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
• • 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
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
  • C08L83/04—Polysiloxanes
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D17/00—Pigment pastes, e.g. for mixing in paints
• • 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
  • G02B1/11—Anti-reflection coatings
  • G02B1/111—Anti-reflection coatings using layers comprising organic materials

Definitions

• the present disclosure relates to a method for storing a dispersion, 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.
• the first method for storing a dispersion includes: A method for storing 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, The concentration of the particles in the liquid is 3.5% by weight or more, The dispersion is stored in an environment of 10° C. or less.
• 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, The concentration of the particles in the liquid is 3.5% by weight or more, a particle-containing liquid production step of producing a particle-containing liquid containing the particles in the dispersion medium; a storage step of storing the particle-containing liquid in an environment of 10°C or less;
• the present invention is characterized by comprising:
• the second method for producing a dispersion according to the present disclosure 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 condensation product of a raw material containing an alkoxysilane, The concentration of the solid content in the liquid is 3.5% by weight or more, a particle-containing liquid production step of producing a particle-containing liquid containing the particles in the dispersion medium; a storage step of storing the particle-containing liquid in an environment of 10°C or less;
• the present invention is characterized by comprising:
• the term "method for producing a dispersion liquid of the present disclosure” includes both the method for producing a first dispersion liquid of the present disclosure and the method for producing a second dispersion liquid of the present disclosure.
• the dispersion of the present disclosure is characterized by being produced by the dispersion production method of the present disclosure.
• the low refractive index layer of the present disclosure is characterized by being obtained by applying the dispersion liquid of the present disclosure and drying it.
• 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.
• pressure-sensitive adhesives and adhesives may be collectively referred to as "adhesive.”
• an agent with relatively weak adhesive or bonding strength e.g., an agent that allows for re-detachment from an adherend
• an agent with relatively strong adhesive or bonding strength e.g., an agent that makes re-detachment from an adherend impossible or extremely difficult
• an agent with relatively strong adhesive or bonding strength e.g., an agent that makes re-detachment from an adherend impossible or extremely difficult
• an agent with relatively strong adhesive or bonding strength e.g., an agent that makes re-detachment from an adherend impossible or extremely difficult
• the first method for storing the dispersion includes the steps of: A method for storing 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, The concentration of the particles in the liquid is 3.5% by weight or more, The dispersion is stored in an environment of 10° C. or less.
• the second method for storing a dispersion includes the steps of: A method for storing a dispersion in which a solid content including particles is dispersed in a dispersion medium, comprising: the particles are a condensation product of a raw material containing an alkoxysilane, The concentration of the solid content in the liquid is 3.5% by weight or more, The dispersion is stored in an environment of 10° C. or less.
• 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, The concentration of the particles in the liquid is 3.5% by weight or more, a particle-containing liquid production step of producing a particle-containing liquid containing the particles in the dispersion medium; a storage step of storing the particle-containing liquid in an environment of 10°C or less;
• the present invention is characterized by comprising:
• the method for producing a dispersion liquid disclosed herein may further include, for example, a concentration step of concentrating the particle-containing liquid, and the particle-containing liquid after the concentration step may be stored in the storage step.
• 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.
• the raw material (monomer) for the particles may contain, for example, an organosilicon compound represented by the following formula (1).
• the raw material may or may not contain other components.
• the organosilicon compound of the following formula (1) has hydroxyl groups, and therefore is capable of hydrogen bonding or intermolecular bonding via the respective hydroxyl groups.
• 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.
• 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.
• 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 as a particle-containing liquid containing the particles in the dispersion medium, for example, by the aforementioned "particle-containing liquid production process.”
• the particle-containing liquid can be produced, for example, as a sol particle liquid in which the particles are dispersed in a dispersion medium.
• the method for producing the sol particle liquid is not particularly limited, and 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, and 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, and for example, the method described in Japanese Patent No. 7182358 may be used.
• the type of dispersion medium in the sol particle liquid is not particularly limited, and 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.
• the particle-containing liquid is produced as a sol particle liquid in which particles of a condensate of a raw material containing alkoxysilane are dispersed in a dispersion medium using the aforementioned "particle-containing liquid production process."
• 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 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; 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.
• 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 media-less grinding is preferable.
• 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.
