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WO2025178131A1 - Procédé de production de liquide de dispersion, liquide de dispersion, couche à faible indice de réfraction, élément optique, dispositif optique, procédé de production de couche à faible indice de réfraction, procédé de production d'élément optique et procédé de production de dispositif optique - Google Patents

Procédé de production de liquide de dispersion, liquide de dispersion, couche à faible indice de réfraction, élément optique, dispositif optique, procédé de production de couche à faible indice de réfraction, procédé de production d'élément optique et procédé de production de dispositif optique

Info

Publication number
WO2025178131A1
WO2025178131A1 PCT/JP2025/006119 JP2025006119W WO2025178131A1 WO 2025178131 A1 WO2025178131 A1 WO 2025178131A1 JP 2025006119 W JP2025006119 W JP 2025006119W WO 2025178131 A1 WO2025178131 A1 WO 2025178131A1
Authority
WO
WIPO (PCT)
Prior art keywords
particles
liquid
refractive index
concentration
low refractive
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2025/006119
Other languages
English (en)
Japanese (ja)
Inventor
大輔 服部
俊哉 吉見
啓介 佐藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nitto Denko Corp
Original Assignee
Nitto Denko Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nitto Denko Corp filed Critical Nitto Denko Corp
Publication of WO2025178131A1 publication Critical patent/WO2025178131A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
    • C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21S—NON-PORTABLE LIGHTING DEVICES; SYSTEMS THEREOF; VEHICLE LIGHTING DEVICES SPECIALLY ADAPTED FOR VEHICLE EXTERIORS
    • F21S2/00—Systems of lighting devices, not provided for in main groups F21S4/00 - F21S10/00 or F21S19/00, e.g. of modular construction
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/1336—Illuminating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
    • F21Y2115/00—Light-generating elements of semiconductor light sources
    • F21Y2115/20—Electroluminescent [EL] light sources

Definitions

  • the present disclosure relates to a method for manufacturing a dispersion, a dispersion, a low refractive index layer, an optical member, an optical device, a method for manufacturing a low refractive index layer, a method for manufacturing an optical member, and a method for manufacturing an optical device.
  • a low-refractive-index air layer is used as a total reflection layer.
  • each optical film component e.g., a light guide plate and a reflector
  • each component is stacked with an air layer in between.
  • problems such as component bending may occur, especially when the components are large.
  • Patent Document 2 uses roll-to-roll coating of a coating liquid.
  • the first method for producing a dispersion includes: A method for producing a dispersion liquid in which particles are dispersed in a dispersion medium, comprising the steps of: the particles are a condensation product of a raw material containing an alkoxysilane, A first pulverization step, a concentration step, and a second pulverization step are carried out in this order; the first pulverization step is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium, The concentration step is a step of concentrating the liquid, the second pulverization step is a step of further pulverizing the particles in the liquid pulverized in the first pulverization step, the viscosity of the liquid after the second pulverization step is greater than the viscosity of the liquid after the first pulverization step, or the concentration of the particles in the liquid after the second pulverization step is greater than the concentration of the particles in the
  • the second method for producing a dispersion includes: A method for producing a dispersion in which a solid content including particles is dispersed in a dispersion medium, comprising the steps of: the particles are a condensate of a raw material containing an alkoxysilane, A first pulverization step, a concentration step, and a second pulverization step are carried out in this order; the first pulverization step is a step of pulverizing the particles in a liquid in which the solid content is dispersed in the dispersion medium, The concentration step is a step of concentrating the liquid, the second pulverization step is a step of further pulverizing the particles in the liquid pulverized in the first pulverization step, the viscosity of the liquid after the second pulverization step is greater than the viscosity of the liquid after the first pulverization step, or the concentration of the solid content in the liquid after the second pulverization step is greater
  • the optical device of the present disclosure is characterized by including the optical element of the present disclosure.
  • the method for manufacturing an optical member disclosed herein is a method for manufacturing an optical member including a low refractive index layer, characterized in that the low refractive index layer is manufactured by the manufacturing method disclosed herein.
  • the disclosed method for manufacturing an optical device is a method for manufacturing an optical device including an optical element, characterized in that the optical element is manufactured by the disclosed manufacturing method.
  • on or “on the surface” can mean on or in direct contact with the surface, or through another layer, etc.
  • the particles are, as described above, a condensation product of raw materials containing alkoxysilane.
  • the alkoxysilane may be, for example, a saturated alkoxysilane or an unsaturated alkoxysilane having a UV-polymerizable unsaturated group.
  • the saturated alkoxysilane may be, for example, a monomer, an oligomer, or a combination thereof.
  • saturated alkoxysilane monomer examples include methyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, diethoxydimethoxysilane, dimethyldimethoxysilane, and dimethyldiethoxysilane. These may be used alone or in combination.
