CN113201162B - Scratch-resistant anti-reflection film - Google Patents
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2463/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/06—Unsaturated polyesters
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- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a scratch-resistant anti-reflection film, which is obtained by coating a hardening layer coating solution on a substrate, heating and curing at 60-80 ℃ until the surface is dry to form a hardening layer, then coating an anti-reflection layer coating solution on the hardening layer, heating and curing at 80-150 ℃ for at least 1min and UV curing to form an anti-reflection layer, wherein the UV curing energy is 600mJ/cm 2 The hardened layer comprises the following material components in parts by weight: 100 parts of dual-curing resin, 1-10 parts of photoinitiator, 1-10 parts of isocyanate, 5-40 parts of blocked isocyanate, 100-850 parts of solvent and 0.5-10 parts of other auxiliary agents; the anti-reflection layer comprises the following material components in parts by weight: 100 parts of light-cured resin, 10-80 parts of hollow nano silicon dioxide particles, 4000-10000 parts of solvent and 1-10 parts of other auxiliary agents; the advantages are that the anti-reflection coating has excellent anti-reflection function, and simultaneously, the anti-reflection coating has strong interlayer adhesion and strong scratch resistance.
Description
Technical Field
The invention relates to an anti-reflection film, in particular to a scratch-resistant anti-reflection film.
Background
Currently, various display touch screens are generally provided with an antireflection film that minimizes reflection of incident light from the outside. The antireflection film has a multilayer structure, and currently, there are two main methods for manufacturing the antireflection film: dry and wet processes. The antireflection film prepared by the dry method has stronger antireflection function than the antireflection film prepared by the wet method, but the dry method has the advantages that the manufacturing process is intermittent lamination, the process of forming each layer is separately carried out, and the equipment cost and the time cost are high. In addition, antireflection films have been commercialized which are realized by providing a multilayer structure such as a hardened layer (high refractive index layer) and an antireflection layer (low reflection coating) on a substrate.
However, it is difficult for the conventional antireflection film to achieve both antireflection performance and scratch resistance. Among them, the antireflection film disclosed in chinese patent publication No. CN109298470A has low reflectance, but has difficulty in having excellent scratch resistance. In addition, the anti-reflection layer of the existing anti-reflection film generally employs a high fluorine-containing material, such as a durable anti-reflection film disclosed in chinese patent publication No. CN101809465A, so that the inter-layer adhesion (interface adhesion) of the anti-reflection layer is weak and the scratch resistance is low.
Disclosure of Invention
The invention aims to provide a scratch-resistant anti-reflection film, which has excellent anti-reflection function, strong interlayer adhesion between an anti-reflection layer and a hardening layer and strong scratch resistance.
The technical scheme adopted by the invention for solving the technical problems is as follows: a scratch-resistant anti-reflection film is prepared by coating a hardening layer coating solution on a substrate, heating and curing at 60-80 ℃ to be surface-dried to form a hardening layer, coating an anti-reflection layer coating solution on the hardening layer, heating and curing at 80-150 ℃ for at least 1min and UV curing to form an anti-reflection layer, wherein the UV curing energy is 600mJ/cm 2 The hardened layer comprises the following material components in parts by weight: 100 parts of dual-curing resin, 1-10 parts of photoinitiator, 1-10 parts of isocyanate, 5-40 parts of blocked isocyanate, 100-850 parts of solvent and 0.5-10 parts of other auxiliary agents; the anti-reflection layer comprises the following material components in parts by weight: 100 parts of light-cured resin, 10-80 parts of hollow nano silicon dioxide particles, 4000-10000 parts of solvent and 1-10 parts of other auxiliary agents.
The dual-curing resin is acrylic resin containing hydroxyl, and the hydroxyl value is 20-200 mgKOH/g, preferably 40-150 mgKOH/g;
the dual-curing resin is one or more of polyurethane acrylic resin, polyester acrylic resin and epoxy acrylic resin.
The blocked isocyanate is suitable for a photocuring system, can be dissolved in an organic solvent, and preferably has an NCO equivalent weight of more than or equal to 200 and a ring opening temperature of 80-150 ℃, preferably 90-100 ℃.
The light-cured resin is acrylic resin with a functional group of more than 3, excellent aliphatic and special modified wear resistance, and comprises one or more of aliphatic polyurethane acrylic resin, aliphatic polyester acrylic resin, epoxy acrylic resin, modified bisphenol A epoxy acrylic resin and fluorine modified polyurethane acrylic resin.
The surface of the hollow nano silicon dioxide particle is provided with hydroxyl groups, and each nm of the hollow nano silicon dioxide particle is 2 The number of hydroxyl groups on the surface is more than or equal to 5, and the particle diameter of the hollow nano silicon dioxide particle is 10nm-100nm, preferably 10nm-30nm.
