CN116239311A - Double-layer anti-reflection coating - Google Patents

Double-layer anti-reflection coating Download PDF

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CN116239311A
CN116239311A CN202211705176.8A CN202211705176A CN116239311A CN 116239311 A CN116239311 A CN 116239311A CN 202211705176 A CN202211705176 A CN 202211705176A CN 116239311 A CN116239311 A CN 116239311A
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layer
sio
modified
sol
composite layer
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鲍田
王东
王金磊
汤永康
徐嘉馨
甘治平
李刚
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China Building Materials Glass New Materials Research Institute Group Co Ltd
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China Building Materials Glass New Materials Research Institute Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/21Oxides
    • C03C2217/23Mixtures
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/40Coatings comprising at least one inhomogeneous layer
    • C03C2217/43Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/445Organic continuous phases
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/40Coatings comprising at least one inhomogeneous layer
    • C03C2217/43Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475Inorganic materials
    • C03C2217/478Silica
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/73Anti-reflective coatings with specific characteristics
    • C03C2217/734Anti-reflective coatings with specific characteristics comprising an alternation of high and low refractive indexes
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/11Deposition methods from solutions or suspensions
    • C03C2218/111Deposition methods from solutions or suspensions by dipping, immersion
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention relates to a double-layer anti-reflection coating, which is characterized in that SiO is sequentially arranged on the surface of a glass substrate from bottom to top 2 ‑TiO 2 Composite layer, modified SiO 2 A composite layer; modified SiO 2 The inner core layer of the dispersed phase particles of the coating film forming matter used in the composite layer is a cationic surfactant micelle template, and the middle layer is modified SiO 2 The shell layer is composed of polyacrylate or organic siloxane modified polyacrylate. The invention has the advantages that: the average transmittance of the double-layer anti-reflection coating in the wave band of 380 nm-1100 nm is 94.2-96.5%, and the pencil hardness is more than or equal to 4H; the functions of wear resistance, weather resistance, pollution resistance, wide spectrum reflection resistance and the like can be effectively improved; the device is used for the photovoltaic module, can improve the long-term high-efficiency working capacity of the photovoltaic module in various actual working environments, improves the life cycle of products, and reduces the cleaning and maintenance cost of a photovoltaic power station; the anti-reflection coating can also be applied to the fields of building glass, solar flat plate collectors and the like.

Description

Double-layer anti-reflection coating
Technical Field
The invention belongs to the technical field of glass surface treatment, relates to the field of surface treatment of building glass and photovoltaic glass, and in particular relates to a double-layer anti-reflection coating.
Background
The existing photovoltaic glass film layer is generally a double-layer silicon oxide anti-reflection film, and the average transmittance of the coated glass is generally about 94% within a wave band of 380-1100 nm due to the limitation of refractive index, so that the further effective improvement is difficult. In addition, complicated outdoor environmental influencing factors such as rain and snow, wind and sand, atmospheric pollution and the like put high demands on the mechanical strength and the dirt resistance of the film. The photovoltaic module has the advantages that the power generation efficiency is reduced, the cleaning cost is improved, and the life cycle of the product is shortened due to the problems of pollution, abrasion, aging and the like of the anti-reflection coating.
Disclosure of Invention
The invention aims to solve the problems that the transmittance of the existing building or photovoltaic glass anti-reflection coating is low (about 94%) within the wave band of 380-1100 nm, the mechanical strength is low, the dirt resistance is poor and the like, and provides a double-layer anti-reflection coating.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a double-layer anti-reflection coating comprises a glass substrate and is characterized in that SiO is sequentially arranged on the surface of the glass substrate from bottom to top 2 -TiO 2 Composite layer, modified SiO 2 A composite layer; wherein the SiO is modified 2 The structure of the dispersed phase particles of the coating film forming substance used in the composite layer is that the inner core layer is a micelle (cationic surfactant) template, and the middle layer is modified SiO 2 The outer shell layer is composed of polyacrylate or organic siloxane modified polyacrylate.