  • the saturated alkoxysilane oligomer is preferably a condensation polymer of one or more of the above-mentioned monomers.
  • the saturated alkoxysilane oligomer can be obtained, for example, by hydrolysis polymerization of a monomer.
  • the alkoxysilane is preferably an alkoxysilane having three or fewer functional groups (saturated bond functional groups).
  • the unsaturated alkoxysilane may be, for example, a monomer, an oligomer, or a combination thereof.
  • the unsaturated alkoxysilane monomer has, for example, an organic group having at least one double bond or triple bond and an alkoxy group.
  • the particles may be, for example, particles of a silsesquioxane condensate, which is a condensate of a raw material containing a trifunctional organosilicon compound.
  • the particles may be, for example, a condensate of a raw material consisting solely of a trifunctional organosilicon compound, or a condensate of a raw material containing a trifunctional organosilicon compound and another monomer.
  • X is 2, 3, or 4, provided that at least a portion of the raw material represented by the formula (1) is a trifunctional organosilicon compound in which X is 3, and R1 is a linear or branched alkyl group.
  • the number of carbon atoms in R1 is, for example, 1 to 6, 1 to 4, or 1 to 2.
  • the linear alkyl group include a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, and a hexyl group
  • examples of the branched alkyl group include an isopropyl group and an isobutyl group.
  • X is, for example, 3 or 4.
  • a trifunctional organosilicon compound in which X is 3 can be represented by formula (1') below.
  • R1 is the same as in formula (1), for example, a methyl group.
  • the organosilicon compound is tris(hydroxy)methylsilane.
  • the organosilicon compound is, for example, a trifunctional silane having three functional groups.
  • a specific example of the silicon compound represented by formula (1) is a compound in which X is 4.
  • the silicon compound is, for example, a tetrafunctional silane having four functional groups.
  • the silicon compound may be, for example, a precursor that forms the silicon compound of formula (1) upon hydrolysis.
  • the precursor may be, for example, any precursor that can generate the silicon compound upon hydrolysis, and a specific example thereof is a compound represented by the following formula (2):
  • X is 2, 3, or 4; R1 and R2 are each a linear or branched alkyl group; R 1 and R 2 may be the same or different; When X is 2, R 1 may be the same or different, R2 may be the same or different.
  • X and R1 are, for example, the same as X and R1 in formula (1) described later.
  • R2 for example, the examples of R1 in formula (1) described later can be used.
  • the production method of the present invention may include, for example, a step of hydrolyzing the precursor.
  • Particles of the condensate of raw materials containing alkoxysilane can be produced, for example, as a sol particle liquid in which particles are dispersed in a dispersion medium.
  • the method for producing the sol particle liquid is not particularly limited, but for example, it can be produced by grinding a gel of the condensate of raw materials containing alkoxysilane in a dispersion medium.
  • the method for producing the gel of the condensate of raw materials containing alkoxysilane is also not particularly limited, but for example, it can be produced by a method similar to the method for producing a gel of silicon compounds described in WO 2019/065999 or WO 2019/065803.
  • the method for grinding the gel of the condensate of raw materials containing alkoxysilane in a dispersion medium is also not particularly limited, but for example, the method described in Japanese Patent No. 7182358 may be used.
  • the type of dispersion medium in the sol particle liquid is also not particularly limited, but for example, it may be the same as the dispersion medium for the sol particle liquid described in WO 2019/065999 or WO 2019/065803.
  • the sol particle liquid can also be produced, for example, by the method described in "Reference Example 1" of the Examples of the present application, which will be described later.
  • the method for producing the dispersion of the present disclosure is not particularly limited, but for example, it can be produced as follows.
  • a liquid in which particles of a condensate of a raw material containing alkoxysilane are dispersed in a dispersion medium is produced as a sol particle liquid.
  • the particles of the condensate of a raw material containing alkoxysilane may be, for example, silsesquioxane condensate particles, as described above.
  • the sol particle liquid can be produced, for example, by the method described above.
  • the concentration of the particles of the condensate of a raw material containing alkoxysilane in the sol particle liquid at this stage is not particularly limited, but may be, for example, 0.5% by weight or more, 1.0% by weight or more, 2.0% by weight or more, 2.5% by weight or more, or 3.0% by weight or more; or, for example, 3.5% by weight or less, 3.4% by weight or less, 3.3% by weight or less, 3.2% by weight or less, or 3.1% by weight or less; for example, 0.5 to 3.5% by weight, 1.0 to 3.4% by weight, 2.0 to 3.3% by weight, 2.5 to 3.2% by weight, or 3.0 to 3.1% by weight.
