CN115448614B - Method for preparing pit structure optical antireflection film based on emulsion polymerization method - Google Patents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
Abstract
The invention belongs to the field of high polymer functional materials, and discloses a method for preparing a pit structure optical antireflection film based on an emulsion polymerization method, which comprises the following steps: (1) Preparing vinyl-terminated polysiloxane-polyacrylate emulsion by taking methyl methacrylate, butyl methacrylate, acrylic acid and vinyl-terminated polysiloxane as monomers; (2) preparing acidic silica sol; (3) Dip-coating acidic silica sol on a substrate, dip-coating vinyl terminated polysiloxane-polyacrylate emulsion after 5-30 s intervals, heat-treating and curing to form a film, and finally calcining to remove polymer latex particles to obtain the anti-reflection coating. Compared with the common antireflection film, the surface morphology of the concave pit structure is more special, and the concave pit structure is an ideal optical material.
Description
Technical Field
The invention belongs to the field of high molecular functional materials, and particularly relates to a method for preparing an optical antireflection film with a pit structure based on an emulsion polymerization method.
Background
In the optical material, the transparent material refers to a material which has no or negligible absorption to visible light (the wavelength is 400-750 nm) (the transmittance of the visible light is more than or equal to 80 percent) and has certain light, heat and mechanical stability. It includes inorganic optical glass, organic polymer transparent material and composite transparent material. Conventional organic polymer transparent materials include polymethyl methacrylate (PMMA), polystyrene (PS), polycarbonate (PC), polyallyldiethylene glycol carbonate (CR-399), and the like. Because the light transmittance of the material can not meet the requirements of the fields of modern society information industry, communication industry and the like on the optical material, in many optical applications, such as lenses, photovoltaic industry, related photoelectric elements, display fields and the like, an optical anti-reflection coating is coated, the light transmittance is increased, the maximum utilization of light is realized, and the conversion rate of light energy is improved. In the research of the antireflection film, a film structure is designed and optimized by adding reasonable additives, nanoimprint technology and the like, so that the antireflection effect is achieved. The film structure is of great importance in the study of optical anti-reflection coatings.
Disclosure of Invention
The invention aims to provide a method for preparing an optical antireflection film with a pit structure based on an emulsion polymerization method.
In order to achieve the purpose of the invention, the technical scheme adopted is as follows:
a method for preparing a pit structure optical antireflection film based on an emulsion polymerization method comprises the following steps:
(1) Preparation of vinyl-terminated polysiloxane-polyacrylate emulsion: sodium Dodecyl Sulfate (SDS) is used as an emulsifier, ammonium Persulfate (APS) is used as an initiator, n-Hexadecane (HD) is used as a co-stabilizer, methyl Methacrylate (MMA), butyl methacrylate (BA), acrylic Acid (AA) and vinyl-terminated polysiloxane (V-PDMS) are used as monomers, and the mass ratio of acrylic acid to methyl methacrylate to butyl methacrylate is 0.04:1:1 to 0.06:1:1, the auxiliary stabilizer accounts for 3.7 to 4 percent of the mass of the monomer, and the initiator accounts for 0.45 to 0.5 percent of the mass of the monomer.
Specifically, methyl Methacrylate (MMA), butyl methacrylate (BA), acrylic Acid (AA), vinyl-terminated polysiloxane (V-PDMS) and n-Hexadecane (HD) are mixed to prepare an oil phase, and the oil phase is uniformly stirred by a mechanical stirring paddle. An aqueous phase was prepared by dissolving Sodium Dodecyl Sulfate (SDS) in deionized water. The two phases (aqueous phase and oil phase) are mixed together and stirred ultrasonically to homogeneity. Then, 1/3 of the mixture was transferred to a four-necked flask equipped with a reflux condenser and a mechanical stirrer. Adding 1/3 of Ammonium Persulfate (APS) aqueous solution as an initiator, continuously stirring, continuously dripping the rest monomer emulsion and the initiator aqueous solution into a flask after the emulsion is blue, continuously carrying out polymerization reaction, and cooling to room temperature after the reaction is finished to obtain the polymer emulsion.
(2) Preparation of acidic silica sol: and adding tetraethoxysilane into the mixed solution of ethanol, distilled water and hydrochloric acid dropwise, and stirring for reaction to obtain the acid-catalyzed silica sol.
Specifically, distilled water, ethanol and hydrochloric acid are sequentially added into a reaction vessel, after uniform stirring, ethyl orthosilicate is dripped into the reaction vessel through a constant pressure funnel, and the acidic silica sol is obtained after stirring and reacting for 6 hours at 30 ℃.
Further, the mol ratio of the tetraethoxysilane, the ethanol, the hydrochloric acid and the water is 1:37:0.02:4.
