CN114153012A - Anti-dazzle hardening film for vehicle-mounted display and preparation method thereof - Google Patents
Anti-dazzle hardening film for vehicle-mounted display and preparation method thereof Download PDFInfo
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- CN114153012A CN114153012A CN202111527623.0A CN202111527623A CN114153012A CN 114153012 A CN114153012 A CN 114153012A CN 202111527623 A CN202111527623 A CN 202111527623A CN 114153012 A CN114153012 A CN 114153012A
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Images
Classifications
-
- 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
-
- 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
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Optical Elements Other Than Lenses (AREA)
- Surface Treatment Of Optical Elements (AREA)
Abstract
The invention belongs to the field of films, and relates to an anti-glare hardened film for vehicle-mounted display and a preparation method thereof. The first coating is formed by curing a coating liquid consisting of polyurethane acrylic resin, a multifunctional monomer, a photoinitiator, a leveling assistant, a dispersant, an organic solvent and organic particles, and the second coating is formed by curing a coating liquid consisting of polyurethane acrylic resin, a photoinitiator and an organic solvent, wherein the coating thickness H1 of the first coating is 2-10 μm, the particle size of the organic particles of the first coating is 3-15 μm, the average roughness Ra of the first coating is 0.1-0.5 μm, and the coating thickness H2 of the second coating satisfies the following relational expression: H2-Ra is more than or equal to 0.1 and less than or equal to 1 mu m. The anti-dazzle hardening film provided by the invention has excellent scratch resistance, anti-dazzle property and high fineness, and solves the problem of poor post-processing adhesion of the anti-dazzle hardening film.
Description
Technical Field
The invention relates to the technical field of protective films, in particular to an anti-dazzle hardening film for vehicle-mounted display and a preparation method thereof.
Background
When the liquid crystal display panel and the touch panel are used, when external light such as an indoor fluorescent lamp or sunlight is incident on the surface of the display device, strong glare is generated, which causes visual discomfort, and the display feeling of visibility is also reduced by reflection or reflection. Therefore, in order to suppress this, an anti-glare treatment is generally applied to the surface of the image display device. Particularly, with the popularization of vehicle-mounted display screens and the increase of the sizes of the display screens, the requirements on the display effect are higher in combination with the application scenes, and besides the traditional anti-glare effect, the definition of the display picture is also required. In order to prevent the contrast and the visibility from being reduced due to the reflection of external light or the mapping of images, the visibility is reduced more obviously particularly in the outdoor lighting scene. Therefore, in order to reduce the image reflection and reflectance using the principle of optical interference, an antireflection layer is generally provided on the outer side of the in-vehicle display panel. At present, most of display screen cover plates of high-end automobiles or new energy automobiles are glass, and in order to prevent glass from splashing and prevent the effects of anti-dazzle and anti-reflection in accidents, a layer of functional film with high hardness, anti-dazzle high definition and anti-reflection is usually attached to the outer side of the glass cover plate at present.
In contrast, a common practice of such a functional thin film is to use a composite film in which an antiglare hard coat layer and an antireflection layer are formed in this order on a transparent substrate. The anti-reflection layer is formed by sputtering a low refractive index layer and a high refractive index layer on the surface of the anti-glare hard coating layer, and the material of the high/low refractive index layer formed by sputtering is generally SiN or TiO2、Nb2O5、Ta2O5、MgF2、SiO2And the like. High molecular polymer and organic particleThe formed anti-dazzle hard coating and the sputtering anti-reflection layer formed by inorganic components have poor adhesion, especially the requirement on the adhesion is higher after long-time outdoor use, so that the AR layer falls off after the anti-dazzle hard coating and the sputtering anti-reflection layer are used for a long time in vehicle display or screen display, the display screen is uneven, and the anti-reflection effect disappears.
Therefore, the application provides a new technical scheme to solve the problem that the anti-dazzle hardened layer is not good in adhesive force with subsequent coating processing, and simultaneously achieves the effects of preventing glass from splashing and preventing dazzle and increasing the transmittance.
Disclosure of Invention
The invention aims to provide an anti-dazzle hardening film for vehicle-mounted display and a preparation method thereof, and the obtained protective film has high stiffness, low shrinkage and high temperature resistance.
In order to solve the technical problems, the invention adopts the technical scheme that: an anti-glare hardened film for vehicle-mounted display comprises a transparent support, and a first coating and a second coating sequentially coated on one surface of the transparent support;
the first coating is formed by curing a coating liquid, and the coating liquid comprises the following substances in parts by weight:
wherein the coating thickness H1 of the first coating is 2-10 μm, and the average roughness Ra of the first coating is 0.1-0.5 μm;
the second coating is formed by coating and curing a coating liquid prepared from the following components in parts by weight:
48-58 parts of polyurethane acrylic resin
1-8 parts of photoinitiator
35-50 parts of an organic solvent,
wherein the coating thickness H2 of the second coating satisfies the relationship: H2-Ra is more than or equal to 0.1 and less than or equal to 1 mu m.