  • the concentration of components other than the dispersion medium in the sol particle liquid at this stage is not particularly limited, but may be, for example, 0.5 wt% or more, 1.0 wt% or more, 2.0 wt% or more, 2.5 wt% or more, or 3.0 wt% or more; or, for example, 3.5 wt% or less, 3.4 wt% or less, 3.3 wt% or less, 3.2 wt% or less, or 3.1 wt% or less; or, for example, 0.5 to 3.5 wt%, 1.0 to 3.4 wt%, 2.0 to 3.3 wt%, 2.5 to 3.2 wt%, or 3.0 to 3.1 wt%.
  • particle size can be measured using, for example, a laser diffraction particle size analyzer or a dynamic light scattering particle size analyzer (DLS), but in the present disclosure, measurement using a dynamic light scattering particle size analyzer (DLS) is preferable as it allows for the calculation of more accurate values based on the target particle size.
  • D50 is also known as the median diameter, and is the particle size at the center of the particle distribution, corresponding to a cumulative frequency of 50%.
  • a "first grinding step” is performed to grind the particles in the sol particle liquid (a liquid in which the particles are dispersed in the dispersion medium).
  • the grinding method used in the first grinding step is not particularly limited, but for example, the method described in Japanese Patent No. 7182358 may be used. Among these, high-pressure medialess grinding is preferable.
  • the pressure used in the first grinding step is not particularly limited, but may be, for example, 30 MPa or more, 50 MPa or more, 70 MPa or more, 100 MPa or more, or 150 MPa or more; or, for example, 350 MPa or less, 300 MPa or less, 250 MPa or less, 200 MPa or less, or 180 MPa or less; for example, 30 to 350 MPa, 50 to 300 MPa, 70 to 250 MPa, 100 to 200 MPa, or 150 to 180 MPa.
  • the particle size D50 of the alkoxysilane-containing raw material condensate particles after the first pulverization step is not particularly limited, and may be, for example, 25 nm or more, 30 nm or more, 35 nm or more, 40 nm or more, or 50 nm or more; or, for example, 350 nm or less, 300 nm or less, 250 nm or less, 200 nm or less, or 150 nm or less; or, for example, 25 to 350 nm, 30 to 300 nm, 35 to 250 nm, 40 to 200 nm, or 50 to 150 nm.
  • concentration step is carried out to concentrate the sol particle liquid after the first pulverization step.
  • the concentration method in the concentration step is not particularly limited, and may be, for example, heating or pressurization, but pressurization is preferred. More specifically, for example, the liquid may be concentrated to a predetermined concentration by pressurization using a filter, or the liquid may be concentrated to a predetermined concentration by partially removing the dispersion medium by heating, etc.
  • the filter is also not particularly limited, and examples include rotary ceramic membrane filters and crossflow filters. An example of the rotary ceramic membrane filter is the Mitsubishi Dynafilter (DyF) product manufactured by Mitsubishi Kakoki Kaisha.
  • a "second grinding step” is performed to further grind the particles in the sol particle liquid after the concentration step.
  • the viscosity of the liquid after the second grinding step is greater than the viscosity of the liquid after the first grinding step, or the concentration of the particles in the liquid after the second grinding step is greater than the concentration of the particles in the liquid after the first grinding step.
  • the viscosity of the liquid after the second grinding step is greater than the viscosity of the liquid after the first grinding step, or the concentration of the solids in the liquid after the second grinding step is greater than the concentration of the solids in the liquid after the first grinding step.
  • the grinding method for the second grinding step is not particularly limited, but the method described in Japanese Patent No. 7,182,358 may be used, for example. Among these, high-pressure media-less grinding is preferable.
  • the pressure in the second pulverization step is not too small, and from the viewpoint of suppressing an increase in refractive index due to the particle size becoming too small, it is preferable that the pressure in the second pulverization step is not too large.
  • the particle diameter D50 of the alkoxysilane-containing raw material condensate particles after the second pulverization step may be, for example, 20 nm or more and 400 nm or less, or may be, for example, 25 nm or more, 30 nm or more, 35 nm or more, 40 nm or more, or 50 nm or more, or may be, for example, 350 nm or less, 300 nm or less, 250 nm or less, 200 nm or less, 150 nm or less, 100 nm or less, or 80 nm or less, or may be, for example, 25 to 350 nm, 30 to 300 nm, 35 to 250 nm, 40 to 200 nm, 50 to 150 nm, or 20 to 100 nm.
  • a "liquid concentration adjustment process” is carried out in which a dispersion medium is added to the sol particle liquid after the second grinding process to adjust the liquid concentration, thereby producing the dispersion liquid of the present disclosure.
  • the viscosity of the dispersion liquid is not particularly limited, but may be, for example, 4 mPa ⁇ s or more and less than 5000 mPa ⁇ s. In order to ensure the film thickness of the low refractive index layer, it is preferable that the viscosity of the dispersion liquid is not too low.
