KR20160014969A - Manufacturing method of inorganic particles dispersed hybrid materials by controlling the particle size of inorganic particles through grinding of inorganic particles - Google Patents

Abstract

The technical idea of the present invention relates to a manufacturing method of a hybrid material having dispersed inorganic particles, through pulverizing inorganic particles and controlling particle sizes. The manufacturing method comprises: a step of preparing inorganic particles; a step of primarily, secondarily, and tertiarily pulverizing the inorganic particles by using milling balls, each having different sizes; a step of obtaining the inorganic particles pulverized so as to have different particle sizes; a step of treating the surface of the inorganic particles with organic silane; a step of separating and drying the silane-treated inorganic particles; and a step of manufacturing a hybrid material by mixing the inorganic particles with different sizes. By using the inorganic particles with different particle sizes to have a crystallization structure or a compact structure, which are manufactured by the method as described in the present invention, a hybrid material having high packing density can be obtained. An effect of improving electric properties, mechanical properties, and chemical durability of appliances to which the hybrid material is applied, is provided.

Description

Technical Field [0001] The present invention relates to a method for producing inorganic particles dispersed in a hybrid material,

The present invention relates to a method for producing an inorganic particle dispersed hybrid material through pulverization and particle size control of inorganic particles, and more particularly, to a method for producing inorganic particle dispersed hybrid materials by controlling the size, milling time, The present invention relates to a process for producing an inorganic particle hybrid material by pulverizing inorganic particles and controlling the particle size of the inorganic particles, which is applied to a hybrid material, by mixing the inorganic particles with a functional organic silane at a suitable ratio.

In general, inorganic particles have excellent physical properties such as corrosion resistance, chemical resistance, abrasion resistance, heat resistance, hardness, moisture and gas barrier properties, and are utilized in such fields as structural materials, protective coating materials, abrasive materials and shielding films. Inorganic particles having such excellent physical properties are required to be applied to electric, electronic, information and energy materials, and active research for application is underway.

In addition to the expensive high temperature process and dry process, the inorganic particles are difficult to produce thick film due to the brittleness of the material itself and there are many limitations in applying a simple wet process.

In order to overcome these limitations, researches on colloidal inorganic particles capable of wet processing without decreasing the existing properties of inorganic particles and dispersion studies for application of inorganic particles to wet materials have been conducted. Conventional inorganic particles are generally used as structural materials, and they can be mixed with a polymer resin such as an organic binder to form a hybrid material, followed by wet coating to improve the mechanical, thermal, and chemical properties of the inorganic material.

The prior art for manufacturing such inorganic particles is disclosed in Korean Patent Application Laid-Open No. 10-2009-0120257, a method of producing a hybrid inorganic insulating film, a hybrid wet insulating film produced thereby, No. 10-2012-0118876 discloses a method for manufacturing a hybrid organic / inorganic hybrid material capable of controlling the refractive index through controlling the particle size of silica nanosol, and Korean Patent Registration No. 10-1269138 Hybrid Packaging Manufacturing Method .

The above-mentioned prior arts are non-crystalline inorganic particles having insufficient crystallinity and related densities of inorganic particles, and they are difficult to have a dense structure because their particle sizes are the same or similar to each other. Therefore, the particle size of inorganic particles having high crystallinity and density is varied, and a hybrid material produced by dispersing these inorganic particles and having a high packing density is required.

Accordingly, an object of the present invention is to provide a process for producing inorganic particles having various particle sizes by controlling the size of the milling balls, milling time and stirring speed at the time of inorganic particle milling, treating the surface with functional organosilane, And to provide a method of manufacturing an inorganic particle dispersion hybrid material by controlling the particle size and the pulverization of the inorganic particles applied to the material.

The above-mentioned object is achieved by a method of manufacturing a semiconductor device, comprising: preparing inorganic particles; Primary, secondary and tertiary pulverization of the inorganic particles through milling balls having different sizes, respectively; Obtaining inorganic particles that have been pulverized to have different particle sizes, respectively; Treating the surface of the inorganic particles with an organosilane; Separating and drying the silane-treated inorganic particles; And a step of mixing the inorganic particles having different sizes to prepare a hybrid material, wherein the inorganic particles are dispersed in the inorganic particles.

