KR100638509B1 - Method for manufacturing screening near infrared ray filter and screening near infrared ray filter using thereof - Google Patents

Abstract

A method for manufacturing a near infrared ray screening filter and a near infrared ray screening filter using the same are provided to form a near infrared ray screening layer by using a spin-coating method. A near infrared ray screening layer is formed by using a spin-coating method. A mixture of a near infrared ray screening composition and an organic solvent is coated on a transparent supporting layer. The near infrared ray screening composition includes a curable resin, a near infrared ray screening dye of 0.1 to 15 weight percent, a hardener of 0.1 to 15 weight percent, and a leveling agent of 0.1 to 3 weight percent. The curable resin includes a thermosetting resin as a base resin. A drying process is performed to evaporate the organic solvent from the near infrared ray screening layer. A hardening process is performed to harden the near infrared ray screening layer.

Description

Method for manufacturing near-infrared shielding filter and near-infrared shielding filter using same {Method for Manufacturing Screening Near Infrared Ray Filter and Screening Near Infrared Ray Filter using

1 is a graph showing the transmittance of preferred Example 1 and Comparative Example 1 according to the present invention.

The present invention relates to a method for manufacturing a near-infrared shielding filter and a near-infrared shielding filter using the same, and more particularly, a dye having a near-infrared shielding function is mixed with a thermosetting resin or an ultraviolet-curable resin to apply a near-infrared shielding layer by spin coating to apply near-infrared shielding. A method of manufacturing a shielding filter and a near-infrared shielding filter using the same.

The conventional near-infrared shielding filter was a method of mixing a dye having a near-infrared shielding function with a pressure-sensitive adhesive. In the case of a pressure-sensitive adhesive composition (published number 10-2004-0049280 and published number 10-2005-0019046), which is a mixture of a pressure-sensitive adhesive and a dye, when a pressure-sensitive adhesive passes a high temperature drying furnace, While decomposing the mixed dye while volatilizing), there was a disadvantage in modifying the physical and chemical properties of the dye, and a technical necessity for protecting the damaged dye was required.

In addition, the roll-to-roll coating method, the COMMA coating method, the die coating method, etc., had a disadvantage in that the ultra-thin film was not evenly applied evenly applying the dye component having a near infrared shielding function.

In particular, in the case of PDP (Plazma Display Panel, hereinafter referred to as 'PDP'), voltage is applied to helium, neon, argon, xenon, etc. injected between two panes, and visible light is emitted by emitting ultraviolet rays generated at this time to the light emitting body. Near-infrared rays, among the harmful rays generated in addition to the visible rays generated from the PDP, may affect the remote control for home appliances such as TVs, air conditioners, video decks, audio devices, and communication devices, or may affect data transmission. There is an urgent need for filters.

The present invention is to overcome the problems of the prior art, a method of manufacturing a near-infrared shielding filter using a spin coating method and a near-infrared shielding through the near-infrared shielding filter using the same, the dye is applied evenly without damaging the dye. In addition, the near-infrared shielding layer is applied to the ultra-thin film by adjusting the rotation speed, coating time, viscosity, etc. using the stin coating method according to the present invention.

The present invention is a method for manufacturing a near-infrared shielding filter for applying a near-infrared shielding composition to a transparent support layer to form a near-infrared shielding layer,

(1) the near-infrared shielding layer is applied by spin coating, the rotation speed is 10rpm to 7,000rpm, the coating time is 1 second to 500 seconds, the near-infrared shielding composition is mixed with an organic solvent and applied to the transparent support layer, The near-infrared shield composition comprises a curable resin, a near-infrared shield dye, a curing agent and a leveling agent, wherein the curable resin is a thermosetting resin as a base resin, in the near-infrared shield composition 100% by weight,

a) the near infrared shielding dye is 0.1% to 15% by weight;

b) 0.1% to 15% by weight of the curing agent; And

c) the spin coating step, characterized in that the leveling agent is 0.1% to 3% by weight;

(2) a drying step of drying at a drying temperature of 15 ° C. to 85 ° C. and a rotational speed of 20 rpm to 5,000 rpm to volatilize the organic solvent applied together to the near infrared shielding layer coated in the spin coating step; And

(3) a method for producing a near-infrared shielding filter comprising a curing step of thermally curing the near-infrared shield layer dried in the drying step at a curing temperature of 70 ° C. to 140 ° C. and a curing time of 30 seconds to 15 minutes, and a near infrared shielding filter using the same. Can be achieved.

Hereinafter, the present invention will be described in detail with reference to the technical configuration.

The near-infrared shielding filter manufacturing method according to the present invention comprises a spin coating step, a drying step and a curing step. Look below.

(1) Spin coating step

In the spin-coating step, an infrared shielding layer is coated on a transparent support layer cut into a predetermined size by mixing an organic solvent with a near-infrared shielding composition including a curable resin, a near-infrared shielding dye, a curing agent, and a leveling agent. When the curable resin also includes a photocurable resin, the near-infrared shielding composition also uses an ultraviolet absorber.

