CN116184539A - High-definition high-wear-resistance low-reflection film - Google Patents

High-definition high-wear-resistance low-reflection film Download PDF

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Publication number
CN116184539A
CN116184539A CN202211645307.8A CN202211645307A CN116184539A CN 116184539 A CN116184539 A CN 116184539A CN 202211645307 A CN202211645307 A CN 202211645307A CN 116184539 A CN116184539 A CN 116184539A
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low
refraction
coating liquid
parts
refractive
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Inventor
李良彬
刘玉磊
齐海潮
王旭亮
李恒
周通
韩捷
李超
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Hefei Lucky Science and Technology Industry Co Ltd
Institute of Advanced Technology University of Science and Technology of China
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Hefei Lucky Science and Technology Industry Co Ltd
Institute of Advanced Technology University of Science and Technology of China
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Priority to CN202211645307.8A priority Critical patent/CN116184539A/en
Publication of CN116184539A publication Critical patent/CN116184539A/en
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/111—Anti-reflection coatings using layers comprising organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
    • B05D3/065—After-treatment
    • B05D3/067—Curing or cross-linking the coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • B05D5/061—Special surface effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14—Protective coatings, e.g. hard coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2201/00—Polymeric substrate or laminate
    • B05D2201/02—Polymeric substrate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2502/00—Acrylic polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2601/00—Inorganic fillers
    • B05D2601/20—Inorganic fillers used for non-pigmentation effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2601/00—Inorganic fillers
    • B05D2601/20—Inorganic fillers used for non-pigmentation effect
    • B05D2601/22—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2602/00—Organic fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/08—Cellulose derivatives
    • C08J2301/10—Esters of organic acids
    • C08J2301/12—Cellulose acetate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract

The invention belongs to the technical field of optical films, and relates to a high-definition high-wear-resistance low-reflection film, which comprises the following components: the anti-glare optical device comprises a transparent support, and a high-refraction anti-glare layer and a low-refraction layer which are sequentially arranged on one optical surface of the transparent support, wherein the high-refraction anti-glare layer is formed by coating high-refraction coating liquid; the low-refraction layer is formed by coating low-refraction coating liquid; the high-refraction coating liquid contains polyurethane acrylic ester, nanometer high-refraction particles and organic particles; the difference delta n1 of the refractive index of the nanometer high refractive particles and the refractive index of the polyurethane acrylic ester is more than or equal to 0.6; the difference delta n2 between the refractive index of the organic particles and the refractive index of the polyurethane acrylic ester is between-0.05 and 0.02. The low reflection film has the characteristics of high definition and high wear resistance, and can be used for flat screens, special-shaped screens, curved screens and the like of vehicle-mounted display.

Description

High-definition high-wear-resistance low-reflection film
Technical Field
The invention belongs to the technical field of vehicle-mounted display screens, and relates to a high-definition high-wear-resistance low-reflection film.
Background
With the increasing emphasis of energy crisis in recent years, new energy automobiles are rapidly developed. As automobile manufacturers further integrate vehicle-mounted intelligent entertainment functions, the demands for applications such as dashboards, central information displays, and rear-seat entertainment displays have grown. As the display screen becomes larger and the resolution becomes higher, the requirements of people on the definition, high wear resistance, anti-glare and the like of the display screen are increasingly strong. The anti-reflection film is attached or compounded on the surface of the display screen, so that the anti-reflection film is a common solution at present.
The prior art has the anti-reflection function of the film by sputtering or evaporating high refractive inorganic materials such as Nb on the surface of the film 2 O 5 、TiO 2 、Si 3 N 4 Inorganic materials of equal and low refractive index, e.g. SIO 2 、MgF 2 Etc. A film with anti-glare, anti-reflection and anti-fingerprint properties as disclosed in chinese patent CN112694847a, comprising: the anti-glare film comprises a film base layer, an adhesive layer, a release film, an anti-glare layer, an anti-reflection layer and an anti-fingerprint layer; one side of the film base layer is sequentially provided with an adhesive layer and a release film from inside to outside; the other side is provided with an anti-glare layer, an anti-reflection layer and an anti-fingerprint layer from inside to outside in sequence. The sputtering or vapor deposition method for manufacturing the low reflection film has the problems of complex structure, low efficiency and high cost, and the film has high brittleness due to the large use of inorganic materials, and can not be applied to a screen with a large bending angle.
