KR20220078242A - Dispersion comprising metal oxide - Google Patents

Abstract

The present invention relates to a metal oxide dispersion, and more particularly, to a monomer; and surface modifiers; Including, and the tetragonal peak intensity (I _t ) and monoclinic peak intensity (I _m ) of the zirconia nanoparticles are controlled, relates to a metal oxide dispersion.

Description

Metal oxide dispersions {DISPERSION COMPRISING METAL OXIDE}

The present invention relates to a metal oxide dispersion comprising zirconia particles.

A composition containing an oxide of metals is usefully used in manufacturing a film for a display or the like. A film for a display is required to have properties such as optical transmittance, optical haze, optical clarity, and refractive index. One example of such a film for display is a brightness enhancing film.

Such a film for display is used for the purpose of increasing the brightness|luminance of a display, etc. It can be applied to word processors, desktop monitors, televisions, video cameras, and displays for automobiles and aircraft.

When such a film for a display is used, optical properties and physical properties on a specific panel surface including refractive index can be preferably improved. As an example, when a brightness enhancing film or the like is provided, by improving the brightness, it is possible to illuminate the display using less power, thereby reducing power consumption, reducing the degree of heat generation and reducing the product The lifespan of the device is extended, so that electronic products can be used more effectively.

The development of such a material for a display film is still insignificant, and in order to produce it more effectively, it is possible to maintain a high refractive index while including a metal oxide, and a metal oxide dispersion having high dispersibility and low viscosity of the metal oxide in the composition There is a need to develop the composition of

In order to solve the above-mentioned problems, the present invention provides a metal oxide dispersion having a high refractive index and a low viscosity through control of the crystalline phase ratio of the zirconia nanopowder.

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.

According to an embodiment of the present invention, zirconia nanoparticles; monomer; and a surface modifier, wherein the tetragonal peak intensity (I _t ) and the monoclinic peak intensity (I _m ) of the zirconia nanoparticles satisfy the following formulas, It relates to a metal oxide dispersion.

[Equation 1]

3< I _t /I _m < 4

According to an embodiment of the present invention, the zirconia nanoparticles, a monoclinic crystal structure 30% to 40%; and 60% to 70% of a tetragonal crystal structure; may include.

According to an embodiment of the present invention, the zirconia nanoparticles may be 40 wt% to 70 wt% of the metal oxide dispersion.

According to an embodiment of the present invention, the monomer is 1 wt% to 50 wt% of the metal oxide dispersion, and the monomer is methyl acrylate, lauryl acrylate, ethoxydiethylene glycol acrylate, methoxytri Ethylene glycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxyacrylic Late, nenopentyl glycol diacrylate, 1,6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylolpropane acrylic acid benzoic acid Ester, trimethylolpropanebenzoic acid ester, methyl methacrylate, 2-ethylhexyl methacrylate, n-stearyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate, phenoxyethyl methacrylate, Methoxy polyethylene methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxybutyl methacrylate heptadecafluordecyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate rate, 1,6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, glycerin dimethacrylate hexamethylene diisocyanate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, Benzyl acrylate, 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, ethyl (2E)-3-hydroxy-2-(3-phenoxybenzyl)acrylate, phenylmetha acrylate, biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitro Benzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophene Nyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ortho-phenylphenol ethyl acrylate, phenyl phenol, biphenyl methacrylate, o-phenyl phenol ethoxy acrylate, 1- (bi Phenyl-2-ylmethyl)-4-phenylpiperazine, 1-(biphenyl-2-ylmethyl)-4-(2-methoxyphenyl)piperazine, 1-(biphenyl-2-ylmethyl)- 4-(2-ethoxyphenyl)piperazine, 1-(biphenyl-2-ylmethyl)-4-(2-isopropoxyphenyl)piperazine, 1-(biphenyl-2-ylmethyl)-4 -(3-methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (4-methoxyphenyl) containing at least one selected from the group consisting of piperazine and bisphenol diacrylate it could be

According to an embodiment of the present invention, the surface modifier includes a silane coupling agent, and the silane coupling agent includes an acrylate group, a (meth)acrylic group, Epoxy group, alkoxy group, vinyl group (vinyl), phenyl group (phenyl), methacryloxy group (methacryloxy), amino group (amino), chlorosilane group (chlorosilanyl), chloropropyl group (chloropropyl) and mer It may be a silane containing at least one selected from the group consisting of a capto group (mercapto).