As a modified technical scheme of the application, the particle size of the organic particles of the first coating is 3-15 μm.
As an improved technical scheme of the application, the polyfunctional monomer is one of ditrimethylolpropane tetraacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate or dipentaerythritol hexaacrylate.
As an improved technical scheme of the application, the leveling auxiliary agent in the first coating is an acrylate leveling agent.
As an improved technical scheme of the application, the organic particles in the first coating are monodisperse organic particles or medium disperse organic particles.
As an improved technical scheme of the application, the solid content of the coating liquid of the second coating layer is 50-60%, and the viscosity of the coating liquid is 30-50 cps.
As an improved technical scheme of the application, the number average molecular weight of the polyurethane acrylic resin in the second coating layer coating liquid is 2000-5000.
As an improved technical scheme of the application, the boiling point of the organic solvent in the second coating layer coating liquid is 110-153 ℃.
As an improved technical scheme of the application, the haze range of the anti-dazzle hardening film is 1-50%.
As an improved technical scheme of the application, the transparent support is one of PET, TAC, PMMA, SRF and COP, and the thickness of the transparent support is 25-100 mu m.
Another object of the present invention is to provide a method for preparing an anti-glare hardened film for vehicle-mounted display, the anti-glare hardened film comprising a second coating layer, a first coating layer and a transparent support in this order from top to bottom, the method comprising the steps of:
preparing a first coating: coating a coating liquid for forming a first coating on a transparent support, drying and carrying out ultraviolet curing to obtain the coating liquid; the haze of the first coating is 2% -60%;
preparing a second coating: coating a second coating layer coating liquid on the surface of the first coating layer, drying and carrying out UV curing to obtain the coating; the second coating is formed after being dried by a multi-stage drying oven and cured by ultraviolet light, and the temperature of the first-stage drying oven is set to be 25-50 ℃; the temperature of the second-stage oven is 40-60 ℃, and the temperature of the third-stage oven is 80-100 ℃;
the UV energy of the ultraviolet light curing first coating and the second coating is 500mJ/cm2～1000mJ/cm2。
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a two-layer structure, the coating thickness and the particle size are optimized, so that the average roughness of the first coating satisfies the condition that Ra is more than or equal to 0.1 mu m and less than or equal to 0.5 mu m, and the thickness of the second coating H2 satisfies the relation that H2-Ra is more than or equal to 0.1 and less than or equal to 1 mu m, so that the anti-dazzle hardening film has excellent anti-dazzle effect and higher definition, and is particularly suitable for surface protection of vehicle-mounted display.
2. According to the invention, the second coating is formed on the surface of the first coating, and the coating is uniformly formed on the surface of the organic particles of the first coating by controlling the viscosity and the surface tension of the coating liquid and optimizing the drying process, so that the downstream anti-reflection coating has better adhesive force when being sputtered, and the problem of poor adhesive force after the coating on the surface of the organic particles is solved.
In conclusion, the anti-glare hardened film for vehicle-mounted display has the comprehensive performance of anti-glare property and high definition, and has the advantage of excellent adhesion of reprocessed coating compared with the anti-glare hardened film in the prior art.
It should be understood that all combinations of the foregoing concepts and additional concepts described in greater detail below can be considered as part of the inventive subject matter of this disclosure unless such concepts are mutually inconsistent.
The foregoing and other aspects, embodiments and features of the present teachings can be more fully understood from the following description taken in conjunction with the accompanying drawings. Additional aspects of the present invention, such as features and/or advantages of exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of specific embodiments in accordance with the teachings of the present invention.
Drawings
The drawings are not intended to be drawn to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures may be represented by a like numeral. For purposes of clarity, not every component may be labeled in every drawing. Embodiments of various aspects of the present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a schematic structural view of an antiglare cured film for on-vehicle display in the present invention.
In the drawings, each reference numeral indicates 1: a transparent support; 2: a first coating layer; 3: a second coating layer; 4: organic particles.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The structural schematic diagram of the antiglare hardened film for vehicle display in the present invention is shown in fig. 1, in which: a transparent support 1; a first coating layer 2; a second coating layer 3; organic particles 4.
The transparent support selected by the invention comprises plastic films or thin plates such as polyethylene terephthalate (PET), cellulose triacetate film (TAC), polymethyl methacrylate (PMMA), super-birefringence polyester film (SRF), cycloolefin polymer film (COP) and the like. In view of display effect and price cost, a TAC film or an SRF film is preferable. The transparent support of the present invention has a thickness of 25 μm to 100 μm, and preferably a thickness of 40 μm to 80 μm. The object is that if the transparent support is too thin, the coating of the anti-glare hardened coating layer is likely to cause appearance problems such as streaks and warpage, and if the transparent support is too thick, the cost is high and the tendency of thinning of the display is not favorable.
