Particle dispersion liquid

Abstract

The present invention provides a particle dispersion containing particles and a liquid medium, the distance between the HSP value of the particles and the HSP value of the liquid medium being 5.50 MPa 0.5 or less.

Description

Technical Field

[0001] The present invention relates to a particle dispersion and the like. Background Art

[0002] In order to manufacture various industrial parts, a particle dispersion containing particles dispersed in a liquid medium is used. For example, Patent Document 1 listed below describes a particle dispersion using silica particles.

[0003] Previous technical literature

[0004] Patent Literature

[0005] Patent Document 1: Japanese Patent Application No. 2015-519442 Summary of the invention

[0006] Technical issues to be solved by the invention

[0007] In a particle dispersion containing particles dispersed in a liquid medium, the particles may aggregate. In this case, excellent dispersibility is required for the particle dispersion when performing a dispersion treatment.

[0008] One object of the present invention is to provide a particle dispersion having excellent dispersibility when subjected to a dispersion treatment.

[0009] Means for solving technical problems

[0010] The present invention, in some aspects, relates to the following [1] to

[14] , etc.

[0011] [1] A particle dispersion comprising particles and a liquid medium, wherein the distance between the HSP value of the particles and the HSP value of the liquid medium is 5.50 MPa 0.5 the following.

[0012] [2] The particle dispersion according to [1], wherein

[0013] The liquid medium comprises an organic solvent.

[0014] [3] The particle dispersion according to [1], wherein

[0015] The liquid medium includes various organic solvents.

[0016] [4] The particle dispersion according to [3], wherein

[0017] The liquid medium includes methyl isobutyl ketone and toluene.

[0018] [5] The particle dispersion according to any one of [2] to [4], wherein

[0019] The content of the organic solvent is 80% by mass or more based on the total mass of the liquid medium.

[0020] [6] The particle dispersion according to any one of [1] to [5], wherein

[0021] The particles include inorganic particles.

[0022] [7] The particle dispersion according to any one of [1] to [6], wherein

[0023] The particles include at least one selected from the group consisting of silicon dioxide, ceria, aluminum oxide, titanium dioxide, boron nitride, and calcium titanate.

[0024] [8] The particle dispersion according to any one of [1] to [7], wherein

[0025] The particles comprise silicon dioxide.

[0026] [9] The particle dispersion according to any one of [1] to [8], wherein

[0027] The particles have a surface treatment agent on the surface of the particles.

[0028]

[10] The particle dispersion according to [9], wherein

[0029] The surface treatment agent includes a silane compound having an alkoxysilyl group.

[0030]

[11] The particle dispersion according to any one of [1] to

[10] , wherein

[0031] The particle size D50 at the cumulative 50% in the volume-based cumulative particle size distribution of the particles is 0.1 to 20 μm.

[0032]

[12] The particle dispersion according to any one of [1] to

[11] , wherein

[0033] The specific gravity of the particles is 1.0 to 8.0 g / cm 3 .

[0034]

[13] The particle dispersion according to any one of [1] to

[12] , wherein

[0035] The content of the particles (including the content of the surface treatment agent when the particles are surface treated) is 30 to 90% by mass based on the total mass of the particle dispersion.

[0036]

[14] The particle dispersion according to any one of [1] to

[13] , wherein

[0037] At 25°C and shear rate of 1 min -1 The viscosity is 350 mPa·s or more.

[0038] Effects of the Invention

[0039] According to one aspect of the present invention, it is possible to provide a particle dispersion liquid having excellent dispersibility when a dispersion treatment is performed. DETAILED DESCRIPTION

[0040] Hereinafter, embodiments of the present invention will be described, but the present invention is not limited to these embodiments at all.

[0041] In this specification, the numerical range represented by "~" means a range that includes the numerical values ​​recorded before and after "~" as the minimum and maximum values, respectively. In the numerical range recorded in stages in this specification, the upper limit or lower limit of the numerical range of a certain stage can be arbitrarily combined with the upper limit or lower limit of the numerical range of another stage. In the numerical range recorded in this specification, the upper limit or lower limit of the numerical range can be replaced by the value shown in the embodiment. "A or B" includes either A and B, or both. Unless otherwise specified, the materials exemplified in this specification can be used alone or in combination of two or more. In the case where there are a variety of substances equivalent to each component in the composition, unless otherwise specified, the content of each component in the composition represents the total amount of the multiple substances present in the composition.

[0042] The particle dispersion according to the present embodiment includes particles and a liquid medium, and the distance between the HSP value of the particles and the HSP value of the liquid medium (hereinafter referred to as "HSP distance between the particles and the liquid medium" as the case may be) is 5.50 MPa. 0.5 the following.

[0043] The particle dispersion involved in the present embodiment has excellent dispersibility (dispersibility of particles) when the dispersion treatment is performed. According to the present inventors' understanding, the dispersibility of particles is preferably compared under the same solid content. By comparing under the solid content of 3% by mass, the difference in dispersibility can be easily confirmed and the dispersibility can be appropriately evaluated. The particle dispersion involved in the present embodiment has excellent dispersibility when the solid content is adjusted to 3% by mass immediately after the mixed solution containing the components of the mixed particle dispersion is subjected to dispersion treatment (for example, dispersion treatment based on pitting corrosion). According to the particle dispersion involved in this embodiment, in the evaluation shown in the examples described later (evaluation when the solid content is adjusted to 3% by mass immediately after the dispersion treatment is performed), the volume fraction of particles with a particle size of D100 or more in a polydisperse state with a particle size variation coefficient (CV: Coefficient of Variation) of 20 or more, or the volume fraction of particles with a particle size of twice the particle size D50 in a monodisperse state with a particle size variation coefficient of less than 20, can be, for example, 7.0% or less (preferably 5.0% or less or less than 5.0%). When the solid content of the particle dispersion is 3% by mass, the evaluation can be performed without adjusting the solid content. The solid content of the particle dispersion can be adjusted by diluting it with a liquid medium of the same composition as the liquid medium of the particle dispersion, or by volatilizing the liquid medium of the particle dispersion.

[0044] In a particle dispersion containing particles dispersed in a liquid medium, the particles may aggregate over time. In contrast, according to one mode of the particle dispersion involved in the present embodiment, even when the particle dispersion just after the dispersion treatment is stored, excellent dispersion stability (storage stability) can be obtained. According to one mode of the particle dispersion involved in the present embodiment, in the evaluation shown in the examples described below (the particle dispersion just after the dispersion treatment is left to stand for 7 days and the solid content is adjusted to 3% by mass), the volume fraction of particles with a particle size of more than 20 in a polydisperse state with a particle size variation coefficient of more than 20 or the volume fraction of particles with a particle size of more than 2 times the particle size D50 in a monodisperse state with a particle size variation coefficient of less than 20 can be obtained, for example, 20.0% or less (preferably 12.0% or less or 5.0% or less).

