CN114895386A - Anti-glare film, manufacturing method and mold manufacturing method - Google Patents
Anti-glare film, manufacturing method and mold manufacturing method Download PDFInfo
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Abstract
The invention discloses an anti-glare film, a manufacturing method and a die manufacturing method, wherein the anti-glare film comprises a light curing mixture and a heat curing mixture; the photocuring mixture comprises a resin prepolymer, an active monomer, a photoinitiator and a leveling agent; the components of the thermosetting mixture comprise a resin prepolymer, a thermal curing agent, a catalyst, a solvent, an anchoring material and other auxiliary agents; the ratio of the light-curing mixture to the heat-curing mixture is 5% to 25%. The technical problems of low contrast ratio and flash point of the anti-glare film in the prior art are solved.
Description
Technical Field
The invention relates to the technical field of anti-glare films, in particular to an anti-glare film, a manufacturing method and a mold manufacturing method.
Background
In daily life, electronic products, particularly display electronic products with high resolution (more than 400ppi resolution) are in indispensable use in work and life of people. Comfort of use and impact on visual health are among the key points for display type products to be competitive. Therefore, the high-resolution display device introduces an anti-reflection and anti-glare functional film to reduce glare caused by external light intensity reflection and glare generated by light scattering inside the device.
Currently, anti-glare films are classified into several categories: 1. silica gel is sprayed and gathered on the surface to form an irregular rough structure; 2. the particles are introduced into the anti-glare coating liquid, and the particles are larger than the film in thickness to form convex-concave structures on the surface or form irregular convex-concave structures on the surface by utilizing the particle inductivity. The anti-glare film has the advantages that the particles are uniformly dispersed through technical control, the concave-convex structure is formed on the surface of the induction film, the reflection can be reduced, but the size of the concave-convex structure is not controllable, and the flash point is generated in high-resolution display. 3. Due to the fact that different surface energies (containing fluorine and silicon) are utilized, the solvent is volatilized to form the Benard cells to form the concave-convex structure, and the requirement on solvent selection is high. 4. Two or more polymers with different properties are used to form phase separation to form a concave-convex structure.
The existing anti-glare film formed by the anti-glare coating liquid containing the particles simultaneously utilizes the combined action of reducing external light reflection light by utilizing surface roughness and forming haze by utilizing the difference of refractive indexes of the internal particles and resin. However, the anti-glare film prepared by the technology is difficult to have high contrast, and has a flash point (Sparkling) problem.
Disclosure of Invention
The invention aims to provide an anti-glare film, a manufacturing method and a die manufacturing method, and solves the technical problems of low contrast ratio and flash point of the anti-glare film in the prior art.
In order to achieve the above object, the present invention proposes an anti-glare film comprising a light-curing mixture and a heat-curing mixture;
the photocuring mixture comprises a resin prepolymer, an active monomer, a photoinitiator and a leveling agent;
the components of the thermosetting mixture comprise a resin prepolymer, a thermal curing agent, a catalyst, a solvent, an anchoring material and other auxiliary agents;
the ratio of the light-curing mixture to the heat-curing mixture is 5% to 25%.
Alternatively, the content of the components of the anti-glare film is:
5 to 20 percent of resin prepolymer;
10 to 60 percent of active monomer;
0.2 to 5 percent of photoinitiator;
5 to 20 percent of thermal curing agent;
the catalyst comprises the following components: 0.5 to 3 percent;
and (3) leveling agent: 0.01 to 2 percent;
8 to 25 percent of anchoring material;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
Optionally, the resin prepolymer comprises a light-curing prepolymer containing carbon-carbon double bonds, and the light-curing mixture comprises the following components:
the photocuring prepolymer containing carbon-carbon double bonds: 5% -20%;
5 to 80 percent of active monomer;
0.2 to 5 percent of photoinitiator;
leveling agent: 0.01 to 2 percent.
Optionally, the resin prepolymer includes an epoxy oligomer and a phenolic resin, the catalyst is a toughening agent, the anchoring material is nanoparticles, and the thermosetting mixture includes:
5 to 20 percent of epoxy resin oligomer;
5 to 20 percent of phenolic resin;
a toughening agent: 1% -10%;
5 to 20 percent of thermal curing agent;
5 to 20 percent of nano particles;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
The invention also provides a manufacturing method of the anti-glare film, which is used for manufacturing the anti-glare film, and the manufacturing method of the anti-glare film comprises the following steps:
determining a first preset mixture ratio of the light-cured mixture and a second preset mixture ratio of the heat-cured mixture according to the proportion of the light-cured mixture of the anti-glare film and the heat-cured mixture of the anti-glare film and the component content;
preparing a photocuring mixture according to the first preset proportion;
preparing a thermosetting mixture according to the second preset proportion;
mixing the light-cured mixture and the heat-cured mixture according to a first preset proportion to form an anti-glare film material composition;
uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film primary finished product;
introducing a first gas to carry out thermosetting on the primary finished product of the anti-glare film at a first temperature within a first preset time length;
carrying out photocuring on the thermally cured primary finished product of the anti-glare film for a second preset time length at a first preset light intensity;
and placing the primary finished product of the anti-glare film subjected to thermal curing and light curing into plasma for a third preset time length to obtain a finished product of the anti-glare film.
