CN111253854A - Anti-reflective coating material containing modified porous silica, preparation method and anti-reflective film - Google Patents
Anti-reflective coating material containing modified porous silica, preparation method and anti-reflective film Download PDFInfo
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- CN111253854A CN111253854A CN202010264701.1A CN202010264701A CN111253854A CN 111253854 A CN111253854 A CN 111253854A CN 202010264701 A CN202010264701 A CN 202010264701A CN 111253854 A CN111253854 A CN 111253854A
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- 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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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/006—Anti-reflective coatings
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- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- 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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses an anti-reflection coating containing modified porous silicon dioxide, a preparation method and an anti-reflection film, wherein the anti-reflection coating comprises the following components in parts by weight: 12-20 parts of urethane acrylate, 15-25 parts of active monomer, 1-7 parts of fluorine modified porous silica, 2-4.5 parts of photoinitiator and 50-70 parts of organic solvent. The fluorine modified porous silicon dioxide is adopted, the agglomeration of the porous silicon dioxide is reduced, the wetting compatibility of the porous silicon dioxide and a resin system is provided, and the fluorine modified porous silicon dioxide can quickly cover the surface of a coating in airflow generated by solvent volatilization by utilizing the surface directional migration capacity of fluorine element to form a low-refractive-index layer. According to the invention, the surface of the coating is directionally covered by the fluorine modified porous silicon dioxide with low refractive index, the high refractive index coating and the low refractive index coating are designed by 1-pass precision coating, and multiple passes of coating with complex process and low yield are not needed.
Description
Technical Field
The invention relates to the technical field of anti-reflection coatings, in particular to an anti-reflection coating containing modified porous silicon dioxide, a preparation method and an anti-reflection film.
Background
Display screens of televisions, notebooks, displays, smart phones, vehicle-mounted displays and the like are subjected to image display overlapping caused by external light reflection, so that image display is unclear, energy consumption of brightness increase and visual fatigue of users are caused. In the fields of smart phones with high outdoor use frequency, vehicle-mounted display and the like, the method of attaching the anti-reflection screen protection film is a good method. The antireflection is achieved by the following method: firstly, the surface is made into a micro-nano structure, such as a bionic moth eye structure. The method has the defects that the nano-imprinting size precision requires high equipment investment, and the nano structure is not scratch resistant and has weak physical properties. And secondly, designing a multi-layer structure with matched refractive indexes according to an optical principle to reduce light reflection. The anti-reflection film realized by the method has adjustable physical properties and is suitable for large-scale mass production.
Chinese patent CN110196461A discloses an anti-reflection film, CN109416415A discloses an anti-reflection film, CN109188572A discloses an anti-reflection film, a polarizer and an image display device, CN108885281A discloses an anti-reflection film and a preparation method thereof, and CN101858994B discloses a low reflection film, all of these prior arts are to design refractive index matching by 2 layers or 3 layers of coatings to realize low reflectivity, and have the disadvantages that multiple coating processes are required, the process production time consumption is long, the yield is low, and the coating thickness of the last low refractive index layer is 100 plus 200nm, which requires high precision of the equipment, so that the equipment investment is large and the process difficulty is high.
Disclosure of Invention
In view of the above, the present invention provides an anti-reflective coating containing modified porous silica, a preparation method thereof and an anti-reflective film, which can effectively solve the problems of the prior art, such as complexity and low yield of products.
In order to achieve the purpose, the invention adopts the following technical scheme:
an anti-reflective coating containing modified porous silicon dioxide comprises the following components in parts by weight: 12-20 parts of urethane acrylate, 15-25 parts of active monomer, 1-7 parts of fluorine modified porous silica, 2-4.5 parts of photoinitiator and 50-70 parts of organic solvent.
Preferably, the reaction functionality of the polyurethane acrylate is more than or equal to 6.
Preferably, the reactive monomer is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetramethacrylate, pentaerythritol trimethacrylate, dipentaerythritol hexaacrylate, and dipentaerythritol pentaacrylate.
Preferably, the particle size of the fluorine modified porous silica is 50nm to 200 nm.
As a preferable scheme, the particle size of the fluorine modified porous silica is 100-120 nm.
Preferably, the photoinitiator is a cleavage type photoinitiator.
Preferably, the organic solvent is one or more of isopropanol, methyl ethyl ketone, ethyl acetate, butyl acetate and methyl isobutyl ketone.
12-20 parts of urethane acrylate, 15-25 parts of active monomer, 1-7 parts of fluorine modified porous silica, 2-4.5 parts of photoinitiator and 50-70 parts of organic solvent are added into a container to be mixed and stirred uniformly.