[0045] According to one mode of the particle dispersion involved in the present embodiment, in the evaluation shown in the later described example (evaluation when the solid content is adjusted to 3 mass % after the particle dispersion just after the dispersion treatment is left to stand for 30 days), the volume fraction of particles with a particle size of D100 or more in a polydisperse state with a particle size variation coefficient of 20 or more, or the volume fraction of particles with a particle size of twice the particle size D50 in a monodisperse state with a particle size variation coefficient of less than 20, can be obtained, for example, 30.0% or less (preferably 15.0% or less or 10.0% or less).

[0046] The purpose of the particle dispersion involved in the present embodiment is not particularly limited. The particle dispersion involved in the present embodiment can be applied to the manufacture or use of laminated plates (copper-clad laminated plates, etc.), grain bonding films, circuit connection components, polishing liquids (CMP polishing liquids, etc.), sealing materials, battery electrode active materials, transfer-type transparent conductive films, etc. For example, the particle dispersion involved in the present embodiment can be used for the manufacture of semiconductor components, and can be used as a slurry for obtaining laminated plates, insulating films (insulating films of sealing materials, etc.) of semiconductor components, etc.

[0047] The HSP distance of a particle relative to the liquid medium can be determined based on the δ d (dispersion term), δ p (polar term) and δ h (hydrogen bond term) and calculated by the following formula. d1 , δ p1 and δ h1 is the particle's δ d , δ p and δ h , δ d2 , δ p2 and δ h2 is the δ of the liquid medium d , δ p and δ h .

[0048] HSP distance = {4×(δ d1 -δ d2 ) 2 +(δ p1 -δ p2 ) 2 +(δ h1 -δ h2 ) 2} 0.5

[0049] Since the δ d , δ p and δ hSince there is a known information source such as a database, for example, the δ of a desired substance can be obtained by referring to the database. d , δ p and δ h The parameters of substances not registered in the database can be calculated using computer software such as HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi).

[0050] Delta of particles d1 , δ p1 and δ h1 It can be calculated by the following procedure. First, the particle dispersion is dried to recover the particles, and the parameter (δ d , δ p and δ h ) are 16 known evaluation solvents. Next, a dispersibility test of the particles of the evaluation object with respect to each evaluation solvent is performed to determine whether each evaluation solvent is a "solvent with excellent dispersibility" or a "solvent with poor dispersibility". The dispersibility test can be performed by the method described in the examples below. Next, in the case of δ d , δ p and δ h After plotting each evaluation solvent in the three-dimensional space (Hansen space) of the coordinate axis, a virtual sphere is created in the three-dimensional space that does not include all "solvents with poor dispersibility" but includes all "solvents with excellent dispersibility". Then, the δ d , δ p and δ h Delta as a particle d1 , δ p1 and δ h1 .

[0051] δ d1 , δ p1 and δ h1 The particle size varies depending on the type of particle material, particle size, particle size distribution (coefficient of variation of particle size), surface treatment content (type of surface treatment agent, amount of surface treatment agent used, surface treatment method, etc.). For example, the larger the particle size, the smaller the particle size. d1 tends to increase, δ p1 and δ h1 And, the larger the coefficient of variation of particle size, the greater the p1 tends to increase, δ h1 The δ of the surface treated particles d1 , δ p1 and δ h1The entire surface-treated particle is taken as the object, taking into account the influence of the surface treatment. d1 , δ p1 and δ h1 , the value at 25°C can be used.

[0052] δ of liquid medium d2 , δ p2 and δ h2 It can be calculated based on the composition of the liquid medium in the particle dispersion. When the liquid medium is a mixture of multiple components, the δ d2 , δ p2 and δ h2 Can be used as the parameters of each component (δ d , δ p or δ h ) and the product of the volume ratio of each component to the entire mixture. d , δ p and δ h , the values ​​in the database of the analysis software HSPiP (Hansen Solubility Parameter in Practice; written by Prof.Steven Abbottand Dr.Yamamoto Hiroshi) can be used. Parameters of components not registered in the database (δ d , δ p and δ h ) can be calculated using a structural analysis software called SMILES. d2 , δ p2 and δ h2 , the value at 25°C can be used.

[0053] The present inventors have found that adjusting the HSP distance of the particles relative to the liquid medium is effective for adjusting the dispersibility of the particles. 0.5 Hereinafter, the particle dispersion involved in the present embodiment has excellent dispersibility. Regarding the main reason for obtaining such an effect, it can be inferred that if the HSP distance is within the above range, the particles and the liquid medium are easily mixed with each other thermodynamically, so excellent dispersibility can be obtained. However, the main reason for obtaining the effect is not limited to this content.

[0054] From the perspective of adjusting the dispersibility, the HSP distance (unit: MPa) of the particle relative to the liquid medium is 0.5) can be in the following ranges. The HSP distance of the particle relative to the liquid medium can be 5.40 or less, 5.35 or less, 5.30 or less, 5.25 or less, 5.20 or less, 5.15 or less, 5.10 or less, 5.05 or less, 5.00 or less, 4.90 or less, 4.80 or less, 4.70 or less, 4.50 or less, 4.30 or less, 4.10 or less, 4.00 or less, 3.90 or less, 3.70 or less, 3.60 or less, 3.50 or less, or 3.45 or less. The HSP distance of the particle relative to the liquid medium may exceed 0, 0.50 or more, 1.00 or more, 1.50 or more, 2.00 or more, 2.50 or more, 3.00 or more, 3.40 or more, 3.45 or more, 3.50 or more, 3.60 or more, 3.70 or more, 3.90 or more, 4.00 or more, 4.10 or more, 4.30 or more, 4.50 or more, 4.70 or more, 4.80 or more, 4.90 or more, 5.00 or more, 5.05 or more, 5.10 or more, 5.15 or more, 5.20 or more, 5.25 or more, or 5.30 or more. From these viewpoints, the HSP distance of the particle relative to the liquid medium may exceed 0 and be 5.50 or less, 3.00 to 5.50, or 3.00 to 5.40.

[0055] In the particle dispersion according to the present embodiment, at least a portion of the particles may be dispersed in a liquid medium. The particles constitute a solid component in the particle dispersion. The particles may be inorganic particles or organic particles.

