Method for producing dispersion, dispersion, low refractive index layer, optical member, optical device, method for producing low refractive index layer, method for producing optical member, and method for producing optical device

Abstract

This invention provides a method for manufacturing a dispersion that ensures the thickness of a low-refractive-index layer and achieves uniform in-plane film thickness. The method involves manufacturing a dispersion in a dispersion medium containing particles that are condensates of a trifunctional organosilicon raw material, specifically condensates of an alkoxysilane raw material. The method includes sequentially performing a first pulverizing step, a concentration step, and a second pulverizing step. The first pulverizing step involves pulverizing the particles in a liquid containing the particles dispersed in the dispersion medium. The concentration step involves concentrating the liquid. The second pulverizing step further pulverizes the particles in the liquid pulverized in the first pulverizing step. The viscosity of the liquid after the second pulverizing step is greater than the viscosity of the liquid after the first pulverizing step, or the concentration of the particles in the liquid after the second pulverizing step is greater than the concentration of the particles in the liquid after the first pulverizing step. The concentration of the particles in the manufactured dispersion is 3.5% by weight or more.

Description

Technical Field

[0001] This disclosure relates to a method for manufacturing a dispersion, a dispersion, a low-refractive-index layer, an optical component, an optical device, a method for manufacturing a low-refractive-index layer, a method for manufacturing an optical component, and a method for manufacturing an optical device. Background Technology

[0002] In optical devices, for example, air layers with low refractive index are used as total reflection layers. Specifically, for example, in liquid crystal devices, optical film components (e.g., light guide plates and reflective plates) are stacked with air layers between them. However, when the components are separated by air layers, there is a risk of problems such as bending of the components, especially when the components are large.

[0003] Therefore, a solution has been proposed to use a low-refractive-index layer instead of an air layer. For example, a method is used where a low-refractive-index layer is formed on a light guide plate to optically isolate the light transmitted to the light guide plate, allowing it to guide light without being affected by external factors such as stains or scratches on the light guide plate. In Patent Document 1, for the aforementioned purpose of protecting light, a method is used to laminate a low-refractive-index layer via an adhesive layer bonded to the light guide plate.

[0004] As a method for forming such a low refractive index layer, for example, Patent Document 2 uses a roll-to-roll coating liquid.

[0005] Existing technical documents

[0006] Patent documents

[0007] Patent Document 1: Japanese Patent No. 6606518

[0008] Patent Document 2: Japanese Patent No. 6599699 Summary of the Invention

[0009] The problem that the invention aims to solve

[0010] In the case where a low-refractive-index layer is stacked via an adhesive layer as in Patent Document 1, the light transmitted in the light guide plate passes through the adhesive layer before undergoing total internal reflection in the low-refractive-index layer. This results in color shift and light scattering originating from the adhesive layer, posing a potential risk of light guide loss. Therefore, a method is proposed to form a low-refractive-index layer by directly applying a coating liquid to the light guide plate without using an adhesive layer.

[0011] However, since the light guide plates are manufactured in batches, different coating methods than the usual die coating used in roll coating are required to directly apply the liquid, such as batch coating machines, spin coating, spray coating, and dip coating. Among these batch coating methods, spin coating is the easiest to ensure in-plane smoothness. However, for the liquid used to form the low-refractive-index layer as described in Patent Document 2, the liquid design is based on a roll-to-roll coating method, and therefore, the liquid design, which takes into account ensuring the film thickness after drying in spin coating and the spread of the liquid during spin coating, is insufficient. Especially in AR / MR glass applications for small devices, it is important to ensure the film thickness and in-plane film thickness uniformity of the low-refractive-index layer in order to maintain the parallelism between the light guide plates. Even for liquid designs used in spin coating, special attention needs to be paid to the proper management / design of parameters such as viscosity and concentration.

[0012] Therefore, the purpose of this disclosure is to provide a method for manufacturing a dispersion that can ensure the film thickness of a low refractive index layer and achieve in-plane film thickness uniformity, a dispersion, a low refractive index layer, an optical component, an optical device, a method for manufacturing a low refractive index layer, a method for manufacturing an optical component, and a method for manufacturing an optical device.

[0013] Problem Solving Methods

[0014] To achieve the above objectives, the method for manufacturing the first dispersion disclosed herein is a method for manufacturing a dispersion in which particles are dispersed in a dispersion medium, wherein...

[0015] The aforementioned particles are condensates of raw materials containing alkoxysilanes.

[0016] The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially.

[0017] The first pulverizing step described above is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium.

[0018] The above-mentioned concentration process is a process of concentrating the above-mentioned liquid.

[0019] The second pulverizing step described above is a step of further pulverizing the particles in the liquid that have been pulverized in the first pulverizing step.

[0020] 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.

[0021] The concentration of the particles in the above-mentioned dispersion is 3.5% by weight or more.

[0022] To achieve the above objectives, the method for manufacturing the second dispersion disclosed herein is a method for manufacturing a dispersion in which a solid component containing particles is dispersed in a dispersion medium, wherein...

[0023] The aforementioned particles are condensates of raw materials containing alkoxysilanes.

[0024] The process consists of three steps: first grinding, second concentration, and third grinding.

[0025] The first pulverizing step described above is a step of pulverizing the particles in a liquid in which the solid components are dispersed in the dispersion medium.

[0026] The above-mentioned concentration process is a process of concentrating the above-mentioned liquid.

[0027] The second pulverizing step described above is a step of further pulverizing the particles in the liquid that have been pulverized in the first pulverizing step.

[0028] 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 component in the liquid after the second pulverization step is greater than the concentration of the solid component in the liquid after the first pulverization step.

[0029] The concentration of the solid component in the above-mentioned dispersion is 3.5% by weight or more.

[0030] It should be noted that, unless otherwise stated, the term "method of manufacturing dispersion of the present disclosure" hereafter includes both the method of manufacturing the first dispersion of the present disclosure and the method of manufacturing the second dispersion of the present disclosure.

[0031] The dispersion disclosed herein is manufactured by the dispersion manufacturing method disclosed herein.

[0032] The low refractive index layer of this disclosure is obtained by coating the dispersion of this disclosure and then drying it.

[0033] The optical components disclosed herein include the low refractive index layer of this disclosure.

[0034] The optical device disclosed herein includes the optical components disclosed herein.

[0035] The method for manufacturing the low-refractive-index layer disclosed herein includes:

[0036] The steps for manufacturing the dispersion of the present disclosure using the method for manufacturing the dispersion of the present disclosure;

[0037] The process of coating the dispersion of this disclosure onto a substrate; and

[0038] The process of drying the above-mentioned dispersion after coating.

[0039] The method for manufacturing an optical component disclosed herein is a method for manufacturing an optical component comprising a low refractive index layer, the method comprising: manufacturing the aforementioned low refractive index layer by the manufacturing method of the present disclosure.

[0040] The method for manufacturing an optical device disclosed herein is a method for manufacturing an optical device including optical components, the method comprising: manufacturing the optical components by the manufacturing method of the present disclosure.

[0041] The effects of the invention

[0042] According to this disclosure, a method for manufacturing a dispersion capable of ensuring the film thickness of a low refractive index layer and achieving in-plane film thickness uniformity, a dispersion, a low refractive index layer, an optical component, an optical device, a method for manufacturing a low refractive index layer, a method for manufacturing an optical component, and an optical device can be provided. Detailed Implementation

[0043] The following examples will illustrate this disclosure in more detail. However, this disclosure is not limited by the following description.