Optionally, the first preset proportioning is: 15 parts by mass of polyester acrylate prepolymer, 5 parts by mass of epoxy acrylate prepolymer, 10 parts by mass of dipentaerythritol hexaacrylate, 35 parts by mass of trimethylolpropane triacrylate, 31.5 parts by mass of tripropylene glycol diacrylate, 3 parts by mass of photoinitiator (819) and 0.5 part by mass of leveling agent.
Optionally, the step of configuring the light-curing mixture according to the first preset ratio includes:
weighing 15 parts by mass of polyester acrylate prepolymer, 5 parts by mass of epoxy acrylate prepolymer, 10 parts by mass of dipentaerythritol hexaacrylate, 35 parts by mass of trimethylolpropane triacrylate and 31.5 parts by mass of tripropylene glycol diacrylate, mixing at a speed of 120r/min-130r/min, stirring for 30 minutes, weighing 3 parts by mass of photoinitiator (819) and 0.5 part by mass of leveling agent, adding into the mixture, continuously stirring for 15 minutes at a speed of 120r/min-130r/min, and standing for defoaming.
Optionally, the second preset proportion is: 15 parts by mass of metal oxide nanoparticles having a particle size of 10 nm are dispersed in 51.9 parts by mass of a mixed solvent of ethyl acetate, 1-methoxy-2-propanol, methyl ethyl ketone and xylene, 3 parts by mass of an epoxy resin oligomer and an epoxy resin oligomer 1210 parts by mass, 68 parts by mass of a phenolic resin ethylene glycol diglycidyl ether, 2.1 parts by mass of a toughening agent, 5 parts by mass of a curing agent 4, 4' -diaminodiphenyl sulfone (DDS), an accelerator 2-methylimidazole (accounting for 0.1% of the epoxy resin), and 5 parts by mass of other auxiliaries.
Optionally, the step of configuring the thermosetting mixture according to the second preset ratio includes:
weighing 15 parts by mass of metal oxide nanoparticles with the particle size of 10 nanometers, dispersing the metal oxide nanoparticles in 51.9 parts by mass of a mixed solvent of ethyl acetate, 1-methoxy-2-propanol, methyl ethyl ketone and xylene, and performing ultrasonic dispersion for 15 minutes to obtain light blue clear liquid. Adding 3 parts by mass of epoxy resin oligomer at a speed of 120r/min-130r/min, and stirring for 120 minutes to enable the epoxy resin oligomer to be modified and coated on the surface of the nano-particles. And then weighing 1210 parts by mass of epoxy resin oligomer, 68 parts by mass of phenolic resin ethylene glycol diglycidyl ether and 2.1 parts by mass of toughening agent, continuously stirring and mixing for 60 minutes, then adding 5 parts by mass of curing agent 4, 4' -Diamino Diphenyl Sulfone (DDS), accelerator 2-methylimidazole (accounting for 0.1 percent of the epoxy resin) and 5 parts by mass of other auxiliary agents, continuously stirring for 15 minutes, and standing for later use.
Optionally, the step of uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film primary finished product comprises:
setting the rotation speed of a spin coater to 300 r/min;
the anti-glare film material composition was coated onto a 250 micron thick PET substrate to form an anti-glare film precursor.
Optionally, the first predetermined ratio is 1:8 or 1:20 or 1:8 or 1: 10.
The invention also provides a manufacturing method of the anti-glare film mold, which comprises the following steps:
aging the primary finished product of the anti-glare film manufactured by the manufacturing method of the anti-glare film to obtain an anti-glare film mold;
carrying out UV transfer printing on the anti-glare film mold to obtain an anti-glare structure film;
coating a UV glue solution on the transferred anti-glare structure film to realize UV curing;
and aging the anti-glare structure film to obtain the anti-glare film mold.
The anti-glare film of the present invention comprises a light-curable mixture and a heat-curable mixture; wherein the photocuring mixture comprises a resin prepolymer, an active monomer, a photoinitiator and a leveling agent; the components of the thermosetting mixture comprise a resin prepolymer, a thermal curing agent, a catalyst, a solvent, an anchoring material and other auxiliary agents; the ratio of the light-curing mixture to the heat-curing mixture is 5% to 25%. Through the scheme, the components of the anti-glare film are improved, the anti-glare film is divided into the light curing mixture and the heat curing mixture, the light curing mixture and the heat curing mixture are respectively matched with different formulas, and finally the light curing mixture and the heat curing mixture are mixed in a special proportion, so that the anti-glare film with the components has the characteristics of high transmittance and high contrast, and simultaneously has no flash point during high-pixel resolution display. Thereby solving the technical problems of lower contrast ratio and flash point of the anti-glare film in the prior art.
Drawings
The invention is further described below with reference to the drawings and examples;
fig. 1 is a product schematic view of an antiglare film in one embodiment.
Fig. 2 is a schematic flow chart illustrating a method for manufacturing the antiglare film in one embodiment.
Detailed Description
Reference will now be made in detail to the present embodiments of the present invention, preferred embodiments of which are illustrated in the accompanying drawings, wherein the drawings are provided for the purpose of visually supplementing the description in the specification and so forth, and which are not intended to limit the scope of the invention.
The invention provides an anti-glare film, a manufacturing method and a die manufacturing method, and aims to solve the technical problems of low contrast ratio and flash point of the anti-glare film in the prior art.