There is also chinese patent CN103314063a which discloses a coating material, an organic-inorganic composite film, and an antireflection member containing an organic-inorganic composite containing inorganic compound particles and a polymer bonded to the above inorganic compound particles. The proportion of voids in the film is 3 to 70% by volume based on the volume of the film. The patent realizes the effect of low reflection by coating a coating containing hollow carbon dioxide on a film through a wet coating process. However, the applicant finds that the surface abrasion resistance of the Chinese patent CN103314063A is poor in the use process in the practical application process.
Therefore, a low reflection film needs to be redesigned to meet the performances of reflection prevention, anti-dazzle, high definition, high wear resistance and the like of the vehicle-mounted display screen.
Disclosure of Invention
The application provides a high-definition and high-wear-resistance low-reflection film which has the characteristics of high definition and high wear resistance and can be used for a planar screen, a special-shaped screen, a curved screen and the like of vehicle-mounted display.
In order to achieve the technical purpose, the technical scheme adopted by the application is as follows:
a high definition, high abrasion resistant, low reflection film comprising: a transparent support, and a high refractive anti-glare layer and a low refractive layer sequentially provided on one optical surface of the transparent support,
the high-refraction anti-glare layer is formed by coating high-refraction coating liquid; the low-refraction layer is formed by coating low-refraction coating liquid;
the high-refraction coating liquid and the low-refraction coating liquid are irradiated by an ultraviolet lamp to be cured into films, and the irradiation energy of the high-refraction coating liquid is 50-120 mJ/cm 2 The irradiation energy of the low-refraction coating liquid is 500-1000 mJ/cm 2 。
As an improved technical scheme of the application, the high-refraction coating liquid comprises the following substances in parts by weight:
30-60 parts of nano high refractive particles;
20-40 parts of organic solvent;
20-40 parts of polyurethane acrylic ester;
0.5-5 parts of organic particles;
0.1-0.5 part of acrylic leveling agent;
0.5-2 parts of photoinitiator, wherein the difference delta n1 between the refractive index of the nanometer high refractive particles and the refractive index of polyurethane acrylic ester is more than or equal to 0.6; the difference delta n2 of the refractive index of the organic particles and the polyurethane acrylic ester is between-0.05 and 0.02.
As the improved technical scheme of this application, after the coating of high refraction coating liquid, through oven drying, then ultraviolet lamp irradiation forms, and the preparation step of high refraction coating liquid is:
(1) Mixing 30-60 parts of nano high refractive particles with 20-40 parts of organic solvent, stirring (0.5-1) for h at the stirring speed of (500-800) r/min, and then putting into a ball mill for ball milling (2-4) h to obtain ball milling liquid;
(2) Adding 20-40 parts of polyurethane acrylic ester into the ball milling liquid, and stirring for 2-4 hours at a stirring speed of (800-1200) r/min;
(3) Reducing the stirring speed to (200-500) r/min, adding 0.5-5 parts of organic particles, 0.1-0.5 part of acrylic leveling agent and 0.5-2 parts of photoinitiator, and stirring (1-2) for h to obtain the high-refraction coating liquid.
As the improved technical scheme of this application, high refraction coating liquid and low refraction coating liquid are through the drying of level four oven, and this oven drying's temperature sets gradually: the temperature of the first-stage oven is 40-60 ℃, the temperature of the second-stage oven is 60-80 ℃, the temperature of the third-stage oven is set to 80-100 ℃, and the temperature of the fourth-stage oven is set to 60-80 ℃.
As an improved technical scheme of the application, the organic particles are selected from one or more of polymethyl acrylate, polyurethane, polybutyl methacrylate and organosilicon in any weight ratio, and the particle size range is 1-3 mu m.
As an improved technical scheme of the application, the nanometer high-refraction particles are zirconium oxide, barium titanate or titanium dioxide, and the particle size range is 20-50 nm.
As an improved technical scheme of the application, the polyurethane acrylic ester is polyurethane (methyl) acrylic resin with the functionality of 6-15.
As an improved technical scheme of the application, the transparent support is a polyethylene terephthalate film (PET), a polymethyl methacrylate film (PMMA) or a cellulose triacetate film (TAC) with a thickness of 25-100 μm.
As an improved technical scheme of the application, the thickness of the high-refraction anti-glare layer is 5-10 mu m; the thickness of the low refractive layer is 80 nm-120 nm.
