KR102450394B1 - Metal oxide dispersion composition for display, and preparing method for the same and optical member - Google Patents

Abstract

The present invention relates to a metal oxide dispersion composition for a display, a manufacturing method thereof, and an optical member for a display, and the metal oxide dispersion composition for a display according to an embodiment of the present invention comprises: a silane-based surface treatment agent; Phosphoric acid-based surface treatment agent; metal oxide particles; and organic solvents.

Description

Metal oxide dispersion composition for display, manufacturing method thereof, and optical member for display

The present invention relates to a metal oxide dispersion composition for a display, a method for producing the same, and an optical member for a display.

Optically transparent polymer materials are widely used as optical coatings and optoelectronic materials because of their low cost, good processability, and high transmittance in the visible region. Recently, transparent materials with high refractive index have been used as materials for optical filters, lenses, reflectors, optical waveguides, antireflection films, solar cells, and light emitting diodes (LEDs).

However, these polymers have a refractive index (n) of 1.3 to 1.7, and since it is difficult to implement a high refractive index only with a polymer material, research on mixing and dispersing an inorganic material having a high refractive index (n = 1.5 to 2.7) with a polymer is in progress. have.

Materials used as high refractive inorganic materials include TiO ₂ (n=2.5~2.7), ZrO ₂ (n=2.1~2.2), ZnO (n=2.0), SnO ₂ (n=2.0), SiO as metal oxide particles. ₂ (n=1.5).

In order to prepare a dispersion having a high refractive index, a high concentration of inorganic particles is filled. However, due to the high concentration of inorganic particles, viscosity characteristics, dispersion stability, and optical characteristics are deteriorated.

Therefore, there is a need for research and development of a metal oxide dispersion capable of reducing the yellowing phenomenon of a film having a low viscosity while implementing a high refractive index.

The present invention is to solve the above problems, and an object of the present invention is to provide a low-viscosity metal oxide dispersion composition for a display capable of reducing yellowing while implementing a high refractive index, a method for manufacturing the same, and an optical member for a display will do

However, the problems to be solved by the present invention are not limited to those mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.

The metal oxide dispersion composition for a display of the present invention includes a silane-based surface treatment agent; Phosphoric acid-based surface treatment agent; metal oxide particles; and organic solvents.

According to an embodiment, the silane-based surface treatment agent is aminosilane, bilysilane, epoxysilane, methacrylsilane, alkylsilane, phenylsilane, chlorosilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenylchlorosilane , dichlorodiphenylsilane, γ-methacryloxypropyltrimethoxysilane, aminopropyltriethoxysilane, (3-aminopropyl)triethoxysilane, [3-(2-aminoethylamino)propyl]triethoxy Silane, 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane, vinyltrichlorosilane, vinylmethylchlorosilane, trimethoxyvinylsilane, triethoxyvinylsilane, dimethyldichlorosilane, methyl Dichlorosilane, methyltrichlorosilane, phenyltrichlorosilane, 3-(trimethylsilyl)propylmethacrylatesilane, 3-(trimethoxysilyl)propyl methacrylate, methallyltrimethylsilane, allyltrimethylsilane, vinyltrimethylsilane , allyloxytrimethylsilane, allyloxy-tert-butyldimethylsilane, vinyltrimethoxysilane, trimethylchlorosilane, trichlorosilane, glycidoxymethyltrimethoxysilane, glycidoxymethyltriethoxysilane, α-glycine Cydoxyethyltrimethoxysilane, α-glycidoxyethyltriethoxysilane, β-glycidoxyethyltrimethoxysilane, β-glycidoxyethyltriethoxysilane, α-glycidoxypropyltrimethoxy Silane, α-glycidoxypropyltriethoxysilane, β-glycidoxypropyltrimethoxysilane, β-glycidoxypropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycy Doxypropyltriethoxysilane, γ-glycidoxypropyltripropoxysilane, γ-glycidoxypropyltributoxysilane, γ-glycidoxypropyltriphenoxysilane, α-glycidoxybutyltrimethoxysilane , α-glycidoxybutyltriethoxysilane, β-glycidoxybutyltriethoxysilane, γ-glycidoxybutyltrimethoxysilane, γ-glycidoxybutyltriethoxysilane, δ-glycidoxy Butyltrimethoxysilane, δ-glycidoxybutyltriethoxysilane, glycidoxymethyldimethoxysilane, glycidoxymethylmethyldiethoxysilane, α-glycidoxyethylmethyldimethoxysilane, α-glycy Doxyethylmethyldiethoxysilane, β-glycidoxyethylmethyldimethoxysilane, β-glycidoxyethylethyldimethoxysilane, α-glycidoxypropylmethyldimethoxysilane, α-glycidox Cypropylmethyldiethoxysilane, β-glycidoxypropylmethyldimethoxysilane, β-glycidoxypropylethyldimethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyldiethoxysilane , γ-glycidoxypropylmethyldipropoxysilane, γ-glycidoxypropylmethyldibutoxysilane, γ-glycidoxypropylmethyldiphenoxysilane, γ-glycidoxypropyl ethyldimethoxysilane, γ-glyc It may include at least one selected from the group consisting of cydoxypropylethyldiethoxysilane, γ-glycidoxypropylvinyldimethoxysilane, and γ-glycidoxypropylvinyldiethoxysilane.

