WO2018110904A2 - Particule inorganique de structure cœur-coque, son procédé de préparation et film optique la contenant - Google Patents

Particule inorganique de structure cœur-coque, son procédé de préparation et film optique la contenant Download PDF

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WO2018110904A2
WO2018110904A2 PCT/KR2017/014347 KR2017014347W WO2018110904A2 WO 2018110904 A2 WO2018110904 A2 WO 2018110904A2 KR 2017014347 W KR2017014347 W KR 2017014347W WO 2018110904 A2 WO2018110904 A2 WO 2018110904A2
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parts
weight
inorganic particles
core
formula
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PCT/KR2017/014347
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English (en)
Korean (ko)
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WO2018110904A3 (fr
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황웅린
김규민
남성희
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주식회사 창강화학
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Publication of WO2018110904A2 publication Critical patent/WO2018110904A2/fr
Publication of WO2018110904A3 publication Critical patent/WO2018110904A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14—Protective coatings, e.g. hard coatings
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
    • G02B5/021—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures
    • G02B5/0226—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place at the element's surface, e.g. by means of surface roughening or microprismatic structures having particles on the surface
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/02—Diffusing elements; Afocal elements
    • G02B5/0268—Diffusing elements; Afocal elements characterized by the fabrication or manufacturing method
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

Definitions

  • the present invention relates to an inorganic particle having a core shell structure, a manufacturing method thereof, and an optical film including the inorganic particle.
  • Optical sheets used in liquid crystals of liquid crystal displays focus on diffuser plates, diffuser films, and light spreading to the outside to scatter light to make light brightness uniform, thereby improving luminance at the front of the panel.
  • the diffusion film diffuses the light emitted through the upper surface of the light guide plate to uniform the luminance and widen the viewing angle.
  • the light passing through the diffusion film has a problem that the front emission luminance is lowered.
  • the apparatus included in the liquid crystal in order to increase the luminance dropped by the diffusion film is a prism sheet.
  • Thermoplastic acrylic resins which are conventionally used as transparent materials for prism sheets, have high light transmittance, excellent optical properties, molding processability, high surface hardness, and mechanical strength, and thus are widely used in various industrial products and optical devices including automobiles and home appliances.
  • the refractive index of the resin used in the prism sheet should be high, excellent in transparency and low in color coordinates.
  • general high-refractive acrylic resin not only shows yellow color but also accelerates yellowing with UV exposure, so the color coordinates increase, so transparency is low, mechanical strength is low, scratch resistance is weak, and price is high. have.
  • An object of the present invention is to provide a material which is excellent in brightness and refractive index, yellowing is suppressed and solution stability is excellent.
  • Another object of the present invention to provide a method for producing the material.
  • Still another object of the present invention is to provide a high refractive optical film including the material.
  • An inorganic particle surrounding the core and including a shell containing at least one lanthanide element is provided.
  • It provides a method for producing an inorganic particle comprising the step of performing a high pressure reaction of the mixture to produce an inorganic particle having a structure surrounded by a lanthanide element on the surface of the particle containing zirconium (Zr) and aluminum (Al).
  • the shell provides a surface-treated inorganic particles, characterized in that the surface is treated with a compound represented by the formula (1) and (2):
  • R 1 is hydrogen, an alkyl group having 1 to 20 carbon atoms, or (n is any number selected from 1 to 100),
  • R 2 is an alkyl group having 1 to 20 carbon atoms
  • the alkyl group is unsubstituted or substituted with a carboxyl group, an aryl group having 6 to 20 carbon atoms, or an aryloxy group.
  • the present invention provides an optical film including the surface treated inorganic particles.
  • the inorganic particles of the core shell structure according to the present invention may exhibit a high refractive index and transmittance by having a structure in which a shell containing a lanthanide element surrounds a core containing zirconium (Zr) and aluminum (Al).
  • the particles surface-treated the inorganic particles are excellent in compatibility with the acrylic resin is not only high solution stability but also excellent effect of suppressing the yellowing of the acrylic resin can be usefully used in optical films such as prism sheet.
  • 1 is a perspective view schematically showing the shape of a prism sheet.
  • the present invention relates to an inorganic particle having a core shell structure, a manufacturing method thereof, and an optical film including the inorganic particle.