  • the viscosity of the dispersion of the present disclosure may be, for example, 5 mPa ⁇ s or more, 6 mPa ⁇ s or more, 7 mPa ⁇ s or more, 8 mPa ⁇ s or more, 9 mPa ⁇ s or more, 10 mPa ⁇ s or more, 11 mPa ⁇ s or more, 12 mPa ⁇ s or more, 13 mPa ⁇ s or more, 14 mPa ⁇ s or more, 15 mPa ⁇ s or more, 16 mPa ⁇ s or more, 17 mPa ⁇ s or more, 18 mPa ⁇ s or more, or 20 mPa ⁇ s or more, and may be, for example, 5000 mPa ⁇ s or less, 4000 mPa ⁇ s or less, 3500 mPa ⁇ s or less.
  • the concentration of the particles of the condensation product of the raw material containing alkoxysilane in the dispersion of the present disclosure is preferably not too low, from the viewpoint of ensuring the film thickness of the low refractive index layer.
  • the concentration of the particles of the condensation product of the raw material containing alkoxysilane in the dispersion is preferably not too high.
  • the concentration of solids in the dispersion of the present disclosure may be, for example, 3.6 wt% or more, 3.8 wt% or more, 4.0 wt% or more, 4.1 wt% or more, 4.2 wt% or more, or 6.0 wt% or more, for example, 39 wt% or less, 38 wt% or less, 37 wt% or less, 36 wt% or less, 35 wt% or less, 15 wt% or less, 12 wt% or less, 10 wt% or less, 8 wt% or less, or 6 wt% or less, for example, 3.6 to 39 wt%, 3.8 to 38 wt%, 4.0 to 37 wt%, 4.1 to 36 wt%, 4.2 to 35 wt%, or 6.0 to 12.0 wt%.
  • a crosslinking auxiliary also called a crosslinking agent
  • a catalyst etc. may be added to promote crosslinking between particles of the condensate of the raw material containing the alkoxysilane for use in producing a low refractive index layer.
  • the crosslinking may be, but is not limited to, a covalent bond between particles of the condensate of the alkoxysilane-containing raw material, either directly or via the crosslinking aid.
  • the crosslinking aid may also be, but is not limited to, a substance having multiple functional groups capable of forming covalent bonds with particles of the condensate of the alkoxysilane-containing raw material.
  • crosslinking aid examples include bis(trimethoxysilyl)alkylene.
  • examples of the bis(trimethoxysilyl)alkylene include bis(trimethoxysilyl)hexane.
  • Other examples of the crosslinking aid include, but are not limited to, those described in Japanese Patent No. 7182358.
  • the concentration of the crosslinking aid in the dispersion of the present disclosure is also not limited to, but is, for example, those described in Japanese Patent No. 7182358.
  • the catalyst may also be, but is not limited to, a photoactive catalyst or a thermally active catalyst, or an acid catalyst or a base catalyst.
  • a substance that generates a catalyst may be used.
  • Examples of the photobase generator include 9-anthrylmethyl N,N-diethylcarbamate (trade name WPBG-018), (E)-1-[3-(2-hydroxyphenyl)-2-propenoyl]piperidine (trade name WPBG-027), 1-(anthraquinon-2-yl)ethyl imidazolecarboxylate (trade name WPBG-140), and 2-nitrophenyl Examples include methyl 4-methacryloyloxypiperidine-1-carboxylate (trade name WPBG-165), 1,2-diisopropyl-3-[bis(dimethylamino)methylene]guanidium 2-(3-benzoylphenyl)propionate (trade name WPBG-266), 1,2-dicyclohexyl-4,4,5,5-tetramethylbiguanidium n-butyltriphenylborate (trade name WPBG-300), and 1,5,7-triazabicyclo[4.4.0]dec-5-ene
  • All of the above-mentioned trade names containing "WPBG” are trade names of Wako Pure Chemical Industries, Ltd.
  • Examples of the photoacid generator include aromatic sulfonium salts (trade name SP-170: ADEKA Corporation), triarylsulfonium salts (trade name CPI101A: SAN-APRO Corporation), and aromatic iodonium salts (trade name Irgacure 250: CIBA JAPAN KK).
  • the concentration of the catalyst or catalyst generator in the dispersion of the present disclosure is not particularly limited, but is as described in, for example, Japanese Patent No. 7182358.
  • the dispersion liquid of the present disclosure can be produced in the above manner.
  • the method for producing the dispersion liquid of the present disclosure is not limited to this, and any production method can be used as long as it satisfies the conditions of the dispersion liquid of the present disclosure.
  • the method for producing the dispersion liquid of the present disclosure may or may not include steps other than the "first pulverization step,” “concentration step,” and “second pulverization step.”
  • the liquid concentration adjustment step may or may not be performed as needed, and the pulverization step is not limited to two steps, the first pulverization step and the second pulverization step, but may include three or more steps.