The first coating of the invention contains ultraviolet light cured resin (polyurethane acrylic resin), photoinitiator, solvent, organic particles and other coating liquid which is cured under the ultraviolet light condition, and the ultraviolet light cured resin suitable for the invention comprises polyurethane acrylic resin and polyfunctional monomer. The anti-dazzle hardening film is attached to the surfaces of a central control screen and an instrument screen of vehicle-mounted display, and people often remove the touch screen by hands in the use process, so that the coating needs to have higher hardness and scratch resistance. The polyurethane acrylic resin can be selected from aliphatic polyurethane acrylic resin or aromatic polyurethane acrylic resin with the functionality of more than 6, and the higher functionality can improve the crosslinking density of the resin coating, so that the coating has higher hardness and scratch resistance. Since the first coating layer is coated with the second coating layer, which is required to have a good spreading on the first coating layer, the multifunctional monomer in the first coating layer is selected from acrylate monomers containing hydroxyl groups, such as di-trimethylolpropane tetraacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate or dipentaerythritol hexaacrylate. In order to ensure the scratch resistance of the first coating, the polyurethane acrylic resin in the first coating has better crosslinking density after curing reaction, so that the excellent scratch resistance is provided, but the basic performance of the coating is reduced after the acrylate monomer is added. The functionality of the acrylate monomer, the reaction rate and the amount added are taken into consideration at this time. In summary, in the first coating formulation provided by the present invention, the amount of the urethane acrylic prepolymer is controlled to be 10 parts by weight to 20 parts by weight, and the amount of the polyfunctional monomer is controlled to be 30 parts by weight to 60 parts by weight.
The second coating is arranged on the surface of the first coating, the leveling property and the construction property of a resin coating and particles in the first coating are required, a leveling agent must be added into the formula of the first coating, the first coating needs to have higher surface tension, the first coating selects a leveling agent which does not reduce the surface tension of the coating, the acrylic leveling agent is preferred, and BYK-350, BYK-355, BYK-390 and the like of Pico chemistry can be selected.
In the present invention, an organic solvent is added to the coating liquid of the first coating layer, and the organic solvent is selected from: alcohols such as methanol, ethanol, propanol; ketones such as acetone, butanone, methyl isobutyl ketone; or esters such as ethyl acetate, butyl acetate, ethyl propionate.
The anti-dazzle hardening film is used in the field of vehicle-mounted display, and the reprocessing of the anti-dazzle hardening film comprises two methods, wherein one method is mainly to carry out vacuum sputtering of an anti-reflection layer (AR) on the surface of an anti-dazzle hardening coating, the method is a mainstream method, and a small part of method is also carried out to carry out wet coating of a low reflection Layer (LR). Because the dry implementation of vacuum sputtering does not reduce the scratch resistance of the coating surface, while the wet implementation of coating a low-reflection layer reduces the scratch resistance of the coating, which is not suitable for the use scene of finger touch. More importantly, the reflectivity of the vacuum sputtering AR layer can be reduced to be below 0.5%, while the reflectivity of the wet coating LR layer is generally 1% -2%, obviously, the anti-reflection and anti-reflection effects of the vacuum sputtering AR layer are better, so that the vacuum sputtering AR layer is selected in more than 90% of the subsequent processing modes applied to the field of vehicle-mounted display at present, and the processing modes of the wet coating LR layer are fewer. The present invention is also primarily discussed in terms of solving the adhesion problem with the AR layer. And then coating OCA glue on the back of the transparent support body of the anti-glare hardening film, and attaching the OCA glue to a central control display screen of vehicle-mounted display, wherein the functions of the OCA glue comprise preventing glass from splashing, preventing glare, increasing the transmission and reducing the reflection. The anti-dazzle hardening film firstly has an anti-dazzle effect, and secondly has the functions of reflection and reflection resistance by sputtering an AR layer or coating an LR layer in the next working procedure, wherein the adhesion and the bonding force of the anti-dazzle layer and the AR layer/the LR layer are very important. In order to realize the anti-dazzle effect, the first coating and the second coating are coated on the transparent support body at one time, the first coating H1 is controlled to be 2-10 mu m, the grain diameter of organic particles of the first coating is 3-15 mu m, the roughness of the first coating is more than or equal to 0.1 mu m and less than or equal to Ra and less than or equal to 0.5 mu m, the thickness H2 of the second coating satisfies the relation that H2 is more than or equal to 0.1 and less than or equal to Ra and less than or equal to 1 mu m, and the coating has the anti-dazzle effect and the high-definition effect by controlling the thickness, the grain diameter and the surface roughness of the coating.