  • Optical sheets used in liquid crystals of liquid crystal displays focus on diffuser plates, diffuser films, and light spreading to the outside to scatter light to make light uniform, thereby improving luminance at the front of the panel.
  • the diffusion film diffuses the light emitted through the upper surface of the light guide plate to uniform the luminance and widen the viewing angle.
  • the light passing through the diffusion film has a problem that the front emission luminance is lowered.
  • the apparatus included in the liquid crystal in order to increase the luminance dropped by the diffusion film is a prism sheet.
  • Thermoplastic acrylic resin which is conventionally used as a transparent material of prism sheet, has high light transmittance, excellent optical properties, molding processability, high surface hardness, and mechanical strength, and is widely used in various industrial products and optical devices including automobiles and home appliances. have.
  • the acrylic resin is exposed to light including ultraviolet rays, yellowing may occur, thereby causing a problem in that transparency is lowered.
  • a method of adding an ultraviolet absorber is known, but in some cases, due to the absorbent added to the acrylic resin, the brightness of the prism sheet is reduced, or the solution stability is low, so that the absorbent is precipitated in the reliability test. There is a limit that causes a defect.
  • the inorganic particles of the core shell structure according to the present invention may exhibit a high refractive index and transmittance by having a structure in which a shell containing a lanthanide element surrounds a core containing zirconium (Zr) and aluminum (Al).
  • the particles surface-treated the inorganic particles are excellent in compatibility with the acrylic resin is not only high solution stability but also excellent effect of suppressing the yellowing of the acrylic resin can be usefully used in optical films such as prism sheet.
  • the present invention provides an inorganic particle of the core shell structure in one embodiment.
  • the inorganic particles according to the present invention includes a core containing zirconium (Zr) and aluminum (Al); And a shell surrounding the core and containing at least one lanthanide element.
  • the core contains zirconium (Zr) as a main component
  • the zirconium (Zr) may be included without particular limitation on the form.
  • the zirconium (Zr) may be present in the core as zirconium (Zr) as a metal or in the form of zirconia (ZrO 2 ) as an oxide.
  • a main component means 80 wt% or more, 90 wt% or more, 95 wt% or more, 96 wt% or more, 97 wt% or more, 98 wt% or more, 99 wt% or more, based on the total weight of the substrate 100 wt%, 95 to 99 wt%, 96 to 99 wt%, or 97 to 100 wt%.
  • the core may include 98 ⁇ 1% by weight of zirconia and 2 ⁇ 1% by weight of aluminum based on 100 parts by weight of the total.
  • the core has a composition containing aluminum (Al) together with zirconium (Zr) as a main component can not only reduce the manufacturing cost of the inorganic particles compared to the case containing zirconium (Zr) alone, but also zirconium ( The light transmittance and luminance of the core itself containing Zr) can be easily controlled.
  • the content of aluminum (Al) may be 0.1 parts by weight to 30 parts by weight, specifically 0.1 parts by weight to 20 parts by weight, 0.1 parts by weight to 15 parts by weight based on 100 parts by weight of zirconium (Zr) contained in the core.
  • the present invention can not only improve the processability of the inorganic particles by adjusting the content of aluminum (Al) in the above range, but can also simultaneously improve the light transmittance and luminance of the film including the same.
  • the core may further include chromium (Cr) together with zirconium (Zr) and aluminum (Al), the content of which is 0.01 parts by weight to 10 parts by weight, specifically, 100 parts by weight of zirconium (Zr). 0.01 to 8 parts by weight, 0.01 to 5 parts by weight, 0.01 to 1 parts by weight, 3 to 7 parts by weight 5 to 10 parts by weight or 4 to 6 parts by weight.
  • the present invention can further suppress the yellowing due to ultraviolet rays without generating a decrease in the properties of the inorganic particles by further including the chromium in the content range in the core.
  • the shell includes a lanthanide element, and the type thereof may be applied without particular limitation as long as it improves optical properties of the core.
  • the shell may contain lanthanum (La), cerium (Ce), ruthelium (Lu), or the like, and specifically, lanthanum (La).
  • the lanthanide element is not particularly limited in form, but may preferably have an oxide form.
  • the lanthanide element may be lanthanide (La 2 O 3 ).