[0056] As constituent materials of inorganic particles, oxides such as silicon dioxide, cerium dioxide, aluminum oxide, titanium dioxide, zirconium oxide, magnesium oxide, yttrium oxide, zinc oxide, and iron oxide can be cited; nitrides such as silicon nitride, titanium nitride, and boron nitride; hydroxides such as cerium hydroxide; metal materials such as copper, nickel, gold, silver, tin, zinc, nickel, platinum, bismuth, indium, and antimony; silicon carbide; calcium carbonate; aluminum sulfate; barium sulfate; potassium titanate; barium titanate; calcium titanate, etc. Inorganic particles can be made by a melting method, a sol-gel method, a liquid phase method, etc. As constituent materials of organic particles, resin materials can be used, and acrylic resins, styrene resins, urea-formaldehyde resins, phenolic resins, epoxy resins, benzoguanamine resins, etc. can be cited. The constituent materials of the particles can be used alone or in combination of two or more. From the viewpoint of easily obtaining excellent dispersibility, the particles may include inorganic particles, may include non-metallic materials, may include at least one selected from the group consisting of silica, ceria, alumina, titania, boron nitride and calcium titanate, and may include silica.

[0057] The particles may or may not be subjected to surface treatment. The particles subjected to surface treatment may have a surface treatment agent on the surface of the particles. The surface treatment method may be a dry treatment or a wet treatment.

[0058] As the surface treatment agent, there can be mentioned silane compounds (e.g., silane coupling agents), titanium compounds (e.g., titanium coupling agents), aluminate compounds (e.g., aluminate coupling agents), etc. The surface treatment agent may have an alkoxy group, an alkoxysilyl group, a phenyl group, a vinyl group, an epoxy group, an acryl group, a methacryloyl group, an amino group, a urea group, a mercapto group, an isocyanate group, etc. From the viewpoint of easily obtaining excellent dispersibility, the surface treatment agent may contain a silane compound, or may contain a silane compound having an alkoxysilyl group.

[0059] From the viewpoint of easily obtaining excellent dispersibility, the silane compound as a silane compound having an alkoxysilyl group may include a silane compound having an alkoxy group bonded to a silicon atom. In the silane compound, from the viewpoint of easily obtaining excellent dispersibility, the number of alkoxy groups bonded to a silicon atom may be 1 to 4, 1 to 3, 2 to 3, or 3 to 4.

[0060] From the viewpoint of easily obtaining excellent dispersibility, the silane compound may include a silane compound having a nitrogen-containing organic group. As the nitrogen-containing organic group, alkylamino, alkylaminoalkyl, arylamino, arylaminoalkyl, heteroarylamino, heteroarylaminoalkyl, etc. may be cited. From the viewpoint of easily obtaining excellent dispersibility, the nitrogen-containing organic group may include an arylaminoalkyl, a phenylaminoalkyl, or a phenylaminopropyl.

[0061] As the silane compound, N-phenyl-3-aminopropyl trimethoxysilane, phenyl trimethoxysilane, vinyl trimethoxysilane, epoxy trimethoxysilane, methacrylic acid trimethoxysilane, amino trimethoxysilane, urea trimethoxysilane, mercaptopropyl trimethoxysilane, isocyanate propyl trimethoxysilane, phenyl amino trimethoxysilane, acrylic acid trimethoxysilane, p-styrene trimethoxysilane, 3-acryloxypropyl trimethoxysilane, 3-methacryloxypropyl trimethoxysilane, 3-isocyanate propyl trimethoxysilane, 3-aminopropyl trimethoxysilane, etc. can be mentioned. From the viewpoint of easily obtaining excellent dispersibility, the silane compound can contain N-phenyl-3-aminopropyl trimethoxysilane.

[0062] The content of the surface treatment agent can be within the following range relative to 100 parts by mass of the particles (excluding the content of the surface treatment agent). From the viewpoint of easily obtaining excellent dispersibility, the content of the surface treatment agent can be 0.01 parts by mass or more, 0.05 parts by mass or more, 0.1 parts by mass or more, 0.3 parts by mass or more, 0.5 parts by mass or more, 0.8 parts by mass or more, or 1.0 parts by mass or more. From the viewpoint of easily obtaining excellent dispersibility, the content of the surface treatment agent can be 10 parts by mass or less, 8.0 parts by mass or less, 5.0 parts by mass or less, 3.0 parts by mass or less, 2.0 parts by mass or less, 1.5 parts by mass or less, or 1.0 parts by mass or less. The content of the surface treatment agent can be 0.8 parts by mass or less or 0.5 parts by mass or less. From these viewpoints, the content of the surface treatment agent can be 0.01 to 10 parts by mass, 0.05 to 5.0 parts by mass, or 0.1 to 2.0 parts by mass.

[0063] From the viewpoint of adjusting dispersibility, the particle diameter D50 at the cumulative 50% in the volume-based cumulative particle size distribution of the particles may be within the following range. The particle diameter D50 may be 0.1 μm or more, more than 0.1 μm, 0.3 μm or more, 0.5 μm or more, 0.8 μm or more, 1.0 μm or more, 1.2 μm or more, 1.5 μm or more, 1.8 μm or more, 2.0 μm or more, 2.2 μm or more, or 2.5 μm or more. The particle size D50 may be 20 μm or less, 15 μm or less, 10 μm or less, 9.0 μm or less, 8.0 μm or less, 7.0 μm or less, 6.0 μm or less, 5.0 μm or less, 4.0 μm or less, 3.0 μm or less, 2.8 μm or less, 2.5 μm or less, 2.2 μm or less, 2.0 μm or less, 1.8 μm or less, 1.5 μm or less, 1.2 μm or less, 1.0 μm or less, 0.8 μm or less, or 0.5 μm or less. From these viewpoints, the particle size D50 may be 0.1 to 20 μm, 0.5 to 20 μm, or 0.5 to 3.0 μm.

[0064] From the viewpoint of adjusting dispersibility and facilitating obtaining a varnish suitable for manufacturing an insulating film of a laminated board, the particle diameter D95 at the cumulative 95% in the volume-based cumulative particle size distribution of the particles may be within the following range. The particle diameter D95 may be 0.3 μm or more, 0.5 μm or more, 1.0 μm or more, 1.5 μm or more, 2.0 μm or more, 2.5 μm or more, 3.0 μm or more, 3.5 μm or more, 4.0 μm or more, or 4.5 μm or more. The particle size D95 can be 30 μm or less, 25 μm or less, 20 μm or less, 15 μm or less, 10 μm or less, 9.0 μm or less, 8.0 μm or less, 7.0 μm or less, 6.0 μm or less, 5.0 μm or less, 4.5 μm or less, 4.0 μm or less, 3.5 μm or less, 3.0 μm or less, 2.5 μm or less, 2.0 μm or less, 1.5 μm or less, 1.0 μm or less, or 0.6 μm or less. From these viewpoints, the particle size D95 can be 0.3 to 30 μm, 0.5 to 30 μm, or 0.5 to 5.0 μm.

