KR101411006B1 - Hard coating film - Google Patents
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- KR101411006B1 KR101411006B1 KR1020100140046A KR20100140046A KR101411006B1 KR 101411006 B1 KR101411006 B1 KR 101411006B1 KR 1020100140046 A KR1020100140046 A KR 1020100140046A KR 20100140046 A KR20100140046 A KR 20100140046A KR 101411006 B1 KR101411006 B1 KR 101411006B1
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Abstract
The present invention relates to a hard coating film which can maintain a pencil hardness of 3H or more and has a low curl even when a coating film thickness of 10 μm or less is used by using two or more kinds of surface-treated inorganic nanoparticles having different particle diameters.
Description
The present invention relates to a hardcoat film. More specifically, the present invention relates to a hard coating film which can maintain a pencil hardness of 3H or more and has a low curl even when the coating film thickness is 10 占 퐉 or less by including two or more inorganic nanoparticles having different particle diameters.
The polarizing plate is generally formed by bonding a cellulose resin film to both sides of a polarizer on a film made of polyvinyl alcohol or the like. Usually, one of the base films has a multilayer structure in which a protective film is adhered for the purpose of preventing surface damage during transportation and the other resin film is laminated with an adhesive layer and a release film. Such a polarizing plate is used as a major component of a liquid crystal display device. In order to exhibit high durability in using such a polarizing plate in various environments, there is an increasing demand for hard hard coating products during the polarizing surface treatment.
In order to realize a product of high hardness in the past, a pencil hardness of 3H or more can be satisfied when the thickness of the hard coating layer is 10 μm or more. However, as the film thickness increases, curling is increased due to an increase in shrinkage upon UV curing, which may cause film breakage in the production of the polarizing plate, which is disadvantageous in terms of manufacturing cost.
Therefore, it is necessary to develop a hard coat film having a hard coat layer which can satisfy a hardness, for example, a pencil hardness of 3H or more at a thickness of 10 탆 or less, and which is less curled.
It is an object of the present invention to provide a hard coating film which can realize a hardness, for example, a pencil hardness of 3H or more even when the thickness of the coating film is 10 μm or less.
Another object of the present invention is to provide a hardcoat film having a pencil hardness of 3H or more and less curling.
The hard coating film of the present invention may contain an ultraviolet curable resin; Photoinitiators; And inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm, 16-30 nm, and 30-100 nm, and having a pencil hardness of 3H or more.
In one embodiment, the hard coat layer may comprise inorganic nanoparticles surface treated with (meta) acrylate having an average particle size (D50) of 5-15 nm and 16-30 nm.
In one embodiment, the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16-30 nm may be 1: 1 to 1: 9.
In one embodiment, the hard coat layer may comprise inorganic nanoparticles having an average particle size (D50) between 5-15 nm and 30-100 nm.
In one embodiment, the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm: inorganic nanoparticles having an average particle diameter (D50) of 30-100 nm may be 1: 1 to 1: 9.
In one embodiment, the hard coat layer may comprise inorganic nanoparticles having an average particle size (D50) between 5-15 nm, 16-30 nm and 30-100 nm.
In one embodiment, inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16 to 30 nm: inorganic nanoparticles having an average particle diameter (D50) of 30 to 100 nm have a weight ratio of 1 : 1 to 4: 1 to 5.
The present invention provides a hard coating film capable of realizing a hardness, for example, a pencil hardness of 3H or more even when the thickness of the coating film is 10 μm or less. In addition, the present invention provides a hardcoat film having less pencil hardness while realizing a pencil hardness of 3H or more.
The hard coating film of the present invention may have a pencil hardness of 3H or more at a thickness of 10 mu m or less, preferably 1-10 mu m. Generally, in order to realize a hard coating film having a high hardness, the thickness of the hard coating layer should be not less than 10 탆, and the pencil hardness may be 3H or more. However, as the thickness increases, the curling becomes severe. However, the hard coating film of the present invention has a pencil hardness of not less than 3H at a thickness of 10 mu m or less, preferably 1-10 mu m, and is characterized by low curling.