According to an embodiment of the present invention, the surface modifier is (3-glycidoxypropyl) trimethoxysilane, (3-glycidoxypropyl) triethoxysilane, (3-glycidoxypropyl) methyl dime Toxysilane, (3-glycidoxypropyl)dimethylethoxysilane, 3-(methacryloxy)propyltrimethoxysilane, 3,4-epoxybutyltrimethoxysilane, 3,4-epoxybutyltriethoxysilane , 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, aminopropyltriethoxysilane, vinyltriethoxysilane, vinyltri -t-butoxysilane, vinyltriisobutoxysilane, vinyltriisopropoxysilane, vinyltriphenoxysilane, aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane; Phenylsilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenylchlorosilane, phenyltrichlorosilane, γglycidoxypropyltriphenoxysilane, γglycidoxypropylmethyldiphenoxysilane, dichlorodiphenylsilane, At least one selected from the group consisting of N-phenyl-γ-aminopropyltrimethoxysilane, dimethoxymethylphenylsilane, diphenyldimethoxysilane, diethoxydiphenylsilane, methylphenyldiethoxysilane, methylphenyldichlorosilane and phenoxytrimethylsilane It may include more than one.

According to an embodiment of the present invention, the surface modifier may be 10 parts by weight to 20 parts by weight based on the total weight of the zirconia nanoparticles in the metal oxide dispersion.

According to an embodiment of the present invention, the metal oxide dispersion further includes a dispersant, and the dispersant includes a polyether acid-based compound, a polyetheramine-based compound, a polyether acid/amine mixture, an ester-based compound including a phosphoric acid group, and It may include at least one selected from the group consisting of polyether-based compounds containing a phosphoric acid group.

According to an embodiment of the present invention, the refractive index of the metal oxide dispersion may be 1.60 or more.

According to an embodiment of the present invention, the viscosity of the metal oxide dispersion may be 400 CP or less.

According to an embodiment of the present invention, the metal oxide dispersion may be solvent-free.

According to an embodiment of the present invention, it relates to an optical member for a flexible display manufactured using the metal oxide dispersion according to the present invention.

The present invention can provide a monomer dispersion of zirconia having a low viscosity and a high refractive index by applying a zirconia nanopowder with a controlled crystal phase ratio. In addition, the dispersion is excellent in dispersibility of the zirconia particles, provides a relatively low viscosity, has excellent flowability and moldability, and can be applied as a display sol dispersion capable of improving the efficiency of a device, that is, a display device. .

Hereinafter, embodiments of the present invention will be described in detail. In describing the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the gist of the present invention, the detailed description thereof will be omitted. In addition, the terms used in this specification are terms used to properly express a preferred embodiment of the present invention, which may vary depending on the intention of a user or operator or a custom in the field to which the present invention belongs. Accordingly, definitions of these terms should be made based on the content throughout this specification.

Throughout the specification, when a part "includes" a certain component, it means that other components may be further included, rather than excluding other components.

Hereinafter, the present invention will be described in detail with reference to Examples with respect to the polishing slurry composition. However, the present invention is not limited to these examples.

The present invention relates to a metal oxide dispersion, and according to an embodiment of the present invention, the metal oxide dispersion comprises: zirconia nanoparticles; monomer; and a surface modifier;

According to an embodiment of the present invention, the zirconia nanoparticles may lower the viscosity of the metal oxide dispersion by controlling the crystal phase ratio of the powder and exhibit a high refractive index. That is, the ratio of the crystalline phases may control the ratio of peak intensity corresponding to the tetragonal and monoclinic systems, the ratio of tetragonal and monoclinic crystal phases, or both in the XRD pattern.