According to one embodiment, the silane-based surface treatment agent may be 10 wt% to 20 wt% of the metal oxide dispersion composition for a display.

According to one embodiment, the phosphoric acid-based surface treatment agent, phosphoric acid ester (phosphoric acid ester), alkenyl polyethylene glycol ether phosphate (Alkenyl polyethylene glycol ether phosphate), an alkylolammonium salt of a copolymer having an acidic group (Alkylolammonium salt a copolymer) with acidic groups), phosphate (Phosphoric acid salt), poly (oxy-1,2-ethanediyl), α-isotridecyl-ω-hydroxy-phosphate (Poly (oxy-1,2-ethanediyl), alpha- isotridecyl-omega-hydroxy-phosphate), phosphoric acid ester salt of a copolymer, polyoxyethylene tridecyl ether phosphate, polyether phosphate, cationic fatty acid phosphate ester, poly It may include at least one selected from the group consisting of oxyethylene lauryl ether phosphate esters and phosphate esters.

According to one embodiment, the phosphoric acid-based surface treatment agent may be 6 wt% to 10 wt% of the metal oxide dispersion composition for a display.

According to an embodiment, the metal oxide particles are ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ selected from the group consisting of It may include at least one.

According to an embodiment, the metal oxide particles may be 30 wt% to 50 wt% of the metal oxide dispersion composition for a display.

According to an embodiment, the metal oxide particles may have an average particle size of 10 nm to 20 nm.

According to an embodiment, the organic solvent is tetrahydrofuran, isopropyl alcohol, n-butanol, ethylene glycol, propylene glycol, methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, CHN, ethyl acetate, butyl acetate, Propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, n-hexane, toluene, xylene, styrene, o-methyl styrene, m-methyl styrene, p-methyl styrene, vinyl toluene, p-methoxy styrene, benzyl acryl Late, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenylyl acrylate, 2-([1,1'-biphenyl]-2-yloxy) ethyl acrylate , Phenoxybenzylacrylate, 3-phenoxybenzyl-3-(1-naphthyl)acrylate, ethyl (2E)-3-hydroxy-2-(3-phenoxybenzyl)acrylate, phenylmethacrylate , Biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate acrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ortho-phenylphenol ethyl acrylate, bisphenol diacrylate, urethane (meth) Acrylate, 2-ethylhexyl (meth) acrylate, isobornyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy Butyl acrylate, methyl ethylene glycol mono (meth) acrylate, methyl triethylene diglycol (meth) acrylate, 1,4-butanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, hydroxyl Cypivalate neopentyl glycol di(meth)acrylate, dicyclopentanyl di(meth)acrylate, caprolactone-modified dicyclopentanyl di(meth)acrylate, ethylene oxide-modified phosphate di(meth)acrylate, arylated cyclo Hexyldi(meth)acrylate, ethylene glycol di(meth)acrylate, 1,6-hexadiol diacrylate, trimethylolpropane tri(meth)acrylate, pentaerythritol tri( group consisting of meth) acrylate, dipentaerythritol penta (meth) acrylate, dipentaerythritol hexa (meth) acrylate, polyol poly (meth) acrylate, urethane (meth) acrylate and glycerin trimethacrylate It may be to include one or more selected from.

According to an embodiment, the organic solvent may be 35 wt% to 45 wt% of the metal oxide dispersion composition for a display.

According to one embodiment, the metal oxide dispersion composition for a display may have a viscosity of 500 cP or less.

According to an embodiment, the liquidus refractive index may be 1.67 or more, and the yellowness (Y.I) may be 40 or less.

A method for preparing a metal oxide dispersion composition for a display according to another embodiment of the present invention includes the steps of preparing metal oxide particles; preparing a mixed solution by adding the metal oxide particles to a solution in which a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent are dissolved in an organic solvent; preparing a metal oxide-organic solvent dispersion by putting beads in the mixed solution at the same weight as the metal oxide particles and dispersing; and removing the undispersed large metal oxide particles from the metal oxide-organic solvent dispersion.

The film composition for a display according to another embodiment of the present invention, the metal oxide dispersion composition for a display according to an embodiment of the present invention or a method for producing a metal oxide dispersion composition for a display according to another embodiment of the present invention The prepared metal oxide dispersion composition for a display; UV photoinitiators; and a monomer for UV curing.

According to one embodiment, the UV photoinitiator, an onium salt-based, diazonium salt-based, sulfonium salt-based compound and an imidazole-based photocationic initiator selected from; and thioxanthone-based, phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, propanone-based, amino ketone-based, ketone-based, benzoin ether acetophenone-based, anthraquinone-based and aromatic phosphine oxide-based compounds It may include at least one selected from the group consisting of a radical photoinitiator.

According to an embodiment, the UV curing monomer is glycidyl acrylate, glycidyl methacrylate, glycidyl methacrylate, glycidyl-alpha-ethyl acrylate, glycidyl-alpha-ene -Propyl acrylate, glycidyl-alpha-butyl acrylate, 3,4-epoxybutyl methacrylate, 3,4-epoxybutyl acrylate, 6,7-epoxypeptyl methacrylate, 6,7-epoxyheptyl Acrylate, 6,7-epoxyheptyl-alpha-ethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl meta It may include at least one selected from the group consisting of acrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, 1,6-hexanediol diacrylate, and trimethylpropane triacrylate.