[0065] The cumulative particle size distribution for obtaining the particle size D50 and the particle size D95 can be measured by a laser diffraction / scattering method.

[0066] From the perspective of adjusting the dispersibility, the specific gravity of the particles (unit: g / cm 3 ) can be within the following ranges. The specific gravity of the particles can be greater than 0.1, greater than 0.5, greater than 1.0, greater than 1.5, or greater than 2.0. The specific gravity of the particles can be less than 8.0, less than 7.0, less than 6.0, less than 5.0, less than 4.0, less than 3.0, or less than 2.5. From these viewpoints, the specific gravity of the particles can be 0.1 to 8.0, 1.0 to 8.0, or 1.0 to 5.0.

[0067] From the perspective of adjusting the dispersibility, the particle δ d1 (Unit: MPa 0.5 ) can be within the following range. d1 It may be 10.0 or more, 11.0 or more, 12.0 or more, 13.0 or more, 14.0 or more, 15.0 or more, 16.0 or more, 16.5 or more, 17.0 or more, 17.5 or more, or 18.0 or more. d1 It can be 25.0 or less, 22.0 or less, 20.0 or less, 19.5 or less, 19.0 or less, 18.5 or less, 18.0 or less, 17.5 or less, 17.0 or less, or 16.5 or less. From these viewpoints, the δ of the particle is d1 It may be 10.0 to 25.0, 16.0 to 20.0, or 16.5 to 19.0.

[0068] From the perspective of adjusting the dispersibility, the particle δp1 (Unit: MPa 0.5 ) can be within the following range. p1 It may be 1.0 or more, 1.5 or more, 2.0 or more, 2.5 or more, 3.0 or more, 3.5 or more, 4.0 or more, 4.5 or more, 5.0 or more, 5.5 or more, 6.0 or more, 6.5 or more, 7.0 or more, or 7.5 or more. p1 It can be 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, 3.5 or less, or 3.0 or less. From these viewpoints, the δ of the particle is preferably 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, 3.5 or less, p1 It may be 1.0 to 15.0, 2.0 to 10.0, or 2.5 to 8.0.

[0069] From the perspective of adjusting the dispersibility, the particle δ h1 (Unit: MPa 0.5 ) can be within the following range. h1 It may be 1.0 or more, 1.5 or more, 2.0 or more, 2.5 or more, 3.0 or more, 3.5 or more, 4.0 or more, 4.5 or more, 5.0 or more, 5.5 or more, 6.0 or more, 6.5 or more, 7.0 or more, 7.5 or more, or 8.0 or more. h1 It can be 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, or 6.0 or less. From these viewpoints, the δ of the particle is h1 It may be 1.0 to 15.0, 3.0 to 10.0, or 5.0 to 8.5.

[0070] From the viewpoint of easily obtaining excellent dispersibility, the content of inorganic particles (excluding the content of the surface treatment agent when the particles are surface treated) can be 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass, based on the total mass of the particles (the total amount of the particles contained in the particle dispersion. When the particles are surface treated, the content of the surface treatment agent is not included).

[0071] As the content of particles (including the content of the surface treatment agent when the particles are surface treated), the content of particles (excluding the content of the surface treatment agent when the particles are surface treated), the content of inorganic particles (including the content of the surface treatment agent when the particles are surface treated) or the content of inorganic particles (excluding the content of the surface treatment agent when the particles are surface treated), from the viewpoint of adjusting dispersibility, the content A1 can be within the following ranges based on the total mass of the particle dispersion. The content A1 can be 0.1% by mass or more, 0.5% by mass or more, 1% by mass or more, 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, 25% by mass or more, 30% by mass or more, 35% by mass or more, 40% by mass or more, 45% by mass or more, 50% by mass or more, 55% by mass or more, 60% by mass or more, 65% by mass or more, 70% by mass or more, or 75% by mass or more. The content A1 may be 99% by mass or less, 95% by mass or less, 90% by mass or less, 85% by mass or less, 80% by mass or less, 75% by mass or less, 70% by mass or less, 65% by mass or less, 60% by mass or less, 55% by mass or less, 50% by mass or less, or 45% by mass or less. From these viewpoints, the content A1 may be 0.1 to 99% by mass, 20 to 95% by mass, or 30 to 90% by mass.

[0072] As the liquid medium, organic solvents, water, resin materials (for example, resin materials that are liquid at 25°C) and the like can be cited. Organic solvents are a general term for organic compounds that have the property of dissolving other substances, and are widely used in coating, cleaning, printing, and the like. The organic solvent can be liquid at 25°C. In the particle dispersion involved in the present embodiment, only one of the organic solvent, water, and resin materials can be used, or at least two of the organic solvent, water, and resin materials can be used in combination. The organic solvent and the resin material can be used alone or in combination of two or more.

[0073] Examples of the organic solvent include ketone compounds such as methyl isobutyl ketone (MIBK), methyl ethyl ketone (MEK), acetone, cyclohexanone, acetophenone, and benzophenone; aromatic hydrocarbon compounds such as benzene, toluene, and xylene; aliphatic hydrocarbon compounds such as pentane, hexane, heptane, octane, nonane, and decane; alicyclic hydrocarbon compounds such as cyclohexane, methylcyclohexane, and decalin; chlorinated hydrocarbon compounds such as chlorobenzene, dichlorobenzene, trichlorobenzene, dichloromethane, chloroform, carbon tetrachloride, and tetrachloroethylene; methanol, ethanol, n-propanol, isopropanol, 1-butanol, 2-butanol, tert-butanol, 1-pentanol , 2-pentanol, 3-pentanol, 2-ethyl-1-hexanol, cyclohexanol, benzyl alcohol and other alcohols; ether compounds such as ethyl ether, ethylene glycol monomethyl ether, anisole, phenyl ether, dioxane, tetrahydrofuran and other ether compounds; ester compounds such as ethyl acetate, butyl acetate, benzyl benzoate, γ-butyrolactone and other ester compounds; nitrile compounds such as acetonitrile; sulfoxide compounds such as dimethyl sulfoxide, diethyl sulfoxide, dipropyl sulfoxide, diphenyl sulfoxide and other sulfoxide compounds; amide compounds such as formamide, 1-methyl-2-pyrrolidone, N-methyl-2-pyrrolidone and other amide compounds; carbonate compounds such as ethylene carbonate and propylene carbonate; acid anhydrides such as acetic anhydride, etc. From the perspective of easily obtaining excellent dispersibility, the liquid medium may contain an organic solvent, may contain methyl isobutyl ketone, may contain multiple organic solvents, and may contain methyl isobutyl ketone and toluene.