• the concentration of the particles of the condensate of the raw material containing the alkoxysilane in the sol particle liquid after the concentration step is not particularly limited, and may be, for example, 3.6% by weight or more, 4.0% by weight or more, 4.5% by weight or more, 5.0% by weight or more, or 5.5% by weight or more; and may be, for example, 40% by weight or less, 30% by weight or less, 20% by weight or less, 18% by weight or less, or 15% by weight or less, and may be, for example, 3.6 to 40% by weight, 4.0 to 30% by weight, 4.5 to 20% by weight, 5.0 to 18% by weight, or 5.5 to 15% by weight.
• the concentration of solids (solid components) in the sol particle liquid after the concentration step is not particularly limited, and may be, for example, 3.6% by weight or more, 3.8% by weight or more, 4.0% by weight or more, 4.1% by weight or more, or 4.2% by weight or more; or, for example, 39% by weight or less, 38% by weight or less, 37% by weight or less, 36% by weight or less, or 35% by weight or less; for example, 3.6 to 39% by weight, 3.8 to 38% by weight, 4.0 to 37% by weight, 4.1 to 36% by weight, or 4.2 to 35% by weight.
• a "second grinding process” is carried out to grind the particles in the sol particle liquid after the concentration process.
• the grinding method for the second grinding process is not particularly limited, but the method described in Japanese Patent No. 7182358 may be used, for example. Among these, high-pressure media-less grinding is preferable.
• the pressure when using high-pressure media-less grinding in the second grinding process 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 second pulverization step may be, for example, 20 nm or more, 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, 400 nm or less, 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; 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.
• the particle diameter D50 of the particles of the condensate of the raw materials containing the alkoxysilane is not too large.
• the viscosity of the dispersion liquid of the present disclosure is likely to be low. In such cases, the viscosity of the dispersion liquid of the present disclosure can be increased, for example, by increasing the concentration of the particles or the solid content in the dispersion liquid of the present disclosure.
• the particle diameter D50 of the particles of the condensate of the raw materials containing the alkoxysilane is not too large.
• a "liquid concentration adjustment process” is carried out in which a dispersion medium is added to the sol particle liquid after the second crushing process to adjust the liquid concentration. If the viscosity of the dispersion liquid is too low, exceeding the range of this disclosure, it will be impossible to ensure the film thickness of the low refractive index layer. If the viscosity of the dispersion liquid is too high, exceeding the range of this disclosure, the film thickness of the low refractive index layer will vary greatly (in-plane film thickness uniformity will not be achieved), or it will be impossible to form the low refractive index layer at all.
• the viscosity of the dispersion of the present disclosure may be, for example, 4 mPa ⁇ s or more, 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, less than 5000 mPa ⁇ s, 4000 mPa ⁇ s or less, 3500 mPa ⁇ s or less, or less than 5000 mPa ⁇ s.
• the viscosity may be, for example, 16 to 5000 mPa s, 17 to 4000 mPa s, 18 to 3500 mPa s, or 20 to 3000 mPa s.
• the concentration of the particles of the condensate of the raw material containing the alkoxysilane in the dispersion may be, for example, 3.5 to 15 wt %.
• the concentration of the condensate particles 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 condensate particles of the raw material containing alkoxysilane in the dispersion of the present disclosure is preferably not too high from the viewpoint of suppressing or preventing the film thickness of the low refractive index layer from varying greatly (not being able to achieve in-plane film thickness uniformity) and from the viewpoint of suppressing or preventing the formation of the low refractive index layer itself from becoming impossible.
• the concentration of the alkoxysilane-containing raw material condensate particles in the dispersion of the present disclosure may be, for example, 3.6% by weight or more, 4.0% by weight or more, 4.5% by weight or more, 5.0% by weight or more, 5.5% by weight or more, or 6% by weight or more, and may be, for example, 40% by weight or less, 35% by weight or less, 30% by weight or less, 25% by weight or less, 20% by weight or less, 15% by weight or less, 12% by weight or less, 10% by weight or less, 8% by weight or less, or 6% by weight or less, and may be, for example, 3.6 to 40% by weight, 4.0 to 35% by weight, 4.5 to 30% by weight, 5.0 to 25% by weight, 5.5 to 20% by weight, or 6.0 to 12.0% by weight.
• the concentration of solids (solid components) in the sol particle liquid after the concentration step is not particularly limited, but may be, for example, 3.5 to 15% by weight.