Wherein the inorganic particles are at least one of silica, alumina, zirconia, and titania, and the milling balls are zirconia balls, and each of the inorganic particles in the first, second and third milling steps It is preferable to use a milling ball having a size of 1.0, 0.3 or 0.1 mm.

The primary, secondary and tertiary pulverization steps are performed in a solvent, and the solvent is water, distilled water, methanol, ethanol, propanol, isopropanol, butanol, ), Toluene, acetone, methyl ethyl ketone, methyl cellosolve, ethyl cellosolve, butyl cellosolve, tetrahydrofuran, Wherein the step of treating the surface of the inorganic particles with the organosilane is carried out by an atmospheric pressure atmospheric pressure stirring reaction or a reflux reaction (hereinafter referred to as " reflux reaction " desirable.

The organosilane may be at least one selected from the group consisting of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, i-propyltrimethoxysilane, Propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethyl Vinyltrimethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-hexyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, - chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3, -trifluoropropyltriethoxysilane. 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2- 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-hydroxypropyltrimethoxysilane, 3- 3-isocyanatopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4-epoxycyclohexyl) ethyl (Meth) acryloxypropyltrimethoxysilane, 3- (meth) acryloxypropyltriethoxysilane, 3- (meth) acryloxypropyltrimethoxysilane, 3- Ureidopropyltrimethoxysilane, 3-ureidopropyltriethoxysilane And a mixture thereof, and at least one member selected from the group consisting of dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di- Di-n-propyldimethoxysilane, di-n-butyldimethoxysilane, di-n-butyldimethoxysilane, di-n-pentyldimethoxysilane, di- Di-n-hexyldimethoxysilane, di-n-hexyldiethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di- di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane, and mixtures thereof. And a mixture thereof.

The inorganic particles pulverized so as to have different particle sizes respectively have a size of 90 to 110 nm, 250 to 350 nm and 700 to 900 nm, respectively, or the inorganic particles pulverized so as to have different particle sizes, respectively, are 40 to 60 nm, 90 to 110 nm And a size of 200 to 400 nm.

According to the structure of the present invention described above, it is possible to obtain a hybrid material having a high packing density through inorganic particles having different particle sizes so as to have a crystallized or dense structure. The electrical properties, mechanical properties and chemical And the durability is improved.

1 is a flow chart of a method for manufacturing an inorganic particle dispersion hybrid material through pulverization and particle size control of inorganic particles according to an embodiment of the present invention.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a method for producing an inorganic particle dispersion hybrid material through pulverization and particle size control of inorganic particles according to an embodiment of the present invention will be described in detail with reference to the drawings.

First, as shown in FIG. 1, inorganic particles are prepared (S1).

The inorganic particles prepare inorganic crystalline silica particles having a size of several to several tens of micrometers. The inorganic silica particles have a size of 20 to 30 micrometers and are directly re-collected from the mine or used as particles obtained by purifying the re-collected particles. In some cases, the inorganic particles may be selected from the group consisting of alumina, zirconia, and titania.

The inorganic particles are pulverized (S2).

The inorganic silica particles prepared in the step S1 are first crushed using a nano milling mill. The primary grinding is carried out using zirconia balls having a size of 1 mm. At this time, the stirring speed is 2000 to 4000 rpm, and the pulverization time is controlled in a unit of time for 2 to 6 hours and is performed in a solvent. The inorganic silica particles to be ground and the zirconia balls are used at a weight ratio of inorganic particles: zirconia balls = 1: 5, and the applied solvent is mixed by mixing the inorganic particles and the balls: solvent at a weight ratio of 1: 1. In this case, it is preferable to use water or distilled water as the solvent. In addition, methanol, ethanol, propanol, isopropanol, butanol, toluene, acetone, Methyl ethyl ketone, Methyl cellosolve, Ethyl cellosolve, Butyl cellosolve, Tetrahydrofuran (THF) and Tetrahydropyran (Tetrahydropyran) , THP), or a solvent in which these are mixed.

In order to minimize the agglomeration between the pulverized inorganic silica particles and the efficient pulverization, an aqueous dispersing agent considering the pH of the particles is added to the particles at a weight ratio of 2 and the pulverization proceeds.