  • the pressure during the first pulverization step and the pressure during the second pulverization step may be the same, and all of the following relational expressions (1) to (3) may be satisfied, which has the effect of suppressing light scattering caused by particle size when light is guided to a low refractive index layer.
  • the particle diameter D50 of the particles after the concentration step is greater than the particle diameter D50 of the particles after the first grinding step.
  • the particle diameter D50 of the particles after the concentration step is greater than the particle diameter D50 of the particles after the second grinding step.
  • the low refractive index layer of the present disclosure is characterized in that it is obtained by coating the dispersion of the present disclosure and drying it.
  • the layer obtained by coating the dispersion of the present disclosure and drying it as necessary may be subjected to, for example, heating or light irradiation.
  • heating or light irradiation for example, particles of the condensate of the raw material containing the alkoxysilane can be crosslinked directly or via the crosslinking auxiliary, thereby increasing the strength.
  • the low refractive index layer of the present disclosure may be produced, for example, by applying the dispersion of the present disclosure to a substrate such as a film and drying it.
  • the film may be, for example, a resin film.
  • a relatively thin material is called a "film” and a relatively thick material is called a "sheet,” but in this disclosure, no particular distinction is made between "film” and "sheet.”
  • the substrate is not particularly limited, and preferred examples include, but are not limited to, thermoplastic resin substrates, glass substrates, inorganic substrates such as silicon, plastics molded from thermosetting resins, semiconductor elements, and carbon fiber materials such as carbon nanotubes.
  • the method for producing the low refractive index layer of the present disclosure is not particularly limited, and it can be produced, for example, by a method similar to that described in WO 2019/065999 or WO 2019/065803.
  • the low refractive index layer of the present disclosure may have a thickness of, for example, 500 nm or more, 700 nm or more, 800 nm or more, 1000 nm or more, nm or more, or 2000 nm or more; or, for example, 10,000 nm or less, 8,000 nm or less, 5,000 nm or less, 4,000 nm or less, or 3,000 nm or less; or, for example, 500 to 10,000 nm, 700 to 8,000 nm, 800 to 5,000 nm, 1000 to 4,000 nm, or 2,000 to 3,000 nm.
  • the low refractive index layer of the present invention may have a porosity of, for example, 30 vol% or more, 35 vol% or more, 40 vol% or more, 45 vol% or more, or 50 vol% or more; and may have a porosity of, for example, 90 vol% or less, 80 vol% or less, 70 vol% or less, or 60 vol% or less, for example, 30 to 90 vol%, 35 to 80 vol%, 40 to 70 vol%, or 50 to 60 vol%.
  • the low refractive index layer of the present invention may have a refractive index of, for example, 1.05 or more, 1.10 or more, or 1.13 or more; and may have a refractive index of, for example, 1.35 or less, 1.30 or less, or 1.25 or less, for example, 1.05 to 1.35, 1.10 to 1.30, or 1.13 to 1.25.
  • the porosity can be measured by the following method.
  • the layer to be measured for porosity is a single layer containing only voids
  • the ratio (volume ratio) of the constituent material of the layer to air can be calculated by a standard method (for example, measuring the weight and volume to calculate the density), and the porosity (volume %) can be calculated from this.
  • the porosity can also be calculated from the refractive index value of the layer, for example. Specifically, the porosity is calculated from the refractive index value measured with an ellipsometer using the Lorentz-Lorenz formula.
  • the refractive index of the low refractive index layer is the numerical value of the refractive index at a wavelength of 550 nm, measured and calculated using the method below.
  • the low refractive index layer of the present disclosure preferably has a thickness variation of, for example, 20% or less, 18% or less, 16% or less, 15% or less, or 10% or less.
  • the lower limit is not particularly limited, but may be, for example, 0 or a value exceeding 0.
  • the thickness variation is the in-plane film thickness (thickness) variation of the low refractive index layer when the dispersion of the present disclosure is applied by spin coating to a light guide plate made of glass or resin with a surface roughness Rz of 50 nm or less and having a diameter or short side of 20 cm or less, and the low refractive index layer has a refractive index of 1.25 or less.
  • the in-plane film thickness (thickness) variation of the low refractive index layer is an index obtained by comparing the standard deviation of film thickness measurements taken at five points in the plane with the average film thickness.
  • the optical member of the present disclosure is characterized by including the low refractive index layer of the present invention.
  • the optical member of the present disclosure may or may not include components other than the low refractive index layer of the present invention.
  • the optical member of the present disclosure may be, for example, a laminate in which the low refractive index layer of the present invention is laminated on a substrate.
  • the substrate is not particularly limited, but may be, for example, as described above.
  • the optical member of the present disclosure may be, for example, a light guide plate with a low refractive index layer, in which the low refractive index layer of the present disclosure is laminated on a light guide plate.
  • another layer such as an adhesive layer may be present between the light guide plate and the low refractive index layer of the present disclosure, but it is preferable that the low refractive index layer of the present disclosure is laminated directly on the light guide plate without any other layer in between.