An antireflection film prepared from the aforementioned antireflection coating containing modified porous silica.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
the fluorine modified porous silicon dioxide is adopted, the agglomeration of the porous silicon dioxide is reduced, the wetting compatibility of the porous silicon dioxide and a resin system is provided, and the fluorine modified porous silicon dioxide can quickly cover the surface of a coating in airflow generated by solvent volatilization by utilizing the surface directional migration capacity of fluorine element to form a low-refractive-index layer. According to the invention, the surface of the coating is directionally covered by the fluorine modified porous silicon dioxide with low refractive index, the high refractive index coating and the low refractive index coating are designed by 1-pass precision coating, multiple passes of coating with complex process and low yield are not needed, and the defect that the coating of the nanoscale low-refractive index layer in the prior art needs nitrogen curing is also solved.
Detailed Description
The invention discloses an anti-reflection coating containing modified porous silicon dioxide, which comprises the following components in parts by weight: 12-20 parts of urethane acrylate, 15-25 parts of active monomer, 1-7 parts of fluorine modified porous silica, 2-4.5 parts of photoinitiator and 50-70 parts of organic solvent. The reaction functionality of the polyurethane acrylate is more than or equal to 6. The active monomer is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetramethacrylate, pentaerythritol trimethacrylate, dipentaerythritol hexaacrylate and dipentaerythritol pentaacrylate. The particle size of the fluorine modified porous silica is 50nm-200 nm. The particle size of the fluorine modified porous silica is 100-120 nm. The photoinitiator is a cracking photoinitiator. The organic solvent is one or more of isopropanol, methyl ethyl ketone, ethyl acetate, butyl acetate and methyl isobutyl ketone.
The invention also discloses a preparation method of the anti-reflection coating containing the modified porous silicon dioxide, which comprises the steps of adding 12-20 parts by weight of urethane acrylate, 15-25 parts by weight of active monomer, 1-7 parts by weight of fluorine modified porous silicon dioxide, 2-4.5 parts by weight of photoinitiator and 50-70 parts by weight of organic solvent into a container, mixing and uniformly stirring.
The invention also discloses an antireflection film prepared from the antireflection coating containing the modified porous silicon dioxide.
The invention is illustrated in more detail below in the following examples:
example 1:
an anti-reflective coating containing modified porous silicon dioxide comprises the following components in parts by weight: 12 parts by weight of a 6-reactive-functionality urethane acrylate (Zhanxin EB 5129), 25 parts by weight of pentaerythritol triacrylate (Yangxing chemical EM 235C), 3 parts by weight of fluorine-modified porous silica (particle size 100nm, pore volume 40%), 2 parts by weight of a photoinitiator (Long-term chemical JRcure-1104), 20 parts by weight of isopropanol and 40 parts by weight of methyl ethyl ketone; when in preparation, the components are added into a container to be mixed and stirred uniformly, and the anti-reflection coating containing the fluorine modified porous silicon dioxide is prepared.
Then, the above anti-reflective coating containing fluorine modified porous silica was coated on a 100 μm polyethylene terephthalate (PET) optical base film, and about 80 μm was placedoDrying in an oven for 1-2min, drying with a dry film thickness of 3-4 μm and a radiation energy of 400-600mJ/cm2And curing to obtain the anti-reflection film.
Example 2:
an anti-reflective coating containing modified porous silicon dioxide comprises the following components in parts by weight: 20 parts by weight of 6-reactive-functionality urethane acrylate (DSM 230A 2), 15 parts by weight of dipentaerythritol hexaacrylate (GB 66G 00), 2 parts by weight of fluorine-modified porous silica (particle size 120nm, pore volume 50%), 3 parts by weight of photoinitiator (Long-term chemical JRcure-1113), 17 parts by weight of isopropanol and 33 parts by weight of methyl ethyl ketone; when in preparation, the components are added into a container to be mixed and stirred uniformly, and the anti-reflection coating containing the fluorine modified porous silicon dioxide is prepared.
Then the anti-reflective coating containing fluorine modified porous silica is coated on a 150 μm polymethyl methacrylate (PMMA) optical base film and placed in a position of about 80oDrying in an oven for 1-2min, drying with a dry film thickness of 3-4 μm and a radiation energy of 400-600mJ/cm2And curing to obtain the anti-reflection film.
Example 3:
an anti-reflective coating containing modified porous silicon dioxide comprises the following components in parts by weight: 12 parts by weight of 9-reactive-functionality urethane acrylate (sartomer CN 9013N), 25 parts by weight of pentaerythritol triacrylate (changxing chemical EM 235C), 5 parts by weight of fluorine-modified porous silica (particle size 100nm, pore volume 30%), 5 parts by weight of photoinitiator (jurcure-1103), 25 parts by weight of isopropanol and 45 parts by weight of methyl ethyl ketone; when in preparation, the components are added into a container to be mixed and stirred uniformly, and the anti-reflection coating containing the fluorine modified porous silicon dioxide is prepared.
Then the anti-reflective coating containing fluorine modified porous silica is coated on a cellulose Triacetate (TAC) optical base film with the thickness of 80 μm, and is placed in a position of about 80oDrying in an oven for 1-2min, drying with a dry film thickness of 3-4 μm and a radiation energy of 400-600mJ/cm2And curing to obtain the anti-reflection film.