Further, the SiO 2 -TiO 2 The composite layer is prepared by the following method: preparing an acidic or neutral SiO with the mass concentration of 2.5% -5% from a silicon source 2 Preparing acidic or neutral TiO with mass concentration of 2% -4% from titanium source by using sol 2 Sol, followed by SiO 2 Sol and TiO 2 Mixing the sol (10% -40%) according to the volume ratio (60% -90%).
Further, the modified SiO 2 The coating film forming matter dispersed phase particles used in the composite layer are prepared by the following method:
(1) Preparation of the inner core layer: adding 0.1% -0.3% of cationic surfactant into a mixed solution of 20% -60% of water and 40% -80% of alcohol solvent at the temperature of 10 ℃ -35 ℃, and stirring the mixed solution for 4-12 hours to form a cationic surfactant micelle template;
(2) Preparation of an intermediate layer: continuously adding ammonia water accounting for 1.0% -1.3% of the mass of the dispersion liquid in the step (1), tetraethoxysilane (TEOS) accounting for 1.5% -2.5% of the mass of the dispersion liquid and a coupling agent accounting for 0.5% -1.5% of the mass of the dispersion liquid, reacting for 2-8 hours at room temperature, and depositing on the surface of a cationic surfactant micelle template through a sol-gel process to obtain modified SiO 2 A layer;
(3) Preparation of the outer shell layer: and adding 18-30% of acrylic ester monomer or mixed solution of cage oligomeric silsesquioxane and acrylic ester monomer into the dispersion liquid, and stirring for 0.5-4 h at 40-80 ℃ to obtain the shell layer, wherein the mixed solution is 0.15-0.50% of initiator.
Further, the organosiloxane used in the organosiloxane modified polyacrylate is one or more of cage polysilsesquioxane with alkyl and alkenyl.
Further, the silicon source is any one of tetraethoxysilane, tetramethoxysilane, tetrapropoxysilane, tetrabutoxysilane.
Further, the titanium source is any one of tetrabutyl titanate, tetraethyl titanate, tetraisopropyl titanate and tetraisobutyl titanate.
Further, the cationic surfactant is one or more of cetyl trimethyl ammonium bromide, dodecyl dimethyl benzyl ammonium chloride, polydiallyl dimethyl ammonium chloride and dimethyl diallyl ammonium chloride/acrylamide copolymer.
Further, the alcohol is one or more of ethanol, isopropanol, n-propanol, diacetone alcohol, ethylene glycol, propylene glycol, 1-methoxy-2-propanol and n-hexanol.
Further, the coupling agent is one or more of gamma-methacryloxypropyl trimethoxy silane, gamma-aminopropyl triethoxy silane, gamma-methacryloxypropyl triisopropoxy silane, gamma-aminopropyl methyl diethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, isopropyl tri (dioctyl pyrophosphoryl oxy) titanate and di (triethanolamine) diisopropyl titanate. ( The silane coupling agent is effective only for film forming material particles containing silicon element, while the titanium coupling agent has wider adaptability, and the effect is not limited to improving the strength of the organic-inorganic hybrid material coating, but also endows a certain degree of flexibility. The titanate coupling agent and the silane coupling agent can be used together to generate a synergistic effect, and the coupling effect is greatly improved. )
Further, the acrylic ester monomer is one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate, lauryl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl methacrylate and 2-hydroxypropyl methacrylate.
Further, the initiator is one of ammonium persulfate, potassium persulfate, hydrogen peroxide and hydrogen peroxide derivatives.