  • the dispersion liquid of the present disclosure can be applied to the light guide plate and dried, and the low refractive index layer of the present disclosure can be produced by the method described above.
  • the optical component of the present disclosure is not limited to a light guide plate, but may also be, for example, a polarizing plate, a retardation film, a reflective polarizer, a brightness enhancement film, a diffusion film, a dye-containing layer, or a transparent or opaque layer or film with optical functionality.
  • the optical device of the present disclosure is not particularly limited, and may be, for example, an image display device or a lighting device.
  • image display devices include liquid crystal displays, organic EL (electroluminescence) displays, and micro LED (light-emitting diode) displays.
  • lighting devices include organic EL lighting.
  • the number of parts (relative amount used) of each substance is in parts by mass (parts by weight) unless otherwise specified.
  • the adhesive used was a pressure-sensitive adhesive (pressure-sensitive adhesive composition) described below.
  • the term "pressure-sensitive adhesive layer” corresponds to the term "adhesive layer.”
  • the terms "pressure-sensitive adhesive layer” and "adhesive layer” are synonymous unless otherwise specified.
  • the concentration of the total solid content (components other than the dispersion medium) in the coating liquid or the concentration (wt %) of particles of the condensate of raw materials containing alkoxysilane was calculated from the ratio of the weight (mass) of the total coating liquid weight (mass) to the weight (mass) of the total solid content in the coating liquid or the weight (mass) of particles of the condensate of raw materials containing alkoxysilane.
  • the viscosity of the coating liquid was measured at a measurement temperature of 25°C using an E-type viscometer with a 1° cone rotor.
  • the refractive index was measured by the above-mentioned method for measuring the refractive index.
  • the particle diameter D50 of the condensate of the raw material containing alkoxysilane was measured by the method described above. As described above, D50 is also called the median diameter, which is the particle diameter at the center of the particle distribution and corresponds to a cumulative frequency of 50%.
  • the film thickness (thickness) and its variation of the low refractive index layer were measured as follows.
  • the low refractive index layer formed on glass was measured for thickness at five points in the plane using a spectroscopic ellipsometer (manufactured by J.A. Woollam), and the average value and standard deviation were calculated. The ratio of this standard deviation to the average value was calculated, and this value was taken as the variation.
  • Reference Example 1 Production of pulverized gel solution for forming low refractive index layer A pulverized gel liquid (sol particle liquid) for forming a low refractive index layer was produced as follows.
  • a pulverization process was carried out under a pressure of 100 MPa using a high-pressure medialess pulverization machine (manufactured by Sugino Machine Co., Ltd., Starburst HJP-25005 type).
  • a high-pressure medialess pulverization machine manufactured by Sugino Machine Co., Ltd., Starburst HJP-25005 type.
  • Example 1 IBA (isobutyl alcohol) was added to the gel pulverized solution obtained in Reference Example 1 to adjust the concentration of the particles of the condensate of the raw material containing alkoxysilane to 3.5 wt%.
  • this gel pulverized solution was subjected to nano-pulverization using Starburst (a trade name of Sugino Machine Co., Ltd.) under a high pressure of 150 MPa, adjusting the pulverization time so that the particle diameter D50 of the particles after pulverization was 150 nm, thereby obtaining a nano-pulverized solution having a particle concentration of 3.5 wt% of the condensate of the raw material containing alkoxysilane (first pulverization step).
  • Starburst a trade name of Sugino Machine Co., Ltd.
  • the solution was concentrated using Mitsubishi Dynafilter (DyF) (a trade name of Mitsubishi Kakoki Co., Ltd.) until the particle concentration of the condensate of the raw material containing alkoxysilane became 5.6 wt% (concentration step).
  • nano-pulverization was performed again using the Starburst under a high pressure of 150 MPa, adjusting the pulverization time so that the particle diameter D50 of the particles after pulverization became 130 nm (second pulverization step).
  • the measurement results of the concentration, viscosity, and particle size of the liquid obtained in each of these steps are shown in Table 1 below.
  • the dispersion was formed into a film on a glass plate by spin coating, dried, and then irradiated with UV at 350 mJ/cm 2 (@360 nm) to crosslink the particles of the condensate of raw materials containing alkoxysilane, thereby producing a low refractive index layer of the present disclosure.
  • the optical properties of the produced low refractive index layer and an appearance evaluation of the film (low refractive index layer) are summarized in Table 1 below.
  • Example 2 A dispersion liquid and a low refractive index layer according to the present disclosure were produced by the same procedure as in Example 1, except that in the first grinding step, the grinding time was adjusted so that the particle diameter D50 of the particles after grinding was 80 nm, and in the second grinding step, the grinding time was adjusted so that the particle diameter D50 of the particles after grinding was 50 nm, and then the amount of IBA added was changed to adjust the solids concentration of the entire liquid to 9.5 wt % (the concentration of particles of the condensate of raw materials containing alkoxysilane was 9.03 wt %).