[0044] In this disclosure, the "solvent" (e.g., a gel manufacturing solvent, a displacement solvent, a low-refractive-index layer manufacturing solvent, etc. used in the manufacture of the dispersion) may not dissolve the gel or its pulverized form, particles, etc., for example, it may disperse or precipitate the gel or its pulverized form in the solvent. For example, organic solvents may be used as the dispersion medium in the dispersion of this disclosure.

[0045] In this disclosure, "adhesive layer" refers to a layer formed by at least one of an adhesive and a bonding agent. In this disclosure, unless otherwise stated, "adhesive layer" can be an "adhesive layer" formed by an adhesive, an "adhesive layer" formed by a bonding agent, or a layer comprising both an adhesive and a bonding agent. Furthermore, in this disclosure, adhesives and bonding agents are sometimes collectively referred to as "adhesives and bonding agents." Generally, agents with weaker adhesive strength (e.g., agents capable of re-peeling the bonded objects) are sometimes referred to as "adhesives," while agents with stronger adhesive strength (e.g., agents where the bonded objects cannot be peeled off or are very difficult to peel off) are referred to as "bonding agents," thus distinguishing between them. In this disclosure, there is no clear distinction between adhesives and bonding agents. Additionally, in this disclosure, there is no clear distinction between "adhesive strength" and "bonding force."

[0046] In this disclosure, unless otherwise stated, “mass%” and “weight%” may be used interchangeably, as may “parts by mass” and “parts by weight”.

[0047] In addition, in this disclosure, "above" or "on the surface" can refer to a state of direct contact with the above or surface, or a state of being separated by other layers, etc.

[0048] [1. Dispersion and its preparation method]

[0049] As described above, the method for manufacturing the first dispersion disclosed herein is a method for manufacturing a dispersion in which particles are dispersed in a dispersion medium, wherein...

[0050] The aforementioned particles are condensates of raw materials containing alkoxysilanes.

[0051] The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially.

[0052] The first pulverizing step described above is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium.

[0053] The above-mentioned concentration process is a process of concentrating the above-mentioned liquid.

[0054] The second pulverizing step described above is a step of further pulverizing the particles in the liquid that have been pulverized in the first pulverizing step described above.

[0055] 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.

[0056] The concentration of the particles in the above-mentioned dispersion is 3.5% by weight or more.

[0057] As described above, the method for manufacturing the second dispersion disclosed herein is a method for manufacturing a dispersion in which a solid component containing particles is dispersed in a dispersion medium, wherein...

[0058] The aforementioned particles are condensates of raw materials containing alkoxysilanes.

[0059] The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially.

[0060] The first pulverizing step described above is a step of pulverizing the particles in a liquid in which the solid components are dispersed in the dispersion medium.

[0061] The above-mentioned concentration process is a process of concentrating the above-mentioned liquid.

[0062] The second pulverizing step described above is a step of further pulverizing the particles in the liquid that have been pulverized in the first pulverizing step described above.

[0063] 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 component in the liquid after the second pulverization step is greater than the concentration of the solid component in the liquid after the first pulverization step.

[0064] The concentration of the solid component in the above-mentioned dispersion is 3.5% by weight or more.

[0065] Furthermore, the dispersion of this disclosure is manufactured using the dispersion manufacturing method of this disclosure.

[0066] [1-1. Particles of a condensate containing an alkoxysilane]

[0067] In the dispersion disclosed herein, as described above, the particles are condensates of raw materials containing alkoxysilanes. The alkoxysilanes can be, for example, saturated alkoxysilanes or unsaturated alkoxysilanes with unsaturated groups capable of ultraviolet polymerization. The saturated alkoxysilanes can be, for example, monomers, oligomers, or combinations thereof. Specific examples of the saturated alkoxysilane monomers include: methyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, diethoxydimethoxysilane, dimethyldimethoxysilane, and dimethyldiethoxysilane, etc., and only one of these may be used, or multiple may be used in combination. The saturated alkoxysilane oligomers are preferably condensates of one or more of the above monomers. The saturated alkoxysilane oligomers can be obtained, for example, by the hydrolytic polymerization of monomers. The aforementioned alkoxysilanes are preferably alkoxysilanes having three or fewer functional groups (saturated functional groups). The aforementioned unsaturated alkoxysilanes can be, for example, monomers, oligomers, or combinations thereof. The aforementioned unsaturated alkoxysilane monomers, for example, possess an organic group having at least one double or triple bond and an alkoxy group.

[0068] In the dispersion disclosed herein, the aforementioned particles may, for example, be particles of a silsesquioxane condensate, which is a condensate of a raw material comprising a trifunctional organosilicon compound. In this case, the aforementioned particles may, for example, be a condensate of a raw material consisting solely of a trifunctional organosilicon compound, or a condensate of a raw material comprising a trifunctional organosilicon compound and other monomers. In the aforementioned raw material (monomer), the content of the trifunctional organosilicon compound may, for example, be 0.1 mol% or more, 10 mol% or more, 30 mol% or more, 50 mol% or more, or 90 mol% or more, and for example, be 100 mol% or less, 99 mol% or less, 90 mol% or less, 70 mol% or less, or 50 mol% or less, and for example, be 0.1 to 100 mol%, 1 to 99 mol%, 10 to 90 mol%, or 30 to 70 mol%.

[0069] The raw materials (monomers) of the above-mentioned particles may, for example, contain organosilicon compounds as shown in formula (1) below. In this case, the raw materials may further contain other components, or may not contain any. Since the organosilicon compounds of formula (1) below have hydroxyl groups, hydrogen bonding or intermolecular force bonding can be achieved, for example, through each hydroxyl group.

[0070] [Chemical Formula 1]

[0071]

[0072] In the above formula (1), for example, X is 2, 3 or 4, wherein at least a portion of the raw materials shown in the above formula (1) is a trifunctional organosilicon compound with X being 3, R 1 It is a straight-chain or branched alkyl group. The above R... 1 The number of carbon atoms is, for example, 1 to 6, 1 to 4, or 1 to 2. Examples of straight-chain alkyl groups include methyl, ethyl, propyl, butyl, pentyl, and hexyl, while examples of branched alkyl groups include isopropyl and isobutyl. X is, for example, 3 or 4.

[0073] In the organosilicon compounds shown in formula (1) above, the trifunctional organosilicon compounds with X = 3 can be represented by the following formula (1'). In the following formula (1'), R 1 Same as formula (1) above, for example, methyl. In R 1 When X is methyl, the above organosilicon compound is tris(hydroxy)methylsilane. When X is 3, the above organosilicon compound is, for example, a trifunctional silane having 3 functional groups.

[0074] [Chemical Formula 2]

[0075]

[0076] Furthermore, as a specific example of the silicon compound shown in formula (1) above, a compound in which X is 4 can be cited. In this case, the silicon compound is, for example, a tetrafunctional silane having four functional groups.

[0077] The aforementioned silicon compound can be, for example, a precursor to the silicon compound of formula (1) formed by hydrolysis. As a precursor, any precursor that can generate the aforementioned silicon compound by hydrolysis is acceptable; as a specific example, a compound represented by formula (2) can be cited.