The invention introduces TiO with high refractive index according to the film optical principle 2 The refractive index of the bottom film is improved, the bottom coating is composite sol, and a high-adhesion high-strength film layer is formed by hydrolysis, polycondensation and drying of a precursor. The surface coating is an organic-inorganic hybrid emulsion system, and the organic-inorganic hybrid hydrophobically modified SiO is prepared through the composition and structural design of the surface coating film forming material particles 2 And (3) a composite layer. Intermediate SiO of the film forming material particles is obtained by deposition on the surface of a micelle template through a sol-gel process 2 And (3) a layer, and then polymerizing on the surface of the layer to generate a shell substance, so as to obtain a disperse phase of the hybrid emulsion core-shell structure. During film formation, the dispersion medium volatilizes, emulsion particles are tightly piled up and deformed under the pushing of capillary force and surface tension, interfaces among the particles gradually disappear, polymer molecular chains mutually permeate and intertwine, and thus a continuous and uniform coating film is formed, and the coating film has the strength and the resistance of an inorganic coating layerWeather resistance and hydrophobic and anti-fouling properties brought by organic coatings.
The invention has the beneficial effects that:
1. the average transmittance of the anti-reflection coating in the wave band of 380 nm-1100 nm is 94.2% -96.5%, and the pencil hardness is more than or equal to 4H; the functions of wear resistance, weather resistance, stain resistance (the transmittance is reduced by 0.5% -2% compared with a control sample in an outdoor one month test period), wide spectrum anti-reflection and the like can be effectively improved;
2. the anti-reflection coating is used for the photovoltaic module, so that the long-term high-efficiency working capacity of the anti-reflection coating in various practical working environments can be improved, the life cycle of a product is prolonged (the average power generation power is improved by 2% -10% in one month), and the cleaning and maintenance cost of a photovoltaic power station is reduced; the anti-reflection coating can also be applied to the fields of building glass, solar flat plate collectors and the like.
Drawings
FIG. 1 is a schematic illustration of a dual layer anti-reflective coating structure;
FIG. 2 is a modified SiO in a bilayer antireflective coating 2 The cross section of the disperse phase particle structure of the coating film forming substance used in the composite layer is schematically shown.
Detailed Description
The invention is further described with reference to fig. 1 and 2:
the preparation method of the double-layer anti-reflection coating comprises the following specific implementation steps:
example 1
(1) 17.5mL of tetra-isobutyl titanate is added into a mixed solution of 150mL of ethanol and 5.30mL of acetylacetone, 3.7mL of deionized water is added after stirring for 20min, the pH of the system is regulated to 3.0 by concentrated HCl, 5.0mL of N, N-dimethylformamide is added, stirring is continued for 2h, and the mixture is sealed and aged for 24h in a room temperature environment to obtain TiO 2 Sol;
(2) 150mL of ethanol and 22.9mL of Tetraethoxysilane (TEOS) are mixed, 7.4mL of deionized water is added after stirring for 20min, the pH value of the system is regulated to 3.0 by concentrated HCl, stirring is continued for 2h, and aging is carried out for 24h in the environment of 40 ℃ to obtain SiO 2 Sol;
(3) Coating film by adopting a lifting mode, fixing the cleaned glass substrate on a lifting frame, immersing the glass substrate inTiO with volume ratio of 1:2 2 With SiO 2 Immersing the glass substrate in the mixed sol for 40s, and then pulling the glass substrate out of the coating solution at a speed of 100 mm/min to form an underlying TiO layer on the glass surface 2 -SiO 2 A film; wet film to be pulled (TiO 2 -SiO 2 Film) is dried in a baking oven at 60 ℃, then is put in a muffle furnace and is heat treated for 10min at 350 ℃ to obtain TiO 2 -SiO 2 A composite layer;
