF DRAWINGS
[0016] Figure 1 is the spectrum scanning diagram of the anti-reflection composite coating solution prepared in Example 1 of the present application after forming a coating layer on a glass substrate.
[0017] Figure 2 is the spectrum scanning diagram of the anti-reflection composite coating solution prepared in Example 2 of the present application after forming a coating layer on a glass substrate.
[0018] Figure 3 is the spectrum scanning diagram of the anti-reflection composite coating solution prepared in Example 3 of the present application after forming a coating layer on a glass substrate.
[0019] Figure 4is a spectrum scanning diagram of a coating layer formed by a prepared anti-reflection composite coating solution of Example 4 of the present application on a glass substrate.
[0020] Figure 5 is a spectrum scanning diagram of a coating layer formed by a prepared anti-reflection composite coating solution of Example 5 of the present application on a glass substrate.
[0021] Figure 6 is a spectrum scanning diagram of a coating layer formed by a prepared anti-reflection composite coating solution of Example 6 of the present application on a glass substrate.
[0022] Figure 7 is a spectrum scanning diagram of a coating layer formed by a prepared anti-reflection composite coating solution of Comparative Example 1 of the present application on a glass substrate.
[0023] Figure 8 is a spectrum scanning diagram of a coating layer formed by a prepared anti-reflection composite coating solution of Comparative Example 2 of the present application on a glass substrate. DETAILED DESCRIPTION
[0024] The endpoints of the ranges and any values disclosed herein are not limited to the precise values stated. The endpoints of the ranges and any values are understood to be approximate values. The exact numerical values of the endpoints of the ranges and any values are understood to be approximations. It is intended to include all values substantially equivalent to the recited values within the range of values and any values.
[0025] The first aspect of the present application provides a mesoporous silica microsphere solution, wherein the raw materials for preparing the solution include a silicon source, a double template agent, an alkaline catalyst, an organic solvent and water.
[0026] The double template agent includes ethyl cellulose and cetyltrimethylammonium bromide (CTAB).
[0027] In the present application, CTAB, as a cationic surfactant, generates small-sized mesopores (2-4 nm) through micellar self-assembly, endows the material with high specific surface area and ordered pore structure, and enhances the light regulation ability; ethyl cellulose, as a macromolecular polymer template, forms large-aperture mesopores or macro-pores (tens to hundreds of nanometers) through physical entanglement or phase separation, and provides a low-refractive skeleton. In the present application, the combination of the double template realizes a hierarchical pore structure (mesopore-macropore composite), and takes into account both high specific surface area and light transmission optimization, significantly reduces the refractive index of the film, and improves the transmission performance. CTAB is a cationic surfactant, the hydrophilic head group of which interacts with inorganic precursors (such as SiO2 sol), and the hydrophobic tail chain forms a micellar core. The hydrophobic chain of ethyl cellulose is adsorbed on the surface of the CTAB micelles, forming a hierarchical pore structure and realizing pore interconnection.
[0028] In the present application, ethyl cellulose is used to replace high-cost or environmentally unfriendly templates, reducing production costs and improving environmental protection. The green process and environmentally friendly characteristics of the template meet the current direction of sustainable development of the materials industry.
[0029] In addition, ethyl cellulose can enhance mechanical stability. The flexible long chains of ethyl cellulose play a "skeleton" role in the sol-gel process, inhibiting the excessive aggregation of CTAB template micelles, reducing the risk of structure collapse during drying or calcination, and obtaining high-integrity spherical micrometer-sized particles. The viscosity regulation of ethyl cellulose can slow down the hydrolysis and polycondensation rate, promote uniform coating of the silica precursor, form well-dispersed and uniform-sized microspheres, and facilitate uniformity of the coating solution.
[0030] In some embodiments of the present application, the mass ratio of ethyl cellulose to cetyltrimethylammonium bromide in the double template is 1-1.5:1, preferably 1.3:1. In the present application, a mass ratio that is too high leads to a decrease in mesopores, and a mass ratio that is too low inhibits macroporous structures. By adjusting the mass ratio of the two, the pore size can be precisely controlled from 10 nm to 200 nm. Within this specific mass ratio range, the porosity can be adjusted to significantly reduce the refractive index of the film, and the transmittance effect is best.
[0031] In some embodiments of the present application, the mass percentage of the double template is 1.25-2.6%, preferably 1.4%.