In one embodiment, an anti-glare film is disclosed that includes a light-curable mixture and a heat-curable mixture; the photocuring mixture comprises a resin prepolymer, an active monomer, a photoinitiator and a leveling agent;
the components of the thermosetting mixture comprise a resin prepolymer, a thermal curing agent, a catalyst, a solvent, an anchoring material and other auxiliary agents; the ratio of the light-curing mixture to the heat-curing mixture is 5% to 25%.
According to the scheme, the components of the anti-glare film are improved, the anti-glare film is divided into a light curing mixture and a heat curing mixture, a dual curing scheme is adopted, the light curing mixture and the heat curing mixture are respectively matched with different formulas, finally the light curing mixture and the heat curing mixture are mixed according to a special proportion, the proportion of the light curing mixture to the heat curing mixture is controlled to be 5% -25%, and the anti-glare film produced according to the proportion has the characteristics of high transmittance and high contrast and does not have a flash point during high-pixel resolution display, as shown in a reference figure 1. Thereby solving the technical problems of lower contrast ratio and flash point of the anti-glare film in the prior art.
In one embodiment, the components of the anti-glare film are present in the following amounts:
5 to 20 percent of resin prepolymer;
10 to 60 percent of active monomer;
0.2 to 5 percent of photoinitiator;
5 to 20 percent of thermal curing agent;
the catalyst comprises the following components: 0.5 to 3 percent;
and (3) leveling agent: 0.01 to 2 percent;
8 to 25 percent of anchoring material;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
Through the scheme, the content of each component can be further limited, the component content imbalance caused by too many single components or single pursuit proportion can be avoided, the difficulty of industrial screening of specific proportion can be further reduced, the formula can be flexibly changed according to the price of raw materials or the difficulty level of obtaining in the limited parameter range, and a better effect can be realized when the precision range is lower. The total content of the components of the anti-glare film is 100%.
Alternatively, in the components of the anti-glare film, the resin prepolymer comprises a light-curing prepolymer with a carbon-carbon double bond and an epoxy resin oligomer, and the reactive monomer comprises a reactive monomer with a carbon-carbon double bond and an epoxy reactive monomer. The heat curing agent is selected from polyamine curing agents. The catalyst is an acid catalyst. The anchoring material refers to nanoparticles with polymerizable functional groups modified on the surface. Titanium oxide, zirconium oxide, and silicon oxide are preferable.
Optionally, the resin prepolymer can be prepared by selecting one of the following contents: 5% -10%; 10% -15%; 15 to 20 percent.
Optionally, the reactive monomer may be prepared by selecting one of the following contents: 10% -20%; 20 to 30 percent; 30% -40%; 40% -50%; 50 to 60 percent.
Optionally, the photoinitiator can be prepared by selecting one of the following contents: 0.2% -1%; 1% -2%; 2% -3%; 3% -4%; 4 to 5 percent.
Optionally, the thermal curing agent may be prepared by selecting one of the following contents: 5% -10%; 10% -15%; 15 to 20 percent.
Optionally, the catalyst can be prepared by selecting one of the following contents: 0.5 to 1 percent; 1% -2%; 2 to 3 percent.
Optionally, the leveling agent can be selected from one of the following contents: 0.01 to 0.5 percent; 0.5 to 1 percent; 1% -1.5%; 1.5 to 2 percent.
Optionally, the anchoring material can be selected from one of the following contents to be mixed according to a proportion of 8-10%; 10% -15%; 15% -20%; 20 to 25 percent.
Optionally, the solvent can be selected from one of the following contents to be mixed according to the proportion of 30-40%; 40% -50%; 50% -60%; 60 to 70 percent.
Optionally, the other additives can be selected from one of the following contents in a ratio of 0.5-1%; 1% -1.5%; 1.5 to 2 percent.
It should be noted that the above mixture ratio needs to be selected according to the principle that the light curing mixture and the heat curing mixture are 5% to 25%, and the range can be finely adjusted according to the principle to ensure that the mixture falls in the content of the components of the anti-glare film.
In an alternative embodiment, the resin prepolymer includes a UV light curing (free radical) prepolymer and a heat curing epoxy resin.
The UV light-cured prepolymer is a resin containing carbon-carbon unsaturated double bonds, and comprises unsaturated polyester, polyurethane acrylate resin, epoxy acrylate resin, polyester acrylate and polyether acrylate resin, acrylated acrylate resin, organic silicon acrylate resin and the like. When the materials are proportioned, one or more of the materials can be selected to realize the UV light curing prepolymer. Preferentially, the UV light curing prepolymer is polyurethane acrylate resin, the viscosity range of the UV light curing prepolymer is 10000-20000 mpa.s, and the UV light curing prepolymer can achieve better viscosity and ensure the structural stability after curing.
The prepolymer to be cured by heating is an epoxy resin, and includes glycidyl ether type epoxy resins, bisphenol a type epoxy resins, and the like.
In an alternative embodiment, the reactive monomer comprises an organic molecule containing a carbon-carbon unsaturated double bond, including at least one of a vinyl-containing aliphatic compound, a vinyl-containing aromatic compound, and a compound containing acrylic anhydride, methacrylic anhydride, and the like, and the reactive monomer further comprises an organic molecule containing an epoxy functional group, including but not limited to, ethylene glycol diglycidyl ether, polyglycidyl ether, propylene oxide butyl ether, propylene oxide phenyl ether, diglycidyl ethyl ether, trimethylolpropane propyl ether, and the like.