Hereinafter, each component included in the hard coat layer will be described in detail.
Inorganic nanoparticle
In the hard coating film of the present invention, the hard coat layer contains inorganic nanoparticles surface-treated with (meth) acrylate, wherein two or more inorganic nanoparticles having different particle diameters, preferably three or more, more preferably three or more, And may include three species.
The inorganic nanoparticles surface-treated with (meth) acrylate are conventionally used to increase the surface hardness in the hard coat layer. However, when the inorganic nanoparticles are arbitrarily used to increase the surface hardness, the thickness of the hard coating layer may become thick, which may cause curling of the ultraviolet curing.
In the present invention, inorganic nanoparticles having different particle diameters are used, and the ratio of the particle diameter and the content of the inorganic nanoparticles is controlled so as to improve not only the hardness of the pencil but also the curling phenomenon.
When two or more kinds of inorganic nanoparticles are used in the hard coat layer of the present invention, two or more kinds selected from inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm, 16-30 nm and 30-100 nm can be used .
In one embodiment, a mixture of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm and inorganic nanoparticles having an average particle diameter (D50) of 16-30 nm can be used. At this time, the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16-30 nm may be 1: 1-1: 9. Within this range, the pencil hardness can be increased without increasing the thickness of the hard coat layer, and there is no curling. Preferably, it may be 1: 2-1: 5.
In another embodiment, a mixture of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm and inorganic nanoparticles having an average particle diameter (D50) of 30-100 nm can be used. At this time, the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm: inorganic nanoparticles having an average particle diameter (D50) of 30-100 nm may be 1: 1-1: 9. Within this range, the pencil hardness can be increased without increasing the thickness of the hard coat layer, and there is no curling. Preferably, it may be 1: 2-1: 5.
In another embodiment, inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm, inorganic nanoparticles having an average particle diameter (D50) of 16-30 nm, and inorganic nanoparticles having an average particle diameter (D50) . Inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16 to 30 nm: inorganic nanoparticles having an average particle diameter (D50) of 30 to 100 nm in a weight ratio of 1: : It can be 1 to 7. Within this range, the pencil hardness can be increased without increasing the thickness of the hard coat layer, and there is no curling. Preferably 1: 2 to 3: 6 to 7 .
The inorganic nanoparticles surface-treated with (meth) acrylate used in the present invention have a uniform magnetic dispersion property and do not scatter transmitted light and have stable dispersion characteristics, so that there is no entanglement between particles, and transparency is high and turbidity is low .
The inorganic nanoparticles may be those whose surface is treated with a (meth) acrylate compound in an amount of 3 to 50% of the total surface area of the inorganic nanoparticles. Within this range, it has uniform dispersibility and transparency.
The inorganic nanoparticles are not particularly limited and may be organic particles, inorganic particles or a mixture thereof. Preferably, one or more of SiO2, Al2O3, CaCO3, TiO2 and the like can be used.
The inorganic nanoparticles may be contained in a non-surface-treated state, but those that have been surface-treated with (meth) acrylate may also be used.
The inorganic nanoparticle surface treatment agent may be at least one selected from the group consisting of a vinyl-based, epoxy-based, methacrylic rock-based, amino-based silane coupling agent and the like, but is not limited thereto. It is a common practice to surface-treat inorganic nanoparticles with a (meth) acrylic rock silane coupling agent for chemical bonding with an acrylate resin.
The method of surface-treating inorganic nanoparticles with (meth) acrylate can be carried out by a conventional method. For example, it can be surface-treated through chemical bonding between inorganic nanoparticles and (meth) acrylate. For the above chemical bonding, the inorganic nanoparticles may be pretreated with at least one silane coupling agent selected from the group consisting of a vinyl-based, epoxy-based, (meth) acrylic rock clock and amino system.