[0074] The liquid medium may contain a hydrophobic organic solvent or may contain a plurality of hydrophobic organic solvents. As the hydrophobic organic solvent, a solvent having a solubility in water of 1 g / 100 mL or less at 25° C. may be used.

[0075] From the perspective of adjusting the dispersibility, the δ of the liquid medium d2 (Unit: MPa 0.5 ) can be within the following range. d2 It may be 10.0 or more, 11.0 or more, 12.0 or more, 13.0 or more, 14.0 or more, 15.0 or more, 16.0 or more, or 16.5 or more. d2 It can be 25.0 or less, 22.0 or less, 20.0 or less, 19.5 or less, 19.0 or less, 18.5 or less, 18.0 or less, 17.5 or less, 17.0 or less, 16.5 or less, 16.0 or less, or 15.5 or less. From these viewpoints, the δ of the liquid medium is preferably 25.0 or less, 22.0 or less, 20.0 or less, 19.5 or less, 19.0 or less, 18.5 or less, 18.0 or less, 17.5 or less, 17.0 or less, 16.5 or less, 16.0 or less, or 15.5 or less. d2 It may be 10.0 to 25.0, 12.0 to 20.0, or 15.0 to 17.0.

[0076] From the perspective of adjusting the dispersibility, the δ of the liquid medium p2 (Unit: MPa 0.5 ) can be within the following range. p2It may be 1.0 or more, 1.5 or more, 2.0 or more, 2.5 or more, 3.0 or more, 3.5 or more, 4.0 or more, 4.5 or more, 5.0 or more, 5.5 or more, or 6.0 or more. p2 It can be 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, or 4.0 or less. From these viewpoints, the δ of the liquid medium is preferably 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, or 4.0 or less. p2 It may be 1.0 to 15.0, 2.0 to 10.0, or 3.5 to 6.5.

[0077] From the perspective of adjusting the dispersibility, the δ of the liquid medium h2 (Unit: MPa 0.5 ) can be within the following range. h2 It may be 1.0 or more, 1.5 or more, 2.0 or more, 2.5 or more, 3.0 or more, 3.5 or more, or 4.0 or more. h2 It may be 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, or 3.5 or less. From these viewpoints, the δ of the liquid medium may be 15.0 or less, 12.0 or less, 10.0 or less, 9.5 or less, 9.0 or less, 8.5 or less, 8.0 or less, 7.5 or less, 7.0 or less, 6.5 or less, 6.0 or less, 5.5 or less, 5.0 or less, 4.5 or less, 4.0 or less, or 3.5 or less. h2 It may be 1.0 to 15.0, 2.0 to 8.0, or 3.0 to 4.5.

[0078] From the viewpoint of easily obtaining excellent dispersibility, the content of the organic solvent can be 20% by mass or more, 30% by mass or more, 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass, based on the total mass of the liquid medium (the total amount of the liquid medium contained in the particle dispersion).

[0079] From the viewpoint of adjusting dispersibility, the content of the liquid medium can be within the following range relative to 100 parts by mass of the particles (including the content of the surface treatment agent when the particles are surface treated) or 100 parts by mass of the particles (excluding the content of the surface treatment agent when the particles are surface treated). The content of the liquid medium can be 10 parts by mass or more, 15 parts by mass or more, 20 parts by mass or more, 25 parts by mass or more, 30 parts by mass or more, 35 parts by mass or more, 40 parts by mass or more, 45 parts by mass or more, 50 parts by mass or more, 60 parts by mass or more, 80 parts by mass or more, 100 parts by mass or more, or 120 parts by mass or more. The content of the liquid medium can be less than 200 parts by mass, less than 150 parts by mass, less than 120 parts by mass, less than 100 parts by mass, less than 100 parts by mass, less than 80 parts by mass, less than 60 parts by mass, less than 50 parts by mass, less than 45 parts by mass, less than 40 parts by mass, or less than 35 parts by mass. From these viewpoints, the content of the liquid medium may be 10 to 200 parts by mass, 20 to 100 parts by mass, or 30 to 60 parts by mass.

[0080] From the viewpoint of adjusting dispersibility, based on the total mass of the particle dispersion, the content of the liquid medium can be within the following range. The content of the liquid medium can be 1% by mass or more, 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, 25% by mass or more, 30% by mass or more, 35% by mass or more, 40% by mass or more, 45% by mass or more, or 50% by mass or more. The content of the liquid medium can be 99.9% by mass or less, 99.5% by mass or less, 99% by mass or less, 95% by mass or less, 90% by mass or less, 85% by mass or less, 80% by mass or less, 75% by mass or less, 70% by mass or less, 65% by mass or less, 60% by mass or less, 55% by mass or less, 50% by mass or less, 45% by mass or less, 40% by mass or less, 35% by mass or less, 30% by mass or less, or 25% by mass or less. From these viewpoints, the content of the liquid medium can be 1 to 99.9% by mass, 5 to 80% by mass, or 10 to 70% by mass.

[0081] From the viewpoint of adjusting dispersibility, based on the total mass of the particle dispersion, the total amount of the particles and the liquid medium (when the particles are surface-treated, the content of the surface treatment agent is included), the total amount of the particles and the liquid medium (when the particles are surface-treated, the content of the surface treatment agent is not included), the total amount of the inorganic particles and the liquid medium (when the inorganic particles are surface-treated, the content of the surface treatment agent is included), or the total amount of the inorganic particles and the liquid medium (when the inorganic particles are surface-treated, the content of the surface treatment agent is not included) can be 50% by mass or more, more than 50% by mass, 70% by mass or more, 80% by mass or more, 90% by mass or more, 92% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass.

[0082] The particle dispersion according to the present embodiment may contain components other than particles and the liquid medium. As such components, for example, components that are soluble in the liquid medium may be used. As components other than particles and the liquid medium, resin materials that are not liquid at 25° C. may be cited.