  • the content of the lanthanide element may be 0.1 part by weight to 20 parts by weight with respect to 100 parts by weight of the core, and specifically 0.1 part by weight to 15 parts by weight, 0.1 to 10 parts by weight, 0.1 to 5 parts by weight, and 1 weight by weight. And 5 parts by weight, 5 parts by weight to 10 parts by weight, 5 parts by weight to 15 parts by weight, 15 parts by weight, 15 parts by weight, 10 parts by weight to 20 parts by weight, or 15 parts by weight to 20 parts by weight.
  • the inorganic particles according to the present invention may have an average particle size of 1 nm to 100 nm, more specifically 1 nm to 100 nm, 5 nm to 80 nm, 5 nm to 60 nm, 10 nm to 40 nm, 10 Nm to 25 nm, 14 nm to 35 nm, 19 nm to 25 nm or 25 nm to 35 nm.
  • Inorganic particles of the core-shell structure according to the present invention may have the above configuration to improve the refractive index and the brightness of the optical film including the same.
  • the inorganic particle having a shell containing the lanthanide element is composed of an inorganic particle composed only of a core and In contrast, it may have a higher refractive index.
  • the inorganic particles may include a shell containing a lanthanide element, thereby improving yellowing when surface-treated with an organic compound, thereby exhibiting low color coordinates.
  • the raw material price is economical compared to the particles consisting of lanthanide (La 2 O 3 ), which can increase the price competitiveness of the product have.
  • the present invention provides a method for producing an inorganic particle of the core shell structure in one embodiment.
  • obtaining a mixture containing a lanthanide element precursor is a step of preparing a mixture by mixing particles containing zirconium (Zr) and aluminum (Al) and a lanthanide element precursor solution.
  • the lanthanide element precursor is not particularly limited as long as it contains a lanthanide element.
  • acetic acid in which the lanthanide element is dissolved may be used as a precursor of the lanthanide element.
  • acetic acid in which lanthanum (La) is dissolved may be used as a precursor of the lanthanide element.
  • the particles containing zirconium (Zr) and aluminum (Al) are not particularly limited as long as the particles contain zirconium (Zr) and aluminum (Al).
  • the particles containing zirconium (Zr) and aluminum (Al) can be prepared by performing the following steps:
  • a zirconium (Zr) precursor and an aluminum precursor are mixed with a stirrer, and the mixture prepared using a high pressure reactor is subjected to a high pressure reaction at 200 ⁇ 100 ° C. and 30 ⁇ 1 atm, and then 1,000 to 1,000 using a bead mill. Can be obtained by milling at a speed of 1,500 rpm.
  • zirconium precursor and the aluminum precursor may be commercially available to those skilled in the art, and examples thereof include zirconium precursors such as zirconium acetate (ZrO (CH 3 COO) 2 ) or aluminum isopropoxide (Al (Oi-Pr)).
  • zirconium precursors such as zirconium acetate (ZrO (CH 3 COO) 2 ) or aluminum isopropoxide (Al (Oi-Pr)).
  • Aluminum precursors, such as 3 ) are mentioned.
  • the mixture including the zirconium precursor and the aluminum precursor may optionally further include a chromium precursor by further mixing the chromium precursor when mixing the zirconium precursor and the aluminum precursor.
  • the average size of the particles containing zirconium (Zr) and aluminum (Al) may be 1 nm to 20 nm.
  • the average size of the particles containing a particular zirconium (Zr) and aluminum (Al) may be 1 to nm 15nm, 2nm to 12nm or 2nm to 1 0 nm. Since the particles containing zirconium (Zr) and aluminum (Al) in the present invention form the core of the inorganic particles according to the present invention, the average size of the particles containing zirconium (Zr) and aluminum (Al) is adjusted to the above range. In this way, the average particle size of the inorganic particles can be controlled to a nanometer level within a specific range.
  • the present invention provides a particle containing zirconium (Zr) and aluminum (Al) by the method described above. Since drying and dispersing steps can be omitted, workability is improved and economics due to process simplification are improved.
  • the step of preparing the inorganic particles is a step of forming a shell on the surface of the particles containing zirconium (Zr) and aluminum (Al) contained in the mixture by performing a reaction at a high pressure of 1 atm or more at normal pressure,
  • the steps include 1) conducting the mixture at a high pressure of at least 1 atm at atmospheric pressure and 2) milling the mixture subjected to the high pressure reaction to induce chemical reaction and dispersing action.