• the solids concentration 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 solids concentration in the dispersion of the present disclosure is preferably not too high from the viewpoint of suppressing or preventing the film thickness of the low refractive index layer from becoming too uneven (making it impossible to achieve in-plane film thickness uniformity) and from the viewpoint of suppressing or preventing the formation of the low refractive index layer itself due to cracks occurring in the low refractive index layer during drying.
• the solids concentration 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, or 4.2 wt % or more, or may be, for example, 39 wt % or less, 38 wt % or less, 37 wt % or less, 36 wt % or less, or 35 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 %, or 4.2 to 35 wt %.
• a cross-linking auxiliary also referred to as a cross-linking agent
• catalyst etc.
• the cross-linking is not particularly limited, but may be, for example, a bond in which particles of the condensate of the raw material containing the alkoxysilane are covalently bonded together, either directly or via the cross-linking auxiliary.
• the cross-linking auxiliary is not particularly limited, but may be, for example, a substance having multiple functional groups capable of forming covalent bonds with particles of the condensate of the raw material containing the alkoxysilane.
• Specific examples of the cross-linking auxiliary include bis(trimethoxysilyl)alkylene.
• Examples of the bis(trimethoxysilyl)alkylene include bis(trimethoxysilyl)hexane.
• Other examples of the cross-linking auxiliary are not particularly limited, but are described, for example, in Japanese Patent No. 7,182,358.
• the concentration of the crosslinking auxiliary in the dispersion of the present disclosure is not particularly limited, but is as described, for example, in Japanese Patent No. 7182358.
• the photocatalyst generator is not particularly limited, but examples include photobase generators (substances that generate a basic catalyst upon light irradiation) and photoacid generators (substances that generate an acidic catalyst upon light irradiation), and photobase generators are preferred.
• 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 be, for example, a porous layer having voids. Furthermore, the low refractive index layer of the present disclosure may be, for example, a porous body in which microporous particles are chemically bonded to each other.
• 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 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 liquid was filled into a polypropylene container and stored in a refrigerator at 4°C (storage step), producing a dispersion according to the present disclosure. The viscosity was measured after one month of refrigerated storage.
• the dispersion according to the present disclosure after one month of storage 0.22 g of the crosslinking aid bis(trimethoxysilyl)hexane, 0.22 g of the photobase catalyst WPBG-266 (Wako), and additional isobutyl alcohol were added, and the mixture was formed into a film by spin coating.
• the film was then dried, and then irradiated with UV light at 350 mJ/cm 2 (@360 nm) to crosslink particles of the condensate of the raw material containing alkoxysilane, producing a low refractive index layer according to the present disclosure.
• a low refractive index layer was produced by the same method using the particle-containing liquid before one month of refrigerated storage, and the optical properties were compared.
• Example 2 A dispersion liquid and a low refractive index layer according to the present disclosure were produced in the same manner as in Example 1, except that an iron metal container was used instead of the polypropylene container described in Example 1. In this example, rust derived from the metal of the container was generated at the contact point between the iron metal container and the liquid and was mixed into the liquid, but a film (low refractive index layer) was successfully produced.
• Example 4 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 dispersion liquid and a low refractive index layer were produced in the same manner as in Example 1, except that the storage temperature of the particle-containing liquid was changed from refrigerated storage at 4°C to room temperature storage at 15 to 25°C.
• Example 2 A dispersion and a low refractive index layer were produced in the same manner as in Example 1, except that the concentration step was not carried out, and the second grinding step was carried out while the concentration of the particles of the condensate of the raw material containing alkoxysilane remained at 3.5 wt %, and the final adjustment isobutyl alcohol was not added.
• “Layer appearance” represents the results of visually observing the appearance of the low-refractive index layers prepared in each Example and Comparative Example to evaluate the in-plane film thickness uniformity.
• “Concentration” represents the total concentration of solids in the dispersions of the present disclosure prepared in each Example or Comparative Example.
• Particle concentration refers to the concentration of siloxane condensate particles in the dispersion of the present disclosure produced in each of the examples or the dispersion produced in each of the comparative examples.
• “Haze” refers to the haze value of the low refractive index layer produced in each of the examples and comparative examples.