[0032] In some embodiments of the present application, the silicon source is selected from at least one of tetraethoxysilane (TEOS), trimethylethoxysilane (TMEO), and ethyltriethoxysilane.
[0033] In some embodiments of the present application, the mass percentage of the silicon source is 6-11.5%, preferably 6-8%, and further preferably 7%.
[0034] In some embodiments of the present application, the basic catalyst is selected from at least one of aqueous ammonia, sodium hydroxide, and tetramethylammonium hydroxide.
[0035] In some embodiments of the present application, the concentration of the aqueous ammonia is 25%.
[0036] In some embodiments of the present application, the mass percentage of the basic catalyst is 2.8-7%, preferably 3-4%.
[0037] In some embodiments of the present application, the organic solvent is selected from at least one of anhydrous ethanol, methanol, and isopropanol.
[0038] In some embodiments of the present application, the mass percentage of the organic solvent is 72.85-78%, preferably 74.1-76.6%, and further preferably 75.75%.
[0039] In some embodiments of the present application, the mass percentage of the water is 8.4-12%, preferably 11.6%.
[0040] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 0.8%, TEOS 6%, CTAB 0.6%, anhydrous ethanol 78%, deionized water 11.6%, ammonia water (25%) 3%.
[0041] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 0.75%, TEOS 7%, CTAB 0.5%, anhydrous ethanol 75.75%, deionized water 12%, ammonia water (25%) 4%.
[0042] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 1.3%, TEOS 8%, CTAB 1.3%, anhydrous ethanol 78%, deionized water 8.4%, ammonia water (25%) 3%.
[0043] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 0.8%, TEOS 6%, CTAB 1.6%, anhydrous ethanol 76.6%, deionized water 12%, ammonia water (25%) 3%.
[0044] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 0.77%, TEOS 11.5%, CTAB 0.54%, anhydrous ethanol 72.85%, deionized water 11.54%, ammonia water (25%) 2.8%.
[0045] In some embodiments of the present application, the raw materials for preparing the solution include, in mass percentage: ethyl cellulose 0.8%, TEOS 5.8%, CTAB 0.6%, anhydrous ethanol 74.1%, deionized water 11.7%, ammonia water (25%) 7%.
[0046] In the present application, the mesoporous silica microsphere solution can be prepared by the following preparation method:
[0047] (1) mixing ethyl cellulose with an organic solvent to obtain an ethyl cellulose solution;
[0048] (2) sequentially adding CTAB, a silicon source and water into the ethyl cellulose solution and mixing uniformly;
[0049] (3) Add base to adjust the solution to alkaline (pH = about 10), stir and react at room temperature, and reserve after reflux.
[0050] The ethyl cellulose also has a certain dispersion effect in the preparation process, reduces the agglomeration of silica particles, and improves the stability of the sol. This is crucial for the uniformity and coating performance of the subsequent antireflection composite coating solution.
[0051] The second aspect of the present application provides an antireflection composite coating solution, wherein the preparation raw materials of the antireflection composite coating solution comprise: the mesoporous silica microsphere solution of the first aspect, a silane coupling agent, an acrylic resin, an organic solvent, and water.
[0052] The film-forming properties of the ethyl cellulose can improve the spreading of the coating solution on the substrate (such as glass and photovoltaic panels), and reduce the generation of cracks. The silicon hydroxyl (-Si-OH) of the CTAB template residue can enhance the chemical bonding with the substrate and improve the durability of the film layer.
[0053] The present application uses mesoporous silica microspheres and organic resins to compound, which significantly enhances the mechanical properties, flexibility and adhesion of the subsequent coating layer, improves the wear resistance and scratch resistance, and is suitable for outdoor photovoltaic environment.
[0054] In some embodiments of the present application, the mass percentage content of the mesoporous silica microsphere solution is 35-40%, preferably 36%.
[0055] In some embodiments of the present application, the silane coupling agent is selected from at least one of γ-methacryloxypropyltrimethoxysilane (KH570), γ-aminopropyltriethoxysilane (KH550), and γ-(2,3-epoxypropoxy) propyltrimethoxysilane (KH560).
[0056] In some embodiments of the present application, the mass percentage content of the silane coupling agent is 0.15-0.25%, preferably 0.2%.
[0057] In some embodiments of the present application, the acrylic resin is water-based acrylic resin. For example, Jili AC-749, AC-779, etc.