  • the pressure of the high-pressure reaction is not particularly limited as long as the pressure is higher than the atmospheric pressure of 1 atm, specifically, 1 atm to 50 atm, 5 atm to 50 atm, 10 atm to 40 atm, 20 atm to 40 atm, and 30 atm. To 45 atm, 25 atm to 35 atm, or 28 atm to 32 atm.
  • the milling is a milling method commonly used in the art to mix the particles containing zirconium (Zr) and aluminum (Al) and the lanthanide element precursor solution as well as to induce chemical reaction and dispersion thereof. It can be applied without limitation. Specifically, the milling may be a milling method that is performed using a bead mill device.
  • the milling may be performed at a speed of 500 rpm to 2,000 rpm, and specifically, may be performed at a speed of 1,000 rpm to 2,000 rpm, 1,000 rpm to 1,500 rpm, or 1,200 rpm to 1,400 rpm.
  • the method for producing an inorganic particle having a core shell structure is a bead mill apparatus in which a mixture of zirconium (Zr) and aluminum (Al) -containing particles and an acetic acid solution in which lanthanum (La) is dissolved is mixed. After injecting into a milling for 3 ⁇ 1 hours at a speed of 1300 ⁇ 100 rpm at 70 ⁇ 5 °C, the milled mixture was subjected to a high pressure reaction at 30 ⁇ 1 atm and then the solvent was removed to remove inorganic particles of the core shell structure It can manufacture.
  • Zr zirconium
  • Al aluminum
  • La acetic acid solution in which lanthanum
  • R 1 is hydrogen, an alkyl group having 1 to 20 carbon atoms, or (n is any number selected from 1 to 100),
  • R 2 is an alkyl group having 1 to 20 carbon atoms
  • the alkyl group is unsubstituted or substituted with a carboxyl group, an aryl group having 6 to 20 carbon atoms, or an aryloxy group.
  • R 1 is hydrogen, an alkyl group having 1 to 4 carbon atoms, or (n is any number selected from 1 to 50),
  • R 2 is an alkyl group having 1 to 10 carbon atoms
  • the alkyl group may be unsubstituted or substituted with a carboxyl group, phenyl group, naphthyl group, anthracenyl group, benzyloxy group, biphenyloxy group or naphthyloxy group.
  • the compound represented by Formula 1 may be at least one compound selected from the group consisting of Formula 1a to Formula 1d:
  • m is any number selected from 1 to 10.
  • Surface-treated inorganic particles according to the present invention by surface treatment of the surface of the inorganic particles having a core shell structure with any one or more of the compounds represented by the formula (1) and 2 to improve the compatibility with the acrylic resin to improve the solution stability of the inorganic particles
  • the yellowing phenomenon of the acrylic resin is improved, when the surface-treated inorganic particles are used in the prism sheet, low color coordinates may be exhibited.
  • the content of the compounds represented by Formulas 1 and 2 may be appropriately adjusted in a range that does not lower the light transmittance and brightness of the surface-treated inorganic particles.
  • the content of the compounds represented by Formulas 1 and 2 may be 10 to 40 parts by weight based on 100 parts by weight of the inorganic particles of the core shell structure which is not surface treated, and more specifically 100 parts by weight of the inorganic particles of the core shell structure. 10 to 20 parts by weight, 15 to 30 parts by weight, 20 to 40 parts by weight, 25 to 40 parts by weight, 30 to 35 parts by weight, or 31 to 33 parts by weight.
  • the present invention provides a method for producing the surface-treated inorganic particles in one embodiment.
  • the manufacturing method includes the step of modifying the shell surface of the inorganic particles by reacting any one or more of the compounds represented by Formula 1 and 2 with the inorganic particles of the core shell structure according to the present invention.
  • Method for producing a surface-treated inorganic particles according to the present invention by reacting a mixture containing inorganic particles of the core shell structure and any one or more of the compounds represented by Formula 1 and 2 at 40 to 60 °C for 30 minutes to 200 minutes
  • the surface of the inorganic particles is first modified, the first surface-treated inorganic particles are remixed with any one or more of the compounds represented by the formulas (1) and (2) and reacted at 40 to 80 ° C. for 2 to 4 hours to perform the second surface treatment. It may include the step.
