Classifications

• • 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
  • C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
  • C09D183/04—Polysiloxanes
• • G—PHYSICS
  • G02—OPTICS
  • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
  • G02B5/00—Optical elements other than lenses
  • G02B5/08—Mirrors

Definitions

• the present disclosure relates to a dispersion, a dispersion set, 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 1 uses a method in which a low refractive index layer is laminated on top of a light guide plate via an adhesive layer that is bonded to the light guide plate in order to protect the light.
• Patent Document 2 uses roll-to-roll coating of a coating liquid.
• the dispersion set of the present disclosure is characterized by comprising the dispersion of the present disclosure and a catalyst-containing liquid containing a catalyst for chemically bonding the particles of the dispersion.
• 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.
• the "solvent" e.g., a solvent for producing a gel, a replacement solvent, a solvent for producing a low refractive index layer, etc. used in producing a dispersion
• the gel, its pulverized material, particles, etc. may be dispersed or precipitated in the solvent.
• an organic solvent may be used as the dispersion medium in the dispersion of the present disclosure.
• 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
• on or “on the surface” can mean on or in direct contact with the surface, or through another layer, etc.
• the first dispersion of the present disclosure comprises: A dispersion liquid in which particles are dispersed in a dispersion medium, the particles are a condensation product of a raw material containing an alkoxysilane, the concentration of the particles in the dispersion is 3.5 to 15% by weight;
• the viscosity of the dispersion 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 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 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.
• the production method of the present invention may include, for example, a step of hydrolyzing the precursor.
• the method for producing the dispersion of the present disclosure is not particularly limited, but for example, it can be produced as follows.
• a sol particle liquid is produced in which particles of a condensate of a raw material containing alkoxysilane are dispersed in a dispersion medium.
• 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%.
• 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 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.
• 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 medialess grinding is preferable.
• it 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; 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; 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 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 the occurrence of cracks in the low refractive index layer during drying, which makes it impossible to form the low refractive index layer itself.
• 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, 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.
• 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 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 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 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 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 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 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%.
• 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.
• 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 the second grinding step was not performed and concentration adjustment and additive mixing were performed after the concentration step.
• 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 2 The same operations as in Example 1 were carried out up to the first grinding step, and then the concentration of particles of the condensate of raw materials containing alkoxysilane was concentrated to 15.1% by weight in the concentration step. As a result, the viscosity of the liquid began to increase immediately after the concentration step, and the viscosity of the liquid was too high to form a low refractive index layer. In addition, particle aggregation progressed during the liquid concentration adjustment and additive mixing steps, and it was not possible to control it within the range of this disclosure.
• the dispersions (coating solutions) of the present disclosure produced in Examples 1 to 4 all ensured a sufficiently large film thickness and produced low refractive index layers with little film thickness variation (achieved in-plane film thickness uniformity).
• the dispersion (coating solution) of Comparative Example 1 had too low a concentration, resulting in a small film thickness of the low refractive index layer.
• the dispersion (coating solution) of Comparative Example 2 had too high a concentration, resulting in a low refractive index layer not being able to be formed.
• the viscosity of the dispersion is 4 mPa s or more and less than 5000 mPa s,
• the dispersion liquid is characterized in that the particle diameter D50 of the particles is 20 nm or more and 400 nm or less.
• the concentration of the particles in the dispersion is 6.0 to 12.0 wt %;
• the viscosity of the dispersion is 4 to 50 mPa s,
• the particle diameter D50 of the particles is 20 to 100 nm; 2.
• a dispersion set comprising: the dispersion according to any one of claims 1 to 6; and a catalyst-containing liquid containing a catalyst for chemically bonding the particles of the dispersion.
• Appendix 8 8. The dispersion set according to claim 7, further comprising a cross-linking auxiliary agent-containing liquid containing a cross-linking auxiliary agent for indirectly bonding the particles together.
• Appendix 9 A low refractive index layer obtained by coating the dispersion according to any one of Supplementary Notes 1 to 6 or the dispersion set according to Supplementary Notes 7 or 8, and drying the coating.
• An optical member comprising the low refractive index layer according to claim 9.
• Appendix 11 11.
• An optical device comprising the optical member according to claim 10.
• the present disclosure can provide a dispersion liquid, dispersion liquid set, low refractive index layer, optical element, optical device, method for manufacturing a low refractive index layer, method for manufacturing an optical element, and method for manufacturing an optical device, which can ensure the film thickness of a low refractive index layer and achieve in-plane film thickness uniformity.
• the applications 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.

Landscapes

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Physics & Mathematics (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Health & Medical Sciences (AREA)
• General Physics & Mathematics (AREA)
• Optics & Photonics (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Wood Science & Technology (AREA)
• Compositions Of Macromolecular Compounds (AREA)

Priority Applications (1)

Applications Claiming Priority (2)

Publications (1)

Family

ID=96847304

Family Applications (1)

Country Status (3)

Citations (3)

• 2025
  • 2025-02-21 TW TW114106508A patent/TW202600743A/zh unknown
  • 2025-02-21 JP JP2025541028A patent/JPWO2025178129A1/ja active Pending
  • 2025-02-21 WO PCT/JP2025/006117 patent/WO2025178129A1/ja active Pending

Patent Citations (3)

Also Published As

Similar Documents

Legal Events