[0078] [Chemical Formula 3]

[0079]

[0080] In equation (2) above, for example, X is 2, 3, or 4.

[0081] R 1 and R 2 Each is a straight-chain or branched alkyl group.

[0082] R 1 With R 2 They can be the same or different.

[0083] R 1 When X is 2, they can be the same or different.

[0084] R 2 They can be the same as each other, or they can be different.

[0085] The above X and R 1 For example, X and R in equation (1) described later. 1 Same. Additionally, the above R... 2 For example, R in equation (1) described later can be used. 1 Examples.

[0086] As a specific example of the silicon compound shown in formula (2) above, a compound with X equal to 3, as shown in formula (2') below, can be cited. In formula (2') below, R 1 and R 2 These are the same as those in equation (2) above. In R 1 and R 2 In the case of methyl, the above-mentioned silicon compound is trimethoxy(methyl)silane (hereinafter also referred to as "MTMS"). The compound shown in formula (1') can be obtained by hydrolyzing the compound shown in formula (2') below.

[0087] [Chemical Formula 4]

[0088]

[0089] When the silicon compound is a precursor as shown in formula (2), the manufacturing method of the present invention may include, for example, a step of hydrolyzing the precursor.

[0090] Particles of condensates containing alkoxysilane raw materials can be manufactured, for example, in the form of a sol-particle liquid in which the particles are dispersed in a dispersion medium. The method for manufacturing the sol-particle liquid is not particularly limited; for example, it can be manufactured by pulverizing a gel of condensates containing alkoxysilane raw materials in a dispersion medium. The method for manufacturing the gel of condensates containing alkoxysilane raw materials is also not particularly limited; for example, it can be manufactured using the same method as that described in International Publication No. 2019 / 065999 or International Publication No. 2019 / 065803 for manufacturing gels of silicon compounds. The method for pulverizing the gel of condensates containing alkoxysilane raw materials in a dispersion medium is also not particularly limited; for example, the method described in Japanese Patent No. 7182358 can be used. The type of dispersion medium in the sol-particle liquid is also not particularly limited; for example, it can be the same as the dispersion medium of the sol-particle liquid described in International Publication No. 2019 / 065999 or International Publication No. 2019 / 065803. In addition, the above-mentioned sol-particle liquid can be manufactured by, for example, the method described in "Reference Example 1" of the embodiments of this application described later.

[0091] [1-2. Methods for preparing dispersions]

[0092] The method for manufacturing the dispersion disclosed herein is not particularly limited, and for example, it can be manufactured as described below.

[0093] First, a liquid containing particles of a condensate of a raw material containing an alkoxysilane is prepared in the form of a sol-particle liquid. As mentioned above, the particles of the condensate of the raw material containing an alkoxysilane can be, for example, particles of a silsesquioxane condensate. The sol-particle liquid can be prepared, for example, by the method described above. The concentration of the particles of the condensate of the raw material containing an alkoxysilane in the sol-particle liquid during this stage is not particularly limited, and can 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, less than 3.5% by weight, less than 3.4% by weight, less than 3.3% by weight, less than 3.2% by weight, or less than 3.1% by weight; or, 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. Furthermore, the concentration of components other than the dispersion medium in the above-mentioned sol-particle liquid during this stage is not particularly limited, and 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 may be, for example, less than 3.5% by weight, less than 3.4% by weight, less than 3.3% by weight, less than 3.2% by weight, or less than 3.1% by weight; or may be, 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.

[0094] It should be noted that, in this disclosure, the particle size can be measured, for example, by a laser diffraction particle size analyzer or a dynamic light scattering particle size analyzer (DLS). Based on the target particle size, measurement using a dynamic light scattering particle size analyzer (DLS) in this disclosure can yield a more accurate value, and is therefore preferred. By measuring the particle size distribution using these methods, the particle size D50 can be calculated. D50, also known as the median particle size, is the median particle size of the particle distribution, with a cumulative frequency corresponding to 50%.

[0095] Next, a "first pulverization step" is performed to pulverize the particles in the above-mentioned sol-particle liquid (the liquid in which the above-mentioned particles are dispersed in the above-mentioned dispersion medium). The pulverization method in the first pulverization step is not particularly limited; for example, the method described in Japanese Patent No. 7182358 can be used. High-pressure, medium-free pulverization is preferred. The pressure in the first pulverization step is not particularly limited; for example, it can be 30 MPa or more, 50 MPa or more, 70 MPa or more, 100 MPa or more, or 150 MPa or more; for example, it can be 350 MPa or less, 300 MPa or less, 250 MPa or less, 200 MPa or less, or 180 MPa or less; for example, it can be 30-350 MPa, 50-300 MPa, 70-250 MPa, 100-200 MPa, or 150-180 MPa. The particle size D50 of the condensate of the above-mentioned raw material containing alkoxysilane after the first pulverization step is not particularly limited. For example, it can be 25nm or more, 30nm or more, 35nm or more, 40nm or more, or 50nm or more. For example, it can be less than 350nm, less than 300nm, less than 250nm, less than 200nm, or less than 150nm. For example, it can be 25~350nm, 30~300nm, 35~250nm, 40~200nm, or 50~150nm.

[0096] Next, a "concentration step" is performed to concentrate the sol-particle liquid obtained after the first pulverization step. The concentration method in this concentration step is not particularly limited; for example, heating or pressurization can be used, but pressurization is preferred. More specifically, for example, a filter can be used to concentrate the liquid to a given concentration by pressurization, or the dispersion medium can be partially removed by heating to concentrate the liquid to a given concentration. The filter is not particularly limited either; examples include rotary ceramic membrane filters and cross-flow filters. For example, a rotary ceramic membrane filter manufactured by Mitsubishi Chemical Machinery Co., Ltd. under the trade name "Mitsubishi DynaFilter (DyF)" is an example of such a rotary ceramic membrane filter. The concentration of the condensate particles of the above-mentioned raw material containing alkoxysilane in the above-mentioned sol particle liquid after the above-mentioned concentration process is not particularly limited. For example, it can be 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. For example, it can be 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. For example, it can be 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 the solid components (solid elements) in the above-mentioned sol-particle liquid after the above concentration process is not particularly limited. For example, it can be 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. For example, it can be 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, it can be 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.

[0097] Next, a "second pulverization step" is performed to further pulverize the particles in the sol-particle liquid after the concentration step described above. In this process, the method for manufacturing the first dispersion disclosed herein is designed to satisfy at least one of the following conditions: 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. In the method for manufacturing the second dispersion disclosed herein, the method is designed to satisfy at least one of the following conditions: 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 components in the liquid after the second pulverization step is greater than the concentration of the solid components in the liquid after the first pulverization step. The pulverization method for the second pulverization step is not particularly limited; for example, the method described in Japanese Patent No. 7182358 can be used. High-pressure, medium-free pulverization is preferred. The pressure in the second pulverizing step described above is not particularly limited. For example, it can be 30 MPa or more, 50 MPa or more, 70 MPa or more, 100 MPa or more, or 150 MPa or more. Alternatively, it can be 350 MPa or less, 300 MPa or less, 250 MPa or less, 200 MPa or less, or 180 MPa or less. For example, it can be 30-350 MPa, 50-300 MPa, 70-250 MPa, 100-200 MPa, or 150-180 MPa. From the viewpoint of fully utilizing the particle size control effect brought about by the pulverizing process, the pressure in the second pulverizing step described above is preferably not too low. From the viewpoint of suppressing the increase in refractive index caused by excessively small particle size, the pressure in the second pulverizing step described above is preferably not too high. The particle size D50 of the condensate of the above-mentioned raw material containing alkoxysilane after the second pulverization process can be set to 20 nm or more and 400 nm or less, 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, less than 350 nm, less than 300 nm, less than 250 nm, less than 200 nm, less than 150 nm, less than 100 nm or less, or less than 80 nm, for example, 25~350 nm, 30~300 nm, 35~250 nm, 40~200 nm, 50~150 nm or 20~100 nm.