  • the compounds represented by Formulas 1 and 2 may have a different structure from the compound reacted with the core shell inorganic particles during the primary surface treatment.
  • the surface treated inorganic particles may be first surface treated with 2-carboxyl acrylate and / or acrylic acid, and o-phenylphenol ethoxy acrylate ( Secondary surface treatment can be with o-phenylphenol ethoxy acrylate, OPPEA, butyl acrylate (BA) and / or benzyl acrylate (BZ).
  • the present invention provides an optical film including the surface treated inorganic particles.
  • the optical film according to the present invention may not only be excellent in light transmittance and brightness of the film including the surface treated inorganic particles, but also may be usefully used as an optical sheet requiring high light transmittance and brightness because the color coordinate of the optical film is low. .
  • the optical film is included in the optical sheet, and may be used as one or more optical layers formed with a micro-pattern, the optical layer is a variety of structures such as the cross-sectional shape of the triangle is repeated according to the shape of the frame (frame) to be molded It may have a form.
  • the micro pattern may be a prism pattern
  • the optical sheet may be a prism sheet.
  • the optical film according to the present invention may further include a curable resin together with the surface-treated inorganic particles, the process of manufacturing the optical film and the optical properties of the optical film produced according to the type of the curable resin can be controlled. have.
  • curable resins examples include 2-phenoxyethyl acrylate, benzyl acrylate, o-phenoxyphenyl ethoxy acrylate, bisphenol epoxy acrylate, florene diacrylate or urethane acrylate, and the like. Each may be used alone or in combination of two or more.
  • the optical film according to the present invention when used as a prism sheet, the optical film may have a structure formulated into a prism sheet itself.
  • the optical film according to the present invention may be a structure that forms a pattern in which a triangular prism shape including a valley and a peak of a hill shape is used when used as a prism sheet.
  • a pattern in which the triangular prism shape is repeated at least one of the valleys and the peaks of the mountain shape may have a structure formed in a round shape.
  • FIG. 1 is a perspective view schematically showing the shape of an optical film (hereinafter, referred to as a 'prism sheet') when using an optical film as a prism sheet.
  • a 'prism sheet' an optical film
  • the prism sheet 100 includes a base film 110 and a pattern portion 120 disposed on the base film 110.
  • the pattern unit 120 includes a plurality of triangular prisms 130 arranged in a pattern structure in which a valley and a peak of a mountain form are repeated.
  • the vertex of each of the triangular prisms 130 is a line formed by crossing two inclined surfaces, and the cross-sectional shape may be defined as a point.
  • the pitch interval between the triangular prism 130 adjacent to each other is 9 ⁇ m to 25 ⁇ m
  • the thickness of the pattern portion 120 may be in the range of 18 ⁇ m to 50 ⁇ m.
  • each of the triangular prisms 130 may have a round shape, which will be described with reference to FIG. 2.
  • FIG. 2 is a schematic diagram of a triangular prism in which the stem part is round;
  • the vertex of the triangular prism 130 may have a round shape.
  • the effect may vary depending on the height at which the round shape of the stem is formed. That is, the first height H from the bottom of the triangular prism 130 to the virtual vertex 140 and the top of the mountain are rounded at the bottom of the triangular prism 130 having the rounded shape.
  • Luminance and luminance uniformity effects may vary according to the ratio h / H of the second height h to.
  • the shape of the prism sheet in the present invention is not particularly limited and may be applied to a prism sheet that has been altered, replaced or improved without departing from the ordinary knowledge in the art.
  • the prism sheet can be applied to various optical devices.
  • it may be applied to a back light unit (BLU) of an optical device.
  • BLU back light unit
  • Zirconium acetate (ZrO (CH 3 COO) 2 ) solution 500 g, containing 30% by weight of zirconium oxide (ZrO 2 )
  • a zirconium (Zr) precursor aluminum isopropoxide, Al (Oi -Pr) 3 ) and chromium precursor chromium acetate hydrate (Cr 2 (OAc) 2 (H 2 O) 2
  • Table 1 below, and 12 ⁇ 0.2 hours at a speed of 500 ⁇ 20 rpm using a stirrer. Was stirred. At this time, it was confirmed whether the aluminum precursor was completely dissolved.