The organic particles in the first coating layer are monodisperse organic particles (the variance of the size distribution of the organic particles is less than or equal to 5 percent, such as MX-300, MX-1000 and MX-1500H of the chemical company of Hokka) or disperse organic particles (the variance of the size distribution of the organic particles is more than 5 percent and less than 15 percent, such as MRN-8HN and MRN-12H of the chemical company of Hokka). For better control of the roughness, the organic particles in the first coating layer are selected from monodisperse organic particles or monodisperse organic particles having a relatively uniform particle size. The polydisperse organic particles have a large particle size distribution range, and many small-particle-size particles and large-particle-size particles exist, so that the control of the roughness of the first coating is not facilitated, the definition is easily reduced, the fog feeling is increased, and the display effect is not facilitated.
There are many effects of preventing glare, and a method of adding various types of spherical particles to a coating layer is generally used, so that the particles are exposed out of the surface of the coating layer to form diffuse reflection to achieve the effect of preventing glare. The first coating of the present invention realizes antiglare and high definition properties of the coating by controlling particle size, coating thickness and roughness. Considering that the anti-glare hardened film of the invention needs to sputter an AR layer on the surface of the anti-glare hardened coating, the AR layer comprises a plurality of oxide coatings, and needs to be sputtered for a plurality of times, each oxide coating is generally 1nm-100nm, the thickness uniformity of the AR layer is very important, and the adhesion between the AR layer and the anti-glare hardened layer is more important. However, the organic particles protruding from the surface of the anti-glare hardened film greatly affect the thickness uniformity and adhesion of the AR layer. In order to solve the problem, the second coating is arranged on the surface of the first coating, the number average molecular weight of polyurethane acrylic resin in the second coating, the boiling point of an organic solvent in the second coating, the solid content and the viscosity of the coating liquid of the second coating, and the temperature and the air speed of a drying box of the second coating are controlled, so that the film-forming resin of the second coating completely and uniformly wraps and covers the organic particles of the first coating, and when an AR layer is sputtered again, the uniformity and the better adhesive force of the AR coating can be realized. In the invention, the number average molecular weight of the polyurethane acrylic resin in the second coating liquid is 2000-5000, and the using amount of the polyurethane acrylic prepolymer is controlled to be 48-58 parts by weight; the boiling point of the organic solvent in the second coating layer coating liquid is 110-153 ℃, and the using amount of the organic solvent is controlled to be 35-50 parts by weight. The solid content of the coating liquid of the second coating layer is 50-60%, the viscosity of the coating liquid is 30-50 cps, and the haze range of the formed anti-dazzle hardening film is 1-50%.
The first coating liquid contains organic particles, and in order to help the leveling of the coating liquid on the transparent support and the directional distribution of the organic particles, a dispersant such as DISPERBYK-130, DISPERBYK-140, DISPERBYK-142, DISPERBYK-163, and DISPERBYK-171 of Bikk chemical is added to the first coating liquid.
The organic solvent suitable for the second coating liquid should satisfy the boiling point requirement, such as one of toluene, nitroethane, butanol, chlorobenzene, and N, N-dimethylformamide, in addition to the solubility.
The photoinitiator (coating solution of the first coating layer or coating solution of the second coating layer) in the present invention may be selected from initiators known in the art of ultraviolet light curing, such as 1-hydroxycyclohexyl phenyl ketone (184), 2-hydroxy-methyl phenyl propane-1-one (1173), benzoin bis methyl ether (651), 2, 4, 6 (trimethylbenzoyl) diphenyl phosphine oxide (TPO), and the like. The addition amount of the photoinitiator is 1 to 8 parts by weight.
The ultraviolet light used in the present invention can be obtained from a high-pressure mercury lamp and the irradiation intensity of the ultraviolet light is 500mJ/cm2-1000mJ/cm2。
The invention also provides a preparation method of the anti-dazzle hardening film for vehicle-mounted display, which comprises the following steps: preparing a first coating: coating a coating liquid for forming a first coating layer on a transparent support, drying and carrying out UV curing to obtain the coating liquid; the haze of the first coating is 2% -60%; preparing a second coating: coating a second coating layer coating liquid on the surface of the first coating layer, drying and carrying out UV curing to obtain the coating; the second coating is formed after being dried by a multi-stage drying oven and cured by ultraviolet light, and the temperature of the first-stage drying oven is set to be 25-50 ℃; the temperature of the second-stage oven is 40-60 ℃, and the temperature of the third-stage oven is 80-100 ℃. In the preparation method, the process conditions of the second coating are more critical, the organic particles of the second coating to be wrapped on the surface of the first coating are considered, the solid content and the viscosity of the coating liquid of the second coating are combined, the second coating firstly passes through the first-stage oven with relatively low drying temperature, the coating liquid slowly flows on the surfaces of the organic particles, the formed coating is relatively uniform, and the sizing effect is achieved. Then through the second level, the temperature rises gradually, can not let the second coating creep again, only plays the effect of volatile solvent, and the tertiary drying cabinet is in order to make the solvent in the coating volatilize totally clean.
The present invention is further illustrated by the following examples, but the embodiments of the present invention are not limited to these examples.