[0098] It should be noted that, from the viewpoint of minimizing the haze value of the low-refractive-index layer produced by the dispersion of this disclosure, the particle size D50 of the condensate containing the alkoxysilane raw material is preferably not large. However, if the D50 is small, the viscosity of the dispersion of this disclosure tends to decrease. In this case, for example, the viscosity of the dispersion of this disclosure can be increased by increasing the concentration of the aforementioned particles or the aforementioned solid components in the dispersion of this disclosure. Furthermore, from the viewpoint of transparency, the particle size D50 of the condensate containing the alkoxysilane raw material is preferably not large.

[0099] Further, a "liquid concentration adjustment step" is performed to adjust the liquid concentration by adding a dispersion medium to the sol-particle liquid after the second pulverization step, thereby producing the dispersion of this disclosure. At this time, the viscosity of the dispersion is not particularly limited, and can be set to 4 mPa·s or more and less than 5000 mPa·s. To ensure the film thickness of the low-refractive-index layer, the viscosity of the dispersion is preferably not too low. To prevent large deviations in the film thickness of the low-refractive-index layer (making it impossible to achieve in-plane film thickness uniformity) or cracks from forming in the low-refractive-index layer during drying, thus preventing the low-refractive-index layer from forming itself, the viscosity of the dispersion is preferably not too high. The viscosity of the dispersion disclosed herein can be, for example, 5 mPa·s or higher, 6 mPa·s or higher, 7 mPa·s or higher, 8 mPa·s or higher, 9 mPa·s or higher, 10 mPa·s or higher, 11 mPa·s or higher, 12 mPa·s or higher, 13 mPa·s or higher, 14 mPa·s or higher, 15 mPa·s or higher, 16 mPa·s or higher, 17 mPa·s or higher, 18 mPa·s or higher, or 20 mPa·s or higher; for example, it can be below 5000 mPa·s, below 4000 mPa·s, or 3500 mPa·s. The concentrations of the condensate particles containing the alkoxysilane-containing raw material in the dispersion are, for example, 16 to 5000 mPa·s, 17 to 4000 mPa·s, 18 to 3500 mPa·s, or 20 to 3000 mPa·s. Furthermore, the concentration of these particles in the dispersion is, for example, within the range of the dispersion produced by the first dispersion manufacturing method of this disclosure, i.e., 3.5% by weight or more. From the viewpoint of ensuring the film thickness of the low refractive index layer, the concentration of these particles in the dispersion of this disclosure is preferably not too low. In addition, to prevent the film thickness deviation of the low refractive index layer from becoming too large (making it impossible to achieve in-plane film thickness uniformity) or to prevent the low refractive index layer from forming due to cracks during drying, the concentration of particles of the condensate of the raw material containing alkoxysilane in the dispersion is preferably not too high.The concentration of the condensate particles of the above-mentioned alkoxysilane-containing raw material in the dispersion of this disclosure can 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, 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. The concentration of the solid component (solid element) in the above-mentioned sol particle liquid after the above-mentioned concentration step is not particularly limited, for example, it is set to be within the range of the dispersion produced by the second dispersion manufacturing method of this disclosure, that is, 3.5% by weight or more. From the viewpoint of ensuring the thickness of the low-refractive-index layer, the concentration of the solid component in the dispersion of this disclosure is preferably not too low. From the viewpoint of suppressing or preventing the deviation of the low-refractive-index layer thickness from increasing (making it impossible to achieve in-plane film thickness uniformity), and preventing the low-refractive-index layer from forming due to cracks generated during drying, the concentration of the solid component in the dispersion of this disclosure is preferably not too high. The concentration of the solid component in the dispersion disclosed herein can 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, 4.2% by weight or more, or 6.0% by weight or more, for example, 39% by weight or less, 38% by weight or less, 37% by weight or less, 36% by weight or less, 35% 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 39% by weight, 3.8 to 38% by weight, 4.0 to 37% by weight, 4.1 to 36% by weight, 4.2 to 35% by weight, or 6.0 to 12.0% by weight. Furthermore, at this time, a crosslinking aid (also called a crosslinking agent), catalyst, etc., that promotes the crosslinking bonding of the particles of the condensate containing the alkoxysilane raw material and is used for the manufacture of a low refractive index layer can be added together with the dispersion medium. The aforementioned crosslinking is not particularly limited, and can be, for example, a bond formed by the particles of the condensate containing the alkoxysilane directly to each other or by means of the aforementioned crosslinking aid through covalent bonds. The aforementioned crosslinking aid is not particularly limited, and can be, for example, a substance having multiple functional groups capable of forming covalent bonds with the particles of the condensate containing the alkoxysilane. Specifically, examples of the aforementioned crosslinking aid include bis(trimethoxysilyl)alkanes. Examples of the aforementioned bis(trimethoxysilyl)alkanes include bis(trimethoxysilyl)hexane. Other examples of the aforementioned crosslinking aid are not particularly limited, such as those described in Japanese Patent No. 7182358.Furthermore, the concentration of the crosslinking aid in the dispersion disclosed herein is not particularly limited, as described, for example, in Japanese Patent No. 7182358. The catalyst is not particularly limited; for example, it can be a photoactive catalyst, a thermally active catalyst, an acid catalyst, or a base catalyst. In addition to the catalyst described above, a catalyst-generating substance (catalyst generator) can be used, or a catalyst-generating substance (catalyst generator) can be used instead of the catalyst described above. For example, in addition to the photoactive catalyst described above, a light-generating substance (photocatalyst generator) can be used, or a light-generating substance (photocatalyst generator) can be used instead of the photoactive catalyst; in addition to the thermally active catalyst described above, a heat-generating substance (thermal catalyst generator) can be used, or a heat-generating substance (thermal catalyst generator) can be used instead of the thermally active catalyst. The photocatalyst generator is not particularly limited, and examples include photoalkali-generating agents (substances that generate alkaline catalysts through light irradiation) and photoacid-generating agents (substances that generate acidic catalysts through light irradiation), with photoalkali-generating agents being preferred. Examples of photoalkali-generating agents include: 9-anthrylmethyl N,N-diethylcarbamate (trade name WPBG-018), (E)-1-[3-(2-hydroxyphenyl)-2-propenoyl]piperidine (trade name WPBG-027), and 1-(anthraquinone-2-yl)ethylimidazolium carboxylate. imidazolecarboxylate (trade name WPBG-140), 2-nitrophenylmethyl 4-methacryloyloxypiperidine-1-carboxylate (trade name WPBG-165), 1,2-diisopropyl-3-[bis(dimethylamino)methylene]guanidinium 2-(3-benzoylphenyl)propionate (trade name WPBG-266), 1,2-dicyclohexyl-4,4,5,5-tetramethylbiguanidinium n-butyltriphenylborate (trade name WPBG-300), and 1,5,7-triazabicyclo[4.4.0]dec-5-ene of 2-(9-oxazan-2-yl)propionate (Tokyo Chemical Industry Co., Ltd.), and compounds containing 4-piperidinemethanol (trade name HDPD-PB100: manufactured by Heraeus Co., Ltd.), etc. It should be noted that all the product names containing "WPBG" mentioned above are product names of Wako Pure Pharmaceutical Co., Ltd.Examples of photoacid-generating agents include: aromatic sulfonium salts (trade name SP-170: ADEKA), triarylsulfonium salts (trade name CPI101A: San-apro), and aromatic iodonium salts (trade name Irgacure250: Ciba Japan). The concentration of the catalyst or catalyst generator in the dispersion disclosed herein is not particularly limited, for example, as described in Japanese Patent No. 7182358.