In the present invention, it is preferable to coat the near-infrared shielding layer at a rotational speed of 10 rpm to 7,000 rpm of the spin coating, and more preferably 100 rpm to 5,000 rpm. Even more preferred spin coating speeds range from 500 rpm to 4,000 rpm.

If the rotational speed of the spin coating is less than 10rpm, the ultra-thin film to be obtained through the present invention can not be obtained as well as the near-infrared shielding composition is not evenly applied to the transparent support layer surface. In addition, when greater than 7,000rpm, the difference in thickness occurs in the central portion and the outer portion of the shielding layer due to the high centrifugal force. In addition, in order to maintain a high rotational speed can be difficult to spin coating apparatus and may affect the durability of the transparent support layer itself.

In the present invention, the viscosity of the near-infrared shielding composition mixed with the organic solvent is preferably 1 cps to 600 cps, and more preferably 10 cps to 450 cps. Even more preferred is 50cps to 300cps.

If the viscosity of the near-infrared shielding composition mixed with the organic solvent is less than 1 cps, the adhesive force is poor, so that it is difficult to easily apply the near-infrared shielding layer. If the viscosity of the near-infrared shielding composition is greater than 600 cps, the adhesive force is too large to control the process.

In addition, in the spin coating step of the present invention, the rotation time is preferably 1 second to 500 seconds, more preferably 3 seconds to 400 seconds. Even more from 10 to 300 seconds. The rotation time may vary depending on the viscosity of the near infrared shielding composition combined with the organic solvent and the thickness of the shielding layer to be coated.

If the rotation time is less than 1 second, it is difficult to secure sufficient time to evenly apply the near-infrared shielding layer to the transparent support layer, and if it is more than 500 seconds, the economic efficiency is poor.

The thickness of the near-infrared shielding layer coated in the spin coating step is preferably 5 nm to 40 μm, more preferably 10 nm to 10 μm. The thickness of the near-infrared shielding layer is affected by the rotational speed, the rotation time, the viscosity of the organic solvent mixed with the near-infrared shielding composition in the spin coating step, and the like. In the present invention, a thinner ultra-thin coating layer may be formed by using a spin coating method instead of a conventional coating method such as a roll-to-roll coating method or a die coating method.

In addition, various near-infrared shielding layers of different components can be coated using a spin coating method, thereby producing a shielding filter having a high-performance near-infrared shielding layer. This will be described later.

As for the transparent support layer used by this invention, it is preferable to use hydrophobic transparent resin film or glass individually or in mixture. Polyethylene terephthalate (PET), triacetyl cellulose (TAC), polyolefin, amorphous polyolefin, cyclo olefin, polybutylene terephthalate, polyamide, poly (methyl methacrylate) copolymer, polyacrylate, polyimide, polyether And various transparent resin films such as polycarbonate, polysulfone, cellophane, aromatic polyamide, polyethylene, polypropylene, and polyvinyl alcohol, and glass substrates such as quartz glass and soda glass. The transparent support layer used in the present invention is not limited to the materials listed above as long as they exhibit the same effect in view of transparency, mechanical strength, thermal stability, moisture shielding, isotropy, economic efficiency, and the like.

The method of manufacturing a transparent support layer using the above-mentioned transparent resin or glass substrate applies a general method of manufacturing a transparent support layer.

In the present invention, in order to form the near-infrared shielding layer by the spin coating method, the transparent support layer preferably has a predetermined thickness. The thickness is preferably 30 µm to 350 µm, more preferably 50 µm to 300 µm, even more preferably 70 µm to 250 µm. If the thickness of the transparent support layer is less than 30㎛, the support strength is weak when coating the shielding layer and warpage may occur in the transparent support layer.If the thickness of the transparent support layer is larger than 350㎛, the production efficiency is not high and the coated transparent support layer is handled. There is a disadvantage that is difficult to do.

The transparent support layer used in the present invention can also use a polarizing film. When the polarizing film is used as the transparent support layer, the polarizing film is prepared according to a general method of manufacturing a polarizing film.

Hereinafter, the organic resin for applying the curable resin, the near-infrared shielding dye, the curing agent and the leveling agent, and the near-infrared shielding composition included in the near-infrared shielding composition will be described. In addition, when using a photo-curable resin as a curable resin also looks at the ultraviolet absorber.

① Curable resin

The curable resin used in the present invention uses at least one of a thermosetting resin or a photocurable resin.

Thermosetting resins and photocurable resins generally use known resins. Among the thermosetting resins, polycondensation type resins include phenol resins, urea resins, melamine resins, and the like, and epoxy resins, polyester resins, and the like. In this invention, these can be used individually or in mixture. As the photocurable resin, UV curable resin is generally used. As a photocurable resin, unsaturated polyester resin, a polyfunctional acrylate resin, a urethane acrylate, an epoxy acrylic resin, an epoxy acrylate resin, etc. can be used individually or in mixture. Curable resins usable in the present invention are of course not limited to the resins listed above as long as they exhibit the same effect.