In an alternative embodiment, the initiator includes a photoinitiator initiated by ultraviolet light and a thermal curing agent initiated by heat to open the epoxy ring, wherein the photoinitiator is selected from free radical photoinitiators, such as 369, 819, 84, TPO (C22H21O2P, trimethylbenzoyl-diphenylphosphine oxide), and the like.
In an alternative embodiment, the thermal curing agent may be a multi-cationic thermal initiator, an acid anhydride, an imidazole, a dicyandiamide such as an aliphatic amine, a polyamide, an alicyclic amine, a modified amine, or the like.
In an alternative embodiment, the catalyst refers to an acid catalyst comprising p-toluenesulfonic acid, dodecylbenzenesulfonic acid, hexafluorophosphoric acid, butylphosphoric acid, derivatives of aromatic phosphates, and various carboxylic acids.
In an alternative embodiment, the anchoring material refers to nanoparticles with polymerizable functional groups for surface modification. The nanoparticles are preferably silicon oxide, zirconium oxide, titanium oxide, but are not limited thereto. The particle diameter of the contained nano-particles is below 0-150nm, and the optimal particle diameter is below 50 nm. The surface of the nano-particle is connected with a modifier through a chemical bond, and the tail end of the modifier is provided with a polymerizable group.
Wherein, the nanoparticles can be inorganic nanoparticles, polymer-inorganic composite nanoparticles, or polymer nanoparticles. The particle diameter of the contained nano-particles is below 0-150nm, and the optimal particle diameter is below 50 nm. The surface of the nano-particle is connected with a modifier through a chemical bond, and the tail end of the modifier is provided with an epoxy group.
In an alternative embodiment, the solvent comprises aliphatic solvents, organic alcohols, lipids, and the like, but is not limited thereto, and preferably a mixture of at least two of ethyl acetate, butyl acetate, methyl ethyl ketone, cyclohexanone, xylene, n-butanol, 1-methoxy-2-propanol, ethylene glycol monobutyl ether, and the like.
In one embodiment, the resin prepolymer comprises a light-curing prepolymer containing carbon-carbon double bonds, and the light-curing mixture comprises the following components:
the photocuring prepolymer containing carbon-carbon double bonds: 5% -20%;
5 to 80 percent of active monomer;
0.2 to 5 percent of photoinitiator;
leveling agent: 0.01 to 2 percent.
By the above embodiments, the photocuring function of the photocuring mixture can be realized. The light-curing prepolymer containing carbon-carbon double bonds can better realize the light-curing process of the anti-glare film, and the anti-glare film mixed with the thermosetting mixture has better physical properties through the photoinitiator, the flatting agent and the active monomer. The component stability of the anti-glare film material is ensured, and the microstructure consistency of the prepared anti-glare film is ensured.
In one embodiment, the resin prepolymer includes an epoxy oligomer and a phenolic resin, the catalyst is a toughening agent, the anchoring material is nanoparticles, and the components of the thermoset mixture include:
5 to 20 percent of epoxy resin oligomer;
5 to 20 percent of phenolic resin;
a toughening agent: 1% -10%;
5 to 20 percent of thermal curing agent;
5 to 20 percent of nano particles;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
By the above embodiment, the thermosetting function of the thermosetting mixture can be achieved. And the anti-glare film mixed with the light curing mixture has better physical characteristics through the toughening agent, the thermal curing agent, the nano particles and the solvent. The component stability of the anti-glare film material is ensured, and the microstructure consistency of the prepared anti-glare film is ensured.
In one embodiment, the anti-glare film is prepared by coating anti-fingerprint liquid (AF) on the surface to prepare an AGAF film or coating a coating with low refractive index and high refractive index on a laminated layer, and then coating the AF liquid to prepare the AGARAF film, and can be used as an anti-glare function protective film on LCD screens, LED screens, OLEDs, QLEDs, Mini LEDs and Micro LEDs high-resolution pixel display screens.
According to the scheme, the anti-glare film can be combined with other functions to form various functional protective films. Can be widely applied to various occasions.
The invention also provides a manufacturing method of the anti-glare film, which is used for manufacturing the anti-glare film as shown in fig. 2, and the manufacturing method of the anti-glare film comprises the following steps:
s1, determining a first preset mixture ratio of the light-cured mixture and a second preset mixture ratio of the heat-cured mixture according to the proportion of the light-cured mixture of the anti-glare film and the heat-cured mixture of the anti-glare film and the component content;
wherein, based on the anti-glare film, the proportion of the light-cured mixture of the anti-glare film and the heat-cured mixture of the anti-glare film is 5-25%, and the component content is 5-20% of the reference resin oligomer; 10 to 60 percent of active monomer; 0.2 to 5 percent of photoinitiator; 5 to 20 percent of thermal curing agent; catalyst: 0.5 to 3 percent; leveling agent: 0.01 to 2 percent; 8 to 25 percent of anchoring material; 30-70% of solvent; 0.5 to 2 percent of other auxiliary agents. According to the two parameters, a plurality of groups of proportions of the photo-curing mixture and the thermosetting mixture can be obtained and respectively set as a first preset proportion and a second preset proportion.
It should be noted that, a set of implementation schemes of the light curing mixture and the heat curing mixture is provided in the anti-glare film, which is only for illustrating the implementation possibilities, and the scheme and the detailed content of the first preset ratio and the second preset ratio at this time cannot be limited accordingly.