As an improved technical scheme, the method and the device have application to the display terminal.
Advantageous effects
Compared with the prior art, the difference delta n1 of the refractive index of the nanometer high refractive particles and the refractive index of the polyurethane acrylic ester in the application is more than or equal to 0.6; the difference delta n2 between the refractive index of the organic particles and the refractive index of the polyurethane acrylate is between-0.05 and 0.02. In practical experiments, the anti-dazzle display screen has the anti-dazzle effect, better definition and more vivid screen color under the same haze, and is suitable for vehicle-mounted display.
The high refraction coating liquid adopts 50-120 mJ/cm 2 The ultraviolet lamp of (2) is solidified, and the film forming substance is in a semi-solidified state; the low-refraction coating liquid adopts 500-1000 mJ/cm 2 The ultraviolet lamp is solidified, and the film forming substance in the high-refraction coating liquid can be crosslinked with the film forming substance in the low-refraction coating liquid, so that the high wear resistance is realized.
In conclusion, the low reflection film provided by the application has the characteristics of high definition and high wear resistance, and can be used for flat screens, special-shaped screens, curved screens and the like of vehicle-mounted display.
Drawings
FIG. 1 is a schematic view of the structure of a film according to the present invention.
In the figure: 1: a transparent support; 2: a high refractive anti-glare layer; 3: a low refractive layer; 21: organic particles; 22: nano high refractive particles.
Detailed Description
In order to make the purpose and technical solutions of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present invention fall within the protection scope of the present invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The preparation method of the high-definition high-wear-resistance low-reflection film comprises the following steps of:
(1) preparation of high refractive coating liquid:
(1) Mixing (30-60) parts by weight of nano high refractive particles and (20-40) parts by weight of organic solvent, stirring (0.5-1) for h at a stirring speed of (500-800) r/min, and then putting into a ball mill for ball milling (2-4) h to obtain ball milling liquid;
(2) Adding (20-40) weight parts of aliphatic polyurethane acrylate into the ball milling liquid, and stirring (2-4) for h at a stirring speed of (800-1200) r/min;
(3) Reducing the stirring speed to (200-500) r/min, adding (0.5-5) parts by weight of organic particles, (0.1-0.5) parts by weight of acrylic leveling agent and (0.5-2) parts by weight of photoinitiator, and stirring (1-2) for a h to obtain the high-refraction coating liquid.
(2) Preparation of high refractive anti-glare layer:
coating high-refraction coating liquid on a transparent support by using a gravure or slit mode, and drying by a four-stage oven, wherein the drying temperature of the oven is set as follows: the temperature of the first-stage oven is 40-60 ℃, the temperature of the second-stage oven is 60-80 ℃, the temperature of the third-stage oven is set to 80-100 ℃, and the temperature of the fourth-stage oven is set to 60-80 ℃.
After drying, the energy is 50-120 mJ/cm 2 The ultraviolet lamp is irradiated and solidified to form a film to obtain the high-refraction anti-glare layer.
(3) Preparation of low refractive layer:
coating low-refraction coating liquid on a transparent support by using a gravure or slit mode, and drying by a four-stage oven, wherein the drying temperature of the oven is set as follows: the temperature of the first-stage oven is 40-60 ℃, the temperature of the second-stage oven is 60-80 ℃, the temperature of the third-stage oven is set to 80-100 ℃, and the temperature of the fourth-stage oven is set to 60-80 ℃.
After drying, the energy is 500-1000 mJ/cm 2 The low refractive layer is obtained by irradiating and curing the ultraviolet lamp to form a film.
The ultraviolet rays used for curing the high refractive coating liquid and the low refractive coating liquid in the present invention can be obtained from a high pressure mercury lamp, a fusion H lamp, or a xenon lamp. In order to achieve the semi-cured state of the high refractive coating liquid, the irradiation light quantity of the high refractive coating liquid is preferably 50 to 120mJ/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating low refractive coatingAfter the solution, the irradiation light quantity of the low refractive coating solution is preferably 500 to 1000mJ/cm in order to crosslink the semi-cured high refractive coating solution and the low refractive coating solution together and to achieve a higher degree of crosslinking of the low refractive coating solution 2 。
In order to enable the solvents in the high-refraction coating liquid and the low-refraction coating liquid to be sufficiently dried, and simultaneously, uniformly spreading particles in the high-refraction coating liquid and the low-refraction coating liquid to realize high definition, the high-refraction coating liquid and the low-refraction coating liquid are dried by a four-stage oven, and the drying temperature of the oven is set as follows: the temperature of the first-stage oven is 40-60 ℃, the temperature of the second-stage oven is 60-80 ℃, the temperature of the third-stage oven is set to 80-100 ℃, and the temperature of the fourth-stage oven is set to 60-80 ℃.