The solvent is any one or a mixture of more of isopropanol, acetone, methyl isobutyl ketone, butanone, propylene glycol methyl ether, propylene glycol monobutyl ether, methyl acetate, ethyl acetate and butyl acetate.
The thickness of the hardened layer is 2 to 50 μm, preferably 3 to 10 μm.
The thickness of the anti-reflection layer is 90 nm-110 nm.
The anti-reflection film has the steel wool resistance of 1500 times/1 kg, the interlayer adhesion force is boiled for two hours, the average reflectivity is less than or equal to 2 percent, the reflectivity at the position of 550nm can be as low as 1.4 percent, and the b value in a CIE Lab color model is in the range of-3 to + 3.
The other auxiliary agents can be any one or a mixture of more of an initiator, a leveling agent, a wetting agent, a defoaming agent, a light stabilizer, a polymerization inhibitor, an antioxidant and an antistatic agent under the condition that the interlayer adhesion is not influenced. A (c)
Compared with the prior art, the scratch-resistant anti-reflection film disclosed by the invention has the advantages that a hardening layer coating liquid is coated on a substrate, the hardening layer is formed by heating and curing at 60-80 ℃ until the surface is dry, then an anti-reflection layer coating liquid is coated on the hardening layer, and the anti-reflection layer is formed by heating and curing at 80-150 ℃ for at least 1min and UV curing in sequence, wherein the UV curing energy is 600mJ/cm 2 In the above-mentioned manner,the hardened layer comprises the following material components in parts by weight: 100 parts of dual-curing resin, 1-10 parts of photoinitiator, 1-10 parts of isocyanate, 5-40 parts of blocked isocyanate, 100-850 parts of solvent and 0.5-10 parts of other auxiliary agents; the anti-reflection layer comprises the following material components in parts by weight: 100 parts of light-cured resin, 10-80 parts of hollow nano silica particles, 4000-10000 parts of solvent and 1-10 parts of other auxiliary agents, in the process of forming a hardened layer, the hardened layer obtained by heating and curing until the surface is dried is not cured completely, N = C = O in the blocked isocyanate has no activity because the blocked isocyanate does not open a ring and cannot react with hydroxyl in the dual-cured resin, in the subsequent process of forming an anti-reflection layer, N = C = O activity is enhanced because the R group of the blocked isocyanate opens a ring at 80-150 ℃, hydroxyl which does not react completely in the hardened layer dual-cured resin, N = C = O in the opened blocked isocyanate reacts with hydroxyl on the surface of the hollow nano silica particles in the anti-reflection layer, and then acrylic group in the dual-cured resin in the hardened layer is crosslinked with the light-cured resin in the anti-reflection layer after being irradiated by high-energy UV light to strengthen the adhesion of the two layers, so that the adhesion between the hardened layer and the anti-reflection layer is increased, and the scratch resistance is enhanced.
Drawings
FIG. 1 is a schematic structural view of a scratch resistant antireflective film of the invention;
FIG. 2 is a flow chart of the preparation of the scratch resistant antireflective film of the invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The first embodiment is as follows: as shown in figure 1, the scratch-resistant anti-reflection film is obtained by coating a hardening layer coating solution on a substrate 1, heating and curing at 65 ℃ until the surface is dry to form a hardening layer 2 with the thickness of 3 mu m, then coating an anti-reflection layer coating solution on the hardening layer 2, and sequentially heating and curing at 90 ℃ for 1min and UV curing to form an anti-reflection layer 3 with the thickness of 100nm, whereinThe UV curing energy is 600mJ/cm 2 The hardening layer 2 comprises the following material components in parts by weight: 100 parts of dual-curing resin (lithopone L-8464), 5 parts of photoinitiator (Irgacure 184), 5 parts of isocyanate (Mitsui chemical D-131N), 10 parts of blocked isocyanate (XB-G282), 280 parts of solvent (methyl isobutyl ketone) and 0.5 part of other auxiliary agent (BYK 300 flatting agent); the anti-reflection layer 3 comprises the following material components in parts by weight: 100 parts of photocurable resin (R0310), 15 parts of hollow silica nanoparticles (a 311), 4500 parts of solvent (methyl isobutyl ketone) and 7 parts of other auxiliaries (Irgacure 184 photoinitiator 5 parts by weight, showa electrician Karenz MT PE1 thiol 1 parts by weight and 1 part by weight of a 219).
The second embodiment: this embodiment is substantially the same as the first embodiment, and the difference is only that: the blocked isocyanate was 40 parts by weight.