The inorganic silica particles prepared in the step S1 are secondarily pulverized using a zirconia ball smaller in size than the first size. At this time, the size of the zirconia balls is 0.3 mm and the agitation speed is 3000 to 5000 rpm so that the agitation speed is higher than that of the first mill. The pulverization time is controlled in units of one hour for 2 to 6 hours and pulverization is carried out under a solvent. The inorganic silica particles and zirconia balls used in the pulverization are used in an inorganic particle: zirconia ball = 1: 5 weight ratio, and the applied solvent is mixed with water or distilled water at an inorganic particle and a ball: solvent ratio of 1: 1.25, .

In order to minimize the agglomeration between the inorganic silica particles and the efficient pulverization, an aqueous dispersing agent considering the pH of the particles is added at a ratio of 3 parts by weight to the particles to carry out the pulverization.

The inorganic silica particles prepared in the step S1 are thirdly pulverized using a zirconia ball having a size smaller than the second size. At this time, the size of the zirconia balls is 0.1 mm, the agitation speed is 3,000 to 5,000 rpm, and the milling time is 2 to 6 hours. The inorganic silica particles and the zirconia balls used in the pulverization are used in an inorganic particle: zirconia ball = 1: 5 weight ratio, and the applied solvent is mixed with water or distilled water at an inorganic particle and a ball: solvent ratio of 1: 1.5, .

In order to minimize the agglomeration between the pulverized inorganic silica particles and the efficient pulverization, an aqueous dispersing agent considering the pH of the particles is added at a ratio of 5 parts by weight to the particles to carry out the pulverization.

To obtain pulverized inorganic particles (S3).

Through the stepwise grinding process as in the step S2, inorganic silica particles having a particle size of 800 nanometers to 1 micrometer can be obtained in the primary grinding, and the initial one to two hours according to the grinding time can be controlled But as the time increases under the same conditions, the wear of the surface proceeds rather than the control of the particle size.

As in the case of the first grinding, it was confirmed that the second and third grinding also had a larger size reduction ratio than the particle size control according to the grinding time. In the same step, the grinding time increased, Is changed to a more spherical shape. In the second milling, inorganic silica particles having a particle size of 300 to 500 nanometers can be obtained, and in the third milling, inorganic silica particles having a particle size of 50 to 150 nanometers can be obtained.

The surface of the inorganic particles is subjected to silane treatment (S4).

The surface of the inorganic silica particles having different particle sizes obtained through the step S3 is subjected to a silane treatment. The inorganic silica particles are dried in a vacuum oven by size, dispersed in toluene, and subjected to first and second silane treatment using methyltrimethoxysilane and aminopropylmethoxysilane, which are organic silanes. It is preferable that the solvent is any one of tetrahydrofuran and tetrahydropyran in addition to toluene. The silane treatment reaction is carried out at 20 to 50 캜 for 24 hours through the Reflux method. Here, the ratio of the inorganic silica particles, the silane and the solvent was in a weight ratio of particle: silane: solvent = 1: 0.3: 4. In the ratio of the silane ratio of 0.3, 0.15 was methyltrimethoxysilane, Lt; / RTI >

In addition to methyltrimethoxysilane and aminopropyltrimethoxysilane, the organosilane may be a silane compound such as methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane i-propyltrimethoxysilane, i-propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n Cyclohexyltrimethoxysilane, phenyltrimethoxysilane, phenyltrimethoxysilane, phenyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3, -trifluoropropyltriethoxy Silane. 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2- 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-hydroxypropyltrimethoxysilane, 3- 3-isocyanatopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4-epoxycyclohexyl) ethyl (Meth) acryloxypropyltrimethoxysilane, 3- (meth) acryloxypropyltriethoxysilane, 3- (meth) acryloxypropyltrimethoxysilane, 3- Ureidopropyltrimethoxysilane, 3-ureidopropyltriethoxysilane And a mixture thereof, and at least one member selected from the group consisting of dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di- Di-n-propyldimethoxysilane, di-n-butyldimethoxysilane, di-n-butyldimethoxysilane, di-n-pentyldimethoxysilane, di- Di-n-hexyldimethoxysilane, di-n-hexyldiethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di- di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane, and mixtures thereof. And a mixture thereof.

The silane-treated inorganic particles are separated and dried (S5).

