CN114076996A - Optical film and preparation method thereof - Google Patents
Optical film and preparation method thereof Download PDFInfo
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- CN114076996A CN114076996A CN202210012356.1A CN202210012356A CN114076996A CN 114076996 A CN114076996 A CN 114076996A CN 202210012356 A CN202210012356 A CN 202210012356A CN 114076996 A CN114076996 A CN 114076996A
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- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
Abstract
The application relates to an optical film and a preparation method thereof, belonging to the technical field of optical films. The preparation method comprises the following steps: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the temperature at the normal temperature for 0.5-1.5 min, drying at the first temperature for 0.5-1 min, drying at the second temperature for 1-2.5 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer. Wherein, the solvent in the high refractive index masking liquid comprises a first solvent capable of eroding the transparent base film, and the mass percentage of the first solvent in the total solvent is 40% or more; the first temperature is less than the second temperature, and the first temperature is less than the boiling point of the solvent. And finally forming a low-refractive-index layer on the surface of the high-refractive-index layer. The optical film prepared by the method can relieve or avoid the generation of interference fringes, can ensure that the antireflection effect of the low-refractive-index layer is better, and can also increase the adhesive force between the high-refractive-index layer and the transparent base film to a certain extent.
Description
Technical Field
The present disclosure relates to the field of optical film technology, and more particularly, to an optical film and a method for manufacturing the same.
Background
In recent years, with the rapid development of display technologies, a thin high-definition display screen is a favorite in the market, and the display screen with high resolution, strong contrast, and colorful colors is diversified, and the display screen with a large visual range angle, a wide color gamut, and a high color reduction degree is emerging continuously, so as to bring colorful visual sensory experience to people.
With the development of artificial intelligence, especially the continuous abundance of vehicle-mounted display contents, portable display devices, such as mobile phones, tablet computers, electronic books, notebook computers, and vehicle-mounted displays, the vehicle-mounted liquid crystal panels are gradually developing toward high definition, high brightness, large size, wide viewing angle, and the like. However, if the outdoor light is strong, the color and definition of the displayed content are often reduced due to the display screen reflecting the external light, which is very disadvantageous to the safe driving of the automobile. Usually, people attach a layer of film for anti-glare treatment on the surface of a display screen to scatter reflected light to different angles, wherein the concave-convex structure on the surface of the anti-glare film can be realized by adding particles into raw materials or mechanically impressing, but the image definition of the anti-glare film subjected to roughening treatment is unsatisfactory.
In order to reduce the influence of external light reflection and weaken the intensity of reflected light, so as to faithfully present the original color and image quality of the display screen, in recent years, composite films with antireflection function are increasingly emerging, and generally, such films are formed by laminating and combining an optically transparent base film, a high refractive index layer (or a hard coating layer) and a low refractive index layer, as shown in fig. 1. When the external incident light irradiates the antireflection composite film through air, the antireflection composite film is formed by combining materials with different refractive indexes, natural light is reflected at the interface of the materials with different refractive indexes, optical path difference is generated by reflected light due to the difference between the refractive indexes and the thicknesses of the materials, and the reflected light can generate interference to form a reflected light intensity offset effect through the composite film designed with different refractive indexes and film thicknesses, so that the intensity of the reflected light can be greatly reduced.
Generally, the larger the difference between the refractive indexes of different materials is, the lower the intensity of the corresponding reflected light is, but if the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is not less than 0.03, interference fringes (such as rainbow fringes shown in fig. 2) can be formed due to the excessively large difference between the refractive indexes of the transparent base film and the high refractive index layer, and actually, the larger the absolute value of the difference between the refractive indexes of the transparent base film and the high refractive index layer is, the more obvious the formed interference fringes are, and the saturation of the image displayed on the display screen can be seriously affected.
Disclosure of Invention
The larger the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is, the easier the interference fringes are formed, and if the refractive index of the high refractive index layer is larger than that of the transparent base film (for example, the transparent base film is a TAC transparent base film or a PMMA transparent base film); meanwhile, the refractive index of the high refractive index layer is larger than that of the low refractive index layer, and the larger the refractive index difference between the high refractive index layer and the low refractive index layer is, the more obvious the antireflection effect is. Since the refractive index of the transparent base film is determined by the properties of the transparent base film itself, once the transparent base film is selected, the refractive index thereof is a certain value, and in order to reduce the refractive index difference between the high refractive index layer and the transparent base film, it is necessary to make the refractive index of the high refractive index layer lower as better; the lower the refractive index of the high refractive index layer is, the smaller the difference between the refractive index of the high refractive index layer and the refractive index of the low refractive index layer is, which is not favorable for the reflection reducing effect of the optical film. Therefore, how to ensure the antireflection effect of the low refractive index layer of the optical film and simultaneously avoid the generation of interference fringes is particularly important for the quality of the optical film.
In view of the above-identified deficiencies, an object of the embodiments of the present application includes providing an optical film and a method for manufacturing the same, which can alleviate or avoid the generation of interference fringes while ensuring that the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is large (the difference between the refractive indexes of the high refractive index layer and the low refractive index layer is also large, and the antireflection effect of the low refractive index layer is good).
In a first aspect, the present application provides a method for preparing an optical film, comprising the steps of: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 0.5-1.5 min, drying at the first temperature for 0.5-1 min, drying at the second temperature for 1-2.5 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer. Wherein, the solvent in the high refractive index masking liquid comprises a first solvent capable of eroding the transparent base film, and the mass percentage of the first solvent in the total solvent is 40% or more; the first temperature is less than the second temperature, and the first temperature is less than the boiling point of the solvent. And finally forming a low-refractive-index layer on the surface of the high-refractive-index layer.