  • Example 3 A dispersion liquid and a low refractive index layer according to the present disclosure were produced by the same procedure as in Example 1, except that in the first grinding step, the grinding time was adjusted so that the particle diameter D50 of the particles after grinding was 80 nm, and in the second grinding step, the grinding time was adjusted so that the particle diameter D50 of the particles after grinding was 65 nm, and then the amount of IBA added was changed to adjust the solids concentration of the entire liquid to 8.0 wt % (the concentration of particles of the condensate of raw materials containing alkoxysilane was 7.73 wt %).
  • Example 1 A low refractive index layer was produced in the same manner as in Example 1, except that the second pulverization step was not carried out and a film (low refractive index layer) was formed directly after the concentration step.
  • Example 2 A low refractive index layer was produced in the same manner as in Example 1, except that the order of the concentration step and the second pulverization step was reversed and the concentration step was performed after the second pulverization step.
  • Particle size D50 after the first grinding process refers to the particle size D50 of siloxane condensate particles in the liquid in each Example and Comparative Example after the first grinding process.
  • Viscosity after concentration process refers to the viscosity of the liquid in each Example and Comparative Example after the concentration process.
  • Conscentration after concentration process refers to the total solids concentration in the liquid in each Example and Comparative Example after the concentration process.
  • Particle concentration after concentration step refers to the concentration of siloxane condensate particles in the liquid of each of the Examples and Comparative Examples after the concentration step.
  • Particle size D50 after concentration step refers to the particle size D50 of siloxane condensate particles in the liquid of each of the Examples and Comparative Examples after the concentration step.
  • Voliscosity after second pulverization step refers to the viscosity of the liquid of each of the Examples and Comparative Examples after the second pulverization step.
  • Conscentration after second pulverization step refers to the concentration of the total solid content in the liquid of each of the Examples and Comparative Examples after the second pulverization step.
  • Particle concentration after second pulverization step refers to the concentration of siloxane condensate particles in the liquid of each of the Examples and Comparative Examples after the second pulverization step.
  • Particle size D50 after second pulverization step refers to the particle size D50 of siloxane condensate particles in the liquid of each of the Examples and Comparative Examples after the second pulverization step.
  • Refractive index of low refractive index layer refers to the refractive index of the low refractive index layer produced in each of the Examples and Comparative Examples.
  • Thickness of low refractive index layer refers to the thickness of the low refractive index layer produced in each of the above examples and comparative examples.
  • Light guiding property refers to the evaluation results of the light guiding property of the low refractive index layer produced in each of the above examples and comparative examples.
  • Haze refers to the haze value of the low refractive index layer produced in each of the above examples and comparative examples.
  • Example 1 As shown in Table 1 above, when the dispersions (coating liquids) of the present disclosure produced using the dispersion manufacturing method of the present disclosure in Examples 1 to 3 were used, a sufficiently large film thickness was ensured when a low refractive index layer was formed. Furthermore, in Example 1, the light conductivity of the low refractive index layer was good, and it was confirmed that a low refractive index layer with little film thickness variation (in-plane film thickness uniformity was achieved) was produced.
  • Comparative Example 1 in which the second pulverization step was not performed, and Comparative Example 2, in which the concentration step and second pulverization step were not performed in the order disclosed herein, the light conductivity of the low refractive index layer was poor, and it was confirmed that the film thickness variation of the low refractive index layer was large (in-plane film thickness uniformity was not achieved). Furthermore, in Comparative Example 3, in which the concentration step was performed before the first pulverization step rather than following the order of the steps disclosed herein, clogging occurred frequently and the concentration step could not be completed, and as a result, a low refractive index layer could not be formed.