Example 1
10g of a urethane acrylic resin (trade name: EB8254, functionality 6), 60g of a polyfunctional monomer (pentaerythritol triacrylate PETIA, Dissmann, trade name: AgiSyn 2884), 8g of a photoinitiator (1173), 0.5g of a leveling assistant (BYK-390), 2g of a dispersant (DISPERBYK-130), 10g of organic particles (general chemical trade name: MX1500H, particle size 15 μm) and 9.5g of ethyl acetate were placed in a stirring pot, stirred at a speed of 2000r/min for 1 hour, further stirred at a speed of 100r/min for 1 hour, and finally stirred uniformly to obtain a first coating liquid.
48g of a urethane acrylic resin (trade name: EB242, number average molecular weight 2700), 2g of a photoinitiator (1173) and 50g of nitroethane were placed in a stirring pot, stirred at a speed of 500r/min for 1 hour, further stirred at a speed of 100r/min for 1 hour, and stirred uniformly to obtain a coating liquid for a second coating layer (solid content: 50%, viscosity: 30 cps).
Coating the coating liquid for the first coating layer on one surface of a PET (polyethylene terephthalate) base material with the thickness of 25 mu m, drying the PET base material by an oven and curing the PET base material by ultraviolet light to obtain the first coating layer, wherein the haze of the first coating layer is 2%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 25 ℃, the temperature of the second-stage drying oven is 50 ℃, and the temperature of the third-stage drying oven is 100 ℃; the UV energy of the UV-curable first coating was 500mJ/cm2UV energy of the UV-curable second coating is 800mJ/cm2. The coating thickness H1 of the first coating was 10 μm, the roughness Ra was 0.5 μm, and the coating thickness H2 of the second coating was 0.6 μm. The evaluation results are shown in Table1 in (c).
Example 2
20g of a urethane acrylic resin (trade name: EB8415, functionality 10), 30g of a polyfunctional monomer (di-trimethylolpropane tetraacrylate, sartomera, trade name: SR355NS), 1g of a photoinitiator (651), 0.1g of a leveling aid (BYK-390), 0.5g of a dispersant (DISPERBYK-142), 9g of organic particles (trade name: MRN-8HN, particle size: 8 μm) and 39.4g of methyl ethyl ketone were placed in a stirring pot, stirred at a speed of 2000r/min for 1h, further stirred at a speed of 100r/min for 1h, and finally stirred uniformly to obtain a first coating liquid.
A coating liquid for a second coating (solid content: 60%, viscosity: 47cps) was obtained by stirring 52g of a urethane acrylic resin (trade name: EB230, number average molecular weight: 5000), 8g of a photoinitiator (184) and 40g of toluene at 500r/min for 1 hour and 100r/min for 1 hour in a stirring pot.
Coating the coating liquid for the first coating on one surface of a PMMA (polymethyl methacrylate) base material with the thickness of 100 mu m, drying the PMMA base material by an oven and curing the PMMA base material by ultraviolet light to obtain the first coating, wherein the haze of the first coating is 30%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 50 ℃, the temperature of the second-stage drying oven is 60 ℃, and the temperature of the third-stage drying oven is 80 ℃; the UV energy of the UV-curable first coating is 800mJ/cm2UV energy of the UV-curable second coating was 500mJ/cm2. The coating thickness H1 of the first coating was 6 μm, the roughness Ra was 0.1 μm, and the coating thickness H2 of the second coating was 0.85. mu.m. The evaluation results are shown in Table 1.
Example 3
15g of urethane acrylic resin (Inssman, trade name: AgiSoSyn 230A2, functionality 6), 55g of multifunctional monomer (dipentaerythritol hexaacrylate, Changxing chemical, trade name: EM266), 3g of photoinitiator (184), 1g of leveling aid (BYK-355), 1g of dispersant (DISPERBYK-171), 5g of organic particles (MRN-12H, trade name: MRN-12H, particle size 12 μm) and 20g of butyl acetate were placed in a stirring pot, stirred at a speed of 2000r/min for 1H, then stirred at a speed of 100r/min for 1H, and finally stirred uniformly to obtain a coating liquid for a first coating.
A coating liquid for a second coating (solid content: 59%, viscosity: 45cps) was obtained by placing 58g of a urethane acrylic resin (trade name: EB8602, number average molecular weight 2000), 1g of a photoinitiator (TPO) and 41g N, N-dimethylformamide in a stirring pot, stirring at 500r/min for 1 hour, further stirring at 100r/min for 1 hour, and stirring uniformly.
Coating the coating liquid for the first coating on one surface of a COP substrate with the thickness of 50 mu m, drying by an oven, and curing by ultraviolet light to obtain the first coating, wherein the haze of the first coating is 60%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 30 ℃, the temperature of the second-stage drying oven is 40 ℃, and the temperature of the third-stage drying oven is 90 ℃; the UV energy of the UV-curable first coating was 600mJ/cm2UV energy of the UV-curable second coating was 1000mJ/cm2. The coating thickness H1 of the first coating was 8 μm, the roughness Ra was 0.35 μm, and the coating thickness H2 of the second coating was 1.35 μm. The evaluation results are shown in Table 1.