Because the high-refractive-index coating liquid contains the first solvent capable of eroding the transparent base film and the content of the first solvent is high, the high-refractive-index coating liquid is coated on the transparent base film and kept at the normal temperature for 0.5-1.5 min, so that the first solvent can obviously erode the surface of the transparent base film; then drying at a low temperature (first temperature), wherein on one hand, part of the first solvent is slowly volatilized, on the other hand, the rest of the first solvent continuously erodes the surface of the transparent base film, the content of the first solvent eroding the surface of the transparent base film is gradually reduced, and the erosion intensity of the first solvent to the transparent base film is gradually weakened; and then drying at a high temperature (second temperature) to completely volatilize the first solvent without eroding the transparent base film. Therefore, the buffer layer of the irregular micro-concavo-convex structure (namely, the concave-convex structure with stronger initial erosion and weakened erosion after low-temperature drying) can be formed on the surface of the transparent base film, so that incident light is scattered when being reflected at the micro-concavo-convex buffer layer at the interface of the transparent base film and the high-refractive-index layer, and interference fringes can be relieved or avoided while the absolute value of the refractive index difference between the transparent base film and the high-refractive-index layer is larger. Meanwhile, when the transparent base film is corroded by the first solvent, other components in the high-refractive-index coating liquid enter the micro-concavo-convex buffer layer and are cured under the ultraviolet illumination condition, the adhesive force between the cured high-refractive-index layer and the transparent base film is enhanced, and the structural stability of the optical film is improved.
In some embodiments of the present application, the transparent base film is a TAC (Triacetyl Cell μ lose) transparent base film, and the first solvent is at least one of butanone, cyclohexanone, cyclopentanone, ethyl acetate, and methylcyclohexanone.
In some embodiments of the present application, the transparent base film is a PMMA (Polymethyl Methacrylate) transparent base film, and the first solvent is at least one of benzene, toluene, and acetone.
In some examples of the present application, the transparent base film is a CPI (Colorless transparent Polyimide) transparent base film, and the first solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide, and N-methylpyrrolidone.
In some embodiments of the present application, the solid content of the high refractive index coating liquid is 15-25%, and the coating amount of the high refractive index coating liquid is 20-42 g/m2. By matching the solid content and the coating amount, the first solvent can be ensured to erode the transparent base film to have enough etching amountThe etching time for keeping normal temperature and the process control of low-temperature drying are combined, so that the erosion degree of the first solvent to the transparent base film and the speed of other components in the high-refractive-index coating liquid migrating into the micro-concavo-convex buffer layer can be ensured, the finally obtained optical film has light or no interference stripes, and meanwhile, the adhesive force between the high-refractive-index layer and the transparent base film is strong.
In some embodiments of the present application, a method of making a low refractive index layer comprises: coating the low-refractive-index coating liquid on the surface of the high-refractive-index layer, drying at 70-100 ℃ for 1-3 min, and then controlling the oxygen concentration to be less than 500 ppm and the light dose to be 300-500 mj/cm2Ultraviolet irradiation under the conditions of (1) to obtain a low refractive index layer.
The low refractive index layer is relatively thin, and ultraviolet curing reaction is carried out under the low oxygen condition, so that oxygen inhibition is avoided, and the abrasion resistance of the optical film is better.
In some embodiments of the present disclosure, the absolute value of the difference between the refractive indices of the high refractive index layer and the transparent base film is in the range of 0.03 to 0.12, and the refractive index of the high refractive index layer is 0.12 to 0.25 greater than that of the low refractive index layer. The high-refractive-index coating liquid contains a refractive-index adjusting liquid; wherein the refractive index adjusting liquid comprises at least one of a titanium oxide dispersion liquid and a zirconium oxide dispersion liquid.
The refractive index of the high refractive index layer can be adjusted by adding the refractive index adjusting liquid, so that the refractive index of the high refractive index layer is larger; the refractive index difference between the high refractive index layer and the low refractive index layer can be larger and can reach 0.12-0.25; meanwhile, the absolute value of the difference of the refractive indexes between the high-refractive-index layer and the transparent base film is large and can reach 0.03-0.12. However, in combination with the first solvent in the high refractive index layer and the method of manufacturing the high refractive index layer, even if the absolute value of the refractive index difference between the high refractive index layer and the transparent base film is large, the generation of interference fringes can be alleviated or avoided, and the performance of the optical film can be made more excellent.
In some embodiments of the present application, the low refractive index coating liquid has a solid content of 2 to 3%, and the coating amount of the low refractive index coating liquid is 3 to 10 g/m2. By the combination of the solid content and the coating amount, the solid content can be ensuredThe thickness of the low refractive index layer after chemical molding meets the use requirement, and the refractive index is low.
In some embodiments of the present disclosure, the high refractive index coating liquid contains an oligomer, the solvent in the high refractive index coating liquid further includes a second solvent capable of dissolving the oligomer, and the mass percentage of the first solvent in the total solvent is 40 to 70%.
Other second solvents capable of dissolving the oligomer are added into the high-refractive-index masking liquid, so that the oligomer has better fluidity, and in the process of forming the micro concave-convex buffer layer on the surface of the transparent base film, the oligomer can enter the micro concave-convex buffer layer more easily, so that after the high-refractive-index layer is formed by subsequent curing, the bonding force between the high-refractive-index layer and the transparent base film is better.
In some embodiments of the present application, if the first solvent comprises a low boiling point solvent, the second solvent comprises a high boiling point solvent; if the first solvent comprises a high boiling point solvent, the second solvent comprises a low boiling point solvent.
Through the matching use of the high-boiling point solvent and the low-boiling point solvent, the high-refractive-index coating liquid can not cause the local transpiration phenomenon of the solvent due to the fact that the drying temperature is closer to the boiling point temperature of the single solvent, and therefore the probability of forming defects such as whitening, air holes and the like of the optical film is reduced.
In a second aspect, embodiments of the present application provide an optical film prepared by the above preparation method. The optical film has good antireflection effect, and can relieve or avoid the generation of interference fringes while the absolute value of the difference between the refractive indexes of the high-refractive-index layer and the transparent base film is large.