  • the stirred precursor mixture was subjected to a first high pressure reaction at 230 ⁇ 2 ° C. and 30 ⁇ 0.5 atm for 3 ⁇ 0.2 hours. Car milling was performed.
  • Example 1 98.5 wt% 1.5 wt% - 0.3 wt%
  • Example 2 98.5 wt% 1.5 wt% - 0.5 wt%
  • Example 3 98.5 wt% 1.5 wt% 0.1 wt% 0.3 wt%
  • the particle size of the inorganic particles prepared in Example 1 was measured twice using a particle size analyzer (model name: ELSZ-1000, manufacturer: Otsuka Electronics), and the average particle size was derived from the measured values. As a result, the particle size of the inorganic particles prepared in Example 1 was found to be 1 nm to 100 nm, specifically 14 nm to 35 nm, and more specifically 10 nm to 25 nm. In addition, the average particle size of the inorganic particles was 29 ⁇ 0.5 nm in the first measurement and 18 ⁇ 0.5 nm in the second measurement, the particle size distribution is 90% or more (about 75.6 ⁇ ⁇ ) particles having an average particle size of 10 nm to 40 nm 0.5%).
  • the inorganic particles of the core shell structures prepared in Examples 1 to 3 were added to 27 ⁇ 0.5 parts by weight based on the weight of ethanol (100 parts by weight), and 2-carboxyethyl acrylate (2- carboxylethyl acrylate, 8.1 ⁇ 0.1 parts by weight), acrylic acid (acrylic acid, 10.8 ⁇ 0.1 parts by weight) and dispersant (trade name: BYK-110, BYK, 2.7 ⁇ 0.05 parts by weight) and then 90 ⁇ at 50 ⁇ 2 °C The reaction was carried out for 5 minutes to prepare an inorganic particle primary surface treated with an acrylic compound.
  • O-phenylphenol ethoxy acrylate (o-phenylphenol ethoxy acrylate, OPPEA, 11.1 parts by weight), butyl acrylate (butyl acrylate, BA, 1.37) in the solution containing the primary modified inorganic particles (100 parts by weight) Parts by weight) and benzyl acrylate (benzyl acrylate, BZ, 1.37 parts by weight) were added, and the reaction was carried out while raising the reaction temperature from 50 ⁇ 2 ° C. to 70 ⁇ 2 ° C. for 3 ⁇ 0.2 hours. Then, the solvent of the mixture was removed to prepare a secondary surface treated inorganic particles.
  • the particle size of the inorganic particles (Example 4) surface-treated with the inorganic particles prepared in Example 1 was measured twice, and the average particle size was measured from the measured values. Derived. As a result, the particle size of the inorganic particles was found to be 1nm to 150nm, specifically 10nm to 60nm, more specifically 15nm to 30nm.
  • the average particle size of the inorganic particles was 25.5 ⁇ 0.5 nm in the first measurement and 24 ⁇ 0.5 nm in the second measurement, the particle size distribution is 70% or more of the particles having an average particle size of 10 nm to 30 nm (about 72.3 ⁇ 0.5%).
  • Zirconium acetate (ZrO (CH 3 COO) 2 ) solution 500 g, containing 30% by weight of zirconium oxide (ZrO 2 )
  • ZrO (CH 3 COO) 2 zirconium oxide
  • Al (Oi -Pr) 3 aluminum isopropoxide
  • the mixture was milled for 3 ⁇ 0.2 hours at a speed of 1300 ⁇ 20 rpm in the presence of a methanol solvent using a bead mill to prepare inorganic particles.
  • Zirconium precursor Aluminum precursor Comparative Example 1 98.5 wt% 1.5 wt%
  • each of the surface treated inorganic particles, difunctional urethane acrylate (difunctional urethane acrylate), tetrafunctional urethane acrylate (tetrafunctional urethane acrylate) and diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide An additional solution consisting of diphenyl (2,4,6-trimethylbenxoyl) phosphine oxide (TPO) was mixed and stirred for 3 hours to prepare a coating composition.
  • the prepared coating composition was coated on a PET film and cured using a metal lamp, thereby obtaining prism sheets having a structure in which inorganic particles prepared in Examples 4 to 6 and Comparative Example 1 were dispersed.