(3) Preparation of pit structure optical antireflection film: dip-coating the acidic silica sol prepared in the step (2) on a substrate, dip-coating a layer of the polymer emulsion prepared in the step (1) after 5-30 s, performing heat treatment to cure the emulsion into a film, and finally calcining the film to remove emulsion particles (the calcining temperature is preferably 500 ℃ and the calcining time is preferably 3 h) to obtain the optical antireflection film.
Specifically, the acidic silica sol prepared in the step (2) is directly dip-coated on a substrate, the polymer emulsion prepared in the step (1) is dip-coated on the substrate after being diluted by 15 times, and then the substrate is put into an oven for heat treatment at 60 ℃ for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses vinyl end-capped polysiloxane and acrylic monomer to carry out emulsion polymerization, prepares acid silica sol by sol-gel method, and uses calcination technology to obtain the special pit structure antireflection film by dip-coating the acid silica sol and polymer emulsion on the surface of the base material in sequence. In addition, the surface morphology of the antireflection film can be controlled by changing the sequence and the interval time of the two dip-coating processes. Compared with the common antireflection film, the surface morphology of the concave pit structure is more special, and the concave pit structure is an ideal optical material.
Drawings
FIG. 1 is an infrared spectrum of a polymer emulsion (a) and a vinyl-terminated polysiloxane (b);
FIG. 2 is a graph showing the change in light transmittance of an antireflection film before and after calcination;
FIG. 3 is a scanning electron microscope image of an antireflection film after calcination;
FIG. 4 is an atomic force microscope image of an antireflection film after calcination;
fig. 5 is a graph of light transmittance of polymer emulsion anti-reflection films at different vinyl-terminated polysiloxane mass fractions on a glass substrate (vinyl-terminated polysiloxane mass fraction=m V-PDMS /(m MMA +m BA +m AA )。
Detailed Description
The invention is further described in detail below in connection with the examples:
example 1:
(1) Preparation of vinyl-terminated polysiloxane-polyacrylate emulsion (24% by mass of V-PDMS)
An oil phase was prepared by mixing 5g of Methyl Methacrylate (MMA), 5g of butyl methacrylate (BA), 0.2g of Acrylic Acid (AA), 2.4-g V-PDMS, and 0.5g of n-Hexadecane (HD), and stirring at 1000rpm for 10 minutes with a mechanical stirring paddle. An aqueous phase was prepared by dissolving 0.3g of Sodium Dodecyl Sulfate (SDS) in 25g of deionized water. The two phases (aqueous and oil) were mixed together, mixed at 1000rpm for 30min, and sonicated in an ice bath for 20min using a sonicator. Then, one third of the mixture was transferred to a four-necked flask equipped with a reflux condenser and a mechanical stirrer. When the flask temperature was 78 ℃, 1/3 of Ammonium Persulfate (APS) aqueous solution (0.06 g APS was dissolved in 1mL of distilled water) was added, stirring was started for 0.5h, after the emulsion was blue, the remaining monomer emulsion and initiator aqueous solution were continuously dropped into the flask within 1.5h, then polymerization was continued for 1.5h, and after the reaction was completed, the temperature was lowered to 30 ℃ to obtain a polymer emulsion.
FIG. 1 is a polymer emulsion (a) and vinyl terminated polymerInfrared spectrogram of siloxane (b), visible from (b), 1014cm -1 、1066cm -1 The part is a telescopic vibration peak of polysiloxane chain segment Si-O-Si, 786cm -1 、1257cm -1 Is Si-CH on polysiloxane chain segment 3 Is characterized by the characteristic peak of polydimethylsiloxane, 1597cm -1 At c=c characteristic absorption peak. Infrared analysis indicated that the synthesized product was vinyl-terminated polysiloxane. It can be seen from (a) that the introduction of vinyl-terminated polysiloxanes into acrylates for emulsion polymerization gave polymers with characteristic peaks of Si-O-Si bonds and with characteristic absorption peaks of c=c disappeared and characteristic absorption peaks of c=o appeared, indicating successful preparation of the polymer emulsion.
(2) Preparation of acidic silica sols
3.6g of distilled water, 86g of absolute ethyl alcohol and 0.02g of hydrochloric acid are sequentially added into a reaction vessel, after uniform stirring, 10.4g of Tetraethoxysilane (TEOS) is dripped into the reaction vessel through a constant pressure funnel, and stirred and reacted for 6 hours at 30 ℃ to obtain acidic silica sol.
(3) Preparation of anti-reflection material
The acidic silica sol is respectively coated on glass, after 5s interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and coated on the substrate coated with the silica sol, and the mass concentration of the polymer emulsion is 6.25%. And (3) placing the mixture into a 60 ℃ oven for heat treatment for 0.5h to cure and form a film, and finally calcining the film in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93%, the light transmittance of the antireflective coating obtained after calcination is 93.2%, and the light transmittance after calcination is improved, as shown in fig. 2.