Example 4
18g of a urethane acrylic resin (Sadoma, trade name: CN9013NS, functionality: 9), 25g of a polyfunctional monomer (dipentaerythritol pentaacrylate, Sadoma, trade name: SR399), 5g of a photoinitiator (651), 0.4g of a leveling aid (BYK-355), 1.5g of a dispersant (DISPERBYK-163), 0.1g of organic particles (Soken chemical, trade name: MX-300, particle size 3 μm) and 40g of methanol were put in a stirring pot, stirred at a speed of 2000r/min for 1h, further stirred at a speed of 100r/min for 1h, and finally stirred uniformly to obtain a first-coating-layer coating liquid.
57g of urethane acrylic resin (trade name: EB8894, number average molecular weight 4000), 8g of photoinitiator (651) and 35g of chlorobenzene were placed in a stirring pot, stirred at a speed of 500r/min for 1 hour, further stirred at a speed of 100r/min for 1 hour, and stirred uniformly to obtain a coating liquid for a second coating layer (solid content: 65%, viscosity: 50 cps).
Coating the coating liquid for the first coating on one surface of a TAC (TAC) base material with the thickness of 40 mu m, drying by an oven and curing by ultraviolet light to obtain the first coating, wherein the haze of the first coating is 43%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 40 ℃, the temperature of the second-stage drying oven is 55 ℃, and the temperature of the third-stage drying oven is 95 ℃; the UV energy of the UV-curable first coating was 600mJ/cm2UV energy of the UV-curable second coating was 1000mJ/cm2. The coating thickness H1 of the first coating was 2 μm, the roughness Ra was 0.24 μm, and the coating thickness H2 of the second coating was 0.74. mu.m. The evaluation results are shown in Table 1.
Example 5
20.1g of a urethane acrylic resin (trade name: SC2152, functionality: 15, from the American Co., Ltd.), 40g of a polyfunctional monomer (pentaerythritol triacrylate PETIA, Dissmann, trade name: AgiSyn 2884), 6.4g of a photoinitiator (651), 0.7g of a leveling aid (BYK-350), 1.8g of a dispersant (DISPERBYK-140), 1g of an organic particle (trade name: MX-1000, particle size: 10 μm) and 30g of acetone were placed in a stirring pot, stirred at a speed of 2000r/min for 1 hour, further stirred at a speed of 100r/min for 1 hour, and finally stirred uniformly to obtain a first-coating-solution.
50g of urethane acrylic resin (trade name: EB8896, number average molecular weight 4500), 4g of photoinitiator (TPO) and 45g of butanol were placed in a stirring pot, stirred at 500r/min for 1 hour, further stirred at 100r/min for 1 hour, and stirred uniformly to obtain a coating liquid for a second coating layer (solid content: 55%, viscosity: 45 cps).
Coating the coating liquid for the first coating layer on one surface of an SRF substrate with the thickness of 80 mu m, drying by an oven, and curing by ultraviolet light to obtain the first coating layer, wherein the haze of the first coating layer is 16%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage oven is 3The temperature of the second-stage drying oven is 60 ℃ and the temperature of the third-stage drying oven is 92 ℃; the UV energy of the UV-curable first coating was 950mJ/cm2UV energy of the UV-curable second coating is 750mJ/cm2. The coating thickness H1 of the first coating was 5 μm, the roughness Ra was 0.47. mu.m, and the coating thickness H2 of the second coating was 0.71. mu.m. The evaluation results are shown in Table 1.
Comparative example 1
4g of a urethane acrylic resin (trade name: EB4666, functionality 4), 66g of a polyfunctional monomer (tripropylene glycol diacrylate TPGDA, Tesmann, trade name: AgiSyn 2815), 8g of a photoinitiator (1173), 0.5g of a leveling aid (BYK-390), 2g of a dispersant (DISPERBYK-130), 10g of organic particles (trade name: MX1500H, particle size 15 μm) and 9.5g of ethyl acetate were placed in a stirring pot, stirred at 2000r/min for 1h, further stirred at 100r/min for 1h and finally stirred uniformly to obtain a first coating liquid.
48g of a urethane acrylic resin (trade name: EB242, number average molecular weight 2700), 2g of a photoinitiator (1173) and 50g of nitroethane were placed in a stirring pot, stirred at a speed of 500r/min for 1 hour, further stirred at a speed of 100r/min for 1 hour, and stirred uniformly to obtain a coating liquid for a second coating layer (solid content: 50%, viscosity: 30 cps).