[0083] 25℃, shear rate 1min -1 The viscosity V1 (unit: mPa·s) of the particle dispersion under 0.5% mol / L can be within the following range. From the viewpoint of suppressing particle precipitation and easily obtaining excellent dispersibility, the viscosity V1 may be 100 or more, 150 or more, 200 or more, 250 or more, 300 or more, 350 or more, 400 or more, 450 or more, 500 or more, 550 or more, 600 or more, 650 or more, 700 or more, or 750 or more. From the viewpoint of suppressing particle precipitation and easily obtaining excellent dispersibility, the viscosity V1 may be 5000 or less, 4000 or less, 3000 or less, 2000 or less, 1500 or less, 1000 or less, 950 or less, 900 or less, 850 or less, 800 or less, 750 or less, 700 or less, 650 or less, 600 or less, 550 or less, 500 or less, 450 or less, 400 or less, 350 or less, 300 or less, or 250 or less. From these viewpoints, the viscosity V1 may be 100 to 5,000, 150 to 2,000, or 200 to 800.

[0084] 25℃, shear rate 10min -1The viscosity V10 (unit: mPa·s) of the particle dispersion under the condition of 1000 to 2000 can be within the following range. From the viewpoint of suppressing the precipitation of particles and easily obtaining excellent dispersibility, the viscosity V10 can be 10 or more, 20 or more, 30 or more, 40 or more, 50 or more, 60 or more, 70 or more, 80 or more, 90 or more, 100 or more, 110 or more, 120 or more, or 130 or more. From the viewpoint of suppressing the precipitation of particles and easily obtaining excellent dispersibility, the viscosity V10 can be 1000 or less, 900 or less, 800 or less, 700 or less, 600 or less, 500 or less, 400 or less, 300 or less, 250 or less, 200 or less, 150 or less, 140 or less, 130 or less, 120 or less, 110 or less, 100 or less, 90 or less, 80 or less, 70 or less, 60 or less, 50 or less, 40 or less, or 30 or less. From these viewpoints, the viscosity V10 may be 10-1000, 15-500, or 20-150.

[0085] Example

[0086] Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.

[0087] <Preparation of materials>

[0088] (particle)

[0089] Silica particles A: manufactured by Admatechs Co., Ltd., product name "SO-32R", particles produced by a melting method, specific gravity 2.2 g / cm 3

[0090] Silica particles B1: manufactured by NIPPON SHOKUBAI CO., LTD., product name "KE-S50", particles produced by a sol-gel method, specific gravity 2.2 g / cm 3

[0091] Silica particles B2: manufactured by NIPPON SHOKUBAI CO., LTD., product name "KE-S150", particles produced by a sol-gel method, specific gravity 2.2 g / cm 3

[0092] Silica particles B3: manufactured by NIPPON SHOKUBAI CO., LTD., product name "KE-S250", particles produced by a sol-gel method, specific gravity 2.2 g / cm 3

[0093] (Surface treatment agent)

[0094] Silane coupling agent: N-phenyl-3-aminopropyltrimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd., product name "KBM-573"

[0095] (Liquid Medium)

[0096] Methyl isobutyl ketone (MIBK)

[0097] Toluene

[0098] <Preparation of particle dispersion>

[0099] (Example 1)

[0100] In a beaker, 100 parts by mass of silica particles A, 0.5 parts by mass of a silane coupling agent, and 3.5×10 -2 1.5 parts by mass of pure water and 42.8 parts by mass of a liquid medium (MIBK: toluene = 1:1 (volume ratio)) were added to obtain a mixed solution. Next, the beaker containing the mixed solution was placed in a 60°C water bath and stirred at a speed of 150 min using two stirring blades (made of Teflon) using a Sany motor. -1 The wet treatment was performed for 1 hour to obtain a mixed liquid having a solid content of 70% by mass.

[0101] Then, using a Nanomizer device (manufactured by Yoshida Machinery Co. Ltd., product name "NM2-2000AR") and a FILMIX device (manufactured by PRIMIX Corporation, product name "FM40-40L"), a dispersion treatment based on pitting was carried out (Nanomizer treatment conditions: 3 passes through the nozzle; FILMIX treatment conditions: 40 m / s, 1 minute), thereby preparing a particle dispersion (silicon dioxide slurry) having a solid content of 70% by mass.

[0102] (Examples 2, 3, 7)

[0103] Except having changed the volume ratio of MIBK and toluene in the liquid medium into the ratio shown in Table 1, it carried out similarly to Example 1, and prepared the particle dispersion liquid (silica slurry) whose solid content was 70 mass %.

[0104] (Example 4)

[0105] 100 parts by mass of silica particles A, 1.0 parts by mass of a silane coupling agent, 7.0×10 -2After mixing 2 parts by weight of pure water, the mixture was left to stand for 24 hours at 60°C and 60% humidity using a thermostatic and hygrostatic apparatus. Next, 42.8 parts by weight of a liquid medium (MIBK:toluene = 1:1 (volume ratio)) was added to obtain a mixed solution having a solid content of 70% by weight.

[0106] Next, the mixed solution was stirred using THINKY CORPORATION (THINKY) product name "THINKY MIXERARE-310" (treatment conditions: 2000 min -1 , 1 minute) to remove the agglomerates of silica particles. Then, using a Nanomizer device (manufactured by Yoshida Machinery Co. Ltd., product name "NM2-2000AR") and a FILMIX device (manufactured by PRIMIX Corporation, product name "FM40-40L"), a dispersion treatment based on pitting was performed (Nanomizer treatment conditions: passing through the nozzle 3 times; FILMIX treatment conditions: 40 m / s, 1 minute), thereby preparing a particle dispersion liquid (silica slurry) with a solid content of 70% by mass.

[0107] (Example 5)

[0108] A particle dispersion (silica slurry) having a solid content of 70% by mass was prepared in the same manner as in Example 4 except that the amount of the silane coupling agent used was changed to 0.5 parts by mass.

[0109] (Examples 6, 10 and Comparative Example 5)

[0110] In a beaker, 100 parts by mass of silica particles B3, 0.5 parts by mass of a silane coupling agent, and 3.5×10 -2 1.5 parts by weight of pure water and 33.3 parts by weight of a liquid medium (mixing ratio of MIBK and toluene: refer to Table 1) were added to obtain a mixed solution. Next, the beaker containing the mixed solution was placed in a 60°C water bath and stirred at a speed of 150 min using two stirring blades (made of Teflon) using a Sany motor. -1 The wet treatment was performed for 1 hour to obtain a mixed liquid having a solid content of 75% by mass.

[0111] Then, using a Nanomizer device (manufactured by Yoshida Machinery Co. Ltd., product name "NM2-2000AR") and a FILMIX device (manufactured by PRIMIX Corporation, product name "FM40-40L"), a dispersion treatment based on pitting was carried out (Nanomizer treatment conditions: passing through the nozzle 3 times; FILMIX treatment conditions: 40 m / s, 1 minute), thereby preparing a particle dispersion (silicon dioxide slurry) with a solid content of 75% by mass.