  • the prepared prism sheets have a pitch between triangular prisms adjacent to each other about 21 ⁇ 2 ⁇ m, and the overall average thickness of the PET film including the prism sheet was adjusted to about 87.5 ⁇ 2 ⁇ m.
  • the prism sheet thus obtained was assembled to an optical module composed of a light source, a light guide plate, and a diffusion sheet, and then the luminance of the prism sheet manufactured using a display luminance meter (model name: BM7, manufacturer: Topcon Corporation) was measured.
  • a display luminance meter model name: BM7, manufacturer: Topcon Corporation
  • the luminance was measured as the luminance measured value of the prism sheet containing inorganic particles containing only zirconium as 100%, and the relative percentage of each prism sheet was measured, and the results are shown in Table 3 below.
  • the prism sheet including the inorganic particles according to the present invention has excellent luminance and refractive index of 120 to 130% and 1.64 or more, respectively.
  • a prism sheet having a structure in which inorganic particles prepared in Examples 4 to 6 and Comparative Example 1 were dispersed was prepared in the same manner as in Experimental Example 1. Then, prepare a laminate in which a 5.5 "BLU, a light guide plate / diffusion sheet is laminated, arrange each of the prepared prism sheets on both sides of the laminate, and keep the distance between the BLU and the luminance meter at 500 mm and display The color coordinates of the prism sheet were measured using a luminometer (model name: SR-3AR, manufacturer: TOPCPN).
  • the prism sheet measuring the color coordinates was placed in an accelerated weather resistance tester (model name: QUV / spray) and left to stand at 50 ⁇ 2 ° C. for 15 minutes.
  • the amount of coordinate change of the color coordinate y was derived. At this time, the coordinate change amount means that the higher the value is more susceptible to yellowing of the sheet, the measured results are shown in Table 4.
  • the prism sheet including the inorganic particles according to the present invention can be seen that the color coordinate is greatly improved so that the amount of change in the color coordinate y is less than 0.003, specifically, 0.0010 to 0.0026. These results indicate that the inorganic particles surface-treated according to the present invention has improved the yellowing phenomenon.

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  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

La présente invention concerne une particule inorganique ayant une structure cœur-coque, son procédé de préparation, et un film optique la contenant. La particule inorganique de structure cœur-coque selon la présente invention peut présenter un indice de réfraction élevé et une transmissivité élevée grâce à une structure dans laquelle un cœur comprenant du zirconium (Zr) et de l'aluminium (Al) est entouré d'une coque comprenant un élément des lanthanides. De plus, une particule résultant du traitement de surface de la particule inorganique selon l'invention manifeste une excellente compatibilité avec une résine acrylique, une excellente transmittance optique, et de faibles coordonnées de couleur et peut par conséquent être utile pour un film optique, tel qu'une feuille de prisme.
PCT/KR2017/014347 2016-12-14 2017-12-08 Particule inorganique de structure cœur-coque, son procédé de préparation et film optique la contenant WO2018110904A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020160170267A KR101929018B1 (ko) 2016-12-14 2016-12-14 코어쉘 구조의 무기입자, 이의 제조방법 및 이를 포함하는 광학필름
KR10-2016-0170267 2016-12-14

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WO2018110904A2 true WO2018110904A2 (fr) 2018-06-21
WO2018110904A3 WO2018110904A3 (fr) 2019-01-24

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5935889A (en) * 1996-10-04 1999-08-10 Abb Lummus Global Inc. Catalyst and method of preparation
JP2008289971A (ja) * 2007-05-23 2008-12-04 Toyota Motor Corp コアシェル構造体及びその製造方法並びに当該コアシェル構造体を含む排ガス浄化用触媒
CA2800142C (fr) * 2010-05-24 2018-06-05 Siluria Technologies, Inc. Catalyseurs nanofils
KR101189462B1 (ko) 2012-04-16 2012-10-12 엘지엠엠에이 주식회사 광학물성이 우수한 투명 폴리메틸(메타)아크릴레이트 수지 조성물
CN104364320B (zh) * 2012-06-11 2016-09-07 长康化工有限公司 有机-无机混合组合物、其制造方法、光学片及光学装置

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KR101929018B1 (ko) 2018-12-13
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