The inorganic nanoparticles surface-treated with (meth) acrylate may be contained in an amount of 10 to 70% by weight, based on the solids content, of a hard coat layer comprising an ultraviolet curable resin, inorganic nanoparticles surface-treated with (meth) acrylate and a photoinitiator. Within this range, there is no decrease in surface hardness, no curling and the haze of the film may not increase. Preferably from 20 to 50% by weight.
The hard coat layer of the present invention may contain an ultraviolet curable resin and a photoinitiator in addition to inorganic nanoparticles.
Ultraviolet curable resin
The ultraviolet ray curable resin is a resin having an acrylate functional group, and examples thereof include urethane resin, polyester resin, polyether resin, acrylic resin, epoxy resin, alkyd resin, spiroacetal resin, polybutadiene resin, polythiol polyene resin, (Meth) acrylate resins of polyfunctional compounds such as polyhydric alcohols and the like. Preferably, a urethane resin can be used.
Specific examples thereof include ethylene glycol diacrylate, neopentyl glycol di (meth) acrylate, 1,6-hexanediol (meth) acrylate, trimethylolpropane tri (meth) acrylate, dipentaerythritol hexa (Meth) acrylate obtained by esterifying a di (meth) acrylate of a polyol poly (meth) acrylate, a bisphenol A-diglycidyl ether, a polyhydric alcohol and a polyvalent carboxylic acid and an anhydride thereof with acrylic acid, , At least one member selected from the group consisting of polysiloxane polyacrylate, urethane (meth) acrylate, pentaerythritol tetramethacrylate and glycerin trimethacrylate, aromatic urethane, alicyclic urethane and urethane acrylate resin But are not limited thereto.
The ultraviolet curable resin having an acrylate-based functional group may include an acrylate compound having a hydroxy group.
Such an acrylate compound having a hydroxy group may be selected from oligomers such as 2-hydroxyethyl acrylate oligomer, 2-hydroxypropyl acrylate oligomer and pentaerythritol triacrylate oligomer, 2-hydroxyethyl (meth) acrylate, 2- Monomers such as hydroxypropyl (meth) acrylate, caprolactone (meth) acrylate, 2,3-dihydroxypropyl (meth) acrylate and 4-hydroxymethylcyclohexyl (meth) acrylate can be used .
The ultraviolet curable resin may be a fluorine-containing resin such as a fluorine-containing epoxy acrylate or a fluorine-containing alkoxysilane. Specific examples thereof include 2- (perfluorodecyl) ethyl (meth) acrylate, 3-perfluorooctyl-2-hydroxypropyl (meth) acrylate, 3- (perfluoro- , 2-epoxypropane, (meth) acrylic acid-2,2,2-trifluoroethyl, (meth) acrylic acid-2,2,2-trifluoromethyl, 3,3,3- But are not limited thereto.
The ultraviolet curable resin may be contained in an amount of 30 to 89% by weight, based on the solids content, of a hard coat layer comprising an ultraviolet curable resin, inorganic nanoparticles surface-treated with (meth) acrylate, and a photoinitiator. Within this range, the hard coat layer has good pencil hardness, good scratch resistance, and no curling. Preferably 50 to 80% by weight.
Photoinitiator
As the photoinitiator, conventionally known photoinitiators conventionally used can be used. For example, benzophenone compounds such as 1-hydroxycyclohexyl phenyl ketone can be used, but are not limited thereto.
The photoinitiator may be contained in an amount of 0.1 to 10% by weight, based on the solids content, of a hard coat layer comprising an ultraviolet curable resin, inorganic nanoparticles surface-treated with (meth) acrylate, and a photoinitiator. Within the above range, pencil hardness and scratch resistance are satisfied without uncured. Preferably 0.3-0.7 wt%.
The hard coating layer of the present invention may further comprise a polyfunctional monomer.
Multifunctional Monomer
The polyfunctional monomer may be a monomer having two or more functional groups, preferably six or more functional groups. For example, the polyfunctional monomer may be at least one selected from the group consisting of a hydroxyl group-containing polyfunctional (meth) acrylate and a fluorine-modified polyfunctional (meth) acrylate.