[0058] In some embodiments of the present application, the mass percentage content of the acrylic resin is 2.5-4%, preferably 3.5%.
[0059] In some embodiments of the present application, the organic solvent is selected from at least one of anhydrous ethanol, methanol, and isopropanol.
[0060] In some embodiments of the present application, the mass percentage content of the organic solvent is 53-58%, preferably 57%.
[0061] In some embodiments of the present application, the water content is 2.75-4.3%, preferably 3.35%.
[0062] In some embodiments of the present application, the preparation raw materials of the antireflection composite plating solution include, in percentage by mass: mesoporous silica microsphere solution 35%, KH570 0.2%, acrylic resin 2.5%, anhydrous ethanol 58%, and deionized water 4.3%.
[0063] In some embodiments of the present application, the preparation raw materials of the antireflection composite plating solution include, in percentage by mass: mesoporous silica microsphere solution 40%, KH570 0.15%, acrylic resin 3.5%, anhydrous ethanol 53%, and deionized water 3.35%.
[0064] In some embodiments of the present application, the preparation raw materials of the antireflection composite plating solution include, in percentage by mass: mesoporous silica microsphere solution 36%, KH570 0.25%, acrylic resin 4%, anhydrous ethanol 57%, and deionized water 2.75%.
[0065] In the present application, the antireflection composite plating solution can be prepared by the following method:
[0066] (1) Add mesoporous silica microsphere solution into organic solvent (ultrasonic for 30 minutes), then add silane coupling agent and water, and stir at room temperature to promote silanization of SiO2 particle surface;
[0067] (2) Add acrylic resin and stir until uniform to obtain the antireflection composite plating solution.
[0068] The third aspect of the present application provides an antireflection coating prepared from the antireflection composite plating solution of the second aspect.
[0069] The antireflection coating of the present application can be prepared by the following method:
[0070] (1) Substrate treatment: clean the substrate surface to ensure no oil stains and dust (use ultrasonic cleaning, isopropanol wiping or ultraviolet ozone treatment);
[0071] (2) Coating process: uniformly coat the antireflection composite plating solution on the substrate surface by spraying, rolling or dipping method;
[0072] (3) High temperature preheating: preheating temperature is 150-250℃, and the duration is 3-5 minutes (the specific temperature is determined according to the substrate thickness and equipment;
[0073] (4) High temperature treatment: heating the substrate (close to the softening point of the substrate, for example, glass is 650-700℃), ensuring that the internal part of the substrate reaches a uniform temperature, heating time is about 3-5 minutes, and the heating time of thick substrate needs to be extended.
[0074] In the high temperature treatment process, the ethyl cellulose can be completely removed without residue, ensuring the purity of the pore structure.
[0075] In the present application, the formed organic-inorganic composite coating can enhance the flexibility and weather resistance of the film layer, and the transmittance reaches ≥97%, and the pencil hardness ≥2H.
[0076] The fourth aspect of the present application provides the use of the anti-reflection coating according to the third aspect in photovoltaic glass.
[0077] The present application will be described in detail below through examples.
[0078] In the following examples and comparative examples, the specific conditions not specified are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be obtained by market purchase.
[0079] Material source:
[0080] Acrylic resin: Jili AC-749.
[0081] Example 1
[0082] This example is used to illustrate the preparation of mesoporous silica microsphere solution and anti-reflection composite coating solution.
[0083] I. Preparation of mesoporous silica microsphere solution
[0084] Formulation: ethyl cellulose 0.8%, TEOS 6%, CTAB 0.6%, anhydrous ethanol 78%, deionized water 11.6%, ammonia water (25%) 3%.
[0085] Preparation steps:
[0086] (1) Dissolve ethyl cellulose in anhydrous ethanol, stir at room temperature for 30 minutes until completely dissolved;
[0087] (2) Add CTAB, TEOS and deionized water in sequence, stir for 20 minutes to make them uniformly mixed;
[0088] (3) Slowly add ammonia water to pH=10, continue to stir for 4 hours, react at room temperature, and reserve after reflux.
[0089] II. Preparation of anti-reflection composite coating solution
[0090] Formula: Mesoporous silica microspheres solution (obtained in the previous step) 35%, KH570 0.2%, acrylic resin 2.5%, anhydrous ethanol 58%, deionized water 4.3%.