Example 2:
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(3) Preparation of an anti-reflection material: respectively dip-coating acidic silica sol on glass, diluting vinyl-terminated polysiloxane-polyacrylate emulsion after 10s interval, dip-coating the diluted emulsion on a substrate coated with the silica sol, placing the substrate in a 60 ℃ oven for heat treatment for 0.5h to cure and form a film, and finally calcining in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93%, the light transmittance of the antireflective coating obtained after calcination is 93.3%, and the light transmittance after calcination is improved, as shown in fig. 2.
Example 3:
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(3) Preparation of an anti-reflection material: respectively dip-coating acidic silica sol on glass, diluting vinyl-terminated polysiloxane-polyacrylate emulsion after 15s interval, dip-coating the diluted emulsion on a substrate coated with the silica sol, placing the substrate coated with the silica sol in an oven with the mass concentration of 6.25 ℃, performing heat treatment for 0.5h to cure and form a film, and finally calcining in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93.1%, the light transmittance of the antireflective coating obtained after calcination is 93.4%, and the light transmittance after calcination is improved, as shown in fig. 2.
Example 4:
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(3) Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after the interval of 20s, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on the substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93.1%, the light transmittance of the antireflective coating obtained after calcination is 93.4%, and the light transmittance after calcination is improved, as shown in fig. 2.
Example 5:
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(3) Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after 30s of interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on the substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93.2%, the light transmittance of the antireflective coating obtained after calcination is 93.5%, and the light transmittance after calcination is improved, as shown in fig. 2.
Fig. 3 a is a scanning electron microscope image of the anti-reflection coating in this experiment, and fig. 4 a is an atomic force microscope image of the anti-reflection coating in this experiment, and a relatively uniform pit structure can be seen, and the structure is favorable for optical anti-reflection, so that the light transmittance after calcination is reduced.
Comparative example 1
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(2) Preparation of anti-reflection material
Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after 60s of interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on the substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 93.3%, the light transmittance of the antireflective coating obtained after calcination is 93%, and the light transmittance after calcination is reduced, as shown in fig. 2.
Comparative example 2
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(2) Preparation of anti-reflection material
Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after 90s of interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on the substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 92.8%, the light transmittance of the antireflective coating obtained after calcination is 92.7%, and the light transmittance after calcination is reduced, as shown in fig. 2.
Comparative example 3
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(2) Preparation of anti-reflection material
Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after 120s of interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on a substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 92.7%, the light transmittance of the antireflective coating obtained after calcination is 92.6%, and the light transmittance after calcination is reduced, as shown in fig. 2.
Comparative example 4
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(2) Preparation of anti-reflection material
Preparation of an anti-reflection material: the acid silica sol is respectively dip-coated on glass, after 150s of interval, the vinyl-terminated polysiloxane-polyacrylate emulsion is diluted and then dip-coated on the substrate coated with the silica sol, the mass concentration of the polymer emulsion is 6.25%, the substrate is put into a 60 ℃ oven for heat treatment for 0.5h to be solidified into a film, and finally the film is calcined in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment is 92.7%, the light transmittance of the antireflective coating obtained after calcination is 91.8%, and the light transmittance after calcination is reduced, as shown in fig. 2.
Fig. 3 b is a scanning electron microscope image of the anti-reflection coating in the experiment, and fig. 4 b is an atomic force microscope image of the anti-reflection coating in the experiment, and the surface is smooth without pit structures, so that the light transmittance is reduced after calcination.
Comparative example 5
(1) The preparation of the vinyl-terminated polysiloxane-polyacrylate emulsion was carried out as in example 1.
(2) The preparation method of the acidic silica sol is the same as in example 1.
(2) Preparation of anti-reflection material
Preparation of an anti-reflection material: the preparation method comprises the steps of firstly diluting and dip-coating vinyl-terminated polysiloxane-polyacrylate emulsion on a substrate coated with silica sol, wherein the mass concentration of the polymer emulsion is 6.25%, dip-coating acidic silica sol on glass after 30s, putting into a 60 ℃ oven for heat treatment for 0.5h to cure and form a film, and finally calcining in a muffle furnace to obtain the anti-reflection coating, wherein the calcining temperature is 500 ℃ and the calcining time is 3h.
The light transmittance before calcination in this experiment was 92.7%, and the light transmittance after calcination was 91%.
Comparative example 5 is mainly different from example 5 in that: the order of dip coating the acidic silica sol and the polymer emulsion is different.