In some embodiments of the present application, the thickness of the transparent base film of the optical film is 25 to 250 μm; the thickness of the high refractive index layer is 3-5
m, the thickness of the low refractive index layer is 0.09-0.11
And m is selected. The thickness of each layer can be such thatThe optical film has good comprehensive performance.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a schematic diagram of light transmission of a prior art optical film;
FIG. 2 is a pictorial representation of a prior art optical film;
FIG. 3 is a process flow diagram of a method for making an optical film according to an embodiment of the present disclosure;
FIG. 4 is a schematic view of light transmission of the optical film provided in example 1 of the present application;
FIG. 5 is a pictorial representation of an optical film provided in example 1 of the present application;
FIG. 6 is a diagram illustrating the evaluation of the magnitude of the reflectivity amplitude;
FIG. 7 is a graph showing a comparison of the reflectance amplitude of an optical film provided in example 1 of the present application and that of comparative example 1;
FIG. 8 is a graph showing a comparison of the reflectance amplitude of an optical film provided in example 1 and comparative example 2 of the present application;
fig. 9 is a graph comparing the reflectivity amplitude of the optical films provided in example 1 and comparative example 3 of the present application.
Detailed Description
In the prior art, generally, the larger the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is, the more easily the interference fringes are formed; the larger the difference between the refractive indexes of the high refractive index layer and the low refractive index layer is, the more obvious the antireflection effect of the optical film is. Then, for some transparent base films, for example: the refracting index on high refracting index layer is greater than the refracting index of transparent base film, in order to reduce the refracting index difference between high refracting index layer and the transparent base film, alleviates or avoids appearing the phenomenon of interference fringe, under the certain circumstances of transparent base film refracting index, generally need reduce the refracting index on high refracting index layer, however, this just makes the refracting index difference on high refracting index layer and low refracting index layer reduce for the effect of the antireflection of optical film is not good. Therefore, the prior art is generally unable to satisfy the requirements of optical films for alleviating or avoiding the contradiction between interference fringes and enhancing the antireflection effect.
The applicant conducts a great deal of research on the basis, and through the preparation method of the optical film and the blending of the components of the high refractive index coating liquid and the low refractive index coating liquid, the optical film can have a better antireflection effect while the interference fringes generated by the optical film are relieved or avoided.
Fig. 3 is a process flow diagram of a method for manufacturing an optical film according to an embodiment of the present disclosure. Referring to fig. 3, the method for manufacturing an optical film provided in the present application includes the following steps:
s110, preparing a high-refractive-index layer: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 0.5-1.5 min, drying at the first temperature for 0.5-1 min, drying at the second temperature for 1-2.5 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer. The high-refractive-index masking liquid comprises an oligomer, a reactive monomer, a photoinitiator and a first solvent. The first solvent can erode the transparent base film, and the mass percentage of the first solvent in the total solvent is 40% or more; the first temperature is less than the second temperature, and the first temperature is less than the boiling point of the solvent.
Because the high-refractive-index coating liquid contains the first solvent capable of eroding the transparent base film and the content of the first solvent is high, the high-refractive-index coating liquid is coated on the transparent base film and kept at the normal temperature for 0.5-1.5 min, so that the first solvent can obviously erode the surface of the transparent base film; then drying at a low temperature (first temperature), wherein on one hand, part of the first solvent is slowly volatilized, on the other hand, the rest of the first solvent continuously erodes the surface of the transparent base film, the content of the first solvent eroding the surface of the transparent base film is gradually reduced, and the erosion intensity of the first solvent to the transparent base film is gradually weakened; and then drying at a high temperature (second temperature) to completely volatilize the first solvent without eroding the transparent base film. Therefore, the buffer layer of the irregular micro-concavo-convex structure (namely, the concave-convex structure with stronger initial erosion and weakened erosion after low-temperature drying) can be formed on the surface of the transparent base film, so that incident light is scattered when being reflected at the micro-concavo-convex buffer layer at the interface of the transparent base film and the high-refractive-index layer, and interference fringes can be relieved or avoided while the absolute value of the refractive index difference between the transparent base film and the high-refractive-index layer is larger. Meanwhile, when the transparent base film is corroded by the first solvent, other components in the high-refractive-index coating liquid enter the micro-concavo-convex buffer layer and are cured under the ultraviolet illumination condition, the adhesive force between the cured high-refractive-index layer and the transparent base film is enhanced, and the structural stability of the optical film is improved.
Alternatively, the method of applying the high refractive index coating liquid may be a slit coating method, a micro-gravure coating method, a blade coating method, a Mayer bar coating method, a roll coating method, and a blade coating method to form the coating layer. If the coating mode is selected from a micro-gravure coating method and a slit coating method, the coating effect can be better.
As an example, the duration of time for which the high refractive index coating liquid is maintained at normal temperature may be 0.5min, 1min, or 1.5 min; the time at the first temperature (low temperature drying) may be 0.5min, 0.8 min or 1 min; the time at the second temperature (high temperature drying) may be 1min, 1.5min, 2min or 2.5 min.
It should be noted that: the solvent in the high refractive index masking liquid can be a single solvent or a mixed solvent, and if the solvent in the high refractive index masking liquid is the single solvent, the first temperature is lower than the boiling point of the single solvent; if the solvent in the high refractive index dope is a mixed solvent, the first temperature is lower than the boiling point of the solvent having the lowest boiling point among the mixed solvents.