[0091] Preparation steps:
[0092] (1) Add mesoporous silica microspheres solution to anhydrous ethanol (ultrasonic for 30 minutes), add KH570 and water, stir at room temperature for 1 hour;
[0093] (2) Add acrylic resin and stir for 30 minutes to form a uniform plating solution.
[0094] Example 2
[0095] This example is used to illustrate the preparation of mesoporous silica microspheres solution and antireflection composite plating solution.
[0096] I. Preparation of mesoporous silica microspheres solution
[0097] Formula: Ethyl cellulose 0.75%, TEOS 7%, CTAB 0.5%, anhydrous ethanol 75.75%, deionized water 12%, ammonia water (25%) 4%.
[0098] Preparation steps:
[0099] (1) Dissolve ethyl cellulose in anhydrous ethanol, stir at room temperature for 30 minutes until completely dissolved;
[0100] (2) Add CTAB, TEOS and deionized water in sequence, stir for 30 minutes to mix evenly;
[0101] (3) Slowly add ammonia water to pH = 10, continue to stir for 3 hours, react at room temperature, and reserve after reflux.
[0102] II. Preparation of antireflection composite plating solution
[0103] Formula: Mesoporous silica microspheres solution (obtained in the previous step) 40%, KH570 0.15%, acrylic resin 3.5%, anhydrous ethanol 53%, deionized water 3.35%.
[0104] The preparation steps are the same as in Example 1.
[0105] Example 3
[0106] This example is used to illustrate the preparation of mesoporous silica microspheres solution and antireflection composite plating solution.
[0107] I. Preparation of mesoporous silica microspheres solution formula
[0108] Formulation: ethyl cellulose 1.3%, TEOS 8%, CTAB 1.3%, anhydrous ethanol 78%, deionized water 8.4%, ammonia water (25%) 3%.
[0109] Preparation steps:
[0110] (1) Dissolve ethyl cellulose in anhydrous ethanol, stir at room temperature for 30 minutes until completely dissolved;
[0111] (2) Add CTAB, TEOS and deionized water in sequence, stir for 30 minutes to mix evenly;
[0112] (3) Slowly add ammonia water to pH = 10, continue stirring for 5 hours, react at room temperature, and reserve after reflux.
[0113] II. Preparation of antireflection composite coating solution
[0114] Formulation: mesoporous silica microsphere solution (obtained in the previous step) 36%, KH570 0.25%, acrylic resin 4%, anhydrous ethanol 57%, deionized water 2.75%.
[0115] The preparation steps are the same as in Example 1.
[0116] Example 4
[0117] This example is used to illustrate the preparation of mesoporous silica microsphere solution and antireflection composite coating solution.
[0118] I. Preparation of mesoporous silica microsphere solution
[0119] Formulation: ethyl cellulose 0.8%, TEOS 6%, CTAB 1.6%, anhydrous ethanol 76.6%, deionized water 12%, ammonia water (25%) 3%.
[0120] Preparation steps:
[0121] (1) Dissolve ethyl cellulose in anhydrous ethanol, stir at room temperature for 30 minutes until completely dissolved;
[0122] (2) Add CTAB, TEOS and deionized water in sequence, stir for 30 minutes to mix evenly;
[0123] (3) Slowly add ammonia water to pH = 10, continue stirring for 5 hours, react at room temperature, and reserve after reflux.
[0124] II. Preparation of antireflection composite coating solution
[0125] Formulation: mesoporous silica microsphere solution (obtained in the previous step) 36%, KH570 0.25%, acrylic resin 4%, anhydrous ethanol 57%, deionized water 2.75%.
[0126] The preparation procedure is the same as that in Example 1.
[0127] Example 5
[0128] This example is used to illustrate the preparation of a mesoporous silica microsphere solution and a transmittance-increasing composite plating solution.
[0129] 1. Preparation formula of mesoporous silica microsphere solution
[0130] Formula: ethyl cellulose 0.77%, TEOS 11.5%, CTAB 0.54%, anhydrous ethanol 72.85%, deionized water 11.54%, ammonia water (25%) 2.8%.
[0131] Preparation procedure:
[0132] (1) Dissolve ethyl cellulose in anhydrous ethanol, and stir at room temperature for 30 minutes until complete dissolution;
[0133] (2) Add CTAB, TEOS and deionized water in sequence, and stir for 30 minutes until they are uniformly mixed;
[0134] (3) Slowly add ammonia water to pH = 10, continuously stir for 5 hours, and react at room temperature, and reserve after reflux.