  • a method for producing a dispersion liquid in which particles are dispersed in a dispersion medium comprising the steps of: the particles are a condensation product of a raw material containing an alkoxysilane, A first pulverization step, a concentration step, and a second pulverization step are carried out in this order; the first pulverization step is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium, The concentration step is a step of concentrating the liquid, the second pulverization step is a step of further pulverizing the particles in the liquid pulverized in the first pulverization step, the viscosity of the liquid after the second pulverization step is greater than the viscosity of the liquid after the first pulverization step, or the concentration of the particles in the liquid after the second pulverization step is greater than the concentration of the particles in the liquid after the first pulverization step, The method is characterized in that the concentration of
  • a method for producing a dispersion in which a solid content including particles is dispersed in a dispersion medium comprising the steps of: the particles are a condensation product of a raw material containing an alkoxysilane, A first pulverization step, a concentration step, and a second pulverization step are carried out in this order; the first pulverization step is a step of pulverizing the particles in the liquid in which the solid content is dispersed in the dispersion medium, The concentration step is a step of concentrating the liquid, the second pulverization step is a step of further pulverizing the particles in the liquid pulverized in the first pulverization step, the viscosity of the liquid after the second pulverization step is greater than the viscosity of the liquid after the first pulverization step, or the concentration of the solid content in the liquid after the second pulverization step is greater than the concentration of the solid content in the liquid after the first pulverization step, The method for producing
  • the pressure during the first pulverization step is equal to or less than the pressure during the second pulverization step, and The manufacturing method according to claim 1 or 2, which satisfies all of the following relational expressions (1) to (3):
  • the pressure during the first pulverization step is greater than the pressure during the second pulverization step, and
  • the manufacturing method according to claim 1 or 2 which satisfies all of the following relational expressions (1) to (3):

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Abstract

Est prévu un procédé de production d'un liquide de dispersion permettant de garantir l'épaisseur de film d'une couche à faible indice de réfraction et d'obtenir une uniformité d'épaisseur de film dans le plan.　Ce procédé de production est destiné à un liquide de dispersion dans lequel des particules sont dispersées dans un milieu de dispersion, le procédé étant caractérisé en ce que : les particules sont des particules d'un condensat d'un matériau contenant un alcoxysilane, c'est-à-dire un condensat d'un matériau contenant un silicium organique trifonctionnel ; une première étape de pulvérisation, une étape de condensation et une seconde étape de pulvérisation sont effectuées dans l'ordre indiqué ; la première étape de pulvérisation consiste à pulvériser les particules dans un liquide dans lequel les particules sont dispersées dans le milieu de dispersion ; l'étape de condensation consiste à condenser le liquide ; la seconde étape de pulvérisation consiste à pulvériser davantage les particules, dans le liquide, pulvérisées à la première étape de pulvérisation ; la viscosité du liquide après la seconde étape de pulvérisation est supérieure à la viscosité du liquide après la première étape de pulvérisation, ou la concentration des particules dans le liquide après la seconde étape de pulvérisation est supérieure à la concentration des particules dans le liquide après la première étape de pulvérisation ; et la densité des particules dans le liquide de dispersion produit est de 3,5 % en poids ou plus.
PCT/JP2025/006119 2024-02-22 2025-02-21 Procédé de production de liquide de dispersion, liquide de dispersion, couche à faible indice de réfraction, élément optique, dispositif optique, procédé de production de couche à faible indice de réfraction, procédé de production d'élément optique et procédé de production de dispositif optique Pending WO2025178131A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002520424A (ja) * 1998-07-09 2002-07-09 ダブリュー・アール・グレース・アンド・カンパニー−コーン インキ受理性コーティングに適した配合物
JP2010521399A (ja) * 2007-03-16 2010-06-24 キャボット コーポレイション エーロゲル粒子及びそれらの製造方法
JP2017066251A (ja) * 2015-09-29 2017-04-06 日東電工株式会社 多孔体ゲル含有液の製造方法、多孔体ゲル含有液、高空隙層の製造方法、高空隙率多孔体の製造方法、および積層フィルムロールの製造方法
JP2017132968A (ja) * 2016-01-29 2017-08-03 日東電工株式会社 ゲル粉砕物含有液の製造方法
JP2018123299A (ja) * 2017-01-31 2018-08-09 日東電工株式会社 低屈折率層含有粘接着シート、低屈折率層含有粘接着シートの製造方法、および光学デバイス
WO2024058165A1 (fr) * 2022-09-12 2024-03-21 株式会社日本触媒 Dispersion de gel d'oxyde de silicium, film transparent à faible indice de réfraction et procédé de fabrication de dispersion de gel d'oxyde de silicium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002520424A (ja) * 1998-07-09 2002-07-09 ダブリュー・アール・グレース・アンド・カンパニー−コーン インキ受理性コーティングに適した配合物
JP2010521399A (ja) * 2007-03-16 2010-06-24 キャボット コーポレイション エーロゲル粒子及びそれらの製造方法
JP2017066251A (ja) * 2015-09-29 2017-04-06 日東電工株式会社 多孔体ゲル含有液の製造方法、多孔体ゲル含有液、高空隙層の製造方法、高空隙率多孔体の製造方法、および積層フィルムロールの製造方法
JP2017132968A (ja) * 2016-01-29 2017-08-03 日東電工株式会社 ゲル粉砕物含有液の製造方法
JP2018123299A (ja) * 2017-01-31 2018-08-09 日東電工株式会社 低屈折率層含有粘接着シート、低屈折率層含有粘接着シートの製造方法、および光学デバイス
WO2024058165A1 (fr) * 2022-09-12 2024-03-21 株式会社日本触媒 Dispersion de gel d'oxyde de silicium, film transparent à faible indice de réfraction et procédé de fabrication de dispersion de gel d'oxyde de silicium

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