The optical film for a display according to another embodiment of the present invention is prepared by UV curing the film composition for a display according to an embodiment of the present invention, and has a yellowness (Y.I) of 40 or less.

An optical member for a display according to another embodiment of the present invention includes an optical film for a display according to an embodiment of the present invention.

The titania dispersion composition according to the present invention includes a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent, thereby reducing yellowness (Y.I) while implementing low viscosity and high refractive index.

In addition, the film composition according to the present invention can manufacture an optical film with improved optical properties and yellowness properties while implementing a high refractive index.

1 is a graph showing the yellowness (YI) for the MPS content of the present invention.
Figure 2 is a graph showing the Haze for the MPS content of the present invention.
3 is a graph showing the viscosity with respect to the MPS content of the present invention.

Hereinafter, embodiments will be described in detail with reference to the accompanying drawings. However, since various changes may be made to the embodiments, the scope of the patent application is not limited or limited by these embodiments. It should be understood that all modifications, equivalents and substitutes for the embodiments are included in the scope of the rights.

Terms used in the examples are used for the purpose of description only, and should not be construed as limiting. The singular expression includes the plural expression unless the context clearly dictates otherwise. In the present specification, terms such as “comprise” or “have” are intended to designate that a feature, number, step, operation, component, part, or combination thereof described in the specification exists, but one or more other features It is to be understood that this does not preclude the possibility of the presence or addition of numbers, steps, operations, components, parts, or combinations thereof.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the embodiment belongs. Terms such as those defined in a commonly used dictionary should be interpreted as having a meaning consistent with the meaning in the context of the related art, and should not be interpreted in an ideal or excessively formal meaning unless explicitly defined in the present application. does not

In addition, in the description with reference to the accompanying drawings, the same components are assigned the same reference numerals regardless of the reference numerals, and the overlapping description thereof will be omitted. In the description of the embodiment, if it is determined that a detailed description of a related known technology may unnecessarily obscure the gist of the embodiment, the detailed description thereof will be omitted.

In addition, in describing the components of the embodiment, terms such as first, second, A, B, (a), (b), etc. may be used. These terms are only for distinguishing the elements from other elements, and the essence, order, or order of the elements are not limited by the terms.

Components included in one embodiment and components having a common function will be described using the same names in other embodiments. Unless otherwise stated, descriptions described in one embodiment may be applied to other embodiments as well, and detailed descriptions within the overlapping range will be omitted.

The metal oxide dispersion composition for a display of the present invention includes a silane-based surface treatment agent; Phosphoric acid-based surface treatment agent; metal oxide particles; and organic solvents.

The titania dispersion composition according to the present invention includes a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent, thereby reducing yellowness (Y.I) while implementing low viscosity and high refractive index.

According to an embodiment, the silane-based surface treatment agent serves to disperse the metal oxide in a solvent by maintaining high transparency and high refractive index in the metal oxide dispersion composition for a display.

According to an embodiment, the silane-based surface treatment agent is aminosilane, bilysilane, epoxysilane, methacrylsilane, alkylsilane, phenylsilane, chlorosilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenylchlorosilane , dichlorodiphenylsilane, γ-methacryloxypropyltrimethoxysilane, aminopropyltriethoxysilane, (3-aminopropyl)triethoxysilane, [3-(2-aminoethylamino)propyl]triethoxy Silane, 3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxysilane, vinyltrichlorosilane, vinylmethylchlorosilane, trimethoxyvinylsilane, triethoxyvinylsilane, dimethyldichlorosilane, methyl Dichlorosilane, methyltrichlorosilane, phenyltrichlorosilane, 3-(trimethylsilyl)propylmethacrylatesilane, 3-(trimethoxysilyl)propyl methacrylate, methallyltrimethylsilane, allyltrimethylsilane, vinyltrimethylsilane , allyloxytrimethylsilane, allyloxy-tert-butyldimethylsilane, vinyltrimethoxysilane, trimethylchlorosilane, trichlorosilane, glycidoxymethyltrimethoxysilane, glycidoxymethyltriethoxysilane, α-glycine Cydoxyethyltrimethoxysilane, α-glycidoxyethyltriethoxysilane, β-glycidoxyethyltrimethoxysilane, β-glycidoxyethyltriethoxysilane, α-glycidoxypropyltrimethoxy Silane, α-glycidoxypropyltriethoxysilane, β-glycidoxypropyltrimethoxysilane, β-glycidoxypropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycy Doxypropyltriethoxysilane, γ-glycidoxypropyltripropoxysilane, γ-glycidoxypropyltributoxysilane, γ-glycidoxypropyltriphenoxysilane, α-glycidoxybutyltrimethoxysilane , α-glycidoxybutyltriethoxysilane, β-glycidoxybutyltriethoxysilane, γ-glycidoxybutyltrimethoxysilane, γ-glycidoxybutyltriethoxysilane, δ-glycidoxy Butyltrimethoxysilane, δ-glycidoxybutyltriethoxysilane, glycidoxymethyldimethoxysilane, glycidoxymethylmethyldiethoxysilane, α-glycidoxyethylmethyldimethoxysilane, α-glycy Doxyethylmethyldiethoxysilane, β-glycidoxyethylmethyldimethoxysilane, β-glycidoxyethylethyldimethoxysilane, α-glycidoxypropylmethyldimethoxysilane, α-glycidox Cypropylmethyldiethoxysilane, β-glycidoxypropylmethyldimethoxysilane, β-glycidoxypropylethyldimethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyldiethoxysilane , γ-glycidoxypropylmethyldipropoxysilane, γ-glycidoxypropylmethyldibutoxysilane, γ-glycidoxypropylmethyldiphenoxysilane, γ-glycidoxypropyl ethyldimethoxysilane, γ-glyc It may include at least one selected from the group consisting of cydoxypropylethyldiethoxysilane, γ-glycidoxypropylvinyldimethoxysilane, and γ-glycidoxypropylvinyldiethoxysilane. Preferably, 3-(trimethylsilyl)propyl methacrylate silane may be used.