As an example of the present invention, the tetragonal peak intensity (I _t ) and the monoclinic peak intensity (I _m ) in the zirconia nanoparticles may satisfy Equation 1 below.

[Equation 1]

3< I _t /I _m < 4

As an example of the present invention, 30% to 40% of the monoclinic crystal structure in the zirconia nanoparticles; or 34% to 40%; and 60% to 70% of a tetragonal crystal structure; Alternatively, it may be 60% to 66%, and in combination with the peak intensity ratio according to Equation 1, it may be advantageous to lower the viscosity of the dispersion while having a high refractive index.

As an example of the present invention, the zirconia nanoparticles may be 40 wt% to 70 wt% of the metal oxide dispersion. When included within the above range, the refractive index of the dispersion is lowered due to the low content of zirconia and the luminance is lowered to prevent a problem that it is difficult to provide a high refractive index cured film, and the dispersion interval between the zirconia particles due to the excessive addition of the zirconia particles is extremely The viscosity of the dispersion is lowered, and the dispersibility is inhibited due to the occurrence of agglomeration between the zirconia particles, and the deterioration of the optical properties can be lowered.

In one embodiment of the present invention, the size of the zirconia particles, 1 nm or more; more than 10 nm; or 50 nm to 100 nm.

According to an embodiment of the present invention, the monomer is a C1-C22 alkyl acrylate-based monomer, a C1-C22 alkoxy acrylate-based monomer, a C6-C24 aryl acrylate-based monomer, and a C1-C22 alkyl (meth)acrylate-based monomer. Monomer, C1-C22 alkoxy (meth) acrylate-based monomer, C6-C24 aryl (meth) acrylate-based monomer, alkylene glycol di (meth) acrylate-based monomer, alkylene glycol diacrylate-based monomer, alkylene glycol It may include at least one selected from the group consisting of an alkyl ether (meth) acrylate-based monomer, an alkylene glycol alkyl ether acrylate-based monomer, and a derivative into which a methacrylate and/or acrylate substituent is introduced.

In addition, the monomer is further substituted by at least one of hydroxy, an aliphatic ring, and an aromatic ring (6 to 30 carbon atoms) in the molecule, and the "alkylene" has 1 to 10 carbon atoms, and 1 to 20 carbon atoms. Included as (n), the “alkyl ether” may include an alkyl group having 1 to 20 carbon atoms. The monomer may include 1 to 6 functional acrylates, for example, bifunctional, trifunctional, and the like.

For example, the monomer is methyl acrylate, lauryl acrylate, ethoxydiethylene glycol acrylate, methoxytriethylene glycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate , 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxy acrylate, nenopentyl glycol diacrylate, 1,6-hexanediol diacrylate, trimethylolpropane tri Acrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylol propane acrylic acid benzoate ester, trimethylol propane benzoic acid ester, methyl methacrylate, 2-ethylhexyl methacrylate, n- Stearyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate, phenoxyethyl methacrylate, methoxy polyethylene methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxybutyl methacrylate Late heptadecafluordecyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate, 1,6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, glycerin di Methacrylate hexamethylene diisocyanate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, benzyl acrylate, 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, 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 Yite, phenylphenol, biphenyl methacrylate, o-phenylphenol ethoxyacrylate, 1-(biphenyl-2-ylmethyl)-4-phenylpiperazine, 1-(biphenyl-2-ylmethyl)- 4-(2-Methoxyphenyl)piperazine, 1-(biphenyl-2-ylmethyl)-4-(2-ethoxyphenyl)piperazine, 1-(biphenyl-2-ylmethyl)-4- (2-isopropoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (3-methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- ( 4-methoxyphenyl) piperazine, bisphenol diacrylate, and the like.

In one embodiment of the present invention, the monomer may be included in an amount of 1 wt% to 50 wt% of the metal oxide dispersion; Or 10 wt% to 50 wt%, when included within the above range, it is possible to provide a coating having high refractive index and flexibility by increasing the dispersibility of the metal oxide and improving hardenability in the subsequent process.