• the dispersions (coating solutions) of the present disclosure produced in Examples 1 to 4 all produced low refractive index layers that were able to ensure a sufficiently large film thickness and had little film thickness variation (achieved in-plane film thickness uniformity). Furthermore, as shown in Table 1 above, the viscosity of the dispersions of the present disclosure produced in Examples 1 to 4 remained almost unchanged even after one month of storage. As a result, even when a low refractive index layer was similarly produced using the particle-containing liquid before one month of storage, its properties were almost identical to those of the low refractive index layers of Examples 1 to 4 shown in Table 1 above.
• the dispersion (coating solution) of Comparative Example 1 was stored at a high temperature, resulting in a large change (increase) in viscosity after storage, and as a result, in-plane film thickness uniformity of the low refractive index layer could not be achieved. Furthermore, the dispersion (coating solution) of Comparative Example 2 had a concentration that was too low, resulting in a small film thickness of the low refractive index layer.
• (Appendix 1) A method for storing 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, The concentration of the particles in the liquid is 3.5% by weight or more, The storage method comprises storing the dispersion in an environment of 10°C or less.
• (Appendix 2) A method for storing a dispersion in which a solid content including particles is dispersed in a dispersion medium, comprising: the particles are a condensation product of a raw material containing an alkoxysilane, The concentration of the solid content in the liquid is 3.5% by weight or more, The storage method comprises storing the dispersion in an environment of 10°C or less.
• (Appendix 5) 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, The concentration of the particles in the liquid is 3.5% by weight or more, a particle-containing liquid production step of producing a particle-containing liquid containing the particles in the dispersion medium; a storage step of storing the particle-containing liquid in an environment of 10°C or less; A manufacturing method comprising: (Appendix 6) 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, The concentration of the solid content in the liquid is 3.5% by weight or more, a particle-containing liquid production step of producing a particle-containing liquid containing the particles in the dispersion medium; a storage step of storing the particle-containing liquid in an environment of 10
• Appendix 8 The manufacturing method according to any one of Appendices 5 to 7, wherein in the storage step, the particle-containing liquid is stored in an environment of 10°C or less by the storage method according to any one of Appendices 1 to 4.
• Appendix 9 A manufacturing method described in any one of Appendices 5 to 8, wherein the viscosity change rate of the particle-containing liquid after storage for one month from immediately after the completion of the concentration step is within ⁇ 30%.
• the viscosity of the dispersion liquid produced is 4 mPa s or more and less than 5000 mPa s, The particle diameter D50 of the particles is 20 nm or more and 400 nm or less.
• the method of any one of appendices 5 to 9. (Appendix 11) A dispersion produced by the production method described in any one of appendices 5 to 10. (Appendix 12) 12. A low refractive index layer obtained by coating the dispersion liquid according to claim 11 and drying it. (Appendix 13) 13. The low refractive index layer according to claim 12, having a refractive index of 1.25 or less. (Appendix 14) 14.
• Appendix 15 An optical member comprising the low refractive index layer according to any one of appendices 12 to 14.
• Appendix 16 16.
• An optical device comprising the optical member according to claim 15.
• Appendix 17 producing the dispersion by the production method described in any one of Supplementary Notes 5 to 10;
• a method for producing a low refractive index layer comprising the steps of: applying the dispersion onto a substrate; and drying the applied dispersion.
• Appendix 18 18. The method of claim 17, wherein the refractive index of the low refractive index layer produced is 1.25 or less.
• Appendix 19 19.
• Appendix 20 20.
• a method for producing an optical member including a low refractive index layer the method comprising producing the low refractive index layer by the method described in any one of appendices 17 to 19.
• a method for manufacturing an optical device including an optical element the method comprising manufacturing the optical element by the manufacturing method described in appendix 20.
• the present disclosure can provide a method for storing a dispersion that can ensure the film thickness of a low refractive index layer and achieve in-plane film thickness uniformity, a method for manufacturing a dispersion, a dispersion, a low refractive index layer, an optical element, an optical device, a method for manufacturing a low refractive index layer, a method for manufacturing an optical element, and a method for manufacturing an optical device.
• the uses of the present disclosure are not particularly limited.
• the optical device of the present disclosure is not particularly limited, and examples thereof include image display devices and lighting devices. Examples of the image display devices include liquid crystal displays, organic EL displays, and micro LED displays. Examples of the lighting devices include organic EL lighting.

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