According to one embodiment, the silane-based surface treatment agent may be 10 wt% to 20 wt% of the metal oxide dispersion composition for a display. When the silane-based surface treatment agent is less than 10% by weight of the metal oxide dispersion composition for a display, the dispersibility of the metal oxide in the dispersion composition is lowered to cause a problem that cloudiness occurs, and when it is more than 20% by weight, the metal Since the silane compound is excessively bound to the surface of the oxide particles, aggregation between the particles may occur, resulting in an increase in viscosity. Preferably, the silane-based surface treatment agent may be 10 wt% to 14 wt% of the metal oxide dispersion composition for a display.

According to one embodiment, the phosphoric acid-based surface treatment agent, phosphoric acid ester (phosphoric acid ester), alkenyl polyethylene glycol ether phosphate (Alkenyl polyethylene glycol ether phosphate), an alkylolammonium salt of a copolymer having an acidic group (Alkylolammonium salt a copolymer) with acidic groups), phosphate (Phosphoric acid salt), poly (oxy-1,2-ethanediyl), α-isotridecyl-ω-hydroxy-phosphate (Poly (oxy-1,2-ethanediyl), alpha- isotridecyl-omega-hydroxy-phosphate), phosphoric acid ester salt of a copolymer, polyoxyethylene tridecyl ether phosphate, polyether phosphate, cationic fatty acid phosphate ester, poly It may include at least one selected from the group consisting of oxyethylene lauryl ether phosphate esters and phosphate esters.

According to one embodiment, the phosphoric acid-based surface treatment agent may be 6 wt% to 10 wt% of the metal oxide dispersion composition for a display. When the phosphoric acid-based surface treatment agent is less than 6% by weight of the metal oxide dispersion composition for display, it cannot secure sufficient dispersibility, resulting in cloudiness in the solution phase, and the ring-change phenomenon may not be suppressed, and when it exceeds 10% by weight, the molecular weight is Due to the chain entanglement of the large phosphoric acid-based surface treatment agent, the viscosity of the dispersion may increase and dispersibility may decrease, and problems may occur in curing and visibility of the coating layer. Preferably, the phosphoric acid-based surface treatment agent may be 6 wt% to 9 wt% of the metal oxide dispersion composition for a display.

According to an embodiment, the metal oxide particles are ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ selected from the group consisting of It may include at least one. Preferably, the metal oxide particles may be ZrO ₂ . The ZrO ₂ particles have a high refractive index, substantially no photocatalytic activity, and excellent light resistance and weather resistance.

According to an embodiment, the metal oxide particles serve to provide high luminance functionality.

According to an embodiment, the metal oxide particles may be 30 wt% to 50 wt% of the metal oxide dispersion composition for a display. When the metal oxide particles are included in less than 30% by weight of the metal oxide dispersion composition for the display, the luminance of the curable composition is lowered, and there may be a problem in that the optical properties of the cured film produced in the post-process are lowered, and more than 50% by weight may occur. In this case, the dispersion interval between the metal oxide particles is extremely low, so that the viscosity of the dispersion is excessively increased, and there may be a problem in that aggregation between the metal oxide particles occurs.

According to an embodiment, the metal oxide particles may have an average particle size of 10 nm to 20 nm. If the average particle size of the metal oxide particles is less than 10 nm, dispersion may be difficult due to an increase in the surface energy of the particles, and if it is more than 20 nm, aggregation occurs or precipitates are formed, resulting in poor coating appearance and reduced refractive index Problems can arise.

According to an embodiment, the organic solvent is tetrahydrofuran, isopropyl alcohol, n-butanol, ethylene glycol, propylene glycol, methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, CHN, ethyl acetate, butyl acetate, Propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, n-hexane, toluene, xylene, styrene, o-methyl styrene, m-methyl styrene, p-methyl styrene, vinyl toluene, p-methoxy styrene, benzyl acryl Late, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenylyl acrylate, 2-([1,1'-biphenyl]-2-yloxy) ethyl acrylate , Phenoxybenzylacrylate, 3-phenoxybenzyl-3-(1-naphthyl)acrylate, ethyl (2E)-3-hydroxy-2-(3-phenoxybenzyl)acrylate, phenylmethacrylate , Biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate acrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ortho-phenylphenol ethyl acrylate, bisphenol diacrylate, urethane (meth) Acrylate, 2-ethylhexyl (meth) acrylate, isobornyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy Butyl acrylate, methyl ethylene glycol mono (meth) acrylate, methyl triethylene diglycol (meth) acrylate, 1,4-butanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, hydroxyl Cypivalate neopentyl glycol di(meth)acrylate, dicyclopentanyl di(meth)acrylate, caprolactone-modified dicyclopentanyl di(meth)acrylate, ethylene oxide-modified phosphate di(meth)acrylate, arylated cyclo Hexyldi(meth)acrylate, ethylene glycol di(meth)acrylate, 1,6-hexadiol diacrylate, trimethylolpropane tri(meth)acrylate, pentaerythritol tri( group consisting of meth) acrylate, dipentaerythritol penta (meth) acrylate, dipentaerythritol hexa (meth) acrylate, polyol poly (meth) acrylate, urethane (meth) acrylate and glycerin trimethacrylate It may be to include one or more selected from. Preferably, tetrahydrofuran may be used.