In the present application, the conditions of the ultraviolet irradiation may be: the light dose is 350-500 mj/cm2Under the conditions of (1) ultraviolet irradiation. Illustratively, the light dose is 350 mj/cm2、400 mj/cm2、450 mj/cm2Or 500 mj/cm2。
In the application, the thickness of the transparent base film is 25-250 μm; optionally, the thickness of the transparent base film is 25-80 μm, 80-150 μm or 150-250 μm. Illustratively, the transparent base film has a thickness of 25 μm, 30 μm, 40 μm, 60 μm, 80 μm, 100 μm, 125 μm, 188 μm, or 250 μm. If the transparent base film is a TAC (cellulose triacetate) transparent base film, the first solvent is at least one of butanone, cyclohexanone, cyclopentanone, ethyl acetate and methylcyclohexanone; the TAC transparent base film can be etched well.
Alternatively, if the first solvent is butanone or/and ethyl acetate based on the TAC transparent base film, the high refractive index layer is prepared by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 50-70 s, drying at the temperature of 48-52 ℃ for 0.5-1 min, drying at the temperature of 88-92 ℃ for 1.5-2 min, and then performing ultraviolet irradiation to obtain the high-refractive-index layer.
Alternatively, if the first solvent is cyclohexanone or/and methylcyclohexanone based on the TAC transparent base film, the high refractive index layer is prepared by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 1-1.5 min, drying at 68-72 ℃ for 40 s-1 min, drying at 102-107 ℃ for 1-1.5 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer.
Alternatively, if the first solvent is cyclopentanone based on the TAC transparent base film, the high refractive index layer is prepared by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the temperature at the normal temperature for 0.5-1 min, drying at the temperature of 58-62 ℃ for 0.5-1 min, drying at the temperature of 93-97 ℃ for 1.5-2 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer.
If the transparent base film is PMMA (polymethyl methacrylate) transparent base film, the first solvent is at least one of benzene, toluene and acetone; the PMMA transparent base film can be etched well.
Alternatively, if the first solvent is toluene or/and benzene based on a PMMA transparent base film, the high refractive index layer is prepared by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 1-1.5 min, drying at the temperature of 58-62 ℃ for 0.5-1 min, drying at the temperature of 95-105 ℃ for 2-2.5 min, and then carrying out ultraviolet irradiation to obtain the high-refractive-index layer.
Alternatively, if the first solvent is acetone based on a PMMA transparent base film, the high refractive index layer is prepared by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the normal temperature for 1-1.5 min, drying at the temperature of 38-42 ℃ for 40 s-1 min, drying at the temperature of 88-92 ℃ for 1.5-2 min, and then performing ultraviolet irradiation to obtain the high-refractive-index layer.
If the transparent base film is a CPI (transparent polyimide) transparent base film, the first solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the CPI transparent base film can be etched better.
Alternatively, the high refractive index layer is prepared based on the first solvent of the CPI clear base film by: and coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the temperature at the normal temperature for 1-1.5 min, drying at the temperature of 53-57 ℃ for 0.5-1 min, drying at the temperature of 108-112 ℃ for 2-2.5 min, and performing ultraviolet irradiation to obtain the high-refractive-index layer.
In the present application, the monomer is one or more of o-phenylphenoxyethyl acrylate, ethylene glycol dimethacrylate, propoxylated neopentyl glycol diacrylate, propoxylated glycerol triacrylate, 1, 4-butanediol diacrylate, 1, 6-hexanediol diacrylate, trimethylolethane triacrylate, ethoxylated pentaerythritol tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, and dipentaerythritol hexaacrylate.
The photoinitiator is 1-hydroxycyclohexyl phenyl ketone (184), 1' - (methylenebis-4, 1-phenylene) bis [ 2-hydroxy-2-methyl-1-propanone ] (127), 2-hydroxy-methylphenylpropane-1-one (1173), 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-propanone (907), benzoin dimethyl ether (651), 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide (TPO), etc.
In the present application, the oligomer may be one or more of urethane acrylate, epoxy acrylate, polyester acrylate, and pure acrylic acid. Optionally, a second solvent capable of dissolving the oligomer is further added to the high-refractive-index coating liquid, and the mass percentage of the first solvent in the total solvent is 40-70%.
Other second solvents capable of dissolving the oligomer are added into the high-refractive-index masking liquid, so that the oligomer has better fluidity, and in the process of forming the micro concave-convex buffer layer on the surface of the transparent base film, the oligomer can enter the micro concave-convex buffer layer more easily, so that after the high-refractive-index layer is formed by subsequent curing, the bonding force between the high-refractive-index layer and the transparent base film is better.
Illustratively, the first solvent accounts for 70% by mass of the total solvent, and the second solvent accounts for 30% by mass of the total solvent; or the first solvent accounts for 60 percent of the total solvent by mass, and the second solvent accounts for 40 percent of the total solvent by mass; or the first solvent accounts for 50 percent of the total solvent by mass, and the second solvent accounts for 50 percent of the total solvent by mass; or the first solvent accounts for 40 percent of the total solvent by mass, and the second solvent accounts for 60 percent of the total solvent by mass.
Alternatively, if the first solvent comprises a low boiling point solvent, the second solvent comprises a high boiling point solvent; if the first solvent comprises a high boiling point solvent, the second solvent comprises a low boiling point solvent. Through the matching use of the high-boiling point solvent and the low-boiling point solvent, the high-refractive-index coating liquid can not cause the local transpiration phenomenon of the solvent due to the fact that the drying temperature is closer to the boiling point temperature of the single solvent, and therefore the probability of forming defects such as whitening, air holes and the like of the optical film is reduced.