[0100] The dispersion of this disclosure can be manufactured as described above. However, the method for manufacturing the dispersion of this disclosure is not limited to this; any manufacturing method can be used as long as it meets the conditions of the dispersion of this disclosure described above. For example, the method for manufacturing the dispersion of this disclosure may include steps other than the "first pulverization step," "concentration step," and "second pulverization step" described above, or it may not include them. For example, the liquid concentration adjustment step described above may or may not be performed as needed, and the pulverization step is not limited to the two stages of the first pulverization step and the second pulverization step described above; it may also include three or more stages.

[0101] It should be noted that the method for manufacturing the dispersion disclosed herein can, for example, be configured such that the pressure during the first pulverization step is the same as the pressure during the second pulverization step, and satisfies all of the following relationships (1) to (3). Thus, for example, it has the effect of suppressing light scattering caused by particle size when light is transmitted to the low refractive index layer.

[0102] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the first pulverization process.

[0103] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the second pulverization process.

[0104] The particle size D50 of the first pulverized particles is greater than or equal to the particle size D50 of the second pulverized particles.

[0105] [2. Low-refractive-index layer and its manufacturing method]

[0106] As described above, the low refractive index layer of this disclosure can be obtained by coating the dispersion of this disclosure with the above-described dispersion and then drying it. The layer obtained by coating the dispersion of this disclosure with the above-described dispersion and then drying it as needed can be subjected to heating or light irradiation, for example. Through heating or light irradiation, for example, the particles of the condensate containing the alkoxysilane raw material can be directly crosslinked and bonded to each other, or crosslinked and bonded with the aid of the above-described crosslinking agent, thereby increasing the strength.

[0107] The low-refractive-index layer of this disclosure can be manufactured, for example, by coating the dispersion of this disclosure onto a substrate such as a film and then drying it. The film can be, for example, a resin film. It should be noted that, generally speaking, a thinner film is sometimes referred to as a "film" and a thicker film as a "sheet" for distinction, but this disclosure does not specifically distinguish between "film" and "sheet". The substrate is not particularly limited; for example, substrates made of thermoplastic resins, glass substrates, inorganic substrates represented by silicon, plastics molded from thermosetting resins, semiconductor components, carbon fiber materials represented by carbon nanotubes, etc., are preferred, but this is not a limitation.

[0108] The method for manufacturing the low-refractive-index layer disclosed herein is not particularly limited, and can be manufactured by, for example, by the same method described in International Publication No. 2019 / 065999 or International Publication No. 2019 / 065803.

[0109] The low refractive index layer of this disclosure can be, for example, a porous layer with voids. Alternatively, the low refractive index layer of this disclosure can be, for example, a porous body in which microporous particles are chemically bonded together.

[0110] The thickness of the low-refractive-index layer disclosed herein can be, for example, 500 nm or more, 700 nm or more, 800 nm or more, 1000 nm or more, or 2000 nm or more; for example, it can be less than 10000 nm, less than 8000 nm, less than 5000 nm, less than 4000 nm, or less than 3000 nm; for example, it can be 500-10000 nm, 700-8000 nm, 800-5000 nm, 1000-4000 nm, or 2000-3000 nm. The porosity of the low-refractive-index layer of the present invention can be, for example, 30% or more by volume, 35% or more by volume, 40% or more by volume, 45% or more by volume, or 50% or more by volume; for example, it can be less than 90% by volume, less than 80% by volume, less than 70% by volume, or less than 60% by volume; for example, it can be 30-90% by volume, 35-80% by volume, 40-70% by volume, or 50-60% by volume. The refractive index of the low refractive index layer of the present invention can be, for example, 1.05 or more, 1.10 or more, or 1.13 or more, or, for example, 1.35 or less, 1.30 or less, or 1.25 or less, or, for example, 1.05 to 1.35, 1.10 to 1.30, or 1.13 to 1.25.

[0111] In the low-refractive-index layer of this disclosure, the porosity can be determined by the following method.

[0112] (Methods for determining porosity)

[0113] If the layer being measured for porosity is a single layer containing voids, the ratio (volume ratio) of the layer's constituent material to air can be calculated using conventional methods (e.g., by measuring weight and volume to calculate density), thus allowing the porosity (volume %) to be calculated. Furthermore, since refractive index and porosity are related, the porosity can also be calculated, for example, based on the refractive index value of the layer. Specifically, for example, the porosity can be calculated using the Lorentz-Lorenz formula based on the refractive index value measured using an ellipsometer.

[0114] In this disclosure, the refractive index of the low-refractive-index layer is set as the value of the refractive index at a wavelength of 550 nm, which is determined and calculated by the method described below.

[0115] (Methods for determining refractive index)

[0116] After a low-refractive-index layer is formed on the glass light guide plate, a prism coupler (made by Metrico) is used to incident a laser beam (λ=407nm) from the side of the glass light guide plate. The refractive index at 407nm is calculated based on the measured value of the total internal reflection angle. Furthermore, based on the wavelength dispersion of the low-refractive-index layer monomers calculated separately using an ellipsometer (made by JA Woollam), the measured value of the refractive index at 407nm is converted to the refractive index at 550nm, and this converted value is used as the refractive index of the low-refractive-index layer.

[0117] The thickness deviation of the low-refractive-index layer disclosed herein is preferably 20% or less, 18% or less, 16% or less, 15% or less, or 10% or less. The lower limit is not particularly limited; for example, it can be 0 or a value greater than 0. Regarding the aforementioned thickness deviation, the in-plane film thickness deviation of the low-refractive-index layer is defined as follows: the dispersion of the disclosed material is spin-coated onto a light guide plate with a diameter or short side of 20 cm or less formed from glass or resin with a surface roughness Rz of 50 nm or less. It should be noted that in this disclosure, the in-plane film thickness deviation of the low-refractive-index layer is an index obtained by comparing the standard deviation of the in-plane measurements of the film thickness at five points with the average film thickness.

[0118] [3. Optical components and optical devices]

[0119] As described above, the optical component of this disclosure includes the low refractive index layer of the present invention. The optical component of this disclosure may include or exclude constituent elements other than the low refractive index layer of the present invention.

[0120] The optical components disclosed herein can be, for example, laminates on a substrate to which the low refractive index layer of the present invention is stacked. The substrate is not particularly limited, for example, as described above.