According to an embodiment, the organic solvent may be 35 wt% to 45 wt% of the metal oxide dispersion composition for a display. When the solvent is less than 35% by weight of the metal oxide dispersion composition for display, the viscosity increases and it is difficult to uniformly disperse the metal oxide. Therefore, it becomes difficult to control the thickness of the coating film during coating.

According to one embodiment, the metal oxide dispersion composition for a display may have a viscosity of 500 cP or less. When the viscosity of the metal oxide dispersion composition for a display exceeds 500 cP, the viscosity may become too high, so that it may be difficult to prepare a liquid with an organic material, and when a film for a display is manufactured, it is difficult to form a homogeneous film layer can occur

According to an embodiment, the liquidus refractive index may be 1.67 or more, and the yellowness (Y.I) may be 40 or less.

The metal oxide dispersion composition for a display according to the present invention has an effect of remarkably improving yellowness compared to a dispersion composition in which only a silane-based surface treatment agent or a phosphoric acid-based surface treatment agent is added while implementing a high refractive index of 1.67 or more.

That is, the metal oxide dispersion composition for a display according to the present invention has a feature that can improve yellowness while implementing high refractive index and low viscosity.

A method for preparing a metal oxide dispersion composition for a display according to another embodiment of the present invention includes the steps of preparing metal oxide particles; preparing a mixed solution by adding the metal oxide particles to a solution in which a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent are dissolved in an organic solvent; preparing a metal oxide-organic solvent dispersion by putting beads in the mixed solution at the same weight as the metal oxide particles and dispersing; and removing the undispersed large metal oxide particles from the metal oxide-organic solvent dispersion.

A method of preparing a metal oxide dispersion composition for a display according to another embodiment of the present invention includes a step of preparing metal oxide particles, a step of preparing a mixed solution, a step of preparing a metal oxide-organic solvent dispersion, and a step of removing large metal oxide particles.

According to an embodiment, the metal oxide particle preparation step is ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ From the group consisting of It may be to prepare at least one selected metal oxide particle. Preferably, the metal oxide particles may be ZrO ₂ .

According to an embodiment, the preparing of the mixed solution may include preparing a mixed solution by adding the metal oxide particles to a solution in which a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent are dissolved in an organic solvent.

According to one embodiment, the mixed solution may be prepared by adding the metal oxide particles to a solution in which a silane-based surface treatment agent is dissolved in an organic solvent and a solution in which a phosphoric acid-based surface treatment agent is dissolved in an organic solvent.

According to one embodiment, in the metal oxide dispersion composition for a display, each characteristic of the silane-based surface treatment agent, the phosphoric acid-based surface treatment agent and the organic solvent is as described above.

According to one embodiment, the solution in which the silane-based surface treatment agent is dissolved in an organic solvent is obtained by adding the silane-based surface treatment agent to the organic solvent, and then using a stirrer bar at a temperature of 20°C to 30°C for 5 minutes to 20 minutes. It can be prepared by mixing.

According to one embodiment, the solution in which the phosphoric acid-based surface treatment agent is dissolved in an organic solvent is obtained by adding the phosphoric acid-based surface treatment agent to the organic solvent, and then using a stirrer bar at a temperature of 20°C to 30°C for 5 minutes to 20 minutes. It can be prepared by mixing.

Then, the metal oxide particles are put in a solution in which the silane-based surface treatment agent is dissolved in an organic solvent and a phosphoric acid-based surface treatment agent is dissolved in an organic solvent, and the stirrer bar is stirred at a temperature of 20 to 30°C for 20 to 40 minutes. A mixed solution can be prepared by using and mixing.

According to one embodiment, the metal oxide-organic solvent dispersion preparation step is to prepare a metal oxide-organic solvent dispersion by putting beads in the mixed solution at the same weight as the metal oxide particle weight and dispersing it.

According to an embodiment, the beads include at least one selected from the group consisting of zirconia, yttria, yttria stabilized zirconia, alumina, titanium dioxide, magnesia, silicon carbide, tungsten carbide, titanium carbide, and silicon nitride. may be doing

According to one embodiment, after the beads are added to the mixed solution, the metal oxide particles may be dispersed for 2 to 4 hours using a paint shaker.

According to an embodiment, the step of removing the large metal oxide particles may include removing the large metal oxide particles that are not dispersed in the metal oxide-organic solvent dispersion.

According to an embodiment, a dispersion composition for a display may be prepared by filtering out undispersed large metal oxide particles from the metal oxide-organic solvent dispersion using a syringe filter of 1 μm.