In the application, the solid content of the high-refractive-index coating liquid is 15-25%, and the coating amount of the high-refractive-index coating liquid is 20-42 g/m2. Through the solid content and the coating amount, the erosion degree of the first solvent to the transparent base film can be controlled, so that the adhesive force of the high-refractive-index layer and the transparent base film can be enhanced while interference fringes are reduced or avoided. Illustratively, the high refractive index dope has a solid content of 15%, 18%, 20%, 22%, or 25%; the coating amount of the high refractive index coating liquid is 20 g/m2、25 g/m2、30 g/m2、35 g/m2Or 42g/m2。
By the solids content and coating amount mentioned aboveThe thickness of the high refractive index layer can be controlled to be 3-5
m; as an example, the thickness of the high refractive index layer may be 3
m、3.5 
m、4 
m、4.2 
m、4.4 
m、4.6 
m、4.8 
m or 5
m。
Optionally, a leveling agent can be added into the high-refractive-index coating liquid, and the leveling agent can be one or more of a fluorine leveling agent, an organic siloxane leveling agent and an organic silicon modified acrylic leveling agent. Alternatively, the leveling agent can be BYK-307, BYK-310, BYK-333, BYK 3560, BYK 3565, BYK-377, BYK-378 of Pico chemistry; FTERGENT 602A of Nieuss, Japan; one or more of F-445, F-470, F-479, F-553, F-556 of Dainippon ink Chemicals.
Wherein, if the leveling agent in the high refractive index coating liquid is at least one of BYK 3560, BYK 3565, FTERGENT 602A and F-470, the surface tension of the high refractive index coating liquid is not influenced, and the high refractive index layer formed by adding the leveling agent has excellent recoating performance, and the subsequent low refractive index coating liquid is diluted by a solvent and then added with a common leveling agent, so that the surface of the high refractive index layer can be wetted very easily, and the formed high refractive index layer has good processability.
And S120, forming a low-refractive-index layer on the surface of the high-refractive-index layer. Coating the low-refractive-index coating liquid on the surface of the high-refractive-index layer, drying at 70-100 ℃ for 1-3 min, and then controlling the oxygen concentration to be less than 500 ppm and the light dose to be 300-500 mj/cm2Ultraviolet irradiation under the conditions of (1) to obtain a low refractive index layer.
The low refractive index layer is very thin, and ultraviolet curing reaction is carried out under the low oxygen condition, so that oxygen inhibition is avoided, and the abrasion resistance of the optical film is better.
Alternatively, the method of applying the low refractive index coating liquid may be a slit coating method, a micro-gravure coating method, a blade coating method, a Mayer bar coating method, a roll coating method, and a blade coating method to form the coating layer. If the coating mode is selected from a micro-gravure coating method and a slit coating method, the coating effect can be better.
Illustratively, the drying conditions of the low refractive index dope are: drying at 70 deg.C for 3 min; or drying at 85 deg.C for 2 min; or drying at 100 deg.C for 1 min; the conditions of ultraviolet irradiation were: in the presence of oxygen concentration of 100 ppm and light dose of 350 mj/cm2Ultraviolet irradiation under the conditions of (1); or in the presence of oxygen at a concentration of 200 ppm and a light dose of 400 mj/cm2Ultraviolet irradiation under the conditions of (1); or in the presence of oxygen concentration of 300 ppm and light dose of 450 mj/cm2Ultraviolet irradiation under the conditions of (1); or in the presence of oxygen at 400 ppm and light dose of 500 mj/cm2Under the conditions of (1) ultraviolet irradiation.
In the application, the absolute value of the difference between the refractive indexes of the high-refractive-index layer and the transparent base film is within 0.03-0.12, and the refractive index of the high-refractive-index layer is 0.12-0.25 larger than that of the low-refractive-index layer. The high-refractive-index coating liquid contains a refractive-index adjusting liquid; wherein the refractive index adjusting liquid comprises at least one of a titanium oxide dispersion liquid and a zirconium oxide dispersion liquid. The low refractive index coating liquid contains a low refractive index coating, a solvent and a flatting agent; wherein, the leveling agent can be consistent with the leveling agent in the high-refractive-index coating liquid.
The refractive index of the high refractive index layer can be adjusted by adding the refractive index adjusting liquid, so that the refractive index value of the high refractive index layer is larger; the refractive index difference between the high refractive index layer and the low refractive index layer is larger and can reach 0.12-0.25; meanwhile, the absolute value of the difference between the refractive index of the high-refractive-index layer and the refractive index of the transparent base film is large and can reach 0.03-0.12. However, in combination with the first solvent in the high refractive index layer and the method of manufacturing the high refractive index layer, even if the absolute value of the refractive index difference between the high refractive index layer and the transparent base film is large, the generation of interference fringes can be alleviated or avoided, and the performance of the optical film can be made more excellent.
It should be noted that: the low refractive index coating is a commercially available low refractive index coating such as: SL-023 produced by Japan wasteland chemical, ELCOM P-5062 produced by daily catalytic synthesis, SL-044 produced by Japan wasteland chemical and the like.
Optionally, the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is 0.04-0.11, and the refractive index of the high refractive index layer is 0.15-0.25 larger than that of the low refractive index layer; or the absolute value of the difference between the refractive indexes of the high refractive index layer and the transparent base film is 0.06-0.11, and the refractive index of the high refractive index layer is 0.15-0.2 larger than that of the low refractive index layer.
In the application, the solid content of the low-refractive-index coating liquid is 2-3%, and the coating amount of the low-refractive-index coating liquid is 3-10 g/m2. Through the matching of the solid content and the coating amount, the thickness of the cured low-refractive-index layer can meet the use requirement, and meanwhile, the refractive index of the low-refractive-index layer can be controlled to be lower. Illustratively, the low refractive index dope has a solid content of 2%, 2.2%, 2.4%, 2.6%, 2.8%, or 3.0%; the coating amount of the low refractive index coating liquid is 3 g/m2、5 g/m2、8 g/m2Or 10 g/m2。
Through the limitation of the solid content and the coating amount, the thickness of the low-refractive-index layer can be controlled to be 0.09-0.11
m; illustratively, the low refractive index layer may have a thickness of 0.09
m、0.10 
m or 0.11
m。
The optical film can be prepared by the method, and comprises a transparent base film, a high-refractive-index layer attached to the surface of the transparent base film, and a low-refractive-index layer attached to the surface of the high-refractive-index layer.