The haze of the high-refraction anti-glare layer is 1% -15%; the thickness is 5-10 μm. The thickness is less than 5 μm, and the hardness and scratch resistance are insufficient; the thickness is more than 10 mu m, the toughness is insufficient, and the glass can not be used for special-shaped screens and curved screens for vehicle-mounted display.
In the present invention, the organic particles play a role of scattering light and preventing glare, and may be selected from polymethyl acrylate, polyurethane, polybutylmethacrylate, silicone or a combination thereof. The applicant found on the basis of a large number of experiments that in order to achieve an anti-glare effect and also have a very high definition, the difference deltan 2 between the refractive index of the organic particles and the refractive index of the urethane acrylate is between-0.05 and 0.02, and the particle size range is selected from 1 μm to 3 μm. The organic particles are added in an amount of 0.5 to 5 parts by weight in order to achieve a haze of 1 to 15%.
In the invention, the difference delta n1 of the refractive index of the nanometer high refractive particles and the polyurethane acrylic ester is more than or equal to 0.6, so that the internal haze of the coating can be improved, fewer organic particles are used under the same haze, and the definition of the coating is higher. The nanometer high refractive particles are selected from zirconium oxide, barium titanate or titanium dioxide which are sold in the market, and in order to avoid the definition reduction caused by the scattering of the particles, the particle size of the nanometer high refractive particles is required to be 20 nm-50 nm through a ball milling process. The addition amount of the nanometer high refractive particles is 30 to 60 weight parts.
In the present invention, in order to provide the high refractive anti-glare layer with sufficient abrasion resistance, a commercially available urethane (meth) acrylic resin having a functionality of 6 to 15 is used as the urethane acrylate. The method specifically relates to the following steps: aliphatic urethane hexa (meth) acrylate, aliphatic urethane nona (meth) acrylate, aliphatic urethane dodeca (meth) acrylate, aliphatic urethane penta (meth) acrylate, aromatic urethane hexa (meth) acrylate, aromatic urethane nona (meth) acrylate, aromatic urethane deca (meth) acrylate, aromatic urethane dodeca (meth) acrylate, aromatic urethane penta (meth) acrylate, and the like. The content of urethane acrylate is preferably 20 to 40 parts by weight.
In the present invention, in order to improve the flatness of the high refractive anti-glare layer, the high refractive coating liquid contains a leveling agent, and the leveling agent suitable for the present invention is selected from commercially available acrylic leveling agents, such as: BYK-350, BYK-352, BYK-354, BYK-355, BYK-361N, BYK-390, BYK-392, BYK-394, BYK-399, level 839, etc. The addition amount of the acrylic leveling agent is 0.1 to 0.5 weight part.
In the present invention, the photoinitiator is a raw material commonly used in the art, and two general types of photoinitiators suitable for the present invention are radical polymerization photoinitiators and cationic polymerization photoinitiators. Exemplary photoinitiators are: radical polymerization photoinitiator: 2-hydroxy-methylphenyl propane-1-one (1173), 1-hydroxycyclohexylphenyl ketone (184), 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-propanone (907), benzoin dimethyl ether (651), 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxide (TPO), xylene ketone (BP), 2-Isopropylthioxanthone (ITX), and the like; cationic polymerization photoinitiator: diaryl iodonium salts, triaryliodonium salts, alkyl iodonium salts, isopropylbenzene ferrocenium hexafluorophosphate salts, and the like. Preferred radical polymerization photoinitiators of the invention are, for example, 2-hydroxy-methylphenyl-propan-1-one (1173) and 1-hydroxycyclohexylphenyl-ketone (184). The addition amount of the photoinitiator is 0.5 to 2 parts by weight.
If necessary, an organic solvent is further added to the high refractive coating liquid in the present invention, and a conventional organic solvent may be used without any limitation, for example: aliphatic hydrocarbons such as hexane, heptane and cyclohexane; aromatic hydrocarbons such as toluene and xylene; halogenated hydrocarbons such as dichloromethane and dichloroethane; alcohols such as methanol, ethanol, propanol and butanol; ketones such as acetone, butanone, methyl ethyl ketone, 2-pentanone, and isophorone; esters such as ethyl acetate and butyl acetate; cellosolve-based solvents such as ethyl cellosolve. The organic solvents may be used singly or in combination of two or more.