(4) Adding 0.1g of Cetyl Trimethyl Ammonium Bromide (CTAB) into a mixed solution of 40mL of ethanol and 10mL of water, and uniformly stirring to form a cationic surfactant micelle template; continuously adding 0.5mL of ammonia water, 0.80 mL Tetraethoxysilane (TEOS) and 0.4 mL gamma-methacryloxypropyl trimethoxysilane, mixing, reacting for 6h at room temperature, and depositing on the surface of a micelle template through a sol-gel process to obtain modified SiO 2 An intermediate layer;
(5) Adding 9.8% of n-butyl acrylate, 10.2% of methacrylic cage-shaped silsesquioxane and 0.3% of ammonium persulfate into the mixed solution obtained in the step (4), and fully stirring at 60 ℃ for 1 h to obtain modified SiO 2 An outer shell layer of film former particles of the coating used in the composite layer;
(6) Coating the film in a lifting mode to coat the TiO with the bottom layer 2 -SiO 2 Immersing the glass substrate of the composite layer into the mixed liquid prepared in the step (5), immersing for 30s, then pulling the glass substrate out of the coating liquid at the speed of 120 mm/min to form a gel film, placing the gel film in a baking oven at 120 ℃ for 15min, and then placing the gel film in a muffle furnace for heat treatment at 500 ℃ for 2min to obtain the double-layer anti-reflection coating. Through detection, the transmittance of the double-layer anti-reflection coating sample in a wave band of 380 nm-1100 nm is 95.4%, the pencil hardness is 5H, the water contact angle is 108 DEG, and the transmittance is reduced by 1.2% compared with a commercial control sample in an outdoor test period of one month.
Example 2
(1) Adding 18mL of tetrabutyl titanate into a mixed solution of 140mL of ethanol and 5.30mL of acetylacetone, stirring for 20min, adding 3.2mL of deionized water, regulating the pH of the system to 2.0 by using concentrated HCl, adding 5.0mL of N, N-dimethylformamide, continuously stirring for 2h, and circulating at room temperatureSealing and aging for 24 hours in the environment to obtain TiO 2 Sol;
(2) Mixing 84 mL isopropanol and 9.8 mL tetramethoxysilane, stirring for 30 min, adding 3.2mL of 0.01mol/L diluted hydrochloric acid, stirring for 2 hr, aging at 40deg.C for 24 hr to obtain SiO 2 Sol;
(3) Coating in a lifting mode, fixing the cleaned glass substrate on a lifting frame, and immersing a sample in TiO with the volume ratio of 3:4 2 With SiO 2 Immersing the glass substrate in the mixed sol for 60s, and then pulling the glass substrate out of the coating solution at a speed of 120 mm/min to form an underlying TiO layer on the glass surface 2 -SiO 2 A film; wet film to be pulled (TiO 2 -SiO 2 Film) is dried in a baking oven at 100 ℃, then is put in a muffle furnace and is heat-treated for 5min at 350 ℃ to obtain TiO 2 -SiO 2 A composite layer;
(4) Adding 0.08g of dodecyl dimethyl benzyl ammonium chloride into a mixed solution of 20mL of isopropanol and 20mL of water, stirring uniformly to form a cationic surfactant micelle template, continuously adding 0.5mL of ammonia water, 0.80. 0.80 mL Tetraethoxysilane (TEOS), 0.35 mL gamma-methacryloxypropyl trimethoxysilane and 0.05mL of isopropyl tri (dioctyl pyrophosphoryl oxy) titanate, reacting for 4h at room temperature, and depositing on the surface of the micelle template through a sol-gel process to obtain modified SiO 2 An intermediate layer;
(5) Continuously adding 10% of methyl acrylate, 12% of methyl methacrylate and 0.25% of ammonium persulfate into the mixed solution, and fully stirring at 50 ℃ for 2h to obtain modified SiO 2 An outer shell layer of film former particles of the coating used in the composite layer;
(6) Coating the mixed solution prepared in the step (5) on the plated bottom layer TiO in a spin coating mode 2 -SiO 2 Coating a surface film on the glass substrate of the composite layer, spin-coating for 30s at 3000 r/min, placing the sample in a baking oven at 120 ℃ for drying for 15min, and then placing in a muffle furnace for heat treatment at 500 ℃ for 2min to obtain the double-layer anti-reflection coating. Through detection, the transmittance of the double-layer anti-reflection coating sample in a wave band of 380 nm-1100 nm is 96.0%, the pencil hardness is 4H, the water contact angle is 110 DEG, and the double-layer anti-reflection coating sample is matched with the market in an outdoor test period of one monthThe decrease in transmittance was reduced by 1.8% compared to the sold control sample.