Coating the coating liquid for the first coating layer on one surface of a PET (polyethylene terephthalate) base material with the thickness of 25 mu m, drying the PET base material by an oven and curing the PET base material by ultraviolet light to obtain the first coating layer, wherein the haze of the first coating layer is 2%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 25 ℃, the temperature of the second-stage drying oven is 50 ℃, and the temperature of the third-stage drying oven is 100 ℃; the UV energy of the UV-curable first coating was 500mJ/cm2UV energy of the UV-curable second coating is 800mJ/cm2. The coating thickness H1 of the first coating was 10 μm, the roughness Ra was 0.5 μm, and the coating thickness H2 of the second coating was 0.6 μm. The evaluation results are shown in Table 1.
Comparative example 2
20g of a urethane acrylic resin (trade name: EB8415, functionality 10), 30g of a polyfunctional monomer (di-trimethylolpropane tetraacrylate, sartomera, trade name: SR355NS), 1g of a photoinitiator (651), 0.1g of a leveling aid (BYK-390), 0.5g of a dispersant (DISPERBYK-142), 9g of organic particles (trade name: MRN-8HN, particle size: 8 μm) and 39.4g of methyl ethyl ketone were placed in a stirring pot, stirred at a speed of 2000r/min for 1h, further stirred at a speed of 100r/min for 1h, and finally stirred uniformly to obtain a first coating liquid.
A coating liquid for a second coating (solid content: 60%, viscosity: 47cps) was obtained by stirring 52g of a urethane acrylic resin (trade name: EB230, number average molecular weight: 5000), 8g of a photoinitiator (184) and 40g of toluene at 500r/min for 1 hour and 100r/min for 1 hour in a stirring pot.
Coating the coating liquid for the first coating on one surface of a PMMA (polymethyl methacrylate) base material with the thickness of 100 mu m, drying the PMMA base material by an oven and curing the PMMA base material by ultraviolet light to obtain the first coating, wherein the haze of the first coating is 30%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 50 ℃, the temperature of the second-stage drying oven is 60 ℃, and the temperature of the third-stage drying oven is 80 ℃; the UV energy of the UV-curable first coating is 800mJ/cm2UV energy of the UV-curable second coating was 500mJ/cm2. The coating thickness H1 of the first coating was 6 μm, the roughness Ra was 0.1 μm, and the coating thickness H2 of the second coating was 1.6. mu.m. The evaluation results are shown in Table 1.
Comparative example 3
15g of urethane acrylic resin (Inssman, trade name: AgiSoSyn 230A2, functionality 6), 55g of multifunctional monomer (dipentaerythritol hexaacrylate, Changxing chemical, trade name: EM266), 3g of photoinitiator (184), 1g of leveling aid (BYK-355), 1g of dispersant (DISPERBYK-171), 5g of organic particles (MRN-12H, trade name: MRN-12H, particle size 12 μm) and 20g of butyl acetate were placed in a stirring pot, stirred at a speed of 2000r/min for 1H, then stirred at a speed of 100r/min for 1H, and finally stirred uniformly to obtain a coating liquid for a first coating.
38g of urethane acrylic resin (trade name: EB8602, number average molecular weight 2000), 1g of photoinitiator (TPO) and 61g N, N-dimethylformamide were placed in a stirring pot, stirred at 500r/min for 1 hour, further stirred at 100r/min for 1 hour, and stirred uniformly to obtain a coating liquid for a second coating layer (solid content: 39%, viscosity: 25 cps).
Coating the coating liquid for the first coating on one surface of a COP substrate with the thickness of 50 mu m, drying by an oven, and curing by ultraviolet light to obtain the first coating, wherein the haze of the first coating is 60%; and then coating the coating liquid for the second coating layer on the surface of the first coating layer, drying by a multi-stage oven, and curing by ultraviolet light to obtain the second coating layer, and finally forming the anti-glare hardened film for vehicle-mounted display. Wherein the temperature of the first-stage drying oven is 30 ℃, the temperature of the second-stage drying oven is 40 ℃, and the temperature of the third-stage drying oven is 90 ℃; the UV energy of the UV-curable first coating was 600mJ/cm2UV energy of the UV-curable second coating was 1000mJ/cm2. The coating thickness H1 of the first coating was 8 μm, the roughness Ra was 0.35 μm, and the coating thickness H2 of the second coating was 0.43. mu.m. The evaluation results are shown in Table 1.
Table 1: test data table for each example and comparative example
Comparing comparative example 1 and example 1, it can be seen that, with the selection of a low functional urethane acrylate and a low functional monomer, the hardness and scratch resistance of the coating layer may be reduced, which is not favorable for screen protection; as can be seen by comparing comparative example 2 and example 2, the second coating thickness H2 was 1.6. mu.m, H2-Ra was 1.5. mu.m, and the relationship 0.1. ltoreq. H2-Ra was not satisfied and 1. mu.m, the anti-glare properties of the resulting anti-glare cured film became poor, and the adhesion after coating became poor. Comparing comparative example 3 and example 3, it can be seen that the second coating thickness H2 was 0.43 μm, H2-Ra was 0.08 μm, the relational expression 0.1. ltoreq. H2-Ra. ltoreq.1 μm, the coating liquid solid content of the second coating was 39%, the coating liquid viscosity was 25cps, the coating liquid of the second coating did not form effective coating on the particle surface, and the adhesion was very poor.