Example three: this embodiment is substantially the same as the first embodiment, and the difference is only that: 10 parts by weight of isocyanate and 5 parts by weight of blocked isocyanate.
Example four: this embodiment is substantially the same as the first embodiment, and the difference is only that: the thickness of the hardened layer 2 was 2 μm.
Example five: this embodiment is substantially the same as the first embodiment, and the differences are only that: the thickness of the hardened layer 2 was 10 μm.
Example six: this embodiment is substantially the same as the first embodiment, and the differences are only that: the curing temperature of the hardened layer 2 becomes 90 ℃.
Example seven: this embodiment is substantially the same as the first embodiment, and the difference is only that: the thickness of the anti-reflection layer 3 was 90nm.
Example eight: this embodiment is substantially the same as the first embodiment, and the difference is only that: the thickness of the anti-reflection layer 3 was 110nm.
Example nine: this embodiment is substantially the same as the first embodiment, and the differences are only that: the heat curing temperature of the anti-reflection layer 3 was 120 ℃.
Example ten: this embodiment is substantially the same as the first embodiment, and the differences are only that: air conditionerThe core silica nanoparticles (A311) were 75 parts by weight, and the UV curing energy was changed to 800mJ/cm 2 。
To verify the benefits of the present invention, several comparative examples were set up as follows for comparison with the present invention.
Comparative example one: essentially the same as example one, except that in this comparative example: the dual-curing resin used for the hardened layer and the light-curing resin used for the anti-reflection layer are both R0310.
Comparative example two: essentially the same as example one, except that in this comparative example: the part of the blocked isocyanate is 0 part by weight.
Comparative example three: essentially the same as example one, except in this comparative example: the curing temperature of the anti-reflective layer was 65 ℃.
Comparative example four: essentially the same as example one, except that in this comparative example: the curing temperature of the hardened layer was raised to 100 ℃.
Comparative example five: essentially the same as example one, except in this comparative example: the UV curing energy of the anti-reflection layer was 300mJ/cm 2 。
The test data of the above examples and comparative examples are shown in table 1.
TABLE 1 test data
| Examples | Average reflectivity | Minimum reflectance | b value (D65) | Steel wire resistant velvet | Water boiling deviceGrid (C) |
| Example one | 2％ | 1.30％ | -1.92 | ο | 5B |
| Example two | 2％ | 1.30％ | -1.92 | Δ | 5B |
| EXAMPLE III | 2％ | 1.30％ | -1.93 | Δ | 5B |
| Example four | 2％ | 1.30％ | -1.92 | Δ | 5B |
| EXAMPLE five | 2％ | 1.30％ | -2.0 | ο | 5B |
| Practice ofExample six | 2％ | 1.30％ | -1.9 | Δ | 2B |
| EXAMPLE seven | 2％ | 1.50％ | -2.78 | ο | 5B |
| Example eight | 2％ | 1.40％ | 1.66 | Δ | 5B |
| Example nine | 2％ | 1.30％ | -1.92 | Δ | 5B |
| Example ten | 1.90％ | 1.20％ | -2.67 | Δ | 5B |
| Comparative example | Average reflectivity | Minimum reflectance | b value (D65) | Steel wire resistant velvet | Water boiling grid |
| Comparative example- | 2％ | 1.30％ | -1.92 | × | 0B |
| Comparative example | 2％ | 1.30％ | -1.92 | × | 0B |
| Comparative example No. three | 2％ | 1.30％ | -1.92 | × | 0B |
| Comparative example No. four | 2％ | 1.30％ | -1.92 | × | 0B |
| Comparative example five | 2％ | 1.30％ | -1.92 | × | 0B |
In table 1, average reflectance, minimum reflectance, and b-value: carrying out darkening treatment on the back surface of the anti-reflection film, measuring the minimum reflectivity of the anti-reflection film in a wavelength region of 380nm to 780nm through an ultraviolet spectrocolorimeter CM3600A, recording the b value at the moment, and finally obtaining the average reflectivity through calculation;
evaluation of scratch resistance: a steel Wool #0000 (steel Wool, japan) of 1000gf, a 2cm × 2cm abrasion-resistant head was pressed to the surface of the antireflection film to make reciprocal friction 2000 times, and the damaged state of the surface of the antireflection film was observed with naked eyes from obliquely above with a three-wavelength type daytime white fluorescent lamp (National Palook, f.l 15 EX-N15W) as a light source; o: no damage was observed; Δ: lesions were observed, but at a level where use was not problematic; x: significant damage was observed;
evaluation of adhesion force: after the antireflection film was boiled in boiling water at 100 ℃ for two hours, the antireflection film was wiped dry, and the adhesion rating of the antireflection film was judged using a 1cm × 1cm hundred grid knife, nitto day 31B Test tape, specifically according to ASTM D3359 Cross-cut Type Test.