[0135] II. Preparation of transmittance-increasing composite plating solution
[0136] Formula: mesoporous silica microsphere solution (obtained in the previous step) 36%, KH570 0.25%, acrylic resin 4%, anhydrous ethanol 57%, deionized water 2.75%.
[0137] The preparation procedure is the same as that in Example 1.
[0138] Example 6
[0139] This example is used to illustrate the preparation of a mesoporous silica microsphere solution and a transmittance-increasing composite plating solution.
[0140] I. Preparation formula of mesoporous silica microsphere solution
[0141] Formula: ethyl cellulose 0.8%, TEOS 5.8%, CTAB 0.6%, anhydrous ethanol 74.1%, deionized water 11.7%, ammonia water (25%) 7%.
[0142] Preparation procedure:
[0143] (1) Dissolve ethyl cellulose in anhydrous ethanol, and stir at room temperature for 30 minutes until complete dissolution;
[0144] (2) Add CTAB, TEOS and deionized water in sequence, and stir for 30 minutes until they are uniformly mixed;
[0145] (3) Slowly add ammonia water to pH = 10, continue stirring for 5 hours, room temperature reaction, after reflux standby.
[0146] II. Preparation of the antireflection composite coating solution
[0147] Formulation: Mesoporous silica microsphere solution (obtained in the previous step) 36%, KH570 0.25%, acrylic resin 4%, anhydrous ethanol 57%, deionized water 2.75%.
[0148] Preparation steps are the same as Example 1.
[0149] Comparative Example 1
[0150] Prepare the mesoporous silica microsphere solution and the subsequent antireflection composite coating solution according to the method of Example 1, except that CTAB is omitted and ethyl cellulose is used as a single template agent.
[0151] Comparative Example 2
[0152] Prepare the mesoporous silica microsphere solution and the subsequent antireflection composite coating solution according to the method of Example 1, except that ethyl cellulose is omitted and CTAB is used as a single template agent.
[0153] Test Example 1
[0154] Use the antireflection composite coating solutions prepared in Examples 1-6 and Comparative Examples 1-2 to prepare antireflection coatings, as follows:
[0155] Uniformly coat the antireflection composite coating solution on the surface of the cleaned substrate by dip coating; after preheating at 200°C for 4 minutes, heat to 650°C and ensure that the internal temperature of the substrate reaches a uniform temperature, heating time is about 3 minutes. After obtaining the coating, the following tests are performed and compared with the blank glass.
[0156] Transmittance test method:
[0157] Use spectrophotometry (standard method) to test transmittance.
[0158] Principle: Use a spectrophotometer to measure the light transmittance in a specific wavelength range (usually 380-1100 nm, covering the solar spectrum).
[0159] Steps:
[0160] Calibrate the instrument using a standard reference sample (blank glass).
[0161] Place the photovoltaic glass sample (sample after coating) in the light path, avoiding contamination or scratching.
[0162] Scan the wavelength range and record the transmittance spectrum curve.
[0163] The weighted average transmittance is calculated (weighted according to the AM1.5 solar spectrum).
[0164] The photovoltaic transmittance is calculated according to the formula in GB / T 30984.1-2015.
[0165]
[0166] In the formula:
[0167] T - photovoltaic transmittance;
[0168] T(λ) - spectral transmittance;
[0169] S λ - relative spectral distribution of solar radiation for air mass AM = 1.5;
[0170] Δλ - wavelength interval, in nanometers (nm);
[0171] S λ Δλ - product of the relative spectral distribution of solar radiation and the wavelength interval, see Appendix A;
[0172] λ - wavelength, in nanometers (nm).
[0173] Pencil hardness test method:
[0174] According to the national standard GB / T 6739-2022, the pencil method is used to test the hardness of paint film.
[0175] Pencil set: standard drawing pencils with hardness ranging from soft to hard (6B→5B→4B→3B→2B→B→HB→F→H→2H→3H→4H→5H→6H→7H→8H→9H).
[0176] Ensure that the pencil core is exposed about 5-6mm, and use 400 grit sandpaper to smooth the tip (form a cylindrical flat head, with no burrs on the edge).
[0177] The angle between the pencil and the paint film surface is 45°, and the test is performed.
[0178] Adhesion test method:
[0179] According to GB / T 9286-2021, the cross-hatch test is used to test the paint and varnish.