The film composition for a display according to another embodiment of the present invention, the metal oxide dispersion composition for a display according to an embodiment of the present invention or a method for producing a metal oxide dispersion composition for a display according to another embodiment of the present invention The prepared metal oxide dispersion composition for a display; UV photoinitiators; and a monomer for UV curing.

According to an embodiment, the UV photoinitiator may include a photocationic initiator, a radical photoinitiator, or both.

According to one embodiment, the UV photoinitiator, an onium salt-based, diazonium salt-based, sulfonium salt-based compound and an imidazole-based photocationic initiator selected from; and thioxanthone-based, phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, propanone-based, amino ketone-based, ketone-based, benzoin ether acetophenone-based, anthraquinone-based and aromatic phosphine oxide-based compounds It may include at least one selected from the group consisting of a radical photoinitiator.

According to an embodiment, the UV photoinitiator may be 2 wt% to 5 wt% of the film composition for a display. When the UV photoinitiator is less than 2% by weight of the film composition for display, curing of the film composition may not be sufficiently achieved and it may be difficult to secure appropriate hardness. can

According to one embodiment, the UV curing monomer may include an acrylate-based resin. The acrylate-based resin is a saturated hydrocarbon-based polymer having no intramolecular double bond, and has excellent resistance to oxidation in terms of its intrinsic properties, and thus has excellent weather resistance.

According to an embodiment, the UV curing monomer is glycidyl acrylate, glycidyl methacrylate, glycidyl methacrylate, glycidyl-alpha-ethyl acrylate, glycidyl-alpha-ene -Propyl acrylate, glycidyl-alpha-butyl acrylate, 3,4-epoxybutyl methacrylate, 3,4-epoxybutyl acrylate, 6,7-epoxypeptyl methacrylate, 6,7-epoxyheptyl Acrylate, 6,7-epoxyheptyl-alpha-ethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl meta It may include at least one selected from the group consisting of acrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, 1,6-hexanediol diacrylate, and trimethylpropane triacrylate.

According to one embodiment, the film composition for a display according to the present invention may further include an acrylic resin.

According to an embodiment, the acrylic resin is hydroxyethyl acrylate (HEA), hydroxyethyl methacrylate (HEMA), hexanediol diacrylate (HDDA), tripropylene glycol diacrylate (TPGDA), ethylene Glycol diacrylate (EGDA), trimethylolpropane triacrylate (TMPTA), trimethylolpropaneethoxy triacrylate (TMPEOTA), glycerin propoxylated triacrylate (GPTA), pentaerythritol tetraacrylate (PETA) , benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenylyl acrylate, 2-([1,1'-biphenyl] -2-yloxy) ethyl acrylate, Phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, phenyl methacrylate, biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2- It may include one or more selected from the group consisting of nitrophenyl methacrylate, 4-nitrophenyl methacrylate, and dipentaerythritol hexaacrylate (DPHA).

The film composition according to an embodiment of the present invention can prepare a low-viscosity composition, and can improve the color of the film from yellowing.

The optical film for a display according to another embodiment of the present invention is prepared by UV curing the film composition for a display according to an embodiment of the present invention, and has a yellowness (Y.I) of 40 or less.

Preferably, the yellowness may be 38 or less.

The optical film for a display according to the present invention has a characteristic of reducing yellowness while implementing a high refractive index of 1.67 or more.

An optical member for a display according to another embodiment of the present invention includes an optical film for a display according to an embodiment of the present invention.

According to an embodiment, the optical member for display may include a polarizing film, a prism sheet, an AR sheet, and the like.

Hereinafter, the present invention will be described in detail with reference to the following Examples and Comparative Examples. However, the technical spirit of the present invention is not limited or limited thereto.

[Example 1]

40 wt% of zirconia particles, 13.2 wt% of MPS (3-(trimethoxysilyl)propylmethacrylate silane) (Sigma-Aldrich) as a silane-based surface treatment agent, 13.2 wt% of a phosphoric acid-based surface treatment agent (Plysurf AL (product name, Daiichi) 7.5 wt% organic solvent An inorganic particle mixture was prepared using 39.3 wt% of tetrahydrofuran.

After that, 0.05 mm beads are added to the mixed solution in the same weight as the zirconia particles, and the dispersion process is performed using a paint shaker, and then the undispersed large metal oxide particles are filtered out using a 1 μm syringe filter to disperse the dispersion for display. A composition was prepared.

[Example 2]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 11.2 wt% of MPS, a silane-based surface treatment agent, was added.

[Example 3]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 10.7 wt% of MPS, a silane-based surface treatment agent, was added.

[Example 4]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 10.5 wt% of MPS, a silane-based surface treatment agent, was added.

[Example 5]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 10.2 wt% of MPS, a silane-based surface treatment agent, was added.

[Example 6]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 9.0 wt% of AL, a phosphoric acid-based surface treatment agent, was added.

[Example 7]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 7.5 wt% of AL, a phosphoric acid-based surface treatment agent, was added.

[Example 8]

In Example 1, a metal oxide dispersion was obtained in the same manner as in Example 1, except that 6.0 wt% of AL, a phosphoric acid-based surface treatment agent, was added.

[Comparative Example 1]

40 wt% of zirconia particles, 9.2 wt% of 3-(trimethoxysilyl)propylmethacrylate silane (Sigma-Aldrich Co.) as a silane-based surface treatment agent, 7.5 wt% of a phosphoric acid-based surface treatment agent (Plysurf AL (product name, Daiichi Co.) 7.5 wt% organic solvent tetrahydro An inorganic particle mixture was prepared using 43.3 wt% of furan.