Examples of the hydroxyl group-containing polyfunctional (meth) acrylate include ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, Hexanediol diacrylate, hexanediol diacrylate, neopentyldiacrylate, pentaerythritol diacrylate, pentaerythritol triacrylate, dipentaerythritol diacrylate, dipentaerythritol triacrylate, dipentaerythritol pentaacrylate (Meth) acrylate, dipentaerythritol hexaacrylate, bisphenol A diacrylate, trimethylol propane triacrylate, novolak epoxy acrylate, propylene glycol di (meth) acrylate, 1,4-butanediol Di (meth) acrylate, and 1,6-hexanediol di (meth) acrylate. But are not limited to these.
When the multifunctional monomer is included, the ultraviolet curable resin is contained in the hard coat layer in an amount of 35-59 wt%, the multifunctional monomer is contained in 10-30 wt%, the inorganic nanoparticles are contained in 30-50 wt% The photoinitiator may be included in an amount of 0.1-5% by weight. Within this range, the pencil hardness and scratch resistance of the hard coat layer may be good. Preferably from 10 to 20% by weight.
The hard coat layer of the present invention can be used in a conventional manner such as a photosensitizer, a photosensitizer, a polymerization inhibitor, a leveling agent, a wettability improver, a surfactant, a plasticizer, an ultraviolet absorbent, an antioxidant, an antistatic agent, a silane coupling agent, And may further include additives. These may be used alone or in combination of two or more.
The hard coating film of the present invention can include a base film and the hard coating layer, and has a structure in which a hard coating layer is formed on a base film.
The base film may be at least one selected from the group consisting of, for example, a cellulose ester resin, a polyester resin, a polycarbonate resin, a norbornene resin, a polyarylate resin and a polysulfone resin. Preferably, a triacetylcellulose film which is an acetylcellulose-based resin can be used.
The thickness of the base film may be 80 占 퐉, and the thickness of the hard coat layer may be 10 占 퐉 or less, preferably 3-8 占 퐉, but is not limited thereto.
The hard coating film of the present invention can be mounted so as to serve as a protecting and supporting polarizer in a polarizing plate.
A method for producing a hard coat film comprises the steps of: preparing a composition for forming a hard coat layer; Applying the composition to a substrate film; Drying said composition; And curing the composition.
In the step of preparing the composition for forming a hard coat layer, each component contained in the hard coat layer of the present invention is added to prepare a composition. The content of each component is as described above. As the composition, a solvent having solubility and swelling property in the ultraviolet curable resin may be used.
As the solvent, a solvent having solubility and swelling property in the ultraviolet curable resin may be used. Specific examples thereof include methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, acetone, diacetone alcohol or polyhydric alcohol as the ketone, methyl cellosolve, ethyl cellosolve, butyl cellosolve or cellosolve acetate as the ethers, ester Methylene chloride, methylene chloride or tetrachloroethane as the halogenated hydrocarbons, nitromethane, acetonitrile, N-methylpyrrolidone or N, N-dimethylformamide as the nitrogen-containing compounds , Or a mixture of two or more of them may be used.
In the application step, the composition for forming a hard coat layer is applied on a base film. As a method of applying the composition to the base film, a bar coating method, a knife coating method, a gravure coating method, a microgravure coating method, a slot die coating method, or the like can be used.
In the drying step, the composition for forming a coated hard coat layer is dried to remove the solvent.
In the ultraviolet curing step, ultraviolet rays are irradiated to cure the dried composition for forming a hard coat layer to form a hard coat layer on the substrate film. Examples of ultraviolet lamps include high-pressure mercury lamps, metal halide lamps, xenon lamps, and microwave type electrodeless lamps. The wavelength range is 250-360 nm, and the light amount may be 180-250 mJ / cm 2, but is not limited thereto.