In the present invention, the curable resin can be composed of only the thermosetting resin, but the photocurable resin can also be used together. In order for the near-infrared shielding layer to have not only the near-infrared shielding effect but also physical properties such as high hardness and transparency, it is more preferable that the photocurable resin used in the present invention uses an ultraviolet curable polyfunctional acrylate resin. In the present invention, the ultraviolet curable polyfunctional acrylate-based resin is dipentaerythritol hexaacrylte, tetramethylolmethane tetraacrylate, tetramethylolmethane triacrylate, trimethanol Propane triacrylate, 1,6-hexanediol diacrylate, 1,6-bis (3-acryloyloxy-2-hydroxypropyloxy) hexane [1, Polyfunctional alcohol derivatives such as 6-bis (3-acryloyloxy-2-hydroxypropyl) hexane], urethane acrylates such as polyethylene glycol diacrylate and pentaerythritol triacrylate, Hexamethylene diisocyanate urethane prepolymer or the like alone or mixed Use open.

It is preferable to use 10 weight%-90 weight% of said ultraviolet curable polyfunctional acrylate-type resin in 100 weight% of curable resin, More preferably, it is 30 weight%-87 weight%. Even more preferably, 50 to 85% by weight is used.

When the UV-curable polyfunctional acrylate-based resin is less than 10% by weight in 100% by weight of the curable resin, it is difficult to obtain high hardness due to the combination of functional groups because the absolute number of functional groups is small, and when it is more than 90% by weight, the near-infrared shielding dye is higher. There is a drawback with poor compatibility.

② NIR shielding dye

As the near-infrared shielding dye used in the present invention, it is possible to use a general near-infrared shielding dye.

Near-infrared shielding dyes used in the present invention are phthalocyanine dyes, naphthalocyanine dyes, anthraquinone dyes, naphthoquinone dyes, cyanine dyes, metal complex dyes, ammonium dyes, aluminum dyes, immonium dyes, di Immonium dyes, polymethine dyes, aromatic dithiol dyes, aromatic diol dyes and the like are used alone or in combination. Phthalocyanine-based dyes having excellent near-infrared absorption effects include phthalocyanine, phthalocyanine complexes, and derivatives having various functional groups in the phthalocyanine skeleton benzene ring.

The more preferred near-infrared shielding dye used in the present invention maintains thermal stability even during the drying and curing steps, and may be used alone or mixed with ammonium dyes, aluminum dyes, immonium dyes, and dimonium dyes to maintain the physical properties of the dyes. It is more preferable to use.

The content of the near-infrared shielding dye used in the present invention is preferably 0.1 to 15% by weight, more preferably 0.5 to 10% by weight, based on 100% by weight of the near-infrared shielding composition. Even more preferably 1% to 5% by weight.

When the content of the near-infrared shielding dye is less than 0.1% by weight, it is difficult to obtain the near-infrared absorbing effect according to the present invention, and the amount of the near-infrared shielding layer becomes thick because the content of the absolute dye must be large. In addition, when greater than 15% by weight may be affected by thermal stability or photo stability due to the dye exposed during thermal curing or photocuring, it is also economical.

③ curing agent

The curing agent in the present invention can be selected and mixed as appropriate depending on the form of the functional group present in the thermosetting resin or photocurable resin, preferably isocyanate compound, epoxy compound, aziridine compound, metal chelate compound, metal alkoxide Metal salts, amine compounds, hydrazine compounds and the like are used alone or in combination.

Isocyanate compounds in the present invention are trimethylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, diphenylmethane isocyanate, xylene diisocyanate aromatic diisocyanate compounds such as diisocyanate, aliphatic diisocyanate such as hexamethyl diisocyanate, and the like are used alone or in combination.

In addition, the epoxy compound in the present invention is a polyethylene glycol diglycidyl ether (diglycidyl ether), diglycidyl ether (diglycidyl ether), trimethylol propane triglycidyl ether (trimethylol propane triglycidyl ether) and the like alone Or mixed.

It is preferable to use 0.1 to 15 weight% of 100% by weight of the hardening | curing agent in a near-infrared shielding composition, More preferably, it is 0.5 to 10 weight%. Even more preferably 1% to 5% by weight.

 In the present invention, the curing agent is an additive used to control the molecular weight or the chain structure of the near-infrared shielding composition. When the curing agent is used in the above-described range, the effect of suppressing phase separation and the like is prominent. If the content of the curing agent is less than 0.1% by weight, it is difficult to expect the function of the curing agent, if the content of more than 15% by weight it is difficult to increase the hardness of the relatively low content of the curable resin.

④ UV absorber

When the photocurable resin is also used as the curable resin in the present invention, it is preferable to use an ultraviolet absorber to prevent deterioration occurring when the photocurable resin is photocured and to improve the durability of the dye.