Example 3
(1) Preparation of TiO according to example 1 2 Sol and SiO 2 Sol, then coating the bottom layer film;
(2) Adding 0.1g of Cetyl Trimethyl Ammonium Bromide (CTAB) into a mixed solution of 40mL of ethanol and 10mL of water, uniformly stirring to form a cationic surfactant micelle template, continuously adding 0.5mL of ammonia water, 0.80 mL of TEOS and 0.4 mL gamma-methacryloxypropyl trimethoxysilane, and reacting 0.1 mL di (triethanolamine) diisopropyl titanate at room temperature for 6h, and depositing on the surface of the micelle template through a sol-gel process to obtain modified SiO 2 An intermediate layer;
(3) Continuously adding n-butyl acrylate accounting for 9.8 percent of the total mass, allyl isobutyl cage-shaped silsesquioxane accounting for 10.2 percent and potassium persulfate accounting for 0.2 percent into the mixed solution, and fully stirring at 60 ℃ for 1 h to obtain modified SiO 2 An outer shell layer of film former particles of the coating used in the composite layer;
(4) Coating the film in a lifting mode to coat the TiO with the bottom layer 2 -SiO 2 Immersing the glass substrate of the composite layer into the mixed liquid prepared in the step (3), immersing for 50s, then pulling the glass substrate out of the coating liquid at the speed of 150 mm/min to form a gel film, placing the gel film in a 100 ℃ oven for drying for 20min, and then placing the gel film in a muffle furnace for heat treatment at 600 ℃ for 1 min to obtain the double-layer anti-reflection coating. Through detection, the transmittance of the double-layer anti-reflection coating sample in a wave band of 380 nm-1100 nm is 96.4%, the pencil hardness is 4H, the water contact angle is 120 DEG, and the transmittance is reduced by 2.0% compared with a commercial control sample in an outdoor test period of one month.
The above examples are necessary descriptions of the coating structure and the main components of the coating in the technical solution of the present application, and the use and regulation of various solvents, film-forming aids, dispersants, emulsifiers, mold inhibitors, thickeners, etc. involved in the coating process and the coating formulation can be reasonably solved through limited experiments according to the process experience in the art, and thus are not described.

Claims (9)

1. A double-layer anti-reflection coating comprises a glass substrate and is characterized in that the surface of the glass substrate is sequentially provided with SiO from bottom to top 2 -TiO 2 Composite layer, modified SiO 2 A composite layer; wherein the SiO is modified 2 The inner core layer of the dispersed phase particles of the coating film forming matter used in the composite layer is a cationic surfactant micelle template, and the middle layer is modified SiO 2 The outer shell layer is composed of polyacrylate or organic siloxane modified polyacrylate.
2. A bilayer antireflective coating according to claim 1, wherein: the SiO is 2 -TiO 2 The composite layer is prepared by the following method: preparing an acidic or neutral SiO with the mass concentration of 2.5% -5% from a silicon source 2 Preparing acidic or neutral TiO with mass concentration of 2% -4% from titanium source by using sol 2 Sol, followed by SiO 2 Sol and TiO 2 Mixing the sol (10% -40%) according to the volume ratio (60% -90%).