In the present invention, the low refractive layer is formed by coating a commercially available low refractive coating liquid containing hollow silica and a fluororesin. In order to achieve a reflectivity of less than 1.5, the refractive index of the low refractive layer is between 1.33 and 1.40; the thickness is 80 nm-120 nm.
In the present invention, the high refractive anti-glare layer and the low refractive layer may be coated by a doctor blade coating method, a Mayer bar coating method, a roll coating method, a blade coating method, a slit coating method, and a gravure coating method, and preferably a slit coating method and a gravure coating method.
The transparent support of the present invention is selected from polyethylene terephthalate film (PET), polymethyl methacrylate film (PMMA) or cellulose triacetate film (TAC) and has a thickness of 25 μm to 100. Mu.m.
The high-definition and high-wear-resistance low-reflection film can be used for display terminals, such as mobile phones and computers … …
The present invention will be further described in detail with reference to the accompanying drawings and examples, but the protection of the present invention is not limited to the following examples.
Example 1
(1) Preparation of high refractive coating liquid:
(1) 30 parts by weight of zirconia [ Jining City, kai Xin material Co., ltd; mixing refractive index 2.13 with 20 parts by weight of butanone, stirring at a stirring speed of 500r/min for 0.5h, and then putting into a ball mill for ball milling for 2h to obtain ball milling liquid with the particle size of 50 nm;
(2) Adding 40 parts by weight of polyurethane acrylic ester W4301[ Guangzhou five elements ] into the ball milling liquid; functionality 6; refractive index 1.53], stirring at 800r/min for 2h;
(3) Reducing the stirring speed to 200r/min, and adding 0.5 weight parts of polymethyl acrylate particles [ water chemistry; particle size 1 μm; refractive index 1.49], acrylic leveling agent BYK-350[ Pick ] 0.1 weight part, photoinitiator 184[ Basoff ] 2 weight part, and stirring for 1h to obtain high refractive coating liquid.
(2) Preparation of high refractive anti-glare layer:
the high-refraction coating liquid is coated on a polymethyl methacrylate film [ Longhua ] with the thickness of 40 mu m by using a gravure mode, and is dried by a four-stage oven, wherein the drying temperature of the oven is set as follows: the first stage oven temperature was 40 ℃, the second stage oven temperature was 60 ℃, the third stage oven temperature was set to 80 ℃, and the fourth stage oven temperature was set to 60 ℃.
After drying, the energy is 50mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to obtain a high refractive anti-glare layer having a thickness of 10. Mu.m.
(3) Preparation of low refractive layer:
coating a low-refraction coating liquid SUBEF-40 (New Material technology Co., ltd., shenwei, guangzhou) on the high-refraction anti-glare layer by using a gravure mode, and drying by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 40 ℃, the second stage oven temperature was 60 ℃, the third stage oven temperature was set to 80 ℃, and the fourth stage oven temperature was set to 60 ℃.
After drying, the energy is 1000mJ/cm 2 The film is formed by irradiation and solidification of an ultraviolet lamp to obtain a low refractive layer with the thickness of 120nm and the refractive index of 1.40. The performance was tested and the results are shown in Table 1.
Example 2
(1) Preparation of high refractive coating liquid:
(1) 37 parts by weight of barium titanate (merck); mixing the refractive index of 2.4 and 25 parts by weight of ethyl acetate, stirring for 0.6h at a stirring speed of 600r/min, and then putting into a ball mill for ball milling for 2.5h to obtain ball milling liquid with the particle size of 40 nm;
(2) Adding 35 parts by weight of polyurethane acrylate UA 9050[ Pasteur ] into the ball milling liquid; functionality 8; refractive index 1.51], stirring at 900/min for 2.5h;
(3) Reducing the stirring speed to 300r/min, and adding 1.5 parts by weight of polybutylmethacrylate particles [ water chemistry; particle size 2 μm; refractive index 1.48, acrylic leveling agent BYK-354 (Pick) 0.2 weight parts, and photo initiator TPO (Basoff) 1.6 weight parts, stirring for 1h to obtain high refractive coating liquid.