In fig. 3 c, which is a scanning electron microscope image of the anti-reflection coating in this experiment, it can be seen that cracks are generated on the surface after calcination, and this structure is not beneficial to optical anti-reflection.
In addition, the applicant has made the following comparative tests:
polymer emulsions with different V-PDMS contents are prepared (the dosages of the rest monomers, the emulsifier and the initiator in the preparation process are the same as those in the embodiment 1, only the V-PDMS content is changed), the polymer emulsions are diluted and then dip-coated on a glass substrate, the mass concentration of the polymer emulsions is 6.25%, the polymer emulsions are put into a 60 ℃ oven for heat treatment for 0.5h to be solidified and formed into films, the light transmittance of the antireflection films with different V-PDMS contents is the highest, the light transmittance of the antireflection films with different V-PDMS contents is 24%, and the polymer emulsion antireflection effect is the best under the use level, so that the polymer emulsions with the V-PDMS content of 24% are adopted in the preparation of the follow-up pit structures.
Based on the verification of the above examples and comparative examples, the pit structure prepared by the present invention is only generated under the specific dip-coating sequence and shorter interval time, and has better anti-reflection effect.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme and the concept of the present invention, and should be covered by the scope of the present invention.
Claims (8)
1. A method for preparing a pit structure optical antireflection film based on an emulsion polymerization method is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparation of vinyl-terminated polysiloxane-polyacrylate emulsion: sodium dodecyl sulfate is used as an emulsifier, ammonium persulfate is used as an initiator, n-hexadecane is used as a co-stabilizer, methyl methacrylate, butyl methacrylate, acrylic acid and vinyl-terminated polysiloxane are used as monomers to prepare vinyl-terminated polysiloxane-polyacrylate emulsion, and the mass ratio of acrylic acid to methyl methacrylate to butyl methacrylate is 0.04-0.06: 1:1, the auxiliary stabilizer accounts for 3.7-4% of the mass fraction of the monomer, and the initiator accounts for 0.45-0.5% of the mass fraction of the monomer;
(2) Preparation of acidic silica sol: dropwise adding tetraethoxysilane into a mixed solution of ethanol, distilled water and hydrochloric acid, and stirring for reaction to obtain acid-catalyzed silica sol;
(3) Preparation of pit structure optical antireflection film: dip-coating the acidic silica sol prepared in the step (2) on a substrate, dip-coating a layer of the polymer emulsion prepared in the step (1) after 5-30 s intervals, performing heat treatment to cure the polymer emulsion into a film, and finally calcining to remove polymer emulsion particles to obtain the anti-reflection coating.
2. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the specific preparation steps of the vinyl-terminated polysiloxane-polyacrylate emulsion in the step (1) are as follows:
methyl methacrylate, butyl methacrylate, acrylic acid, vinyl-terminated polysiloxane and n-hexadecane are mixed to prepare an oil phase, and the oil phase is uniformly stirred by a mechanical stirring paddle; dissolving sodium dodecyl sulfate in distilled water to prepare a water phase, mixing the water phase and the oil phase together, and stirring and carrying out ultrasonic treatment uniformly; then, 1/3 of the mixed solution was transferred to a four-necked flask equipped with a reflux condenser and a mechanical stirrer; adding 1/3 ammonium persulfate aqueous solution as initiator, stirring for polymerization, continuously dripping the rest monomer emulsion and initiator aqueous solution after the emulsion is blue, continuously polymerizing, and cooling to room temperature after the reaction is finished to obtain the polymer emulsion.
3. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 2, wherein the method comprises the following steps: the emulsion polymerization temperature in the specific preparation step of the vinyl-terminated polysiloxane-polyacrylate emulsion of step (1) was 78 ℃.
4. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the specific preparation steps of the acidic silica sol in the step (2) are as follows:
distilled water, ethanol and hydrochloric acid are sequentially added into a reaction vessel, after uniform stirring, tetraethoxysilane is dripped into the reaction vessel through a constant pressure funnel, and the acidic silica sol is obtained through stirring reaction, wherein the reaction temperature is 30 ℃, and the reaction time is 6 h.
5. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the specific preparation steps of the pit structure optical antireflection film in the step (3) are as follows: the acidic silica sol and the polymer emulsion are directly and sequentially dip-coated on the substrate, and the mass concentration of the polymer emulsion is 6% -7%.
6. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the curing temperature in the step (3) is 60 ℃ and the curing time is 0.5h.
7. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the calcination temperature is 500 ℃ and the calcination time is 3 hours.
8. The method for preparing the pit structure optical antireflection film based on the emulsion polymerization method according to claim 1, wherein the method comprises the following steps: the mol ratio of the tetraethoxysilane to the ethanol to the hydrochloric acid to the water is 1:37:0.02:4.
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