S2, preparing a photocuring mixture according to the first preset proportion;
s3, preparing a thermosetting mixture according to the second preset proportion;
s4, mixing the light-cured mixture and the heat-cured mixture according to a first preset proportion to obtain an anti-glare film material composition;
wherein the first predetermined proportion is required to fall within 5-25%, and the conversion is in a form of a ratio of 1:20-1:4, and the anti-glare film material composition is obtained by mixing the materials.
Note that the composition of the antiglare film material at this time is only a preliminary material, and a series of treatments are required to be performed subsequently.
S5, uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film primary finished product;
in an alternative embodiment, the step of uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film precursor comprises: the spin coater is set to rotate at a speed of 300r/min, and the anti-glare film material composition is coated on a PET substrate with the thickness of 250 microns to form an anti-glare film primary finished product.
The substrate includes a sheet or plate of a high molecular polymer, such as PET (polyethylene terephthalate), PC, PMMA, or the like, or glass.
S6, introducing a first gas at a first temperature within a first preset time length to thermally cure the primary finished product of the anti-glare film;
in which the inner layer is cured by thermal curing, and the photo-curing mixture and the thermosetting mixture are mixed in the above process, so that the process of thermal curing is uniformly performed on the primary anti-glare film product when thermal curing is performed.
Taking an alternative embodiment as an example, carbon dioxide is introduced to perform thermal baking curing at a temperature of 80 ℃, the curing time is 30 minutes, that is, the first temperature is 80 ℃, the first preset time length is 30 minutes, and the first gas is carbon dioxide.
S7, carrying out photocuring on the thermally cured primary finished product of the anti-glare film for a second preset time length at a first preset light intensity;
taking an alternative embodiment as an example, the thermally cured anti-glare film primary finished product is taken out and irradiated for 7 seconds by using an ultraviolet electrodeless lamp under the protection of nitrogen atmosphere at a first preset light intensity (light intensity). The first preset light intensity needs to be set according to actual conditions, and the second preset time length can be set to be 7 seconds. It should be noted that the first preset light intensity and the second preset time length may be changed according to the situation. Or taking out the primary finished product of the anti-glare film after heat curing, and irradiating for 7 seconds by using an ultraviolet electrodeless lamp with a full ultraviolet band under the light intensity of 1400mW/cm2 and under the protection of a nitrogen atmosphere.
Wherein, in the above process, the purpose of the light irradiation is to cure the resin uv to form different phase states. In the foregoing process, the light-curing mixture and the thermosetting mixture are mixed, and thus, when the light-curing is performed at this time, the light-curing process is uniformly performed on the primary product of the antiglare film. The primary finished product of the anti-glare film respectively subjected to thermal curing and light curing has a stable internal structure.
It should be noted that the thermal curing and the photo-curing in steps 6 to 7 are dual curing, and dual curing refers to a mixed system of radical photo-initiation curing acrylate and heating curing epoxy resin, and the photo-initiation wavelength band of the UV resin has different absorption peaks from 200nm to 405 nm. The catalyst catalyzes the mutual linking of the resin material and the anchoring material under the external stimulation (UV illumination and heating), and from the anchoring material, a high molecular chain grows, so that a framework film layer with loose outside and a corrugated structure inside is formed. The surface structure of the film layer does not have a wrinkle structure of phase separation AG, and further treatment is needed, so that a skeleton structure is highlighted, and a structure of diffraction optics AG is obtained.
And S8, placing the primary finished product of the anti-glare film after thermal curing and light curing into plasma for a third preset time length to obtain a finished product of the anti-glare film.
The double curing system is heated to cure the inner layer, the material of the UV system is mixed with the material of the thermal solid system to be brought to the surface of the integral material through volatilization of the solvent, and then the UV curing is carried out on the surface of the coating through UV light curing according to the thermally cured bottom layer structure and the thermally cured material doped in the material of the UV system, so that the surface structure which takes the thermally cured material as the core and is formed along the surface grains of the thermally cured material and then subjected to the UV curing is formed. When the solidified solvent is volatilized, the surface is firstly solidified on the bottom layer and then solidified to form a random micro-wrinkle structure on the surface of the film due to different upper and lower solidification rates, and the random micro-wrinkle structure generates an anti-dazzle effect. The plasma bombards and removes loose materials on the surface of the primary finished product of the Anti-glare film subjected to heat drying and UV irradiation, so that a lower skeleton structure is exposed, and a milky film sample with surface grains is obtained, wherein the surface of the sample has an Anti-glare (Anti-glare) structure, and the surface of the Anti-glare film prepared from the material composition has a random micro-wrinkle structure, wherein the line width of a microstructure is 2-6 um, and the line density is about 65-80%. In the above embodiments, based on the principle of diffraction optics and the device structure, the surface of the finished anti-glare film has a random micro-wrinkle structure, as shown in fig. 1, which produces a high haze effect and has high transmittance. Thereby solving the technical problems of lower contrast ratio and flash point of the anti-glare film in the prior art.
In an alternative embodiment, the step of placing the pre-finished anti-glare film product after thermal curing and photo-curing into plasma for a third preset time period to obtain a finished anti-glare film product comprises:
and (3) placing the treated sample in oxygen plasma for treating for 10 minutes, wherein the vacuum degree is 10-3Pa, the plasma frequency is 2.45GHz, and the strength is 260W. The oxygen plasma bombards and removes loose materials on the surface of the membrane after the previous heat drying and light irradiation, so that a lower skeleton structure is exposed, and a milky membrane sample with surface grains is obtained, wherein the surface of the sample has a phase separation AG structure. Wherein, a vacuum environment is required during plasma processing. That is, the chamber is first evacuated to a desired vacuum and then treated with a small amount of oxygen. The frequency and intensity cannot be changed to achieve the AG effect described in this patent. It should be noted that the loose material is the material portion which can not combine with other materials to form a stable dense structure, and the material portion can be removed by bombardment in the oxygen plasma, so that only the dense structure is left.