The ultraviolet absorber used in the present invention is preferably used alone or mixed with a salicylate ultraviolet absorber, a benzophenone ultraviolet absorber, a benzotriazole ultraviolet absorber, a cyanoacrylate ultraviolet absorber, and a benzoate ultraviolet absorber. Do.

More specifically, the ultraviolet absorber is phenyl salicylate, p-tert-butylphenyl salicylate, p-octylphenyl salicylate, 4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-octoxybenzophenone, 2-hydroxy-4-dodecyloxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy- 4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2-hydroxy-4-methoxy-5-sulfobenzophenone, bis (2-methoxy-4 -Hydroxy-5-benzoylphenyl) methane, 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, 2- (2'-hydroxy-5'-tert-butylphenyl) benzotriazole, 2- (2'-hydroxy-3 ', 5'-di-tert-butylphenyl) benzotriazole, 2- (2'-hydroxy-3'-tert-butyl-5'-methylphenyl) -5- Chlorobenzotriazole, 2- (2'-hydroxy-3 ', 5'-di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2'-hydroxy-3', 5-di -tert-amylphenyl) benzotriazole, 2- (2'-hydroxy-4'-octoxy Yl) benzotriazole, 2- (2'-hydroxy-3 '-(3', 4 ', 5', 6'-tetrahydrophthalimidomethyl) -5'-methylphenyl) benzotriazole, 2, 2'-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6- (2H-benzotriazolyl-2-yl) phenol], 2- (2'-hydroxy-5'- Methacryloxyphenyl) -2H-benzotriazole, 2,2'-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6-[(2H-benzotriazol-2-yl) Phenol], and 2- (2'-hydroxy-3 ', 5'-di-t-amylphenyl) benzotriazole, 2-ethylhexyl-2-cyano-3,3'-diphenylacrylate, Ethyl-2-cyano-3,3'-diphenyl acrylate or the like is used alone or in combination.

In the present invention, the content of the ultraviolet absorber is preferably used in an amount of 0.1 wt% to 15 wt%, more preferably 0.5 wt% to 10 wt%, in 100 wt% of the near-infrared shielding composition. Even more preferably 1% to 5% by weight.

⑤ Leveling agent

In the present invention, to level the surface of the near-infrared shielding layer, a leveling agent is mixed with the near-infrared shielding composition. The leveling agent can be used by mixing a ketone or an ester solvent with a silicone resin. As a leveling agent by this invention, it is preferable to use a silicone diacrylate and a silicone polyacrylate compound individually or in mixture.

The content of the leveling agent is preferably 0.1 wt% to 3 wt%, more preferably 0.5 wt% to 2 wt%, based on 100 wt% of the near-infrared shielding composition. When the leveling agent is less than 0.1% by weight, it is difficult to expect the leveling effect, and when the leveling agent is greater than 3% by weight, the surface hardness of the near infrared ray shielding layer may be weakened.

⑥ organic solvent

In the present invention, an organic solvent is used to apply the near infrared shielding layer.

A proper organic solvent is used in consideration of the applicability of the near infrared shielding layer, the adhesion to the transparent support layer, and the enhancement of the shielding function of the near infrared shielding composition.

The organic solvent used in the present invention may be a C1-8 saturated hydrocarbon alcohol such as methanol, isopropanol, butanol, t-butanol, isobutanol, or acetone, methyl ethyl ketone, or methyl isobutyl ketone. Saturated hydrocarbon-based diketones having 1 to 8 carbon atoms, such as 1 to 8 saturated hydrocarbon ketones and acetyl acetone, ethyl acetate of esters, ethyl hydrocarbons of 1 to 8 carbon atoms such as butyl acetate, and ethyl alcohols of ether alcohols. Solves, methyl cellosolves, butyl cellosolves, 1-methoxy-2-propanol, and N-methyl pyrrolidone, ethyl cellosolve acetate, diacetone alcohol, and the like are used alone or in combination.

The organic solvent is preferably used in an amount of 20 parts by weight to 110 parts by weight based on 100 parts by weight of the near-infrared shielding composition to be applied, and more preferably 30 parts by weight to 80 parts by weight. When the content of the organic solvent is less than 20 parts by weight based on 100 parts by weight of the near-infrared shielding composition, applicability and adhesion with the transparent support layer are inferior. This takes long and loses profitability.

(2) drying step

In the drying step, the organic solvent applied together with the near-infrared shield composition in the spin coating step is volatilized.

In the drying step, not only the organic solvent remaining in the coating liquid may be more effectively removed by performing the drying process by the rotating process, but the near-infrared shielding composition may be more easily adsorbed onto the transparent support layer, thereby completing the drying step in a short time.

The drying temperature performed in the drying step is preferably 15 ℃ to 85 ℃, more preferably 25 ℃ to 75 ℃. If the drying temperature is lower than 15 ℃ it takes a long time to remove the organic solvent, if the drying temperature is higher than 85 ℃ may affect the physical properties of the dye.