[0121] The optical component disclosed herein can be, for example, a light guide plate with a low refractive index layer of the present disclosure laminated on a light guide plate. In this case, there may be other layers such as an adhesive layer between the light guide plate and the low refractive index layer of the present disclosure, but preferably the low refractive index layer of the present disclosure is directly laminated on the light guide plate without the aid of other layers. In this case, for example, the dispersion 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 manufactured by the above method.

[0122] The optical components disclosed herein are not limited to light guide plates, but may include, for example, polarizing plates, phase difference films, reflective polarizers, brightness enhancement films, diffusion films, pigmented layers, or transparent and opaque layers or films with optical functions.

[0123] The optical device (optical apparatus) disclosed herein is not particularly limited, and may be, for example, an image display device or an illumination device. Examples of image display devices include liquid crystal displays, organic EL (ElectroLuminescence) displays, and micro-LED (Light Emitting Diode) displays. Examples of illumination devices include organic EL illumination.

[0124] Example

[0125] The embodiments of this disclosure will now be described. However, this disclosure is not limited to the following embodiments.

[0126] It should be noted that, in the following reference examples, embodiments, and comparative examples, unless otherwise stated, the parts (relative amounts) of each substance are parts by mass (parts by weight). In the following reference examples, embodiments, and comparative examples, the adhesive (adhesive composition) described later was used as the adhesive. In the following reference examples, embodiments, and comparative examples, "adhesive layer" is equivalent to "adhesive bonding layer." That is, in the following reference examples, embodiments, and comparative examples, unless otherwise stated, "adhesive layer" and "adhesive bonding layer" have the same meaning.

[0127] <Method for determining the concentration of the topical solution>

[0128] The overall concentration (excluding the dispersion medium) of the solid components in the coating solution or the concentration (by weight) of the particles of the condensate of the raw material containing alkoxysilane is calculated based on the ratio of the overall weight (mass) of the coating solution to the overall weight (mass) of the aforementioned solid components in the coating solution or the weight (mass) of the particles of the aforementioned condensate of the raw material containing alkoxysilane.

[0129] <Methods for determining the viscosity of coating solutions>

[0130] The viscosity of the coating solution was measured at a test temperature of 25°C using an E-type viscometer equipped with a 1° conical rotor.

[0131] <Methods for Determining Refractive Index>

[0132] The refractive index was determined using the method described above.

[0133] <Methods for determining particle size>

[0134] The particle size D50 of the condensate containing alkoxysilane was determined using the method described above. It should be noted that, as mentioned earlier, D50 is also known as the median particle size, representing the median particle size of the particle distribution, with a cumulative frequency corresponding to 50%.

[0135] <Methods for Measuring Film Thickness>

[0136] The thickness (thickness) and its deviation of the low-refractive-index layer were measured as follows. For the low-refractive-index layer formed on the glass, the thickness at five points in the plane was measured using a spectroscopic ellipsometer (JA Woollam), and the average value and standard deviation were calculated. The proportion of the standard deviation to the average value was calculated, and this value was taken as the deviation.

[0137] <Evaluation Methods for Light Guiding Properties>

[0138] For a glass plate that is a substrate with a low refractive index layer, the state of guiding light was evaluated by visual observation using an LED that shines light into it from the end, according to the following criteria.

[0139] White cloudiness during light guiding is NG (×)

[0140] No white haze during light guiding (remains transparent) OK (○)

[0141] <Methods for measuring haze>

[0142] A 100mm × 100mm laminate (void layer / glass substrate) was used as the test sample. The test sample was placed in a spectrophotometer (manufactured by Nippon Denshoku Kogyo Co., Ltd.: SH7000), and the haze value was measured. More specifically, regarding the haze value, diffuse transmittance and total transmittance were measured, and the haze value calculated based on these values ​​using the following formula was used as the measured haze value.

[0143] Haze value (%) = [Diffuse transmittance (%) / Total transmittance (%)] × 100 (%)

[0144] [Reference Example 1: Preparation of Gel Pulverizing Solution for Low Refractive Index Layer Formation]

[0145] A gel pulverizing solution (sol particle liquid) for forming low refractive index layers was manufactured as described below.

[0146] (1) Gel formation of silicon compounds

[0147] 9.5 kg of methyltrimethoxysilane (MTMS), a precursor of silicon compounds, was dissolved in 22 kg of dimethyl sulfoxide (DMSO) to prepare mixture A. 5 kg of a 0.01 mol / L aqueous solution of oxalic acid was added to mixture A, and the mixture was stirred at room temperature for 30 minutes, thereby hydrolyzing MTMS to produce mixture B containing tri(hydroxy)methylsilane.

[0148] 3.8 kg of ammonia (28% by weight) and 2 kg of pure water were added to 55 kg of DMSO. Then, the above mixture B was added in addition, and the mixture was stirred at room temperature for 15 minutes to gel the tri(hydroxy)methylsilane, thereby obtaining a mixture C containing a gel-like silicon compound.

[0149] (2) Aging treatment

[0150] The mixture C containing the gel-like silicon compound prepared as described above was poured into a 30cm×30cm×5cm stainless steel container and aged directly at 40°C for 20 hours to perform a maturation treatment.

[0151] (3) Crushing process

[0152] Next, isobutanol, used as a replacement solvent, was poured into the gel synthesized in the aforementioned stainless steel container. The gel was then slowly cut into cuboids measuring 1.5cm × 2cm × 5cm by inserting a cutting tool into the gel from the top. The cut gel was transferred to another container, maintaining its shape, and four times the volume of isobutanol was added. After standing for 6 hours, four solvent replacements were performed. The gel (gel-like silicon compound) was then pulverized using a continuous emulsification dispersion (Milder MDN304, manufactured by Pacific Machinery Co., Ltd.) to obtain a coarsely pulverized liquid. Further, pulverization was performed at 100MPa using a high-pressure medialess pulverizer (Star Burst HJP-25005, manufactured by SUGINO MACHINE). This yielded an isobutanol dispersion (liquid containing the pulverized gel) containing nano-sized particles (the pulverized gel).

[0153] [Example 1]

[0154] IBA (isobutanol) was added to the gel pulverization solution obtained in Reference Example 1 to adjust the particle concentration of the condensate containing the alkoxysilane to 3.5% by weight. Next, the gel pulverization solution was nano-pulverized using Star Burst (a trade name of SUGINOMACHINE) at 150 MPa under high pressure, adjusting the pulverization time, until the particle size D50 of the pulverized particles reached 150 nm, resulting in a nano-pulverized solution with a particle concentration of 3.5% by weight of the condensate containing the alkoxysilane (first pulverization step). Next, the liquid was concentrated using Mitsubishi DynaFilter (DyF) (a trade name of Mitsubishi Chemical Machinery Co., Ltd.) until the particle concentration of the condensate containing the alkoxysilane reached 5.6% by weight (concentration step). Then, the same Star Burst was used again at 150 MPa under high pressure, adjusting the pulverization time, and nano-pulverization was performed until the particle size D50 of the pulverized particles reached 130 nm (second pulverization step). It should be noted that the concentration, viscosity, and particle size of the liquids obtained in each of these processes are shown in Table 1 below. After the second pulverization process described above, 0.22 g of bis(trimethoxysilyl)hexane as a crosslinking aid and 0.22 g of WPBG-266 (Wako Corporation) photocatalyst were added to 100 g of the liquid, and IBA (isobutanol) was further added to adjust the overall solid content concentration of the liquid to 4.2% by weight (the particle concentration of the condensate containing the alkoxysilane raw material was 3.86% by weight), thus producing the dispersion of this disclosure. The dispersion was spin-coated onto a glass plate to form a film, which was then dried and subjected to a 350 mJ / cm² test. 2 UV irradiation at 360 nm crosslinks the particles of the condensate containing alkoxysilane raw materials, thus producing the low refractive index layer of this disclosure. The optical properties of the produced low refractive index layer and the appearance evaluation of the film (low refractive index layer) are summarized in Table 1 below.