(2) Preparation of high refractive anti-glare layer:
the high-refraction coating liquid is coated on a polymethyl methacrylate film [ Longhua ] with the thickness of 60 mu m in a slit mode, and is dried by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 45 ℃, the second stage oven temperature was 65 ℃, the third stage oven temperature was set at 85 ℃, and the fourth stage oven temperature was set at 65 ℃.
After drying, the energy is 65mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to obtain a high refractive anti-glare layer having a thickness of 8.5. Mu.m.
(3) Preparation of low refractive layer:
coating a low-refraction coating liquid FNAR-0125 (Ningbo Funa New Material technology Co., ltd.) on the high-refraction anti-glare layer by using a gravure mode, and drying by a four-stage oven, wherein the drying temperature of the oven is set as follows: the first stage oven temperature was 45 ℃, the second stage oven temperature was 65 ℃, the third stage oven temperature was set at 85 ℃, and the fourth stage oven temperature was set at 65 ℃.
After drying, the energy is 850mJ/cm 2 The film is formed by irradiation and solidification of an ultraviolet lamp to obtain a low refractive layer with the thickness of 110nm and the refractive index of 1.38. The performance was tested and the results are shown in Table 1.
Example 3
(1) Preparation of high refractive coating liquid:
(1) 45 parts by weight of titanium dioxide [ DuPont; mixing the refractive index of 2.55 and 30 parts by weight of toluene, stirring for 0.7h at a stirring speed of 650r/min, and then putting into a ball mill for ball milling for 3h to obtain ball milling liquid with the particle size of 35 nm;
(2) Adding 30 parts by weight of polyurethane acrylic ester DPCA-60[ chemical industry; functionality 6; refractive index 1.50], stirring for 3h at a stirring speed of 1000 r/min;
(3) Reducing the stirring speed to 300r/min, and adding 2.5 parts by weight of polyurethane particles [ industrial on root; particle size 2 μm; refractive index 1.45], 0.3 weight part of acrylic leveling agent level 839[ courtesy ], and 1.2 weight parts of photoinitiator 1173[ basf ], and stirring for 1.5h to obtain high-refractive coating liquid.
(2) Preparation of high refractive anti-glare layer:
the high-refraction coating liquid is coated on a cellulose triacetate film [ Kernica ] with the thickness of 25 mu m by using a slit mode, and is dried by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 50deg.C, the second stage oven temperature was 70deg.C, the third stage oven temperature was 90deg.C, and the fourth stage oven temperature was 70deg.C.
After drying, the energy is 85mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to obtain a high refractive anti-glare layer having a thickness of 7.5. Mu.m.
(3) Preparation of low refractive layer:
the low-refraction coating liquid SL023 (barren chemistry) is coated on the high-refraction anti-glare layer in a slit mode, and is dried by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 50deg.C, the second stage oven temperature was 70deg.C, the third stage oven temperature was 90deg.C, and the fourth stage oven temperature was 70deg.C.
After drying, the energy is 750mJ/cm 2 The film is formed by irradiation and solidification of an ultraviolet lamp to obtain a low refractive layer with the thickness of 100nm and the refractive index of 1.36. The performance was tested and the results are shown in Table 1.
Example 4
(1) Preparation of high refractive coating liquid:
(1) 52 parts by weight of titanium dioxide [ DuPont; mixing the ethanol with the refractive index of 2.55 and 35 parts by weight, stirring for 1h at a stirring speed of 700r/min, and then putting the mixture into a ball mill for ball milling for 3.5h to obtain ball milling liquid with the particle size of 25 nm;
(2) Adding 25 parts by weight of polyurethane acrylic ester CN9013NS [ sardol ] into the ball milling liquid; functionality 9; refractive index 1.48], stirring for 3.5h at a stirring speed of 1100 r/min;
(3) 3.5 parts by weight of organosilicon particles [ Yongqi materials technology (Shanghai) Co., ltd.) are added; particle size 2 μm; refractive index 1.43], 0.4 weight part of acrylic leveling agent BYK-361N [ Pick ], 0.8 weight part of photoinitiator 907[ Basoff ], and stirring for 2 hours to obtain high-refractive coating liquid.
(2) Preparation of high refractive anti-glare layer:
the high refractive coating liquid was coated on a polyethylene terephthalate film [ lerkic ] having a thickness of 75 μm using a gravure method, and was dried by a four-stage oven at the following drying temperatures: the first stage oven temperature was 55deg.C, the second stage oven temperature was 75deg.C, the third stage oven temperature was 95deg.C, and the fourth stage oven temperature was 75deg.C.