The oxygen plasma bombards and removes loose materials on the surface of the primary finished product of the anti-glare film subjected to heat drying and light irradiation, so that a lower skeleton structure is exposed, a milky anti-glare film finished product with surface grains is obtained, and the surface of the anti-glare film finished product has a phase separation AG structure. When the anti-glare film is cured by heat curing and light curing, the upper and lower curing rates of the primary finished product of the anti-glare film are different, aggregation motion of nanoparticles is caused by products under different curing conditions, such as core particles after heat curing, so that fluctuation similar to ripples can be formed on the surface of the liquid, the light curing is performed to form a fixed structure in a quick surface drying manner, and the inner layer is heated and cured to form a random micro-wrinkle structure on the surface of the finished product of the anti-glare film.
The contents of the photo-curing prepolymer and the reactive monomer in the resin prepolymer and the particle size of the nanoparticles for anchoring have an influence on the structural size of the random micro-wrinkles on the surface. With the content of the photocuring prepolymer and the active monomer reduced by 5% from 20%, the width size of the random microstructure is reduced to 5-0.5 microns from 20-15 microns; the smaller the particle size of the nanoparticles, the larger the range of random microstructure size adjustment. The particle size is too large, the random degree is reduced, the particles tend to be round and convex, and the particles have flash points when displayed in high pixels. Therefore, the particle size of the nanoparticles is controlled to be less than 200nm, preferably 1 to 50 nm. Meanwhile, the surface of the nano particles is modified with a modifying agent with polymerizable groups, so that the dispersibility of the nano particles in a system is improved, the nano particles are not agglomerated and are not settled, and the particles and a resin material are combined by chemical bonds during polymerization and solidification. The component stability of the anti-glare film material is ensured, and the microstructure consistency of the prepared anti-glare film is ensured.
The haze formed by the random microstructure on the film surface prepared by the anti-glare film material composition is 75-85%, and a light (UV) transfer printing mold can be manufactured on the basis of an anti-glare film finished product through a UV transfer printing mold preparation process. And the depth of the microstructure on the surface of the film is finely adjusted through reprinting and flushing, so that the UV transfer printing mold with different haze can be prepared. Thereby facilitating mass production.
Optionally, the step of placing the heat-cured and light-cured primary finished anti-glare film product into plasma for a third preset time period to obtain a finished anti-glare film product further includes:
coating anti-fingerprint liquid (AF) on the surface of the finished anti-glare film to prepare an AGAF film; or the like, or, alternatively,
and coating a coating with low refractive index and high refractive index on the laminated layer of the finished anti-glare film, and coating AF liquid to prepare the AGARAF film.
By the mode, the finished anti-glare film can be used for LCD screens, LED screens, OLEDs, QLEDs, Mini LEDs and Micro LEDs high-resolution pixel display screens, namely, the anti-glare functional protective film is pasted on the anti-glare film.
Optionally, the first preset proportioning is: 15 parts by mass of polyester acrylate prepolymer, 5 parts by mass of epoxy acrylate prepolymer, 10 parts by mass of dipentaerythritol hexaacrylate, 35 parts by mass of trimethylolpropane triacrylate, 31.5 parts by mass of tripropylene glycol diacrylate, 3 parts by mass of photoinitiator (819) and 0.5 part by mass of leveling agent.
Optionally, the step of configuring the photo-curing mixture according to the first preset ratio includes:
weighing 15 parts by mass of polyester acrylate prepolymer, 5 parts by mass of epoxy acrylate prepolymer, 10 parts by mass of dipentaerythritol hexaacrylate, 35 parts by mass of trimethylolpropane triacrylate and 31.5 parts by mass of tripropylene glycol diacrylate, mixing at a speed of 120r/min-130r/min, stirring for 30 minutes, weighing 3 parts by mass of photoinitiator (819) and 0.5 part by mass of leveling agent, adding into the mixture, continuously stirring for 15 minutes at a speed of 120r/min-130r/min, and standing for defoaming.
The formulation and method of disposing the photocurable mixture are not limited to the specific formulation and method of disposing, and other formulations and methods of disposing may be used under the precondition.
Optionally, the second preset proportioning is: 15 parts by mass of metal oxide nanoparticles having a particle size of 10 nm are dispersed in 51.9 parts by mass of a mixed solvent of ethyl acetate, 1-methoxy-2-propanol, methyl ethyl ketone and xylene, 3 parts by mass of an epoxy resin oligomer and an epoxy resin oligomer 1210 parts by mass, 68 parts by mass of a phenolic resin ethylene glycol diglycidyl ether, 2.1 parts by mass of a toughening agent, 5 parts by mass of a curing agent 4, 4' -diaminodiphenyl sulfone (DDS), an accelerator 2-methylimidazole (accounting for 0.1% of the epoxy resin), and 5 parts by mass of other auxiliaries.