After that, 0.05 mm beads are added to the mixed solution at the same weight as the metal oxide particles, and the dispersion process is performed using a paint shaker, and then the undispersed large metal oxide particles are filtered out using a 1 μm syringe filter to form a dispersion composition was prepared.

[Comparative Example 2]

40% by weight of zirconia particles, 3-(trimethoxysilyl)propylmethacrylate silane (Sigma-Aldrich) 26.3% by weight as a silane-based surface treatment agent, 7.5% by weight as an organic solvent as a phosphoric acid-based surface treatment agent (Plysurf AL (product name, Daiichi)) An inorganic particle mixture was prepared using 26.2 wt% of furan.

After that, 0.05 mm beads are added to the mixed solution at the same weight as the metal oxide particles, and the dispersion process is performed using a paint shaker, and then the undispersed large metal oxide particles are filtered out using a 1 μm syringe filter to form a dispersion composition was prepared.

[Comparative Example 3]

Metal oxide particles 40% by weight, 3-(trimethoxysilyl)propylmethacrylate silane (Sigma-Aldrich) 11.2% by weight as a silane-based surface treatment agent, phosphate-based surface treatment agent (Plysurf AL (product name, Daiichi Corporation) 9.0% by weight as an organic solvent An inorganic particle mixture was prepared using 39.8 wt% of hydrofuran.

After that, 0.05 mm beads are added to the mixed solution at the same weight as the metal oxide particles, and the dispersion process is performed using a paint shaker, and then the undispersed large metal oxide particles are filtered out using a 1 μm syringe filter to form a dispersion composition was prepared.

The silane-based surface treatment agent content, phosphoric acid-based surface treatment agent content, viscosity, zirconia particle size, Haze, Y.I and refractive index for the dispersion composition for display of Examples 1 to 8 and the dispersant composition of Comparative Examples 1 to 3 were measured. The measurement results are as follows.

silane
surface treatment agent
(weight%) phosphate
surface treatment agent
(weight%) viscosity
(cp) granularity
(nm) Haze
(%) Y.I. refractive index Comparative Example 1 9.2 7.5 545 13.6 19.88 45.96 1.672 Example 1 13.2 360 16.61 13.83 36.88 1.672 Example 2 11.2 293 12.6 11.52 32.96 1.671 Example 3 10.7 278 11.2 11.82 33.86 1.672 Example 4 10.5 321 12.4 11.65 33.35 1.671 Example 5 10.2 410 14.5 16.92 34.59 1.672 Comparative Example 2 26.3 705 13.5 15.18 40.3 1.666 Example 6 11.2 9.0 316 11.8 17.74 33.85 1.672 Example 7 11.2 7.5 307 12.9 15.67 33.64 1.672 Example 8 11.2 6.0 281 13.8 16.18 33.46 1.672 Comparative Example 3 11.2 5.0 640 15.4 18.21 34.85 1.672

1 is a graph showing the yellowness (Y.I) for the MPS content of the present invention, FIG. 2 is a graph showing the haze for the MPS content of the present invention, and FIG. 3 is a graph showing the viscosity for the MPS content of the present invention to be.

As can be seen from the results of Table 1 and FIGS. 1 to 3, the content of the silane-based surface treatment agent is in the range of 13.2 wt% to 10.2 wt%, and the phosphoric acid-based surface treatment agent has a refractive index of 1.670 when it has a range of 6 wt% to 9 wt% As described above, it was confirmed that a dispersion composition of metal oxide particles for a display having a viscosity of 500 cP or less and Y.I 40 or less could be prepared.

As described above, although the embodiments have been described with reference to the limited drawings, those skilled in the art may apply various technical modifications and variations based on the above. For example, the described techniques are performed in a different order than the described method, and/or the described components of the system, structure, apparatus, circuit, etc. are combined or combined in a different form than the described method, or other components Or substituted or substituted by equivalents may achieve an appropriate result.

Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.

Claims (18)