After drying, the energy is 100mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to obtain a high refractive anti-glare layer having a thickness of 6. Mu.m.
(3) Preparation of low refractive layer:
coating low-refraction coating liquid ABC-B80-55[ Nanjing grain materials science and technology Co., ltd.) on the high-refraction anti-glare layer by using a gravure mode, and drying by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 55deg.C, the second stage oven temperature was 75deg.C, the third stage oven temperature was 95deg.C, and the fourth stage oven temperature was 75deg.C.
After drying, the energy is 650mJ/cm 2 The film is formed by irradiation and solidification of an ultraviolet lamp to obtain a low refractive layer with the thickness of 90nm and the refractive index of 1.34. The performance was tested and the results are shown in Table 1.
Example 5
(1) Preparation of high refractive coating liquid:
(1) 60 parts by weight of zirconia [ merck; mixing the refractive index of 2.13 and 40 parts by weight of butyl acetate, stirring for 1h at a stirring speed of 800r/min, and then putting into a ball mill for ball milling for 4h to obtain ball milling liquid with the particle size of 20 nm;
(2) Adding 20 parts by weight of polyurethane acrylic ester 6196-100[15 ] functionality into the ball milling liquid; a changxing chemistry; refractive index 1.47], stirring for 4 hours at a stirring speed of 1200 r/min;
(3) Reducing the stirring speed to 500r/min, and adding 5 parts by weight of polymethyl acrylate [ fully ground; particle size 3 μm; refractive index 1.49], acrylic leveling agent BYK-392[ Pick ] 0.5 weight parts, photoinitiator 651[ Basoff ] 0.5 weight parts, stirring for 2 hours to obtain high refractive coating liquid.
(2) Preparation of high refractive anti-glare layer:
the high-refraction coating liquid is coated on a polyethylene terephthalate film [ Lekai ] with the thickness of 100 mu m by using a gravure mode, and is dried by a four-stage oven, wherein the drying temperature of the oven is set as follows: the first stage oven temperature was 60 ℃, the second stage oven temperature was 80 ℃, the third stage oven temperature was set to 100 ℃, and the fourth stage oven temperature was set to 80 ℃.
After drying, the energy is 120mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to obtain a high refractive anti-glare layer having a thickness of 5. Mu.m.
(3) Preparation of low refractive layer:
coating a low-refraction coating liquid HFC-1[ anti-coating ] on a high-refraction anti-glare layer in a gravure mode, and drying by a four-stage oven, wherein the drying temperature of the oven is sequentially set as follows: the first stage oven temperature was 60 ℃, the second stage oven temperature was 80 ℃, the third stage oven temperature was set to 100 ℃, and the fourth stage oven temperature was set to 80 ℃.
After drying, the energy is 500mJ/cm 2 The film was cured by irradiation with an ultraviolet lamp to give a low refractive layer having a thickness of 80nm and a refractive index of 1.33. The performance was tested and the results are shown in Table 1.
Comparative example 1
The same procedure as in example 1 was employed, and the energy of the ultraviolet lamp irradiating the high refractive coating liquid was changed from 50mJ/cm 2 Is changed to 500mJ/cm 2 Its performance was tested.
Comparative example 2
The same procedure as in example 5 was used to test the properties of the high refractive index coating liquid without adding zirconia particles.
The test method of each performance is as follows:
(1) Refractive index
The level difference meter test was performed using the prince KOBRA.
(2) Reflectivity of
Measured according to the method defined in JIS Z8722. The reflectance at 380nm to 780nm was measured, and the average value was taken as the test result.
(3) Definition of definition
Measured according to the method specified in ASTM D1003.
(4) Haze degree
Measured according to the method specified in GB/T2410.
(5) Wear resistance
The number of rubs when scratches were generated was recorded by measuring the steel wool by the method specified in HG/T4303 using 0000#, and loading 1 kg.
Table 1: test data sheet for each embodiment
Δn1 Δn2 Reflectivity of Definition of definition Haze degree Wear resistance
Example 1 0.6 -0.04 1.45％ 94％ 1％ 220 times
Example 2 0.89 -0.03 1.34％ 88％ 3％ 200 times
Example 3 1.05 -0.01 1.26％ 82％ 7％ 190 times
Example 4 1.07 -0.05 1.03％ 76％ 12％ 150 times
Example 5 0.66 0.02 0.95％ 73％ 15％ 130 times
Comparative example 1 0.6 -0.04 1.44％ 93％ 1％ 50 times
Comparative example 2 / 0.02 0.98％ 62％ 11％ 120 times
The foregoing is a description of embodiments of the invention, which are specific and detailed, but are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.