The test methods for the properties in the table are as follows:
(1) haze, transmittance, clarity test
A transmission haze imaging instrument (Debyk, model: BYK-4725) was used to measure haze, light transmittance, and sharpness.
(2) Pencil hardness test
Film hardness tester using pencil scratch [ manufactured by shanghai pushen chemical machinery ltd; the model is as follows: "BY" ], a load of 500g, and pencil hardness was measured.
(3) Anti-glare property evaluation method
The surface-treated films of examples and comparative examples were bonded to a liquid crystal display using a transparent optical adhesive
In (Apple iPad Air 3, dark gray, off state), when observed from a position 50cm vertically away from the center of the liquid crystal display under an illumination of 250lux, 100 arbitrary persons visually determined whether or not their own image (face) can be clearly observed on the liquid crystal display. As a result of the evaluation, the case of 70 or more persons who did not observe clear images was "o", the case of 30 or more persons and less than 70 persons was "Δ", and the case of less than 30 persons was "x".
(4) Adhesion of coating film
Taking 3 pieces of anti-dazzle hardening film with the size of A4, and sputtering a first low-refractive-index film layer, a first high-refractive-index film layer, a second low-refractive-index film layer and a second high-refractive-index film layer on the surface of the anti-dazzle hardening film in sequence, wherein the low-refractive-index film layer is an SiON film layer, and the high-refractive-index film layer is an Si film layer3N4The coating thickness of the film layer, the low refractive index layer and the high refractive index layer is 30nm +/-5 nm. The adhesion was then measured with a white knife and the adhesion of the low and high refractive index layers to the antiglare cured layer was observed, according to standard ASTM D3359.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (10)
1. An anti-glare hardened film for vehicle-mounted display, which comprises a transparent support and is characterized by further comprising a first coating layer and a second coating layer which are sequentially coated on one surface of the transparent support;
the first coating is formed by curing a coating liquid, and the coating liquid comprises the following substances in parts by weight:
wherein the coating thickness H1 of the first coating is 2-10 μm, and the average roughness Ra of the first coating is 0.1-0.5 μm;
the second coating is formed by coating and curing a coating liquid prepared from the following components in parts by weight:
48-58 parts of polyurethane acrylic resin
1-8 parts of photoinitiator
35-50 parts of an organic solvent,
wherein the coating thickness H2 of the second coating satisfies the relationship: H2-Ra is more than or equal to 0.1 and less than or equal to 1 mu m.
2. The antiglare hardened film for vehicle displays of claim 1, wherein the first coating layer has an organic particle size of 3 μm to 15 μm.
3. The antiglare hardened film of claim 1, wherein the polyfunctional monomer is one of ditrimethylolpropane tetraacrylate, pentaerythritol triacrylate, dipentaerythritol pentaacrylate or dipentaerythritol hexaacrylate.
4. The antiglare hardened film for vehicle displays of claim 1, wherein the leveling aid in the first coating layer is an acrylate leveling agent.
5. The antiglare hardened film for vehicle displays of claim 1, wherein the organic particles in the first coating layer are monodisperse organic particles or monodisperse organic particles.
6. The antiglare hardened film for on-vehicle displays of claim 1, wherein the second coating layer has a coating liquid solid content of 50% to 60% and a coating liquid viscosity of 30cps to 50 cps.
7. The antiglare hardened film for on-vehicle display as claimed in claim 1, wherein the number average molecular weight of the urethane acrylic resin in the second coating layer coating liquid is 2000-; the boiling point of the organic solvent in the second coating layer coating liquid is 110-153 ℃.
8. The antiglare hardened film for vehicle displays of claim 1, wherein the antiglare hardened film has a haze ranging from 1% to 50%.
9. The antiglare hardened film for vehicle displays of claim 1, wherein the transparent support is one of PET, TAC, PMMA, SRF, COP, and has a thickness of 25 μm to 100 μm.
10. A method for producing an antiglare hardened film for vehicle displays according to claims 1 to 9, wherein the antiglare hardened film comprises a second coat layer, a first coat layer and a transparent support in this order from top to bottom, the production comprising the steps of:
preparing a first coating: coating a coating liquid for forming a first coating on a transparent support, drying and carrying out ultraviolet curing to obtain the coating liquid; the haze of the first coating is 2% -60%;
preparing a second coating: coating a second coating layer coating liquid on the surface of the first coating layer, drying, and curing by ultraviolet light to obtain the coating; the second coating is formed after being dried by a multi-stage drying oven and cured by ultraviolet light, and the temperature of the first-stage drying oven is set to be 25-50 ℃; the temperature of the second-stage oven is 40-60 ℃, and the temperature of the third-stage oven is 80-100 ℃;
the UV energy of the ultraviolet light curing first coating and the second coating is 500mJ/cm2～1000mJ/cm2。
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