From an analysis of the data in Table 1, it can be seen that: the reflectivity of the anti-reflection films of the first embodiment to the tenth embodiment can reach 1.3 percent at the lowest, and the interlayer adhesion and the scratch resistance performance are excellent. Specifically, the use of the dual-curing resin and the blocked isocyanate, together with the appropriate curing temperature and UV curing conditions, enhances the interlayer adhesion and crosslinking density between the anti-reflection layer and the hardened layer, thereby enhancing the scratch resistance of the anti-reflection film. On the other hand, although the addition amount of the hollow nano-silica particles in the anti-reflection layer is increased, the anti-reflection effect is also enhanced, but the crosslinking density of the anti-reflection layer is affected, the UV energy is further increased, and although the crosslinking density can be enhanced to a certain extent, the scratch resistance of the anti-reflection layer is still reduced, such as a slight whitening phenomenon of the anti-reflection layer observed by naked eyes after the friction of the steel wool in the example ten.
Claims (10)
1. A scratch-resistant anti-reflection film is characterized in that a hardening layer coating solution is coated on a substrate, the hardening layer coating solution is heated and cured to be surface-dried at the temperature of 60-80 ℃ to form a hardening layer, then an anti-reflection layer coating solution is coated on the hardening layer, and the anti-reflection layer coating solution is sequentially heated and cured at the temperature of 80-150 ℃ for at least 1min and UV-cured to form an anti-reflection layer, so that the scratch-resistant anti-reflection film is obtained, wherein the UV-cured energy is 600mJ/cm 2 The hardened layer comprises the following material components in parts by weight: 100 parts of dual-curing resin, 1 to 10 parts of photoinitiator, 1 to 10 parts of isocyanate, 5 to 40 parts of closed isocyanate, 100 to 850 parts of solvent and 0.5 to 10 parts of other auxiliary agents; the anti-reflection layer comprises the following material components in parts by weight: 100 parts of light-cured resin, 10 to 80 parts of hollow nano silicon dioxide particles, 4000 to 10000 parts of solvent and 1 to 10 parts of other auxiliary agents; the dual-curing resin is acrylic resin containing hydroxyl; the surface of the hollow nano silicon dioxide particle is provided with hydroxyl.
2. The scratch-resistant antireflection film according to claim 1, wherein the hydroxyl value of the hydroxyl group-containing acrylic resin is 20 to 200mgKOH/g.
3. The scratch resistant, antireflective film according to claim 2 wherein the dual cure resin is one or more of a polyurethane acrylic resin, a polyester acrylic resin and an epoxy acrylic resin.
4. The scratch-resistant anti-reflection film as claimed in claim 1, wherein the blocked isocyanate is suitable for a photocuring system, can be dissolved in an organic solvent, and has an NCO equivalent weight of preferably not less than 200 and a ring opening temperature of 80-150 ℃.
5. The scratch-resistant and antireflection film according to claim 1, wherein the photocurable resin is an acrylic resin having a functional group of 3 or more and being aliphatic and specially modified, and having excellent abrasion resistance, and comprises one or more of aliphatic urethane acrylic resin, aliphatic polyester acrylic resin, epoxy acrylic resin, modified bisphenol a epoxy acrylic resin, and fluorine-modified urethane acrylic resin.
6. The scratch resistant, antireflective film according to claim 1 wherein the hollow nanosilica particles have a surface per nm 2 The number of the hydroxyl groups on the surface is more than or equal to 5, and the particle size of the hollow nano silicon dioxide particles is 10nm-100nm.
7. The scratch-resistant anti-reflective film according to claim 1, wherein the solvent is any one or a mixture of isopropyl alcohol, acetone, methyl isobutyl ketone, butanone, propylene glycol methyl ether, propylene glycol monobutyl ether, methyl acetate, ethyl acetate, and butyl acetate.
8. The scratch-resistant antireflection film according to claim 1, wherein the thickness of the cured layer is 2 to 50 μm.
9. The scratch-resistant antireflection film according to claim 1, wherein a thickness of the antireflection layer is 90nm to 110nm.
10. The scratch-resistant anti-reflection film according to claim 1, characterized in that the anti-reflection film has a steel wool resistance of 1500 times/1 kg, an interlayer adhesion force of water boiling for two hours of 5B with hundred grids, an average reflectivity of 360nm to 740nm of less than or equal to 2%, a reflectivity at 550nm of 1.4%, and a b value in a CIE Lab color model of-3 to + 3.
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