silane-based surface treatment agent;
Phosphoric acid-based surface treatment agent;
metal oxide particles; and
organic solvents;
including,
The silane-based surface treatment agent is 3-(trimethylsilyl)propylmethacrylatesilane, 3-(trimethoxysilyl)propyl methacrylate, methallyltrimethylsilane, allyltrimethylsilane, vinyltrimethylsilane, allyloxytrimethylsilane and is selected from the group consisting of allyloxy-tert-butyldimethylsilane,
The silane-based surface treatment agent is 10 wt% to 14 wt% of the metal oxide dispersion composition for a display,
The phosphoric acid-based surface treatment agent is 6 wt% to 9 wt% of the metal oxide dispersion composition for a display,
The organic solvent is 35 wt% to 45 wt% of the metal oxide dispersion composition for display,
a viscosity of 500 cP or less,
The yellowness (YI) is 40 or less,
A metal oxide dispersion composition for a display.
delete delete According to claim 1,
The phosphoric acid-based surface treatment agent,
Phosphoric acid ester, Alkenyl polyethylene glycol ether phosphate, Alkylolammonium salt a copolymer with acidic groups, Phosphoric acid salt, poly (oxy-1,2-ethanediyl), α-isotridecyl-ω-hydroxy-phosphate (Poly(oxy-1,2-ethanediyl), alpha-isotridecyl-omega-hydroxy-phosphate), phosphoric acid of the copolymer Phosphoric acid ester salt of a copolymer, polyoxyethylene tridecyl ether phosphate ester, polyether phosphate, cationic fatty acid group phosphate ester, polyoxyethylene lauryl ether phosphate ester and phosphate esters ) to include at least one selected from the group consisting of,
A metal oxide dispersion composition for a display.
delete According to claim 1,
The metal oxide particles,
ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ Which comprises at least one selected from the group consisting of,
A metal oxide dispersion composition for a display.
According to claim 1,
The metal oxide particles, 30% to 50% by weight of the metal oxide dispersion composition for the display,
A metal oxide dispersion composition for a display.
According to claim 1,
The metal oxide particles,
which has an average particle size of 10 nm to 20 nm,
A metal oxide dispersion composition for a display.
According to claim 1,
The organic solvent is
Tetrahydrofuran, isopropyl alcohol, n-butanol, ethylene glycol, propylene glycol, methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, CHN, ethyl acetate, butyl acetate, propylene glycol monomethyl ether, propylene glycol monomethyl ether Acetate, n-hexane, toluene, xylene, styrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, vinyl toluene, p-methoxy styrene, benzyl acrylate, benzyl methacrylate, phenyl acrylate, Diphenyl acrylate, biphenyl acrylate, 2-biphenylyl acrylate, 2-([1,1'-biphenyl] -2-yloxy) ethyl acrylate, phenoxybenzyl acrylate, 3-phenoxy Benzyl-3-(1-naphthyl)acrylate, ethyl (2E)-3-hydroxy-2-(3-phenoxybenzyl)acrylate, phenyl methacrylate, biphenyl methacrylate, 2-nitrophenyl Acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4 -Chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ortho-phenylphenol ethyl acrylate, bisphenol diacrylate, urethane (meth) acrylate, 2-ethylhexyl (meth) acrylic Late, isobornyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxybutyl acrylate, methylethylene glycol mono (meth) ) acrylate, methyltriethylenediglycol (meth)acrylate, 1,4-butanediol di(meth)acrylate, neopentylglycol di(meth)acrylate, hydroxypivalate neopentylglycol di(meth)acrylate , dicyclopentanyl di(meth)acrylate, caprolactone-modified dicyclofentanyl di(meth)acrylate, ethylene oxide-modified phosphate di(meth)acrylate, arylated cyclohexyldi(meth)acrylate, ethylene glycol di (meth)acrylate, 1,6-hexadiol diacrylate, trimethylolpropane tri(meth)acrylate, pentaerythritol tri(meth)acrylate, dipentaerythritol penta(meth) ) acrylate, dipentaerythritol hexa (meth) acrylate, polyol poly (meth) acrylate, urethane (meth) acrylate and glycerin trimethacrylate comprising at least one selected from the group consisting of,
A metal oxide dispersion composition for a display.
delete delete According to claim 1,
The liquidus refractive index is 1.67 or more,
A metal oxide dispersion composition for a display.
preparing metal oxide particles;
preparing a mixed solution by adding the metal oxide particles to a solution in which a silane-based surface treatment agent and a phosphoric acid-based surface treatment agent are dissolved in an organic solvent;
preparing a metal oxide-organic solvent dispersion by putting beads in the mixed solution at the same weight as the metal oxide particles and dispersing; and
removing undispersed large metal oxide particles from the metal oxide-organic solvent dispersion;
containing,
The method for preparing the metal oxide dispersion composition for a display according to claim 1 .
A metal oxide dispersion composition for a display prepared by the method for preparing the metal oxide dispersion composition for a display of claim 1 or the metal oxide dispersion composition for a display of claim 13;
UV photoinitiators; and
UV curing monomers;
containing,
A film composition for a display.
15. The method of claim 14,
The UV photoinitiator is
a photocationic initiator selected from onium salt-based, diazonium salt-based, sulfonium salt-based compounds and imidazole-based compounds; and
Thioxanthone-based, phosphorus-based, triazine-based, benzophenone-based, benzoin-based, oxime-based, propanone-based, amino ketone-based, ketone-based, benzoin ether acetophenone-based, anthraquinone-based and aromatic phosphine oxide-based compounds radical photoinitiators;
Which comprises at least any one selected from the group consisting of
A film composition for a display.
15. The method of claim 14,
The UV curing monomer is
Glycidyl acrylate, glycidyl methacrylate, glycidyl methacrylate, glycidyl-alpha-ethyl acrylate, glycidyl-alpha-ene-propyl acrylate, glycidyl-alpha-butylacrylic rate, 3,4-epoxybutyl methacrylate, 3,4-epoxybutyl acrylate, 6,7-epoxypeptyl methacrylate, 6,7-epoxyheptyl acrylate, 6,7-epoxyheptyl-alpha-ethyl Acrylates, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl methacrylate, tripropylene glycol diacrylate, dipropylene glycol which comprises at least one selected from the group consisting of diacrylate, 1,6-hexanediol diacrylate, and trimethylpropane triacrylate,
A film composition for a display.
It is prepared by UV curing the film composition for a display of claim 14,
yellowness (YI) of 40 or less;
Optical film for display.
Including the optical film for display of claim 17,
Optical member for display.

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