The rotational speed performed in the drying step is preferably to dry the organic solvent at 20rpm to 5,000rpm, more preferably 50rpm to 4,000rpm. Even more preferred rotational speeds are from 70 rpm to 3,000 rpm.

If the rotational speed of the drying step is less than 20rpm, it is difficult to sufficiently obtain the drying effect by the rotation, if the rotational speed of more than 5,000rpm drying efficiency is lower than the rotational speed.

(3) curing step

In the curing step, the near-infrared shielding layer formed through the spin coating step and the drying step is cured. When the base resin is composed of only a thermosetting resin in the near-infrared shielding composition, only the thermosetting is performed, and when the thermosetting resin and the photocurable resin are used together, it is preferable to perform photocuring after the thermosetting first. Photocuring is preferably UV curing. If necessary, when the curable resin is composed of only photocurable resins, only photocuring can be performed.

1) In case of using thermosetting resin and photosetting resin together

When the near-infrared shielding composition is composed of a thermosetting resin and a photocurable resin, the thermosetting process is first performed. The temperature condition of the thermosetting step is preferably in the range of 40 ° C to 80 ° C, more preferably 50 ° C to 70 ° C. If the thermal curing temperature is less than 40 ℃ is not enough to heat the curing, greater than 80 ℃ may affect the physical properties of the dye or transparent support layer.

The heat curing time is preferably 10 seconds to 5 minutes, more preferably 1 minute to 3 minutes. The thermosetting time can be changed corresponding to the thermosetting temperature conditions. If the thermal curing time is less than 10 seconds, even if the thermal curing temperature is high, it is difficult to secure a sufficient thermal curing effect, and if the thermal curing time exceeds 5 minutes, productivity may be degraded and may affect the physical properties of the dye.

The photocuring process is performed after the thermosetting process. Photocuring in the present invention proceeds to UV curing, UV curing is preferably UV curing in the energy range of 5mJ to 40mJ, more preferably 10mJ to 20mJ.

When the amount of UV curing energy is less than 5mJ, sufficient photocuring effect is not obtained, and when the amount of UV curing energy is larger than 40mJ, excessive UV curing may affect the physical properties of the dye.

2) When only thermosetting resin is used

When the base resin is made of only the thermosetting resin, the thermosetting temperature proceeds to a higher temperature than when using the photosetting resin together. At this time, it is preferable that temperature conditions are 70 degreeC-140 degreeC, More preferably, it is 80 degreeC-120 degreeC.

If the thermosetting temperature is less than 70 ℃ does not sufficiently cure the thermosetting resin, if it is larger than 140 ℃ may affect the physical properties and durability of the dye or transparent support layer.

When only the thermosetting resin is used as the curable resin, the curing time is preferably longer than when using the photocurable resin together. The curing time is preferably 30 seconds to 15 minutes, more preferably 1 minute to 10 minutes.

The curing time is determined in correspondence with the curing temperature. When using only a thermosetting resin, if the curing time is shorter than 30 seconds, sufficient thermosetting effect cannot be obtained. If the curing time is longer than 15 minutes, the thermosetting resin can be sufficiently cured, but The near-infrared shielding function can be impaired.

In the present invention, the thermosetting resin or the photocurable resin can be combined with a dye having a near-infrared shielding function to protect the dye, thereby increasing the heat resistance of the dye. In addition, the dye is evenly applied by spin coating, and ultra-thin coating is possible.

In the present invention, it is also possible to coat two or more near-infrared shielding layers by repeatedly performing the spin coating step of coating the near-infrared shielding composition and the drying step of drying the same. When coating two or more near-infrared shielding layers, the near-infrared shielding composition of the same component and content may be used, and the near-infrared shielding composition of the other component and content may be used as needed.

In addition, when applying two or more coating layers, it is also possible to apply a near-infrared shielding layer (first coating layer) and another functional layer (second coating layer) together.

In the present invention, the second coating layer is coated with at least one coating layer from an antireflection layer, a low reflection layer, an unreflective layer, an antiglare layer, a low refractive index layer, a high refractive index layer, a hard coating layer, an electromagnetic shielding layer, an antistatic layer, etc. together with a near infrared shielding layer. .

The scope of the present invention also extends to the near infrared shielding filter manufactured by the above-described method for manufacturing the near infrared shielding filter. In addition, the scope of the present invention extends to an image display apparatus to which a near-infrared shielding filter manufactured by the present invention is applied, and such an image display apparatus is a cathode-ray tube (CRT), a liquid crystal display (LCD, liquid). At least one of a group consisting of a crystal dispaly, a plasma display panel (PDP) and an organic light emitting diode (OLED).

Hereinafter, the present invention will be described in more detail with reference to preferred examples of the present invention and comparative examples compared with the present invention.