In the application, the first solvent capable of eroding the transparent base film is added into the high-refractive-index coating liquid, and when the high-refractive-index layer is prepared, the high-refractive-index coating liquid is placed on one surface of the transparent base film and kept at the normal temperature for 0.5-1.5 min, then is dried at the first temperature for 0.5-1 min, then is dried at the second temperature for 1-2.5 min, then is subjected to ultraviolet irradiation to obtain the high-refractive-index layer (the first temperature is lower than the second temperature, and the first temperature is lower than the boiling point of the solvent), and then is subjected to ultraviolet irradiation to obtain the high-refractive-index layer.
Through the cooperation of the first solvent and the forming method of the high-refractive-index layer, the buffer layer of the irregular micro-concavo-convex structure (namely, the concave-convex structure which is strong in initial erosion and weakened in erosion after keeping at normal temperature) can be formed on the surface of the transparent base film, so that incident light is scattered when being reflected at the micro-concavo-convex structure on the interface of the transparent base film and the high-refractive-index layer, and interference fringes can be relieved or avoided while the absolute value of the difference between the refractive indexes of the transparent base film and the high-refractive-index layer is large.
Optionally, because the high refractive index coating solution further includes a second solvent capable of dissolving the oligomer, in the process of maintaining the normal temperature and drying, the oligomer is easy to enter the micro-concavo-convex structure, and is cured under the ultraviolet irradiation condition, so that the adhesion between the cured high refractive index layer and the transparent base film is enhanced, the bonding force between the high refractive index layer and the transparent base film is better, and the weather resistance of the optical film is improved.
Optionally, since the refractive index adjusting liquid can be added into the high refractive index coating liquid, one of the main components in the low refractive index coating liquid is the low refractive index coating, the refractive index difference between the high refractive index layer and the low refractive index layer can be made larger, and meanwhile, the absolute value of the refractive index difference between the high refractive index layer and the transparent base film is also larger, so that not only can the generation of interference fringes be relieved or avoided, but also the antireflection effect of the low refractive index layer can be made better, and the performance of the optical film can be made more excellent.
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Implement group one
This implementation group provides an optical film, and it includes from the lower supreme transparent base film that stacks gradually and adheres to the high refractive index layer on transparent base film, adheres to the low refractive index layer on the high refractive index layer. The components and some reaction conditions for preparing the optical film are shown in table 1:
TABLE 1 compositions of optical films and partial reaction conditions
The preparation method of the optical film comprises the following steps:
(1) preparing a high-refractive-index coating liquid: mixing the polyurethane acrylate oligomer, the active monomer and the solvent in the table 1 according to the proportion in the table 1, stirring for 35 min, adding the photoinitiator and the leveling agent in the table 1, and continuously stirring for 20 min to prepare the high-refractive-index coating liquid.
(2) Coating the high-refractive-index coating liquid on the surface of the substrate 60
m thick TAC-based film (Korea Xiaoxing)Production, model number: PG 601S), coating amount of the high refractive index coating solution and maintaining time at normal temperature are shown in Table 1, and drying is carried out at 50 deg.C for 0.5min and then at 90 deg.C for 2min, and the passing dose is 350 mj/cm2The high refractive index layer was obtained by ultraviolet irradiation with a high pressure mercury lamp.
(3) Coating low refractive index coating liquid LR1 on the high refractive index layer, drying at 80 deg.C for 2min, and adjusting oxygen concentration to 200 ppm and light dose to 350 mj/cm2The low refractive index layer was obtained under ultraviolet irradiation from a high-pressure mercury lamp.
Carry out group two
This implementation group provides an optical film, and it includes from the lower supreme transparent base film that stacks gradually and adheres to the high refractive index layer on transparent base film, adheres to the low refractive index layer on the high refractive index layer. The components and some reaction conditions for preparing the optical film are shown in table 2:
TABLE 2 compositions of optical films and partial reaction conditions
The preparation method of the optical film comprises the following steps:
(1) preparing a high-refractive-index coating liquid: and mixing the polyurethane acrylate oligomer, the active monomer and the solvent in the table 2 according to the proportion in the table 2, stirring for 35 min, adding the photoinitiator and the leveling agent in the table 2, and continuously stirring for 20 min to prepare the high-refractive-index coating liquid.
(2) Coating the high-refractive-index coating liquid on the surface of the substrate 40
On a TAC base film (manufactured by Konika, Japan, model: KC4 UAW) having a thickness of m, the coating amount of the high refractive index coating liquid, the time for keeping the room temperature and the drying manner are shown in Table 2, and the passing light dose is 350 mj/cm2The high refractive index layer was obtained by ultraviolet irradiation with a high pressure mercury lamp.
(3) Coating low refractive index coating liquid LR1 on the high refractive index layer, drying at 80 deg.C for 2min, and oxygen concentration 150 ppm, light dose at 300 mj/cm2The low refractive index layer was obtained under ultraviolet irradiation from a high-pressure mercury lamp.
Implementation group III
This implementation group provides an optical film, and it includes from the lower supreme transparent base film that stacks gradually and adheres to the high refractive index layer on transparent base film, adheres to the low refractive index layer on the high refractive index layer. The ingredients and some reaction conditions for preparing the optical film are shown in table 3:
TABLE 3 compositions of optical films and partial reaction conditions
The preparation method of the optical film comprises the following steps:
(1) preparing a high-refractive-index coating liquid: and mixing the polyurethane acrylate oligomer, the active monomer and the solvent in the table 3 according to the proportion in the table 3, stirring for 35 min, adding the photoinitiator and the leveling agent, and continuously stirring for 20 min to obtain the high-refractive-index coating liquid.