According to an embodiment of the present invention, when the surface modifier is included within the above range, the metal oxide sol dispersion effectively sols the zirconia particles while maintaining a high refractive index, a low viscosity level suitable for forming a film, and an effective light transmittance. It can perform a role of dispersing in the dispersion. Through this, even when the metal oxide dispersion of the present invention is filled with a high concentration of zirconia particles, stable dispersibility is ensured, so that it may be possible to prepare a metal oxide sol maintaining high transparency.

In one embodiment of the present invention, the surface modifier includes a silane coupling agent, and the silane coupling agent includes an acryl group, a (meth)acrylic group, Epoxy group, alkoxy group, vinyl group (vinyl), phenyl group (phenyl), methacryloxy group (methacryloxy), amino group (amino), chlorosilane group (chlorosilanyl), chloropropyl group (chloropropyl) and mer It may be a silane containing at least one selected from the group consisting of a capto group (mercapto). The acrylate-based monomer and the methacrylate-based monomer may be substituted with a phenyl group.

For example, the surface modifier is (3-glycidoxypropyl) trimethoxysilane, (3-glycidoxypropyl) triethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, (3 -glycidoxypropyl) dimethylethoxysilane, 3-(methacryloxy)propyltrimethoxysilane, 3,4-epoxybutyltrimethoxysilane, 3,4-epoxybutyltriethoxysilane, 2-(3 ,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, aminopropyltriethoxysilane, vinyltriethoxysilane, vinyltri-t-butoxy silane, vinyltriisobutoxysilane, vinyltriisopropoxysilane, vinyltriphenoxysilane, aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane; and phenylsilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenylchlorosilane, phenyltrichlorosilane, γ-glycidoxypropyltriphenoxysilane, γ-glycidoxypropylmethyldiphenoxysilane, dichlorodi phenylsilane, N-phenyl-γ-aminopropyltrimethoxysilane, dimethoxymethylphenylsilane, diphenyldimethoxysilane, diethoxydiphenylsilane, methylphenyldiethoxysilane, methylphenyldichlorosilane, phenoxytrimethylsilane, and the like.

As an example of the present invention, the surface modifier is 10 parts by weight to 20 parts by weight based on the total weight of the zirconia nanoparticles in the metal oxide dispersion, and when included within the range, the progress rate of the surface treatment reaction of the zirconia particles is appropriately adjusted It can be maintained to increase the dispersibility of the zirconia particles in the dispersion composition, and the excessively used surface treatment agent is attached to the surface of the zirconia particles to induce agglomeration between the zirconia particles, thereby lowering the dispersibility degradation.

According to an embodiment of the present invention, the metal oxide dispersion further includes a dispersant, and the dispersant includes a polyether acid-based compound, a polyetheramine-based compound, a polyether acid/amine mixture, an ester-based compound including a phosphoric acid group, and It may include at least one selected from the group consisting of polyether-based compounds containing a phosphoric acid group.

As an example of the present invention, the dispersant may be 1 wt% to 20 wt% of the metal oxide dispersion. When the dispersant is included in less than 1% by weight, compatibility with the resin composition made of an organic compound to be used in the post-process is lowered, and when it is included in more than 20% by weight, the dispersant is excessively bound to the surface of the zirconia particles and the refractive index is lowered. There may be problems with degradation.

According to an embodiment of the present invention, the metal oxide dispersion may further include an organic solvent, and the solvent is for facilitating dispersion, and may be 30% to 50% by weight. The solvent can be completely (almost) removed for subsequent processing to form a process solvent-free sol dispersion.

As an example of the present invention, when the organic solvent is less than 30% by weight of the metal oxide dispersion, it is out of the minimum range for the role of the dispersion medium and causes a decrease in dispersibility and inhibition of viscosity and optical properties, and a solvent removal time of more than 50% by weight This increases, the refractive index and luminance of the optical film made of the metal oxide dispersion may decrease, and there may be problems in that the transmittance of the cured film is lowered and the haze is increased.