Example 1

1) The near-infrared shielding composition coated in the spin coating step is 100% by weight of the near-infrared shielding composition using a thermosetting resin as a base resin, 4% by weight of the near-infrared shielding dye mixed with ammonium-based dyes and hexamethylene diisocyanate. 3 weight% of the hardening | curing agent which mixed the isophorone diisocyanate, and 1.5 weight% of silicone polyacrylate compound leveling agents were used. 70 parts by weight of the organic solvent methanol was used based on 100 parts by weight of the near-infrared shielding composition. In the spin coating step, the spin speed was performed for 40 seconds under the condition of 1,000 rpm. The near infrared shielding composition mixed with the organic solvent has a viscosity of 100 cps and the thickness of the near infrared shielding layer is 2 μm.

2) In the drying step it was carried out at 60 ℃ at 700 rpm rotation speed conditions.

3) The curing step was thermoset at 100 ℃ for 3 minutes.

Example 2

1) The near-infrared shielding composition coated in the spin coating step is a thermosetting resin and a photocurable resin as a base resin, and ultraviolet rays mixed with phenyl salicylate and p-tert-butylphenyl salicylate in 100% by weight of the near-infrared shielding composition. 4% by weight of absorbent was used. Other components and content conditions of the near-infrared shielding composition are the same as in Example 1.

2) The drying step is the same as in Example 1.

3) The curing step was first heat-cured at 60 ℃ for 2 minutes, and then UV-cured with 15mJ energy amount.

Example 3

1) The near-infrared shielding composition coated in the spin coating step is 5% by weight of the near-infrared shielding dye mixed with ammonium-based dyes and aluminum-based dyes in 100% by weight of the near-infrared shielding composition using a thermosetting resin as a base resin, and hexamethylene diisocyanate. 3 weight% of the hardening | curing agent which mixed and isophorone diisocyanate, and 2 weight% of silicone polyacrylate compound leveling agents were used. 80 parts by weight of the organic solvent methanol was used based on 100 parts by weight of the near-infrared shielding composition. In the spin coating step, the spin speed was performed for 40 seconds under the condition of 1,000 rpm. The near infrared shielding composition mixed with the organic solvent has a viscosity of 100 cps and the thickness of the near infrared shielding layer is 1.7 μm.

2) In the drying step it was carried out at 60 ℃ at 700 rpm rotation speed conditions.

3) The curing step was thermoset at 100 ℃ for 3 minutes.

Example 4

1) The near-infrared shielding composition coated in the spin coating step is a thermosetting resin and a photocurable resin as a base resin, and ultraviolet rays mixed with phenyl salicylate and p-tert-butylphenyl salicylate in 100% by weight of the near-infrared shielding composition. 3% by weight of absorbent was used. Other components of the near infrared shielding composition and content conditions are the same as in Example 3.

2) The drying step is the same as in Example 3.

3) The curing step was first heat-cured at 60 ℃ for 2 minutes, and then UV-cured with 15mJ energy amount.

Comparative Example 1

The same near-infrared shielding composition as in Example 1 was coated by a roll-to-roll coating method.

Comparative Example 2

The same near-infrared shielding composition as in Example 1 was coated by a die coating method.

Comparative Example 3

A near-infrared shielding filter was prepared by mixing the same near-infrared shielding composition as in Example 1 with an adhesive.

Comparative Example 4

A near-infrared shielding filter was prepared by mixing the same near-infrared shielding composition as in Example 2 with an adhesive.

Table 1 below is a table showing near-infrared transmittance of a preferred embodiment of the present invention and a comparative example compared with the present invention.

Wavelength (nm) Example 1 Example 2 Example 3 Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 1,000 5.5% 5.2% 5.3% 5.1% 5.9% 5.6% 5.7% 5.9% 980 6.1% 6.3% 6.4% 6.7% 16.5% 16.3% 16.4% 16.5% 960 4.8% 4.6% 4.6% 4.4% 6.7% 6.4% 6.7% 6.3% 940 5.3% 5.7% 5.3% 5.5% 6.6% 6.5% 6.8% 6.5% 920 5.5% 5.7% 5.8% 5.6% 9.2% 9.7% 9.8% 9.6% 900 6.2% 6.5% 6.2% 6.8% 10.4% 10.9% 10.9% 10.7% 880 7.1% 7.3% 7.7% 7.9% 12.3% 12.0% 12.6% 12.0% 860 8.2% 8.5% 8.3% 8.5% 14.8% 14.4% 14.3% 14.6% 840 8.2% 8.6% 8.3% 8.9% 14.6% 14.4% 14.5% 14.5% 820 8.4% 8.7% 8.2% 8.9% 14.5% 14.3% 14.2% 14.4% 800 9.8% 9.4% 9.3% 9.8% 16.8% 16.5% 16.4% 16.9%

The larger the effect of shielding the near infrared wavelength region of 800 nm to 1,000 nm, the lower the transmittance. As shown in Table 1, the transmittances of Examples 1 to 4 were about 6% to 10%, whereas the transmittances of Comparative Examples 1 to 4 were about 8% to 15%. Therefore, when the near-infrared shielding filter by this invention is used, a higher shielding rate can be obtained.