Comparative example:
an anti-reflective coating comprises the following components in parts by weight: 12 parts by weight of a 6-reactive-functional urethane acrylate (Zhanxin EB 5129), 25 parts by weight of pentaerythritol triacrylate (Yangxing chemical EM 235C), 3 parts by weight of porous silica (particle size 100nm, pore volume 40%), 2 parts by weight of a photoinitiator (Long-term chemical JRcure-1104), 20 parts by weight of isopropanol and 40 parts by weight of methyl ethyl ketone; when in preparation, the components are added into a container to be mixed and stirred uniformly, and the anti-reflection coating is prepared.
The anti-reflective coating was then applied to a 100 μm polyethylene terephthalate (PET) optical base film, which was placed in a chamber of about 80 angstromsoDrying in an oven for 1-2min, drying with a dry film thickness of 3-4 μm and a radiation energy of 400-600mJ/cm2And curing to obtain the anti-reflection film.
The properties are shown in the following table:
performance of | Example 1 | Example 2 | Example 3 | Comparative example |
Hardness of | H | 2H | H | H |
Reflectivity of light | 1.6 | 1.3 | 2.1 | 3.6 |
Hardness: testing according to GB/T6739-2006.
Reflectance ratio: the wavelength average reflectance at 380-780nm was measured using a U-4100 spectroscopic spectrometer (manufactured by Hitachi, Japan).
The design of the invention is characterized in that: the fluorine modified porous silicon dioxide is adopted, the agglomeration of the porous silicon dioxide is reduced, the wetting compatibility of the porous silicon dioxide and a resin system is provided, and the fluorine modified porous silicon dioxide can quickly cover the surface of a coating in airflow generated by solvent volatilization by utilizing the surface directional migration capacity of fluorine element to form a low-refractive-index layer. According to the invention, the surface of the coating is directionally covered by the fluorine modified porous silicon dioxide with low refractive index, the high refractive index coating and the low refractive index coating are designed by 1-pass precision coating, multiple passes of coating with complex process and low yield are not needed, and the defect that the coating of the nanoscale low-refractive index layer in the prior art needs nitrogen curing is also solved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (9)
1. An antireflective coating comprising modified porous silica, characterized by: comprises the following components in parts by weight: 12-20 parts of urethane acrylate, 15-25 parts of active monomer, 1-7 parts of fluorine modified porous silica, 2-4.5 parts of photoinitiator and 50-70 parts of organic solvent.
2. The modified porous silica-containing antireflective coating of claim 1, wherein: the reaction functionality of the polyurethane acrylate is more than or equal to 6.
3. The modified porous silica-containing antireflective coating of claim 1, wherein: the active monomer is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetramethacrylate, pentaerythritol trimethacrylate, dipentaerythritol hexaacrylate and dipentaerythritol pentaacrylate.
4. The modified porous silica-containing antireflective coating of claim 1, wherein: the particle size of the fluorine modified porous silica is 50nm-200 nm.
5. The antireflective coating containing modified porous silica as claimed in claim 4, wherein: the particle size of the fluorine modified porous silica is 100-120 nm.
6. The modified porous silica-containing antireflective coating of claim 1, wherein: the photoinitiator is a cracking photoinitiator.
7. The modified porous silica-containing antireflective coating of claim 1, wherein: the organic solvent is one or more of isopropanol, methyl ethyl ketone, ethyl acetate, butyl acetate and methyl isobutyl ketone.
8. A process for the preparation of an antireflective coating comprising modified porous silica as claimed in any one of claims 1 to 7, wherein: adding 12-20 parts by weight of polyurethane acrylate, 15-25 parts by weight of active monomer, 1-7 parts by weight of fluorine modified porous silica, 2-4.5 parts by weight of photoinitiator and 50-70 parts by weight of organic solvent into a container, mixing and uniformly stirring.
9. An antireflection film characterized by: prepared from the antireflective coating comprising modified porous silica according to any one of claims 1 to 7.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113896839A (en) * | 2021-10-15 | 2022-01-07 | 江苏锐辰光电技术有限公司 | Hollow porous silica microsphere reinforced photocuring 3D printing composite material |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2005338868A (en) * | 2005-06-27 | 2005-12-08 | Hoya Corp | Method for producing plastic spectacle lens excellent in ultraviolet absorbency |
CN106338783A (en) * | 2015-09-17 | 2017-01-18 | 湖北航天化学技术研究所 | Anti-glare anti-reflection optical film, and preparation method and application thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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JP2005338868A (en) * | 2005-06-27 | 2005-12-08 | Hoya Corp | Method for producing plastic spectacle lens excellent in ultraviolet absorbency |
CN106338783A (en) * | 2015-09-17 | 2017-01-18 | 湖北航天化学技术研究所 | Anti-glare anti-reflection optical film, and preparation method and application thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113896839A (en) * | 2021-10-15 | 2022-01-07 | 江苏锐辰光电技术有限公司 | Hollow porous silica microsphere reinforced photocuring 3D printing composite material |
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