According to an embodiment of the present invention, the refractive index of the metal oxide dispersion is 1.60 or more; Alternatively, the refractive index is 1.670 or more, which has excellent compatibility with a component or composition applied together in a subsequent process, and can form a coating having characteristics of high luminance efficiency, high transmittance and high refractive index.

According to an embodiment of the present invention, the viscosity of the metal oxide dispersion is 400 CP or less; 100 to 400; or 100 to 300, and the metal oxide dispersion is solvent-free, and may be a sol dispersion. When the viscosity is high, the viscosity becomes too high, so it is difficult to prepare a liquid with an organic material, and there may occur a problem that the dispersibility of the zirconia particles in the dispersion is lowered, and when manufacturing a film, it becomes difficult to form a homogeneous film layer, There may be a problem of deterioration of characteristics. The viscosity may be measured using a DV2T LV Spindle (manufactured by Brookfield). In addition, the viscosity may be measured at a temperature of 25° C. and shear rate = 1.0 (1/s)/.

According to an embodiment of the present invention, it relates to an optical member for a flexible display manufactured using the metal oxide dispersion according to the present invention.

As an example of the present invention, the optical member may be, for example, an optical member for a display such as a diffusion film for an electronic device, an optical film, a polarizing film, a prism sheet, an AR sheet, a film for display, and the like.

In one embodiment of the present invention, the optical member may include a substrate; and a coating (film, film, thin film, etc.) prepared from a composition comprising a metal oxide dispersion or a metal oxide dispersion according to the present invention formed on at least a portion of the substrate. When the optical member is manufactured, the composition including the metal oxide dispersion or the metal oxide dispersion may form a coating in a trace amount or close to zero or in a process solvent-free state.

As an example of the present invention, the substrate is appropriately selected according to the use for the optical film, and may be a transparent substrate. The transparent substrate may be applied without limitation as long as it is a film having transparency. For example, between polyester such as polyethyleneterephthalate (PET), polyethylene such as ethylene vinyl acetate (EVA), and cyclic olefin polymer (COP), cyclic olefin copolymer (COC), polyacrylate (PAC), polycarbonate (PC), polyethylene (PE), polymethylmethacrylate (PMMA), polyether ether Ketones (polyetheretherketon, PEEK), polyethylenenaphthalate (PEN), polyetherimide (PEI), polyimide (polyimide, PI), triacetylcellulose (TAC), MMA (methyl methacrylate), or fluorine-based It may be a film including a resin or the like, and may also be an inorganic substrate having flexibility.

Hereinafter, the present invention will be described in more detail through examples, but the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.

Example 1

Hydrothermal-zirconia nanoparticles were synthesized using the hydrothermal synthesis method, and the synthesized zirconia particles were tetragonal 65.4% and monoclinic 34.6%, and the tetragonal to monoclinic peak ratio was 3.70 (XRD pattern).

In a 100mL container for a paint shaker, 28.9 g of tetrahydrofuran (Tetrahydrofuran, hereinafter referred to as 'THF') and 2.1 g of silane having a methacryl group (3-(methacryloxy) propyltrimethoxysilane, particle solids 10-20% content) and mixed for 10 minutes at room temperature using a stirrer bar. Next, 38 g of synthesized zirconia powder was added to the solution, and a mixed solution was formed for 30 minutes at room temperature using a stirrer bar. Thereafter, 200 g of 0.05 mm beads were added to the mixture and dispersed for 3 hours using a paint shaker to obtain a 40 wt% zirconia-THF solvent dispersion. Thereafter, the zirconia-THF solvent dispersion was mixed with an acrylate-based monomer (biphenylmethyl acrylate, 40 wt%) to remove the solvent under reduced pressure to obtain a zirconia-monomer (40 wt%) dispersion. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Example 2

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method, and the zirconia particles synthesized at this time were tetragonal 64.2% and monoclinic 35.8%, and the tetragonal and monoclinic peak ratios were 3.48. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Example 3

Hydrothermal-zirconia nanoparticles were synthesized using the hydrothermal synthesis method, and the zirconia particles synthesized at this time were tetragonal 65.8% and monoclinic 34.2%, and the tetragonal and monoclinic peak ratios were 3.36. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 1