[0112] (Example 8 and Comparative Examples 1 to 3)

[0113] In a beaker, 100 parts by mass of silica particles B1, 0.5 parts by mass of a silane coupling agent, and 3.5×10 -2 1.5 parts by mass of pure water and 122 parts by mass of a liquid medium (mixing ratio of MIBK and toluene: refer to Table 1) were added to obtain a mixed solution. Next, the beaker containing the mixed solution was placed in a 60°C water bath and stirred at a speed of 150 min using two stirring blades (made of Teflon) using a Sany motor. -1 The wet treatment was performed for 1 hour to obtain a mixed liquid having a solid content of 45% by mass.

[0114] Then, using a Nanomizer device (manufactured by Yoshida Machinery Co. Ltd., product name "NM2-2000AR") and a FILMIX device (manufactured by PRIMIX Corporation, product name "FM40-40L"), a dispersion treatment based on pitting was carried out (Nanomizer treatment conditions: passing through the nozzle 3 times; FILMIX treatment conditions: 40 m / s, 1 minute), thereby preparing a particle dispersion (silicon dioxide slurry) with a solid content of 45% by mass.

[0115] (Examples 9, 11, 14 and Comparative Example 4)

[0116] In a beaker, 100 parts by mass of silica particles B2, 0.5 parts by mass of a silane coupling agent, and 3.5×10 -2 1.5 parts by weight of pure water and 42.8 parts by weight of a liquid medium (mixing ratio of MIBK and toluene: refer to Table 1) were added to obtain a mixed solution. Next, the beaker containing the mixed solution was placed in a 60°C water bath and stirred at a speed of 150 min using two stirring blades (made of Teflon) using a Sany motor. -1 The wet treatment was performed for 1 hour to obtain a mixed liquid having a solid content of 70% by mass.

[0117] Then, using a Nanomizer device (manufactured by Yoshida Machinery Co. Ltd., product name "NM2-2000AR") or a FILMIX device (manufactured by PRIMIX Corporation, product name "FM40-40L"), a dispersion treatment based on pitting was carried out (Nanomizer treatment conditions: 3 passes through the nozzle, 3 treated products; FILMIX treatment conditions: 40 m / s, 1 minute), thereby preparing a particle dispersion (silicon dioxide slurry) having a solid content of 70% by mass.

[0118] (Example 12)

[0119] A particle dispersion (silica slurry) having a solid content of 70% by mass was prepared in the same manner as in Example 4 except that only MIBK was used as the liquid medium.

[0120] (Example 13)

[0121] A particle dispersion (silica slurry) having a solid content of 70% by mass was prepared in the same manner as in Example 5 except that only MIBK was used as the liquid medium.

[0122] <HSP value of particles>

[0123] The particle dispersion (silicon dioxide slurry) was dried at 130° C. for 1 hour to recover powdered particles. The particle diameter D50 (hereinafter referred to as “particle diameter A”) and particle diameter D100 of the particles were obtained based on real image observation using a scanning electron microscope (SEM).

[0124] Then, after 0.02 g of the particles were placed in 16 containers (screw bottles), 20 mL of 16 organic solvents were placed in each container to prepare a test solution (particle content: about 0.1 mass %). As 16 organic solvents, MIBK (methyl isobutyl ketone), toluene, methanol, cyclohexanol, acetone, acetonitrile, formamide, benzyl benzoate, dimethyl sulfoxide, ethyl acetate, ethanol, acetic anhydride, γ-butyrolactone, MEK (methyl ethyl ketone), 1-butanol and cyclohexane were used. The test solution was dispersed for 5 minutes using an ultrasonic dispersing device (manufactured by ASONE Co., Ltd., product name "VS-D100"). Then, the particle size distribution (cumulative particle size distribution, volume distribution) of the particles in the test solution was measured using a particle size distribution meter (manufactured by Shimadzu Corporation, product name "SALD-7500"). For the case where the above 16 organic solvents were used, the particle size D50 (hereinafter referred to as "particle size B") was obtained based on the measurement results of the particle size distribution. In addition, the particle size distribution of standard particles (MBP1-10) with determined particle size distribution was measured in advance to confirm that the measurement content was appropriate.

[0125] Based on the measurement results of the particle size distribution, the coefficient of variation (CV) of the particle size was obtained for each of the 16 organic solvents. The case where the coefficient of variation was 20 or more was judged as a polydisperse state, and the case where the coefficient of variation was less than 20 was judged as a monodisperse state. For the 16 organic solvents, it was determined whether they were "solvents with poor dispersibility" or "solvents with excellent dispersibility" based on the following criteria.

[0126] For the benchmark of agglomeration in a monodisperse state, a particle diameter twice the particle diameter A (assuming the particle diameter when two particles are in contact) is used as a threshold value, and an organic solvent when the particle diameter B is above the threshold value is judged as a "solvent with poor dispersibility", and an organic solvent when the particle diameter B is less than the threshold value is judged as a "solvent with excellent dispersibility".

[0127] On the other hand, with regard to the benchmark for agglomeration in a polydisperse state, since the distribution of particle sizes is wide, from the perspective of setting a benchmark that easily targets agglomerated particles, the particle size D100 is used as a threshold, and an organic solvent is judged as a "solvent with poor dispersibility" when the particle size B is above the threshold, and an organic solvent is judged as a "solvent with excellent dispersibility" when the particle size B is less than the threshold.

[0128] Next, the analysis software HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi) was used to calculate thed , δ p and δ h The above 16 organic solvents are plotted in the three-dimensional space (Hansen space) as the coordinate axis. d , δ p and δ h , the values ​​of the database of the above-mentioned analysis software were used.

[0129] Next, a virtual sphere was created in the three-dimensional space that did not include all of the above-mentioned "solvents with poor dispersibility" but included all of the above-mentioned "solvents with excellent dispersibility". Then, the δ d , δ p and δ h Delta as a particle d1 , δ p1 and δ h1 The δ of the particles in the examples and comparative examples d1 , δ p1 and δ h1 Shown in Table 1.

[0130] <HSP value of liquid medium>

[0131] As the δ of MIBK and toluene used as liquid medium d , δ p and δ h , using the values ​​from the database of the analysis software HSPiP (Hansen Solubility Parameter in Practice; written by Prof. Steven Abbott and Dr. Yamamoto Hiroshi). The δ d2 , δ p2 and δ h2 The parameters of each solvent (δ d , δ p or δ h ) and the total value of the product of the volume ratio of each solvent. d2 , δ p2 and δ h2 The results are shown in Table 1. Since the amount of pure water mixed with the silane coupling agent was small, the influence of the pure water was not considered.