3. A bilayer antireflective coating according to claim 1, wherein: the modified SiO 2 The coating film forming matter dispersed phase particles used in the composite layer are prepared by the following method:
(1) Preparation of the inner core layer: adding 0.1% -0.3% of cationic surfactant into a mixed solution of 20% -60% of water and 40% -80% of alcohol solvent at the temperature of 10 ℃ -35 ℃, and stirring the mixed solution for 4-12 hours to form a cationic surfactant micelle template;
(2) Preparation of an intermediate layer: continuously adding ammonia water accounting for 1.0% -1.3% of the mass of the dispersion liquid in the step (1), tetraethoxysilane (TEOS) accounting for 1.5% -2.5% of the mass of the dispersion liquid and a coupling agent accounting for 0.5% -1.5% of the mass of the dispersion liquid, reacting for 2-8 hours at room temperature, and depositing on the surface of a cationic surfactant micelle template through a sol-gel process to obtain modified SiO 2 A layer;
(3) Preparation of the outer shell layer: and adding 18-30% of acrylic ester monomer or mixed solution of cage oligomeric silsesquioxane and acrylic ester monomer into the mixed solution, and stirring for 0.5-4 h at 40-80 ℃ to obtain the shell layer, wherein the mixed solution is 0.15-0.50% of initiator.
4. A bilayer antireflective coating according to claim 1, wherein: the organosiloxane used in the organosiloxane modified polyacrylate is one or more of cage-type oligomeric silsesquioxane with alkyl and alkenyl.
5. A bilayer antireflective coating according to claim 2, wherein: the silicon source is any one of tetraethoxysilane, tetramethoxysilane, tetrapropoxysilane and tetrabutoxysilane; the titanium source is any one of tetrabutyl titanate, tetraethyl titanate, tetraisopropyl titanate and tetraisobutyl titanate.
6. A bilayer antireflective coating according to claim 3 wherein: the cationic surfactant is one or more of cetyl trimethyl ammonium bromide, dodecyl dimethyl benzyl ammonium chloride, polydiallyl dimethyl ammonium chloride and dimethyl diallyl ammonium chloride/acrylamide copolymer; the alcohol is one or more of ethanol, isopropanol, n-propanol, diacetone alcohol, ethylene glycol, propylene glycol, 1-methoxy-2-propanol and n-hexanol.
7. A bilayer antireflective coating according to claim 3 wherein: the coupling agent is one or more of gamma-methacryloxypropyl trimethoxy silane, gamma-aminopropyl triethoxy silane, gamma-methacryloxypropyl triisopropoxy silane, gamma-aminopropyl methyl diethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, isopropyl tri (dioctyl pyrophosphoric acyloxy) titanate and di (triethanolamine) diisopropyl titanate.
8. A bilayer antireflective coating according to claim 3 wherein: the acrylic ester monomer is one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate, lauryl acrylate, 2-hydroxy ethyl acrylate, 2-hydroxy propyl acrylate, 2-hydroxy ethyl methacrylate and 2-hydroxy propyl methacrylate.
9. A bilayer antireflective coating according to claim 3 wherein: the initiator is one of ammonium persulfate, potassium persulfate, hydrogen peroxide and hydrogen peroxide derivatives.
CN202211705176.8A 2022-12-29 2022-12-29 Double-layer anti-reflection coating Pending CN116239311A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102649835A (en) * 2012-04-26 2012-08-29 华南理工大学 Organic-inorganic hybrid high-silicon-content acrylic ester emulsion and preparation method thereof
CN109942205A (en) * 2019-03-26 2019-06-28 常州大学 A kind of preparation method of glass surface antireflective automatic cleaning coating

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102649835A (en) * 2012-04-26 2012-08-29 华南理工大学 Organic-inorganic hybrid high-silicon-content acrylic ester emulsion and preparation method thereof
CN109942205A (en) * 2019-03-26 2019-06-28 常州大学 A kind of preparation method of glass surface antireflective automatic cleaning coating

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马立云: ""宽谱增透双层TiO2-SiO2/SiO2薄膜的制备与性能"", 《材料导报》, vol. 33, no. 2, 25 November 2019 (2019-11-25), pages 161 - 164 *

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