Hereinafter, the configuration and operation of the present invention will be described in more detail with reference to preferred embodiments of the present invention. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense.
The contents not described here are sufficiently technically inferior to those skilled in the art, and a description thereof will be omitted.
Specific specifications of the components used in the following examples and comparative examples are as follows.
1. UV curable resin: HX-920UV (Kyoeisha)
2. Polyfunctional monomer: DPHA (SK cytec)
3. Inorganic nanoparticles surface-treated with (meth) acrylate
- Optisol-SST650U (average particle diameter: 12 nm, Ranco)
- Optisol-SST350T1 (average particle diameter: 22 nm, Ranco)
- Optisol-SST2350T3 (average particle diameter: 50 nm, Ranco)
4. Photoinitiator: Irgacure 184 (Ciba Specialty)
5. Base film: triacetylcellulose film (thickness: 80 占 퐉, Normal TAC, Hyosung)
Example 1-3: Preparation of Hard Coat Film
45 parts by weight of an ultraviolet curable resin, 14.9 parts by weight of a polyfunctional monomer, and an average particle diameter (D50) (nm) and a content (parts by weight) of inorganic nanoparticles were measured in 10 g of ethyl acetate as a solvent and 20 g of methyl ethyl ketone, And the mixture was stirred for 20 minutes. Then, 0.1 part by weight of a photopolymerization initiator was added and stirred for 10 minutes to prepare a composition for forming a hard coat layer.
The resulting composition was coated on a triacetyl cellulose film with a # 16 meyer bar coater to a thickness of 7 μm and dried at 80 ° C. for 40 seconds. Dried, and then irradiated with ultraviolet rays at a light quantity of 180 mJ / cm 2 with a high-pressure mercury lamp to cure the hard coat film to give a hard coat film having a thickness of 7 μm.
Comparative Example 1-2: Preparation of hard coat film
A hard coat film having a thickness of 7 탆 was prepared in the same manner as in Example 1 except that the content of the component was changed to the content shown in Table 1 below. In Table 1, the unit of the content is parts by weight.
Experimental Example: Measurement of Physical Properties of Hard Coating Film
The hard coating films prepared in the Examples and Comparative Examples were measured for physical properties shown in Table 2 below, and the results are shown in Table 2 below.
≪ Method for measuring physical properties &
1. Pencil Hardness: A pencil hardness tester (Shinto Scientific, Heidon) was used with a Mitsubishi evaluation pencil (UNI) to draw 5 mm 5 times at a rate of 0.5 mm / sec under a load of 500 kg / cm 2, The pencil hardness was evaluated.
2. Curling: A film sample of 100 mm x 100 mm was prepared and the height (H) of the four corners was measured at the highest point on the floor.
3. Scratch resistance: The number of scratches was checked after rubbing with a steelwool (# 0000) at a speed of 1000 g, a speed of 50 mm / sec, and a distance of 100 mm by reciprocating 10 times, and it was evaluated whether or not a scratch occurred.
4. Rainbow (interference fringe) existence test: In order to prevent the back reflection, a black tape was attached to the opposite surface of the hard coating layer, and after the visual inspection under the triple wavelength fluorescence on the surface of the hard coating layer, it was evaluated as the following evaluation criteria.
<Rainbow Evaluation Criteria>
1: No rainbow in all directions.
2: Weak
3: Strongly occurred
As shown in Table 2, the hard coating film of the present invention had a pencil hardness of 3.6H even at a coating film thickness of 7 占 퐉, showing almost no curling. On the other hand, in Comparative Examples 1 and 2 including only one kind of inorganic nanoparticles having an average particle diameter of 12 nm, pencil hardness was much lower than that of the present invention, curling was remarkable, and scratch resistance was not good.
Claims (15)
The inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm and the inorganic nanoparticles having an average particle diameter (D50) of 16 to 30 nm each have a surface area of 3 to 50% Lt; / RTI >
Wherein the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5-15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16-30 nm is 1: 1 to 1: 9.
The inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm and the inorganic nanoparticles having an average particle diameter (D50) of 30 to 100 nm each have a (meth) acrylate content of 3 to 50% Lt; / RTI >
Wherein the weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm: inorganic nanoparticles having an average particle diameter (D50) of 30 to 100 nm is 1: 1 to 1: 9.
The inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm, inorganic nanoparticles having an average particle diameter (D50) of 16 to 30 nm, and inorganic nanoparticles having an average particle diameter (D50) of 31 to 100 nm, 3 to 50% of the total surface area is surface-treated with (meth) acrylate,
The inorganic nanoparticles having an average particle diameter (D50) of 5 to 15 nm: inorganic nanoparticles having an average particle diameter (D50) of 16 to 30 nm: a weight ratio of inorganic nanoparticles having an average particle diameter (D50) of 31 to 100 nm is 1: : 1.5 to 5. < / RTI >
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| KR1020100140046A KR101411006B1 (en) | 2010-12-31 | 2010-12-31 | Hard coating film |
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| KR1020100140046A KR101411006B1 (en) | 2010-12-31 | 2010-12-31 | Hard coating film |
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| KR101411006B1 true KR101411006B1 (en) | 2014-06-23 |
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| KR20170016298A (en) * | 2015-08-03 | 2017-02-13 | 주식회사 엘지화학 | Coating composition for flexible plastic film |
| KR20170016297A (en) * | 2015-08-03 | 2017-02-13 | 주식회사 엘지화학 | Flexible plastic film |
| US11168191B2 (en) | 2015-08-03 | 2021-11-09 | Lg Chem, Ltd. | Flexible plastic film |
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| KR101622001B1 (en) * | 2012-12-27 | 2016-05-17 | 제일모직주식회사 | Hard coating film and method for preparing the same |
| KR101853888B1 (en) * | 2016-11-30 | 2018-06-08 | 존스미디어 주식회사 | High elongation / high hardness hard coating compositions and coating films |
| KR101725026B1 (en) * | 2016-12-06 | 2017-04-07 | 황중국 | Composition for hard coating film having high hardness and Film for protecting display panel having high hardness |
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| KR20170016298A (en) * | 2015-08-03 | 2017-02-13 | 주식회사 엘지화학 | Coating composition for flexible plastic film |
| KR20170016297A (en) * | 2015-08-03 | 2017-02-13 | 주식회사 엘지화학 | Flexible plastic film |
| KR20190129813A (en) * | 2015-08-03 | 2019-11-20 | 주식회사 엘지화학 | Flexible plastic film |
| KR20190130536A (en) * | 2015-08-03 | 2019-11-22 | 주식회사 엘지화학 | Flexible plastic film |
| KR102094450B1 (en) * | 2015-08-03 | 2020-03-27 | 주식회사 엘지화학 | Flexible plastic film |
| US10626292B2 (en) | 2015-08-03 | 2020-04-21 | Lg Chem, Ltd. | Coating composition for flexible plastic film |
| KR20200044780A (en) * | 2015-08-03 | 2020-04-29 | 주식회사 엘지화학 | Coating composition for flexible plastic film |
| KR102107737B1 (en) | 2015-08-03 | 2020-05-07 | 주식회사 엘지화학 | Flexible plastic film |
| KR102107738B1 (en) * | 2015-08-03 | 2020-05-07 | 주식회사 엘지화학 | Flexible plastic film |
| KR102107736B1 (en) * | 2015-08-03 | 2020-05-07 | 주식회사 엘지화학 | Coating composition for flexible plastic film |
| KR102294400B1 (en) * | 2015-08-03 | 2021-08-26 | 주식회사 엘지화학 | Coating composition for flexible plastic film |
| US11161951B2 (en) | 2015-08-03 | 2021-11-02 | Lg Chem, Ltd. | Coating composition for flexible plastic film |
| US11168191B2 (en) | 2015-08-03 | 2021-11-09 | Lg Chem, Ltd. | Flexible plastic film |
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