(2) Coating the high-refractive-index coating liquid on the surface of the substrate 40
On a PMMA substrate film (manufactured by Japan Large House, type: OXIS-ZU), the coating amount of the coating liquid with high refractive index, the time for keeping the temperature at normal temperature and the drying mode are shown in Table 3, and the light dose is 350 mj/cm2The high refractive index layer was obtained by ultraviolet irradiation with a high pressure mercury lamp.
(3) Coating low refractive index coating liquid LR2 on the high refractive index layer, drying at 90 deg.C for 2min, and adjusting oxygen concentration to 350 ppm and light dose to 500 mj/cm2The low refractive index layer was obtained under ultraviolet irradiation from a high-pressure mercury lamp.
Implementation group four
This implementation group provides an optical film, and it includes from the lower supreme transparent base film that stacks gradually and adheres to the high refractive index layer on transparent base film, adheres to the low refractive index layer on the high refractive index layer. The ingredients and some reaction conditions for preparing the optical film are shown in table 4:
TABLE 4 compositions of optical films and partial reaction conditions
The preparation method of the optical film comprises the following steps:
(1) preparing a high-refractive-index coating liquid: and mixing the polyurethane acrylate oligomer, the active monomer and the solvent in the table 4 according to the proportion in the table 4, stirring for 35 min, adding the photoinitiator and the leveling agent, and continuously stirring for 20 min to obtain the high-refractive-index coating liquid.
(2) Coating the high-refractive-index coating liquid on 80
On the CPI base film (manufactured by Kolon, Korea, No. C80) having a thickness of m, the amount of the coating liquid having a high refractive index and the time for maintaining the room temperature are shown in Table 4, dried at 55 ℃ for 0.5min and then at 110 ℃ for 2min, and passed through a light dose of 350 mj/cm2The high refractive index layer was obtained by ultraviolet irradiation with a high pressure mercury lamp.
(3) Coating low refractive index coating liquid LR3 on the high refractive index layer, drying at 95 deg.C for 2min, and adjusting oxygen concentration to 250 ppm and light dose to 450 mj/cm2The low refractive index layer was obtained under ultraviolet irradiation from a high-pressure mercury lamp.
The formulation of the low refractive index dope is shown in table 5:
TABLE 5 formulation of low refractive index coating
Test example 1
Examples 1 to 8 and comparative examples 1 to 7 provide optical films whose production conditions are shown in table 6 and whose properties are shown in tables 7 and 8. Wherein, the calculation method or the test method of each parameter in table 6, table 7 and table 8 is as follows:
table 6 summary of preparation conditions of optical films
Wherein, 1, the proportion (%) of the first solvent in the total solvent:
the weight ratio of the first solvent to the total solvent is calculated, the preparation process of the coating liquid with high refractive index is carried out in a relatively closed container, and the volatilization amount of the solvent is small and negligible.
2. Coating thickness test:
the thickness of the high refractive index layer and the thickness of the low refractive index layer of the optical film were measured using the principle of light diffraction using a german NXT coating thickness gauge ETA-SST thickness measuring system.
3. Transmittance, haze:
the transmittance and haze of the optical film were measured by the transmitted light method using a Japanese electrochromic NDH 2000N haze measuring instrument in accordance with JIS K-7105.
4. Average reflectance (%), average amplitude of reflection band (%):
cutting the optical film sample into 8cm
8cm, sticking a black adhesive tape on the back of the coating, and measuring the average reflectivity of 6-degree angles in a visible light region with the wavelength of 380-780 nm by using a Japan Shimadzu UV-2600i ultraviolet-visible spectrophotometer. As shown in fig. 6, 7, 8 and 9, the average value of the reflectivity difference between the peak and the trough in each amplitude is calculated, which is the average amplitude of the reflection band.
5. Refractive index of the high refractive index layer, refractive index of the low refractive index layer, absolute value of refractive index difference between the high refractive index layer and the transparent base film, refractive index difference between the high refractive index layer and the low refractive index layer:
the refractive indices of the high refractive index layer and the low refractive index layer at a wavelength of 633nm were measured using a U.S. Metricon M-2010 prism coupler using the principle of prism coupling, the refractive index of the transparent base film was supplied by the supplier, and the difference in refractive index was obtained by mathematical calculation.
6. Interference fringes and base film expression:
and (3) attaching optical glue to the back of the membrane in a darkroom with the illumination of 800-1200 lux by using a three-wavelength lamp, attaching the optical glue to a black acrylic plate, observing the appearance of interference fringes of the optical membrane by eyes at an angle of 45-90 ℃ by an inspector and judging according to the following standard.
[ decision criteria ]
No red-green color difference on film surface
Slight red-green color difference delta of film surface
The red-green color difference of the film surface is obvious
7. Adhesion of the high refractive index layer after boiling in water:
and (3) placing the film coated on the surface of the transparent base film and cured to obtain the high-refractive-index layer in boiling water at 100 ℃ for 1 hour, wiping the film, drawing hundreds of grids on the surface of the coating by using a hundreds of grids cutter according to the standard ASTM D-3359, sticking a 3M 600 type adhesive tape on the drawn hundreds of grids, quickly tearing off the adhesive tape in the 180-degree direction, and observing the falling-off condition of the hundreds of grids by using a magnifier.
5B: the coating does not fall off completely;
4B: the drop area of the louver coating is less than 5 percent;
3B: the falling area of the grid coating is 5% -15%;
2B: the falling area of the louver coating is 15-35 percent;
1B: the falling area of the grid coating is 35-65%;
0B: the area of the grid coating falling off is more than 65 percent.
8. Pencil hardness:
the pencil hardness of the optical film was measured using an Elcometer 3086 pencil hardness meter in accordance with the jis k-5600 standard. Measurement method: using a Mitsubishi pencil having a hardness of 2H to 3H, 5 lines were drawn under a load of 750g, and then the presence or absence of scratches of the optical film coating was observed and judged according to the following criteria.