[0132] <Calculation of HSP distance>

[0133] Particle-based delta d1 , δ p1 and δ h1 , and the δ of the liquid medium d2 , δp2 and δ h2 The HSP distance of the particle relative to the liquid medium was calculated by the following formula. The HSP distance is shown in Table 1.

[0134] HSP distance = {4×(δ d1 -δ d2 ) 2 +(δ p1 -δ p2 ) 2 +(δ h1 -δ h2 ) 2} 0.5

[0135] <Viscosity measurement>

[0136] The viscosity at 25°C and a shear rate of 1 min was measured using an E-type viscometer (manufactured by Toki Sangyo Co., Ltd., product name "TV-22"). -1 and 10min -1 The results are shown in Table 2.

[0137] <Measurement of particle size>

[0138] The particle dispersion (silicon dioxide slurry) just prepared (after dispersion treatment based on pitting. The same below) was diluted with the liquid medium of each embodiment or each comparative example to obtain a test liquid with a solid content of 3% by mass. Next, the particle size distribution (cumulative particle size distribution, volume distribution) of the particles in the test liquid was measured using a particle size distribution meter (made by Shimadzu Corporation, product name "SALD-7500") using a laser diffraction / scattering method. And, based on the particle size distribution, D50 and D95 ​​were obtained as average particle sizes. These average particle sizes are shown in Table 2.

[0139] The particle size distribution is measured by the following procedure: In addition, the particle size distribution of standard particles (MBP1-10) whose particle size distribution is determined is measured in advance, and the appropriateness of the measurement content is confirmed.

[0140] (1) About 0.5 mL of the liquid medium of each Example or each Comparative Example was dropped onto a glass substrate for measurement, and then covered with a slide glass to prevent air bubbles from entering, thereby obtaining a test body.

[0141] (2) After the test object was mounted on the sample holder, a blank measurement was performed using only the liquid medium.

[0142] (3) About 0.5 mL of the test liquid (solid content: 3% by mass) was dropped onto a glass substrate for measurement, and then covered with a slide glass to prevent air bubbles from entering, thereby obtaining a test body.

[0143] (4) After the test body was mounted on a sample holder, the particle size distribution was measured. The particle size distribution was monitored and the constant distribution was measured.

[0144] <Evaluation of dispersibility>

[0145] Based on the measurement results of the particle size distribution obtained by the above-mentioned measurement of the particle size, the coefficient of variation (CV) of the particle size was obtained. The case where the coefficient of variation was 20 or more was judged as a polydisperse state, and the case where the coefficient of variation was less than 20 was judged as a monodisperse state. In the particle dispersion obtained using silica particles A, the coefficient of variation was 55 (polydisperse), in the particle dispersion obtained using silica particles B1, the coefficient of variation was 12 (monodisperse), in the particle dispersion obtained using silica particles B2, the coefficient of variation was 17 (monodisperse), and in the particle dispersion obtained using silica particles B3, the coefficient of variation was 18 (monodisperse).

[0146] For the benchmark of agglomeration in a monodisperse state, a particle size twice the particle size D50 (the particle size when two particles are assumed to be in contact) is used as a threshold value, and the volume fraction of particles with a particle size above the threshold value is calculated. On the other hand, for the benchmark of agglomeration in a polydisperse state, since the distribution of particle sizes is wide, from the perspective of setting a benchmark that is easy to use agglomerated particles as an object, a particle size D100 is used as a threshold value, and the volume fraction of particles with a particle size above the threshold value is calculated. In the particle dispersion obtained using silica particles A, the particle size D100 is 5 μm. The volume fraction of particles with a particle size above the threshold value is shown in Table 2. As shown in Table 2, in each example, the volume fraction (just after preparation) is 7.0% or less.

[0147] After the above-mentioned particle dispersion liquid just prepared in each embodiment was left to stand for 7 days, 20 vibration stirrings were implemented by hand within 10 seconds, and then diluted with the liquid medium of each embodiment, thereby obtaining a test liquid with a solid content of 3% by mass. Then, the particle size distribution (cumulative particle size distribution, volume distribution) of the particles was measured in the same order as the above-mentioned evaluation method. The volume fraction of particles with a particle size above the same threshold value as above is shown in Table 2.

[0148] After the particle dispersions just prepared in Examples 1 to 5 were left to stand for 30 days, they were vibrated and stirred 20 times by hand within 10 seconds, and then diluted with the liquid medium of each Example to obtain a test solution with a solid content of 3% by mass. Then, the particle size distribution (cumulative particle size distribution, volume distribution) of the particles was measured in the same order as the above evaluation method. The volume fraction of particles with a particle size above the same threshold as above is shown in Table 2.

[0149] [Table 1]

[0150]

[0151] [Table 2]

[0152]

Claims

1. A particle dispersion comprising particles and a liquid medium, The distance between the HSP value of the particle and the HSP value of the liquid medium is 5.50 MPa 0.5 the following.

2. The particle dispersion according to claim 1, wherein The liquid medium comprises an organic solvent.

3. The particle dispersion according to claim 1, wherein The liquid medium includes various organic solvents.

4. The particle dispersion according to claim 3, wherein The liquid medium includes methyl isobutyl ketone and toluene.

5. The particle dispersion according to any one of claims 2 to 4, wherein The content of the organic solvent is 80% by mass or more based on the total mass of the liquid medium.

6. The particle dispersion according to any one of claims 1 to 4, wherein The particles include inorganic particles.

7. The particle dispersion according to any one of claims 1 to 4, wherein The particles include at least one selected from the group consisting of silicon dioxide, ceria, aluminum oxide, titanium dioxide, boron nitride, and calcium titanate.

8. The particle dispersion according to any one of claims 1 to 4, wherein The particles comprise silicon dioxide.

9. The particle dispersion according to any one of claims 1 to 4, wherein The particles have a surface treatment agent on the surface of the particles.

10. The particle dispersion according to claim 9, wherein The surface treatment agent includes a silane compound having an alkoxysilyl group.

11. The particle dispersion according to any one of claims 1 to 4, wherein The particle size D50 at the cumulative 50% in the volume-based cumulative particle size distribution of the particles is 0.1 to 20 μm.

12. The particle dispersion according to any one of claims 1 to 4, wherein The specific gravity of the particles is 1.0 to 8.0 g / cm 3 .

13. The particle dispersion according to any one of claims 1 to 4, wherein The content of the particles is 30 to 90% by mass based on the total mass of the particle dispersion. When the particles are surface treated, the content of the particles includes the content of the surface treatment agent.

14. The particle dispersion according to any one of claims 1 to 4, wherein At 25°C, shear rate 1 min -1 The viscosity is 350 mPa·s or more.

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