Claims (10)

1. A high definition, high abrasion resistant, low reflection film comprising: a transparent support, and a high refractive anti-glare layer and a low refractive layer sequentially provided on one optical surface of the transparent support, characterized in that,
the high-refraction anti-glare layer is formed by coating high-refraction coating liquid; the low-refraction layer is formed by coating low-refraction coating liquid;
the high-refraction coating liquid and the low-refraction coating liquid are irradiated by an ultraviolet lamp to be cured into films, and the irradiation energy of the high-refraction coating liquid is 50-120 mJ/cm 2 The irradiation energy of the low-refraction coating liquid is 500-1000 mJ/cm 2 。
2. The high-definition, high abrasion-resistant and low reflection film according to claim 1, wherein said high refraction coating liquid comprises the following substances in parts by weight:
30-60 parts of nano high refractive particles;
20-40 parts of organic solvent;
20-40 parts of polyurethane acrylic ester;
0.5-5 parts of organic particles;
0.1-0.5 part of acrylic leveling agent;
0.5-2 parts of photoinitiator;
the difference delta n1 of the refractive index of the nanometer high refractive particles and the refractive index of the polyurethane acrylic ester is more than or equal to 0.6;
the difference delta n2 between the refractive index of the organic particles and the refractive index of the polyurethane acrylic ester is between-0.05 and 0.02.
3. The high-definition, high-abrasion-resistance and low-reflection film according to claim 1, wherein the high-refraction coating liquid is prepared by the steps of:
(1) Mixing 30-60 parts of nano high refractive particles with 20-40 parts of organic solvent, stirring (0.5-1) for h at the stirring speed of (500-800) r/min, and then putting into a ball mill for ball milling (2-4) h to obtain ball milling liquid;
(2) Adding 20-40 parts of polyurethane acrylic ester into the ball milling liquid, and stirring for 2-4 hours at a stirring speed of (800-1200) r/min;
(3) Reducing the stirring speed to (200-500) r/min, adding 0.5-5 parts of organic particles, 0.1-0.5 part of acrylic leveling agent and 0.5-2 parts of photoinitiator, and stirring (1-2) for h to obtain the high-refraction coating liquid.
4. A high definition, high abrasion resistant, low reflection film according to claim 2 or 3 wherein said high refractive coating fluid and low refractive coating fluid are dried by a four stage oven, the oven drying temperature being set in sequence: the temperature of the first-stage oven is 40-60 ℃, the temperature of the second-stage oven is 60-80 ℃, the temperature of the third-stage oven is set to 80-100 ℃, and the temperature of the fourth-stage oven is set to 60-80 ℃.
5. A high definition, high abrasion resistant, low reflection film according to claim 2 or 3 wherein said organic particles are selected from the group consisting of polymethyl acrylate, polyurethane, polybutyl methacrylate, and silicone, or any combination thereof, having a particle size in the range of 1 μm to 3 μm.
6. A high definition, highly abrasion resistant, low reflection film according to claim 2 or 3 wherein said nano high refractive particles are zirconia, barium titanate or titanium dioxide having a particle size in the range of 20nm to 50nm.
7. A high definition, high abrasion resistant low reflection film according to claim 2 or 3 wherein said urethane acrylate is a urethane (meth) acrylic resin having a functionality of 6 to 15.
8. The high-definition, high abrasion-resistant low reflection film according to claim 1, wherein said transparent support is a polyethylene terephthalate film (PET), a polymethyl methacrylate film (PMMA) or a cellulose triacetate film (TAC) having a thickness of 25 μm to 100 μm.
9. The high-definition, high abrasion-resistant, low reflection film according to claim 1, wherein the high refractive anti-glare layer has a thickness of 5 μm to 10 μm; the thickness of the low refractive layer is 80 nm-120 nm.
10. A high definition, high abrasion resistant low reflection film according to any of claims 1-3, 8-9, having application to display terminals.
CN202211645307.8A 2022-12-20 2022-12-20 High-definition high-wear-resistance low-reflection film Pending CN116184539A (en)

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