[ decision criteria ]
0-2 scratches determine 'Pass'
3-5 scratches determine 'NG'
9. Steel wool abrasion resistance:
the Shenzhen Zhijia instrument ZJ-339-GSR steel wool resistance tester is used and is 2cm
2cm #0000 Steel wool at 500gf/cm2The surface of the optical film was rubbed back and forth 10 times under the load of (3), and the number of scratches was observed.
[ decision criteria ]
0 strip of scratch
1-10 scratches of delta
Scratch>10 strips
Table 7 properties of optical films provided in examples 1 to 8
Table 8 properties of the optical films provided in comparative examples 1 to 6
FIG. 4 is a schematic view of light transmission of the optical film provided in example 1 of the present application; fig. 5 is a real image of the optical film provided in embodiment 1 of the present application. As can be seen from fig. 4 and 5, the optical film provided in example 1 of the present application has a micro concavo-convex structure on the surface of the transparent base film, and thus the phenomenon of "rainbow texture" does not occur.
FIG. 6 is a diagram illustrating the evaluation of the magnitude of the reflectivity amplitude; FIG. 7 is a graph showing a comparison of the reflectance amplitude of an optical film provided in example 1 of the present application and that of comparative example 1; FIG. 8 is a graph showing a comparison of the reflectance amplitude of an optical film provided in example 1 and comparative example 2 of the present application; fig. 9 is a graph comparing the reflectivity amplitude of the optical films provided in example 1 and comparative example 3 of the present application. As can be seen from fig. 6-9, the larger the reflectivity amplitude of the optical film, the more severe the rainbow patterns; the optical film provided in example 1 is excellent in performance and prevents the occurrence of interference fringes.
As can be seen from the combination of tables 6, 7 and 8, the optical film prepared by the present invention has the advantages of low rainbow patterns, low reflectivity, good abrasion resistance, etc. In comparison with example 1, in comparative example 1, the first solvent is not added, the first solvent is less added in comparative example 2, and the time for maintaining the room temperature is shorter in comparative example 3, under the above conditions, the base film is not etched or the etching degree is light, and the interference fringes on the surface of the optical film are more obvious. Comparative example 4 was maintained at the normal temperature for an excessively long time, so that the base film was excessively etched, causing wrinkles in the base film, affecting the appearance of the optical film. Comparative example 5 is dried at a lower temperature once, the solvent volatilization time is longer, although the base film is etched for a long time, the adhesive force of the optical film after water boiling is smaller and the steel wool friction resistance is weaker because the drying temperature is lower and the high boiling point solvent remains, the appearance of the optical film is also influenced, and the wrinkling phenomenon of the base film can occur. Comparative example 6 was dried at a higher temperature once, the etching of the base film was not significant, and the interference fringes on the surface of the optical film were significant.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (10)
1. A method for preparing an optical film, comprising the steps of:
coating the high-refractive-index coating liquid on one surface of the transparent base film, keeping the temperature at normal temperature for 0.5-1.5 min, then drying at a first temperature for 0.5-1 min, then drying at a second temperature for 1-2.5 min, and then carrying out ultraviolet irradiation to obtain a high-refractive-index layer; wherein, the solvent in the high refractive index masking liquid comprises a first solvent capable of eroding the transparent base film, and the first solvent accounts for 40 percent or more of the total solvent by mass; the first temperature is lower than the second temperature, and the first temperature is lower than the boiling point of the solvent;
and finally forming a low-refractive-index layer on the surface of the high-refractive-index layer.
2. The production method according to claim 1, wherein the transparent base film is a TAC transparent base film, and the first solvent is at least one of butanone, cyclohexanone, cyclopentanone, ethyl acetate, and methylcyclohexanone;
or, the transparent base film is a PMMA transparent base film, and the first solvent is at least one of benzene, toluene and acetone;
or, the transparent base film is a CPI transparent base film, and the first solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
3. The preparation method according to claim 1, wherein the solid content of the high refractive index coating liquid is 15-25%, and the coating amount of the high refractive index coating liquid is 20-42 g/m2。
4. The production method according to claim 1, wherein the production method of the low refractive index layer comprises:
coating the low-refractive-index coating liquid on the surface of the high-refractive-index layer, drying at 70-100 ℃ for 1-3 min, and then controlling the oxygen concentration to be less than 500 ppm and the light dose to be 300-500 mj/cm2Ultraviolet irradiation under the conditions of (1) to obtain a low refractive index layer.
5. The production method according to claim 1, wherein an absolute value of a difference in refractive index between the high refractive index layer and the transparent base film is in a range of 0.03 to 0.12, and the high refractive index layer has a refractive index larger than that of the low refractive index layer by 0.12 to 0.25;
the high-refractive-index coating liquid contains refractive-index adjusting liquid; wherein the refractive index adjusting liquid comprises at least one of a titanium oxide dispersion liquid and a zirconium oxide dispersion liquid.
6. The preparation method according to claim 4, wherein the low refractive index coating liquid has a solid content of 2 to 3%, and the coating amount of the low refractive index coating liquid is 3 to 10 g/m2。
7. The method according to any one of claims 1 to 6, wherein the high refractive index coating liquid contains an oligomer, the solvent in the high refractive index coating liquid further comprises a second solvent capable of dissolving the oligomer, and the first solvent accounts for 40 to 70% by mass of the total solvent.
8. The production method according to claim 7, wherein if the first solvent includes a low boiling point solvent, the second solvent includes a high boiling point solvent;
if the first solvent comprises a high boiling point solvent, the second solvent comprises a low boiling point solvent.
9. An optical film produced by the production method according to any one of claims 1 to 8.
10. The optical film according to claim 9, wherein the thickness of the transparent base film of the optical film is 25 to 250 μm; the thickness of the high refractive index layer is 3-5
m, the thickness of the low refractive index layer is 0.09-0.11
m。
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