1 is a graph showing the transmittance of preferred Example 1 and Comparative Example 1 according to the present invention. As shown in Figure 1 it can be seen that the transmittance of Example 1 is 2% to 3% smaller, 5% to 7% lower than the transmittance of Comparative Example 1.

In the above, this invention was demonstrated in detail with reference to an Example and a comparative example centering on a structure. However, the scope of the present invention is not limited to the above embodiments but may be embodied in various forms of embodiments within the appended claims. Without departing from the gist of the invention as claimed in the claims, any person of ordinary skill in the art is considered to be within the scope of the claims described in the present invention to the extent possible to vary.

In addition, the preferred range, more preferred range, and even more preferred range limitation in the present invention is to maximize the effect even more, it is possible to obtain a more satisfactory technical effect by narrowing the limited range.

The present invention can obtain the effect of evenly applying the dye without damaging the dye having a near infrared shielding function by forming a near infrared shielding layer using a spin coating method based on the above-described technical configuration. In addition, in the stin coating method according to the present invention, the near-infrared shielding layer is coated with an ultra-thin film by adjusting the rotational speed, coating time, viscosity, and the like. The effect of forming a shielding layer can also be obtained.

Claims (18)

In the near-infrared shielding filter manufacturing method of applying a near-infrared shielding composition to a transparent support layer to form a near-infrared shielding layer, (1) the near-infrared shielding layer is applied by spin coating, the rotation speed is 10rpm to 7,000rpm, the coating time is 1 second to 500 seconds, The near-infrared shield composition is applied to the transparent support layer by mixing with an organic solvent, the near-infrared shield composition comprises a curable resin, a near-infrared shield dye, a curing agent and a leveling agent, The curable resin is a thermosetting resin as a base resin, in 100% by weight of the near-infrared shielding composition, a) the near infrared shielding dye is 0.1% to 15% by weight; b) 0.1% to 15% by weight of the curing agent; And c) the spin coating step, characterized in that the leveling agent is 0.1% to 3% by weight; (2) a drying step of drying at a drying temperature of 15 ° C. to 85 ° C. and a rotational speed of 20 rpm to 5,000 rpm to volatilize the organic solvent applied together to the near infrared shielding layer coated in the spin coating step; And (3) applying the near-infrared shield layer to the transparent support layer, including a curing step of thermally curing the near-infrared shield layer dried in the drying step at a curing temperature of 70 ° C. to 140 ° C. and a curing time of 30 seconds to 15 minutes. Near-infrared shielding filter manufacturing method characterized in that. In the near-infrared shielding filter manufacturing method of applying a near-infrared shielding composition to a transparent support layer to form a near-infrared shielding layer, (1) the near-infrared shielding layer is applied by spin coating, the rotation speed is 10rpm to 7,000rpm, the coating time is 1 second to 500 seconds, The near-infrared shielding composition is applied to the transparent support layer by mixing with an organic solvent, the near-infrared shielding composition comprises a curable resin, a near-infrared shielding dye, a swab absorber, a curing agent and a leveling agent, The curable resin is a thermosetting resin and a photocurable resin as a base resin, in 100% by weight of the near-infrared shielding composition, a) the near infrared shielding dye is 0.1% to 15% by weight; b) 0.1 wt% to 15 wt% of the ultraviolet absorbent; c) 0.1 to 15 weight percent of said curing agent; And d) the spin coating step, characterized in that 0.1% to 3% by weight of the leveling agent; (2) a drying step of drying at a drying temperature of 15 ° C. to 85 ° C. and a rotational speed of 20 rpm to 5,000 rpm to volatilize the organic solvent applied together to the near infrared shielding layer coated in the spin coating step; And (3) in curing the near-infrared shield layer dried in the drying step a) thermosetting process of thermosetting at a curing temperature of 40 ℃ to 80 ℃, curing time 10 seconds to 5 minutes, b) a method of manufacturing a near-infrared shielding filter comprising a curing step of undergoing a photocuring process in the energy range of 5 mJ to 40 mJ after the thermosetting process. The method of claim 2, The ultraviolet absorbent is phenyl salicylate, p-tert-butylphenyl salicylate, p-octylphenyl salicylate, 4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2- Hydroxy-4-octoxybenzophenone, 2-hydroxy-4-dodecyloxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4- Methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2-hydroxy-4-methoxy-5-sulfobenzophenone, bis (2-methoxy-4-hydrate Hydroxy-5-benzoylphenyl) methane, 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, 2- (2'-hydroxy-5'-tert-butylphenyl) benzotriazole, 2- (2'-hydroxy-3 ', 5'-di-tert-butylphenyl) benzotriazole, 2- (2'-hydroxy-3'-tert-butyl-5'-methylphenyl) -5-chlorobenzo Triazole, 2- (2'-hydroxy-3 ', 5'-di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2'-hydroxy-3', 5-di-tert -Amylphenyl) benzotriazole, 2- (2'-hydroxy-4'-octoxyphenyl) benzoate Azole, 2- (2'-hydroxy-3 '-(3', 4 ', 5', 6'-tetrahydrophthalimidomethyl) -5'-methylphenyl) benzotriazole, 2,2'-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6- (2H-benzotriazol-2-yl) phenol], 2- (2'-hydroxy-5'-methacryloxyphenyl ) -2H-benzotriazole, 2,2'-methylenebis [4- (1,1,3,3-tetramethylbutyl) -6-[(2H-benzotriazol-2-yl) phenol], and 2- (2'-hydroxy-3 ', 5'-di-t-amylphenyl) benzotriazole, 2-ethylhexyl-2-cyano-3,3'-diphenylacrylate, ethyl-2- A method for manufacturing a near-infrared shielding filter, characterized in that at least one of cyano-3,3'-diphenyl acrylate. The method according to claim 1 or 2, The near-infrared shielding composition of the near-infrared shielding composition mixed with the organic solvent is characterized in that 1cps to 600cps. The method according to claim 1 or 2, The near-infrared shielding layer coated in the spin coating step has a thickness of 5nm to 40㎛ characterized in that the near-infrared shielding filter manufacturing method. The method according to claim 1 or 2, The thickness of the transparent support layer is a near infrared shielding filter manufacturing method, characterized in that 30㎛ to 350㎛. The method according to claim 1 or 2, The organic solvent is a near-infrared shielding filter manufacturing method, characterized in that 20 to 110 parts by weight based on 100 parts by weight of the near-infrared shielding composition. The method according to claim 1 or 2, At least two near infrared shielding layers are applied to the transparent support layer by performing the spin coating step and the drying step at least twice. The method according to claim 1 or 2, The second coating layer is applied to the near-infrared shielding layer, wherein the second coating layer is at least one of an antireflection layer, a low reflection layer, an unreflective layer, an anti-glare layer, a low refractive index layer, a hard coating layer, an electromagnetic shielding layer, and an antistatic layer. Near infrared shielding filter manufacturing method. The method according to claim 1 or 2, The near-infrared shielding dyes include phthalocyanine dyes, naphthalocyanine dyes, anthraquinone dyes, naphthoquinone dyes, cyanine dyes, metal complex dyes, ammonium dyes, aluminum dyes, immonium dyes, dimonium dyes, A method for producing a near-infrared shield filter comprising at least one of a polymethine dye, an aromatic dithiol dye, and an aromatic diol dye. The method according to claim 1 or 2, The hardening agent is a near-infrared shielding filter manufacturing method, characterized in that at least one of isocyanate compound, epoxy compound, aziridine compound, metal chelate compound, metal alkoxide metal salt, amine compound, hydride compound. The method of claim 11, The isocyanate compound is trimethylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, diphenylmethane isocyanate, aromatic diisocyanate compound, aliphatic diisocyanate A near infrared shielding filter manufacturing method, characterized in that at least one of the compounds (aliphatic diisocyanate). The method of claim 11, The epoxy compound is at least one of polyethylene glycol diglycidyl ether (diglycidyl ether), diglycidyl ether (diglycidyl ether), trimethylol propane triglycidyl ether (trimethylol propane triglycidyl ether) Near infrared shielding filter manufacturing method. The method according to claim 1 or 2, The leveling agent manufacturing method of near-infrared shielding filter, characterized in that the silicone diacrylate compound or silicone polyacrylate compound alone or mixed. The method according to claim 1 or 2, The organic solvent includes a saturated hydrocarbon alcohol having 1 to 8 carbon atoms, a saturated hydrocarbon ketone having 1 to 8 carbon atoms, a saturated hydrocarbon diketone having 1 to 8 carbon atoms, a saturated hydrocarbon ester having 1 to 8 carbon atoms, and an ethyl alcohol of ether alcohols. Manufacture of near-infrared shielding filter comprising at least one of rosolve, methyl cellosolve, butyl cellosolve, 1-methoxy-2-propanol, N-methyl pyrrolidone, ethyl cellosolve acetate, diacetone alcohol Way. The method according to claim 1 or 2, The thermosetting resin is a near-infrared shielding filter manufacturing method comprising at least one of phenol resin, urea resin, melamine resin, epoxy resin, polyester resin. The method according to claim 1 or 2, The transparent support layer is polyethylene terephthalate (PET), triacetyl cellulose (TAC), polyolefin, amorphous polyolefin, cyclo olefin, polybutylene terephthalate, polyamide, poly (methyl methacrylate) copolymer, polyacrylate, poly A method for producing a near-infrared shielding filter comprising at least one of an imide, polyether, polycarbonate, polysulfone, cellophane, aromatic polyamide, polyethylene, polypropylene, polyvinyl alcohol, quartz glass, and soda glass. The near-infrared shielding filter manufactured by the near-infrared shielding filter manufacturing method in any one of Claims 1-5.

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