The step of preparing the thermosetting mixture according to the second preset ratio comprises:
weighing 15 parts by mass of metal oxide nanoparticles with the particle size of 10 nanometers, dispersing the metal oxide nanoparticles in 51.9 parts by mass of a mixed solvent of ethyl acetate, 1-methoxy-2-propanol, methyl ethyl ketone and xylene, and performing ultrasonic dispersion for 15 minutes to obtain light blue clear liquid. Adding 3 parts by mass of epoxy resin oligomer at a speed of 120r/min-130r/min, and stirring for 120 minutes to enable the epoxy resin oligomer to be modified and coated on the surface of the nano-particles. And then weighing 1210 parts by mass of epoxy resin oligomer, 68 parts by mass of phenolic resin ethylene glycol diglycidyl ether and 2.1 parts by mass of toughening agent, continuously stirring and mixing for 60 minutes, then adding 5 parts by mass of curing agent 4, 4' -Diamino Diphenyl Sulfone (DDS), accelerator 2-methylimidazole (accounting for 0.1 percent of the epoxy resin) and 5 parts by mass of other auxiliary agents, continuously stirring for 15 minutes, and standing for later use.
The formulation and manner of disposing the thermosetting mixture are not limited to the specific formulation and manner of disposing, and other formulations and manners of disposing may be used under the precondition.
Optionally, the step of uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film primary finished product comprises:
setting the rotation speed of a spin coater to 300 r/min;
the anti-glare film material composition was coated onto a 250 micron thick PET substrate to form an anti-glare film primary finished product.
At the moment, the spin coater is set to rotate at a speed of 300r/min, so that the coating uniformity and the coating thickness can be controlled within a reasonable range, and the influence of the base material on the subsequent photocuring and thermocuring effects can be reduced by coating the anti-glare film material composition on the PET base material with the thickness of 250 micrometers.
Optionally, the first predetermined ratio is 1:8 or 1:20 or 1:8 or 1: 10.
In the first case, the mixture is cured as a photocurable mixture a: and mixing the thermosetting mixture B in a ratio of 1:8, coating and curing the mixture to obtain the anti-glare film.
In the second case, the mixture is cured as a photocurable mixture a: the thermosetting mixture B was mixed in a ratio of 1: 20. The coating and curing are carried out in the same manner as the above steps to obtain the anti-glare film.
In a third case, the ratio of photocurable mixture a: the thermosetting mixture B is mixed in a ratio of 1:8, and 2% of fluorocarbon resin LF710 is added to be stirred, dissolved and dispersed. The coating and curing are carried out in the same manner as the above steps to obtain the anti-glare film.
In the fourth case, the average particle diameter of the metal oxide nanoparticles in the thermosetting mixture B was about 20 nm. The light curing mixture A and the heat curing mixture B are mixed into a just glaring film material composition according to the ratio of 1: 10. The coating and curing are the same as above to obtain the anti-glare film.
In the fifth case, the thermosetting mixture B was mixed at a ratio of 1:5, and stirred to obtain the antiglare film material composition.
The invention also provides a manufacturing method of the anti-glare film mold, which comprises the following steps:
aging the primary finished product of the anti-glare film manufactured by the manufacturing method of the anti-glare film to obtain an anti-glare film mold;
carrying out UV transfer printing on the anti-glare film mold to obtain an anti-glare structure film;
coating a UV glue solution on the transferred anti-glare structure film to realize UV curing;
and aging the anti-glare structure film to obtain the anti-glare film mold.
The following two examples illustrate the application of the antiglare film:
1. preparing an anti-glare film mold: step 1, taking a finished product of the anti-glare film prepared by the anti-glare film manufacturing method as an original film, and aging to prepare an anti-glare film mold; and 2, copying the anti-glare structure film through UV transfer printing. And 3, preparing a UV glue solution, coating the solution on the transferred anti-glare structural film, wherein the depth of the random microstructure can be adjusted to be shallow, and performing UV curing to obtain the anti-glare structural film, wherein the tested haze is about 40%. And 4, aging the anti-dazzle film with the haze of about 40% again to manufacture the anti-dazzle film mold.
2. Anti-glare film applications: preparation of an AGAF film: a silica gel film is selected as a base material, and an anti-glare (AG) structure is copied by using a prepared anti-glare film mold with the haze of 40% through a UV transfer technology (dispensing, glue pressing, curing and separating). And coating a layer of anti-fingerprint (AF) liquid on the surface of the AG structural film by using a spraying process, and baking at 120 ℃ for 30 minutes to obtain the AGAF film. The AGAF film has a hydrophobic angle of more than 110 degrees and good wear resistance. The silicon rubber film back film is removed, and the film can be directly attached to a high-pixel display screen (such as a mobile phone, a computer and the like) to be used as an anti-dazzle protective film.
Optionally, the UV glue solution is an ethanol solution of 2% UV transfer glue. The above is only for illustrating an optional real-time scheme, and in practical application, the structural depth of the UV transfer printing mold can be further finely adjusted by coating a diluted UV glue solution;
for example: 1. changing the thickness of the coating layer by changing the coating pressure, thereby changing the structural depth;
2. by changing the concentration of the solution, for example, after dilution, the thickness of the coating layer is reduced, and the depth of the generated structure is reduced;
3. by changing the material proportion of the solution, the solution has higher viscosity, and the generated structural morphology can be changed.