The inorganic silica particles having different sizes each of which the organosilane has been surface-treated are washed and centrifuged to obtain only the pure inorganic silica particles treated with the organosilane and dried. In order to solve the problem of aggregation among the particles during the drying process, the particles are finely ground in a mortar and then mixed at a constant weight ratio in order to maximize the filling efficiency by the particle size obtained by the pulverization step.

And a hybrid material is manufactured (S6).

The inorganic silica particles having different mixed particle sizes are efficiently mixed according to the filling efficiency of each size. Efficient homogeneously mixed crystalline inorganic silica particles are mixed again with an epoxy system to form a hybrid material. The epoxy system is composed of bisphenol A epoxy resin, a carboxylic anhydride curing agent, a polyglycol as a flow agent, and a curing catalyst, Tertiary amine, in a ratio of 100: 95: 15 : 0.2 weight ratio.

Hereinafter, data on the physical properties of the hybrid material prepared through steps S1 to S6 are shown. The surface-treated inorganic silica particles having different particle sizes prepared through the above processes were mixed with each other at a weight ratio of 2: 3: 5 to the crystalline inorganic silica particles having a size of about 800 nanometers, 300 nanometers, and 100 nanometers The inorganic silica particles are blended in an amount of 10 to 40 parts by weight per 100 parts by weight of the epoxy system to prepare a hybrid material. The hybrid material is immersed in a sample holder having a certain ratio of length / length / height according to the standard so as to measure the tensile strength, flexural strength and impact strength, and then cured at 80 ° C for 6 hours. Then, the conditions were changed to 130 DEG C for 10 hours to cure, and finally a molded sample was obtained. Tensile strength, flexural strength and impact strength were measured at room temperature using the obtained samples.

Table 1 below shows the results depending on the presence or absence of the inorganic silica particles having different particle sizes.

Samples made with silica-free epoxy systems Samples mixed with silica particles having different surface-treated particle sizes
(Ratio based on crystalline inorganic silica particle size
800 nm: 300 nm: 100 nm = 2: 3: 5) Tensile Strength (MPa) 75 ~ 85 87.5 to 97.5 Flexural Strength (MPa) 130 ~ 140 145-155 Impact strength (kJ / m 2) 11-13 15 ~ 18

As shown in Table 1, by increasing the chemical crosslinking through the surface treatment of the inorganic silica particles and mixing the inorganic silica particles having different particle sizes to increase the filling efficiency, the tensile strength, the bending strength and the impact strength are increased as compared with the epoxy system alone . Through the hydrophobic treatment of the surface of the inorganic silica particles and the subsequent functionalization of the functional groups capable of chemical cross-linking with the epoxy system without solvent, the efficiency of mixing and molding can be improved by increasing the filling efficiency of particles of different sizes, It can be confirmed that

 The inorganic silica particles obtained by mixing the particles of the surface-treated inorganic silica particles having different particle sizes of 300 nm, 100 nm and 50 nm in a weight ratio of 2: 3: 5 prepared through steps S1 to S6 were dissolved in methyl ethyl ketone (Methyl ethyl ketone) solvent. The epoxy-urethane-silica hybrid material was prepared by mixing 10 to 50 parts by weight of an epoxy-urethane copolymerized binder epoxy system dissolved in 40 parts by weight of solid particles after redispersing the inorganic silica particles: solvent = 15: 85 weight ratio. These hybrid materials were spin-coated on a glass substrate at 1000 rpm for 30 seconds, cured at 150 ° C for 30 minutes, and samples were then obtained through a cured film having a thickness of about 10 μm. The obtained samples were used to measure the pencil hardness and adhesion of the film at room temperature.

Table 2 below shows the physical properties according to the content of the inorganic silica particles (300 nm: 100 nm: 50 nm = 2: 3: 5) in which the crystalline silica particles having different particle sizes are mixed.

Mixed inorganic silica content 0 parts by weight 10 parts by weight 20 parts by weight 30 parts by weight 40 parts by weight 50 parts by weight Pencil hardness 2H 3H 4H 5H 6H 7H Adhesion 3B 3B 4B 5B 5B 5B

In Table 2, pencil hardness and adhesive strength were measured according to ASTM (American Society for Testing and Materials), and adhesive strength was measured using a tape test. As shown in Table 2, even though the content of the inorganic silica particles was increased by chemical crosslinking through hardening rather than simple mixing with the epoxy-urethane copolymerization epoxy system through the surface treatment of the silica, there was no decrease in the adhesive strength, And it increased with increasing contents.