[0155] [Example 2]

[0156] In the first pulverization step, the pulverization time was adjusted so that the particle size D50 of the pulverized particles reached 80 nm. In the second pulverization step, the pulverization time was adjusted so that the particle size D50 of the pulverized particles reached 50 nm. Then, the amount of IBA added was changed, and the overall solid component concentration of the liquid was adjusted to 9.5% by weight (the concentration of particles of the condensate containing the alkoxysilane raw material was 9.03% by weight). Otherwise, the dispersion of the present disclosure and the low refractive index layer of the present disclosure were manufactured by the same operation as in Example 1.

[0157] [Example 3]

[0158] In the first pulverization step, the pulverization time was adjusted so that the particle size D50 of the pulverized particles reached 80 nm. In the second pulverization step, the pulverization time was adjusted so that the particle size D50 of the pulverized particles reached 65 nm. Then, the amount of IBA added was changed, and the overall solid component concentration of the liquid was adjusted to 8.0% by weight (the concentration of particles of the condensate of the raw material containing alkoxysilane was 7.73% by weight). Otherwise, the dispersion of the present disclosure and the low refractive index layer of the present disclosure were manufactured by the same operation as in Example 1.

[0159] [Comparative Example 1]

[0160] The second pulverization step was skipped, and the film (low refractive index layer) was directly formed after the concentration step. Otherwise, the low refractive index layer was manufactured in the same manner as in Example 1.

[0161] [Comparative Example 2]

[0162] By changing the order of the concentration process and the second pulverization process, and performing the concentration process after the second pulverization process, a low refractive index layer was manufactured in the same manner as in Example 1.

[0163] [Comparative Example 3]

[0164] A concentration process was performed before the first pulverizing process, but frequent liquid blockage prevented the concentration process from being completed. As a result, the formation of a low-refractive-index layer was not achieved.

[0165] For the low-refractive-index layers of the embodiments and comparative examples manufactured as described above, the optical properties and appearance of the films (low-refractive-index layers) were evaluated using the methods described above. The evaluation results are summarized in Table 1 below. It should be noted that in Table 1 below, "viscosity after the first pulverization process" represents the viscosity of the liquids in the embodiments and comparative examples after the first pulverization process. "concentration after the first pulverization process" represents the overall concentration of the solid components in the liquids in the embodiments and comparative examples after the first pulverization process. "particle concentration after the first pulverization process" represents the concentration of siloxane condensate particles in the liquids in the embodiments and comparative examples after the first pulverization process. "particle size D50 after the first pulverization process" represents the particle size D50 of the siloxane condensate particles in the liquids in the embodiments and comparative examples after the first pulverization process. "viscosity after the concentration process" represents the viscosity of the liquids in the embodiments and comparative examples after the concentration process. "concentration after the concentration process" represents the overall concentration of the solid components in the liquids in the embodiments and comparative examples after the concentration process. "Particle concentration after concentration process" refers to the concentration of siloxane condensate particles in the liquids of the above-described embodiments and comparative examples after the concentration process. "Particle size D50 after concentration process" refers to the particle size D50 of the siloxane condensate particles in the liquids of the above-described embodiments and comparative examples after the concentration process. "Viscosity after second pulverization process" refers to the viscosity of the liquids of the above-described embodiments and comparative examples after the second pulverization process. "Concentration after second pulverization process" refers to the overall concentration of solid components in the liquids of the above-described embodiments and comparative examples after the second pulverization process. "Particle concentration after second pulverization process" refers to the concentration of siloxane condensate particles in the liquids of the above-described embodiments and comparative examples after the second pulverization process. "Particle size D50 after second pulverization process" refers to the particle size D50 of the siloxane condensate particles in the liquids of the above-described embodiments and comparative examples after the second pulverization process. "Refractive index of the low-refractive-index layer" refers to the refractive index of the low-refractive-index layer manufactured in the above-described embodiments and comparative examples. "Thickness of the low-refractive-index layer" refers to the thickness of the low-refractive-index layer manufactured in the above embodiments and comparative examples. "Light guiding property" refers to the evaluation result of the light guiding property of the low-refractive-index layer manufactured in the above embodiments and comparative examples. "Haze" refers to the haze value of the low-refractive-index layer manufactured in the above embodiments and comparative examples.

[0166]

[0167] As shown in Table 1 above, the dispersions (coating solutions) of this disclosure manufactured according to the dispersion manufacturing method in Examples 1-3 all ensured a sufficiently large film thickness when forming a low-refractive-index layer. Furthermore, according to Example 1, since the low-refractive-index layer has good light conductivity, it can be confirmed that a low-refractive-index layer with small film thickness deviation (achieving in-plane film thickness uniformity) can be manufactured. In contrast, the low-refractive-index layers of Comparative Example 1 (which did not perform the second pulverization step) and Comparative Example 2 (which did not perform the concentration step and the second pulverization step in the order of this disclosure) had poor light conductivity, thus confirming a large film thickness deviation (failing to achieve in-plane film thickness uniformity). Additionally, Comparative Example 3 (which performed the concentration step before the first pulverization step, but not in the order of this disclosure) frequently experienced liquid blockage, failing to complete the concentration step, and consequently, also failed to form a low-refractive-index layer.

[0168] The present disclosure has been described above with reference to the embodiments and examples, but the present disclosure is not limited to the embodiments and examples described above. Various modifications that can be understood by those skilled in the art can be made to the structure and details of the present disclosure within its scope. Furthermore, each embodiment can be appropriately combined with other embodiments.

[0169] This disclosure may also be described, for example, as shown in the following notes. However, the following notes are examples, and this disclosure is not limited to these methods.

[0170] (Postscript 1)

[0171] A manufacturing method for producing a dispersion of particles dispersed in a dispersion medium, wherein...

[0172] The particles are condensates of raw materials containing alkoxysilanes.

[0173] The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially.

[0174] The first pulverizing step is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium.

[0175] The concentration process is a process of concentrating the liquid.

[0176] The second pulverizing step is a step of further pulverizing the particles in the liquid after the first pulverizing step.

[0177] 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 particles in the liquid after the second pulverization step is greater than the concentration of particles in the liquid after the first pulverization step.

[0178] The concentration of the particles in the manufactured dispersion is 3.5% by weight or more.

[0179] (Postscript 2)

[0180] A manufacturing method comprising dispersing a solid component containing particles in a dispersion medium, wherein...

[0181] The particles are condensates of raw materials containing alkoxysilanes.

[0182] The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially.

[0183] The first pulverizing step is a step of pulverizing the particles in a liquid in which the solid components are dispersed in the dispersion medium.

[0184] The concentration process is a process of concentrating the liquid.