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method. At this time, tetragonal 72.6% and monoclinic 27.4% of the synthesized zirconia particles were obtained, and the tetragonal to monoclinic peak ratio was 5.90. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 2

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method, and 68.7% tetragonal and 31.3% monoclinic of the synthesized zirconia particles were obtained, and the tetragonal to monoclinic peak ratio was 5.65. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 3

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method, and the zirconia particles synthesized at this time were tetragonal 64.1% and monoclinic 35.9%, and the tetragonal to monoclinic peak ratio was 4.01. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 4

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method. At this time, tetragonal 56.1% and monoclinic 43.9% of the synthesized zirconia particles were obtained, and the tetragonal to monoclinic peak ratio was 2.23. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 5

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method, and the zirconia particles synthesized at this time were 49.0% tetragonal and 51.0% monoclinic, and the tetragonal to monoclinic peak ratio was 1.62. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

Comparative Example 6

Hydrothermal-zirconia nanoparticles were synthesized using a hydrothermal synthesis method, and the zirconia particles synthesized at this time were tetragonal 25.4% and monoclinic 74.6%, and the tetragonal and monoclinic peak ratios were 0.61. A monomer dispersion was prepared in the same manner as in Example 1. The viscosity and refractive index of the prepared monomer dispersion are shown in Table 1.

<Measuring method of refractive index>

When a sample of the coating solution prepared according to this example is dropped onto a prism at room temperature (25° C.) and the set temperature is reached by pressing the start key, the measurement starts automatically. The result is the refractive index of the composition, and the result is shown in the table.

Measuring device: ATAGO / JAPAN

Model Name: RX-5000 Alpha

<Viscosity measurement method>

Viscosity was measured using DV2T LV Spindle equipment.

zirconia crystal phase Zirconia-monomer dispersion tetragonal intensity (I _t ) Monoclinic Intensity (I _m ) I _t / I _m
Ratio tetragonal ratio (%) Monoclinic rate (%) refractive index Viscosity (cP) Example 1 5220 1410 3.70 65.4 34.6 1.6728 360.4 Example 2 3953 1063 3.48 64.2 35.8 1.6722 302.1 Example 3 5493 1637 3.36 65.8 34.2 1.6719 232.2 Comparative Example 1 4913 833 5.90 72.6 27.4 1.6720 4,079 Comparative Example 2 3427 607 5.65 68.7 31.3 1.6725 1,322 Comparative Example 3 4233 1053 4.01 64.1 35.9 1.6725 876.0 Comparative Example 4 5243 2347 2.23 56.1 43.9 1.6658 1,037 Comparative Example 5 4223 2607 1.62 49.0 51.0 1.6710 1,178 Comparative Example 6 2070 3423 0.61 25.4 74.6 1.6732 1,991

Looking at Table 1, the ratio of tetragonal and monoclinic peak intensities is greater than 3 and less than 4, and the ratio of tetragonal and monoclinic zirconia mixed crystalline phases (tetragonal ratio 60-66%, monoclinic ratio 34-40% crystalline phase) ratio), the effect of reducing the viscosity while having a high refractive index can be confirmed.

As described above, although the embodiments have been described by way of limited embodiments, various modifications and variations are possible by those skilled in the art from the above description. For example, even if the described techniques are performed in an order different from the described method, and/or the described components are combined or combined in a form different from the described method, or replaced or substituted by other components or equivalents Appropriate results can be achieved. Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.

Claims (12)