The present invention produced mixed silica particles through efficient mixing of inorganic particles having different particle sizes prepared through pulverization of inorganic silica particles. Silane hydrophobization treatment of the prepared silica surface and solvent dispersion were followed to treat functional groups capable of chemical cross-linking with the epoxy-urethane copolymerization epoxy system. Through this, it was confirmed that not only the efficiency in mixing, dispersing, coating, molding and drying with the epoxy system was improved, but also the mechanical and chemical properties were improved by the high packing density.

Claims (8)

Disclosed is a method for producing an inorganic particle dispersed hybrid material by pulverizing inorganic particle and controlling particle size,
Preparing inorganic particles;
Primary, secondary and tertiary pulverization of the inorganic particles through milling balls having different sizes, respectively;
Obtaining inorganic particles that have been pulverized to have different particle sizes, respectively;
Treating the surface of the inorganic particles with an organosilane;
Separating and drying the silane-treated inorganic particles;
And a step of mixing the inorganic particles having different sizes to produce a hybrid material. The inorganic particle dispersion hybrid material is produced by pulverizing and controlling the particle size of the inorganic particles. The method according to claim 1,
Wherein the inorganic particles are at least one of silica, alumina, zirconia, and titania. The method for producing inorganic particles dispersed hybrid materials by pulverization and particle size control of inorganic particles . The method according to claim 1,
The milling ball is a zirconia ball,
A milling ball having a size of 1.0, 0.3, or 0.1 mm is used in each of the primary, secondary and tertiary pulverization steps, and a method for manufacturing inorganic particle dispersion hybrid material . The method according to claim 1,
The primary, secondary and tertiary pulverization steps are carried out under a solvent,
The solvent may be water, distilled water, methanol, ethanol, propanol, isopropanol, butanol, toluene, acetone, methyl ethyl ketone, At least one selected from the group consisting of methyl cellosolve, ethyl cellosolve, butyl cellosolve, tetrahydrofuran (THF) and tetrahydropyran (THP) Wherein the inorganic particles are dispersed in the dispersion medium. The method according to claim 1,
Wherein the step of treating the surface of the inorganic particles with organosilane comprises:
Wherein the inorganic particles are dispersed in an aqueous medium at room temperature under atmospheric pressure stirring or reflux reaction. 6. The method of claim 5,
The organosilane may be,
Methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, i-propyltrimethoxysilane, i- Propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethoxysilane, n- Trimethoxysilane, trimethoxysilane, trimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-chloropropyltrimethoxysilane , 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3, -trifluoropropyltriethoxysilane. 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2- 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-hydroxypropyltrimethoxysilane, 3- 3-isocyanatopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4-epoxycyclohexyl) ethyl (Meth) acryloxypropyltrimethoxysilane, 3- (meth) acryloxypropyltriethoxysilane, 3- (meth) acryloxypropyltrimethoxysilane, 3- Ureidopropyltrimethoxysilane, 3-ureidopropyltriethoxysilane And a mixture thereof, and at least one member selected from the group consisting of dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di- Di-n-propyldimethoxysilane, di-n-butyldimethoxysilane, di-n-butyldimethoxysilane, di-n-pentyldimethoxysilane, di- Di-n-hexyldimethoxysilane, di-n-hexyldiethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di- di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane, and mixtures thereof. Wherein the inorganic particles are one selected from the group consisting of the inorganic particles and the mixture thereof. A method for producing a hybrid inorganic particle dispersion material. The method according to claim 1,
Wherein the inorganic particles that have been pulverized so as to have different particle sizes have a size of 90 to 110 nm, 250 to 350 nm, and 700 to 900 nm, respectively, and a method for producing inorganic particle dispersion hybrid material . The method according to claim 1,
Characterized in that the inorganic particles pulverized so as to have different particle sizes each have a size of 40 to 60 nm, 90 to 110 nm and 200 to 400 nm, respectively, and a method for producing an inorganic particle dispersion hybrid material .

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