In the above embodiment, an AG structure mold with different haze (20% -80%) is prepared by using the prepared anti-glare film primary finished product as a master and fine-tuning the structure size of the random micro-wrinkles through an AG structure mold preparation process. Then, the method for manufacturing the anti-glare film for a high pixel resolution screen can be mass-produced by using UV shape transfer printing, and simultaneously, the anti-glare property and high contrast are obtained and the flash point is prevented.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Claims (10)
1. An anti-glare film comprising a light-curable mixture and a heat-curable mixture;
the photocuring mixture comprises a resin prepolymer, an active monomer, a photoinitiator and a leveling agent;
the components of the thermosetting mixture comprise a resin prepolymer, a thermal curing agent, a catalyst, a solvent, an anchoring material and other auxiliary agents;
the ratio of the light-curing mixture to the heat-curing mixture is 5% to 25%.
2. The anti-glare film according to claim 1, wherein the components of the anti-glare film are contained in amounts of:
5 to 20 percent of resin prepolymer;
10 to 60 percent of active monomer;
0.2 to 5 percent of photoinitiator;
5 to 20 percent of thermal curing agent;
the catalyst comprises the following components: 0.5 to 3 percent;
and (3) leveling agent: 0.01 to 2 percent;
8 to 25 percent of anchoring material;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
3. The anti-glare film according to claim 1 or 2, wherein the resin prepolymer comprises a light-curing prepolymer containing a carbon-carbon double bond, and the light-curing mixture comprises:
the photocuring prepolymer containing carbon-carbon double bonds: 5% -20%;
5 to 80 percent of active monomer;
0.2 to 5 percent of photoinitiator;
and (3) leveling agent: 0.01 to 2 percent.
4. The anti-glare film of claim 1 or claim 2, wherein the resin prepolymer comprises an epoxy oligomer and a phenolic resin, the catalyst is a toughening agent, the anchoring material is nanoparticles, and the components of the thermosetting mixture comprise:
5 to 20 percent of epoxy resin oligomer;
5 to 20 percent of phenolic resin;
the toughening agent is as follows: 1% -10%;
5 to 20 percent of thermal curing agent;
5% -20% of the nano particles;
30-70% of solvent;
0.5 to 2 percent of other auxiliary agents.
5. A method for producing an anti-glare film, the method for producing an anti-glare film according to any one of claims 1 to 4, the method comprising:
determining a first preset mixture ratio of the light-cured mixture and a second preset mixture ratio of the heat-cured mixture according to the proportion of the light-cured mixture of the anti-glare film and the heat-cured mixture of the anti-glare film and the component content;
preparing a photocuring mixture according to the first preset proportion;
preparing a thermosetting mixture according to the second preset proportion;
mixing the light-cured mixture and the heat-cured mixture according to a first preset proportion to form an anti-glare film material composition;
uniformly coating the anti-glare film material composition on a substrate to form an anti-glare film primary finished product;
within a first preset time span and at a first temperature, introducing a first gas to carry out thermosetting on the primary finished product of the anti-glare film;
carrying out photocuring on the thermally cured primary finished product of the anti-glare film for a second preset time length at a first preset light intensity;
and placing the primary finished product of the anti-glare film subjected to thermal curing and light curing into plasma for a third preset time length to obtain a finished product of the anti-glare film.
6. The method of manufacturing an anti-glare film according to claim 5, wherein the first predetermined ratio is: 15 parts by mass of polyester acrylate prepolymer, 5 parts by mass of epoxy acrylate prepolymer, 10 parts by mass of dipentaerythritol hexaacrylate, 35 parts by mass of trimethylolpropane triacrylate, 31.5 parts by mass of tripropylene glycol diacrylate, 3 parts by mass of photoinitiator (819) and 0.5 part by mass of leveling agent.
7. The method of making an anti-glare film of claim 5, wherein the second predetermined ratio is: 15 parts by mass of metal oxide nanoparticles having a particle size of 10 nm are dispersed in 51.9 parts by mass of a mixed solvent of ethyl acetate, 1-methoxy-2-propanol, methyl ethyl ketone and xylene, 3 parts by mass of an epoxy resin oligomer and an epoxy resin oligomer 1210 parts by mass, 68 parts by mass of a phenolic resin ethylene glycol diglycidyl ether, 2.1 parts by mass of a toughening agent, 5 parts by mass of a curing agent 4, 4' -diaminodiphenyl sulfone (DDS), an accelerator 2-methylimidazole (accounting for 0.1% of the epoxy resin), and 5 parts by mass of other auxiliaries.
8. The method of claim 5, wherein the step of placing the pre-anti-glare film product after thermal curing and photo-curing into plasma for a third predetermined period of time to obtain a final anti-glare film product further comprises:
coating anti-fingerprint liquid (AF) on the surface of the finished anti-glare film to prepare an AGAF film; or the like, or, alternatively,
and coating a coating with low refractive index and high refractive index on the laminated layer of the finished anti-glare film, and coating AF liquid to prepare the AGARAF film.
9. The method of making an anti-glare film of claim 5, wherein the first predetermined ratio is 1:8, or 1:20, or 1:8, or 1: 10.
10. The manufacturing method of the anti-glare film mold is characterized by comprising the following steps of:
aging the primary finished product of the anti-glare film manufactured by the method for manufacturing the anti-glare film according to any one of claims 5 to 9 to obtain an anti-glare film mold;
carrying out UV transfer printing on the anti-glare film mold to obtain an anti-glare structure film;
coating a UV glue solution on the transferred anti-glare structure film to realize UV curing;
and aging the anti-glare structure film to obtain the anti-glare film mold.
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