zirconia nanoparticles;
monomer; and
surface modifier;
including,
The tetragonal peak intensity (I _t ) and the monoclinic peak intensity (I _m ) of the zirconia nanoparticles satisfy the following formula,
Metal Oxide Dispersion:
[Equation 1]
3< I _t /I _m < 4
According to claim 1,
The zirconia nanoparticles are
30% to 40% monoclinic crystal structure; and
tetragonal crystal structure 60% to 70%;
which includes,
Metal Oxide Dispersion.
According to claim 1,
The zirconia nanoparticles, 40% to 70% by weight of the metal oxide dispersion,
Metal Oxide Dispersion.
According to claim 1,
The monomer is 1% to 50% by weight of the metal oxide dispersion,
The monomer is methyl acrylate, lauryl acrylate, ethoxydiethylene glycol acrylate, methoxytriethylene glycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydr Oxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxy acrylate, nenopentyl glycol diacrylate, 1,6-hexanediol diacrylate, trimethylolpropane triacrylate, penta Erythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylol propane acrylic acid benzoate ester, trimethylol propane benzoic acid ester, methyl methacrylate, 2-ethylhexyl methacrylate, n-stearyl methacrylate Late, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate, phenoxyethyl methacrylate, methoxypolyethylene methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxybutyl methacrylate heptadecafluor Decyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate, 1,6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, glycerin dimethacrylate hexa Methylene diisocyanate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, benzyl acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenyl Lyl acrylate, 2-([1,1'-biphenyl]-2-loxy) ethyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-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, phenylphenol , biphenyl methacrylate, o-phenylphenol ethoxy acrylate, 1- (biphenyl-2-ylmethyl) -4-phenylpiperazine, 1- (biphenyl-2-ylmethyl) -4- (2 -Methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-ethoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-iso Propoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (3-methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (4-methoxy phenyl) comprising at least one selected from the group consisting of piperazine and bisphenol diacrylate,
Metal Oxide Dispersion.
According to claim 1,
The surface modifier includes a silane coupling agent,
The silane coupling agent is an acrylate group, a (meth)acrylic group, Epoxy group, alkoxy group, vinyl group (vinyl), phenyl group (phenyl), methacryloxy group (methacryloxy), amino group (amino), chlorosilane group (chlorosilanyl), chloropropyl group (chloropropyl) and mer It is a silane containing at least one selected from the group consisting of a capto group (mercapto),
Metal Oxide Dispersion.
According to claim 1,
The surface modifier is (3-glycidoxypropyl) trimethoxysilane, (3-glycidoxypropyl) triethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, (3-glycidoxy Propyl) dimethylethoxysilane, 3-(methacryloxy)propyltrimethoxysilane, 3,4-epoxybutyltrimethoxysilane, 3,4-epoxybutyltriethoxysilane, 2-(3,4-epoxy) Cyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, aminopropyltriethoxysilane, vinyltriethoxysilane, vinyltri-t-butoxysilane, vinyltri Isobutoxysilane, vinyltriisopropoxysilane, vinyltriphenoxysilane, aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, phenylsilane, phenyltrimethoxysilane, phenyltriethoxy Silane, phenylchlorosilane, phenyltrichlorosilane, γ-glycidoxypropyltriphenoxysilane, γ-glycidoxypropylmethyldiphenoxysilane, dichlorodiphenylsilane, N-phenyl-γ-aminopropyltrimethoxy A metal oxide dispersion comprising at least one selected from the group consisting of silane, dimethoxymethylphenylsilane, diphenyldimethoxysilane, diethoxydiphenylsilane, methylphenyldiethoxysilane, methylphenyldichlorosilane and phenoxytrimethylsilane.
According to claim 1,
The surface modifier, 10 to 20 parts by weight based on the total weight of the zirconia nanoparticles in the metal oxide dispersion,
Metal Oxide Dispersion.
According to claim 1,
The metal oxide dispersion further comprises a dispersing agent,
The dispersing agent comprises at least one selected from the group consisting of polyether acid-based compounds, polyether amine-based compounds, polyether acid/amine mixtures, ester-based compounds including phosphoric acid groups, and polyether-based compounds including phosphoric acid groups.
Metal Oxide Dispersion.
According to claim 1,
The refractive index of the metal oxide dispersion is 1.60 or more,
Metal Oxide Dispersion.
According to claim 1,
The viscosity of the metal oxide dispersion will be 400 CP or less,
Metal Oxide Dispersion.
According to claim 1,
The metal oxide dispersion is a solvent-free,
Metal Oxide Dispersion.
Claim 1 prepared using the metal oxide dispersion,
Optical member for flexible display.