[0180] Cross-hatch tool: multi-blade cutting knife (blade spacing 1mm), use the tool to cut 6 parallel lines on the paint film surface, the depth needs to penetrate the coating to the substrate. Turn 90° and cut another set of 6 parallel lines, forming 25 squares (5x5).
[0181] The adhesive tape is closely attached to the grid area, and the bubbles are removed by pressing with fingers. After standing for 60±30 seconds, the adhesive tape is quickly torn away at an angle of 60° (it is recommended to complete within 0.5-1 seconds). The surface paint film peeling grade is set to 0-5 levels. The 0 level has the best effect.
[0182] Artificial aging paint film transmittance test:
[0183] The test is carried out according to GB / T 30984.1-2015 Solar Energy Glass.
[0184] The sample is irradiated under a wavelength of 280-320nmz ultraviolet lamp for 168h, and the transmittance of the sample is tested. The test method is consistent with the previous transmittance method. The higher the transmittance, the better the aging resistance.
[0185] The results are shown in Table 1.
[0186] Table 1
[0187]
[0188] As can be seen from the results in Table 1, by using a double template agent and optimizing the amount of each component, a mesoporous silica microsphere solution is obtained. When used for preparing a photovoltaic glass coating, improved transmittance, hardness, adhesion and aging resistance can be obtained.
[0189] The preferred embodiments of the present application are described in detail above, but the present application is not limited thereto. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, including the combination of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as disclosed by the present application, and all fall within the protection scope of the present application.
Claims
1. A mesoporous silica microsphere solution, characterized by, The raw materials for preparing the solution include: a silicon source, a double template agent, an alkaline catalyst, an organic solvent and water. The double template agent includes ethyl cellulose and cetyltrimethylammonium bromide.
2. The mesoporous silica microsphere solution of claim 1, wherein, In the double template agent, the mass ratio of ethyl cellulose and cetyltrimethylammonium bromide is 1-1.5:1, preferably 1.3:
1. Preferably, the mass percentage of the double template agent is 1.25-2.6%, preferably 1.4%.
3. The mesoporous silica microsphere solution according to claim 1 or 2, wherein, The silicon source is selected from at least one of tetraethoxysilane, trimethylethoxysilane and ethyl triethoxysilane. Preferably, the mass percentage of the silicon source is 6-11.5%, preferably 6-8%, further preferably 7%.
4. The mesoporous silica microsphere solution according to any one of claims 1-3, wherein, The alkaline catalyst is selected from at least one of ammonia, sodium hydroxide and tetramethylammonium hydroxide. Preferably, the concentration of the ammonia is 25%. Preferably, the mass percentage of the alkaline catalyst is 2.8-7%, preferably 3-4%.
5. The mesoporous silica microsphere solution according to any one of claims 1-4, wherein, The organic solvent is selected from at least one of anhydrous ethanol, methanol and isopropanol. Preferably, the mass percentage of the organic solvent is 72.85-78%, preferably 74.1-76.6%, further preferably 75.75%. Preferably, the mass percentage of the water is 8.4-12%, preferably 11.6%.
6. An antireflection composite coating solution, characterized by comprising: The raw materials for preparing the anti-reflective composite coating solution include: the mesoporous silica microsphere solution of any one of claims 1-5, a silane coupling agent, an acrylic resin, an organic solvent and water.
7. The antireflection composite plating solution according to claim 6, wherein The mass percentage of the mesoporous silica microsphere solution is 35-40%, preferably 36%. Preferably, the silane coupling agent is selected from at least one of γ-methacryloyloxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane and γ-(2,3-epoxypropoxy)propyltrimethoxysilane. Preferably, the mass percentage of the silane coupling agent is 0.15-0.25%, preferably 0.2%.
8. The antireflection composite plating solution according to claim 7, wherein The acrylic resin is an aqueous acrylic resin. Preferably, the mass percentage of the acrylic resin is 2.5-4%, preferably 3.5%. Preferably, the organic solvent is selected from at least one of anhydrous ethanol, methanol and isopropanol. Preferably, the mass percentage of the organic solvent is 53-58%, preferably 57%. Preferably, the mass percentage of the water is 2.75-4.3%, preferably 3.35%.
9. An anti-reflective coating prepared from the anti-reflective composite coating solution of any one of claims 6-8.
10. Use of the anti-reflective coating of claim 9 as a coating for photovoltaic glass.