[0185] The second pulverizing step is a step of further pulverizing the particles in the liquid after the first pulverizing step.

[0186] 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 component in the liquid after the second pulverization step is greater than the concentration of the solid component in the liquid after the first pulverization step.

[0187] The concentration of the solid component in the manufactured dispersion is 3.5% by weight or more.

[0188] (Note 3)

[0189] According to the manufacturing method described in Appendix 1 or 2, wherein,

[0190] The pressure during the first crushing process is at or below the same level as the pressure during the second crushing process, and satisfies all of the following relationships (1) to (3):

[0191] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the first pulverization (1).

[0192] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the second pulverization (2).

[0193] The particle size D50 of the first pulverized particle is greater than or equal to the particle size D50 of the second pulverized particle (3).

[0194] (Note 4)

[0195] According to the manufacturing method described in Appendix 1 or 2, wherein,

[0196] The pressure during the first crushing process is greater than the pressure during the second crushing process, and all of the following relationships (1) to (3) are satisfied:

[0197] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the first pulverization (1).

[0198] The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the second pulverization (2).

[0199] The particle size D50 of the first pulverized particles is less than or equal to the particle size D50 of the second pulverized particles (3).

[0200] (Note 5)

[0201] The manufacturing method according to any one of Appendices 1 to 4, wherein,

[0202] The pressure in the first crushing process is above 50 MPa.

[0203] (Note 6)

[0204] A dispersion, which is manufactured by any one of the manufacturing methods described in Appendix 1 to 5.

[0205] (Note 7)

[0206] A low refractive index layer is obtained by coating with the dispersion described in Appendix 6 and then drying it.

[0207] (Postscript 8)

[0208] According to Appendix 7, the low refractive index layer has a refractive index of 1.25 or less.

[0209] (Note 9)

[0210] The low-refractive-index layer, as described in Appendix 7 or 8, has a thickness of 800 nm or more.

[0211] (Postscript 10)

[0212] An optical component comprising a low refractive index layer as described in any one of Appendices 7 to 9.

[0213] (Postscript 11)

[0214] An optical device comprising the optical components described in Appendix 10.

[0215] (Postscript 12)

[0216] A method for manufacturing a low refractive index layer, the method comprising:

[0217] The process of manufacturing the dispersion by any one of the manufacturing methods described in Appendices 1 to 5,

[0218] The process of coating the dispersion onto the substrate, and

[0219] The process of drying the dispersion after coating.

[0220] (Postscript 13)

[0221] According to the manufacturing method described in Appendix 12, wherein,

[0222] The refractive index of the manufactured low-refractive-index layer is below 1.25.

[0223] (Postscript 14)

[0224] According to the manufacturing method described in Appendix 12 or 13, wherein,

[0225] The thickness of the low-refractive-index layer manufactured is above 800 nm.

[0226] (Postscript 15)

[0227] A method for manufacturing an optical component, comprising a low-refractive-index layer, the method comprising:

[0228] The low-refractive-index layer is manufactured by any one of the manufacturing methods described in Appendices 12 to 14.

[0229] (Postscript 16)

[0230] A method for manufacturing an optical device, comprising optical components, the method comprising:

[0231] The optical component is manufactured using the manufacturing method described in Appendix 15.

[0232] Industrial applicability

[0233] As described above, according to this disclosure, a method for manufacturing a dispersion capable of ensuring the film thickness of a low-refractive-index layer and achieving in-plane film thickness uniformity can be provided, along with the dispersion, the low-refractive-index layer, optical components, and optical devices. The application of this disclosure is not particularly limited. For example, the optical devices disclosed are not particularly limited, and examples include image display devices and illumination devices. Examples of such image display devices include liquid crystal displays, organic EL displays, and micro-LED displays. Examples of such illumination devices include organic EL illumination.

[0234] This application claims priority based on Japanese Patent Application No. 2024-026039, filed on February 22, 2024, the entire disclosure of which is incorporated herein by reference.

Claims

1. A manufacturing method for producing a dispersion of particles dispersed in a dispersion medium, wherein, The particles are condensates of raw materials containing alkoxysilanes. The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially. The first pulverizing step is a step of pulverizing the particles in a liquid in which the particles are dispersed in the dispersion medium. The concentration process is a process of concentrating the liquid. The second pulverizing step is a step of further pulverizing the particles in the liquid that have been pulverized in the first pulverizing 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 particles in the liquid after the second pulverization step is greater than the concentration of particles in the liquid after the first pulverization step. The concentration of the particles in the manufactured dispersion is 3.5% by weight or more.

2. A manufacturing method comprising a dispersion of a solid component containing particles dispersed in a dispersion medium, wherein, The particles are condensates of raw materials containing alkoxysilanes. The first pulverizing step, the concentration step, and the second pulverizing step are performed sequentially. The first pulverizing step is a step of pulverizing the particles in a liquid in which the solid components are dispersed in the dispersion medium. The concentration process is a process of concentrating the liquid. The second pulverizing step is a step of further pulverizing the particles in the liquid after the first pulverizing 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 component in the liquid after the second pulverization step is greater than the concentration of the solid component in the liquid after the first pulverization step. The concentration of the solid component in the manufactured dispersion is 3.5% by weight or more.

3. The manufacturing method according to claim 1 or 2, wherein, The pressure during the first crushing process is at or below the same level as the pressure during the second crushing process, and satisfies all of the following relationships (1) to (3): The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the first pulverization (1). The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the second pulverization (2). The particle size D50 of the first pulverized particle is greater than or equal to the particle size D50 of the second pulverized particle (3).

4. The manufacturing method according to claim 1 or 2, wherein, The pressure during the first crushing process is greater than the pressure during the second crushing process, and all of the following relationships (1) to (3) are satisfied: The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the first pulverization (1). The particle size D50 of the particles after the concentration process is greater than the particle size D50 of the particles after the second pulverization (2). The particle size D50 of the first pulverized particles is less than or equal to the particle size D50 of the second pulverized particles (3).

5. The manufacturing method according to any one of claims 1 to 4, wherein, The pressure in the first crushing process is above 50 MPa.

6. A dispersion, which is manufactured by the manufacturing method according to any one of claims 1 to 5.

7. A low refractive index layer obtained by coating with the dispersion of claim 6 and drying it.

8. The low refractive index layer according to claim 7, wherein the refractive index is 1.25 or less.

9. The low refractive index layer according to claim 7 or 8, wherein the thickness is 800 nm or more.

10. An optical component comprising a low refractive index layer as described in any one of claims 7 to 9.

11. An optical device comprising the optical component of claim 10.

12. A method for manufacturing a low refractive index layer, the method comprising: The process of manufacturing the dispersion by the manufacturing method according to any one of claims 1 to 5 The process of coating the dispersion onto the substrate, and The process of drying the dispersion after coating.

13. The manufacturing method according to claim 12, wherein, The refractive index of the manufactured low-refractive-index layer is below 1.

25.

14. The manufacturing method according to claim 12 or 13, wherein, The thickness of the low-refractive-index layer manufactured is above 800 nm.

15. A method for manufacturing an optical component, comprising a low-refractive-index layer, the method comprising: The low-refractive-index layer is manufactured by the manufacturing method according to any one of claims 12 to 14.

16. A method for manufacturing an optical device, comprising optical components, the method comprising: The optical component is manufactured using the manufacturing method described in claim 15.

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