WO2020066152A1 - 被覆炭化珪素粒子粉体 - Google Patents
被覆炭化珪素粒子粉体 Download PDFInfo
- Publication number
- WO2020066152A1 WO2020066152A1 PCT/JP2019/023511 JP2019023511W WO2020066152A1 WO 2020066152 A1 WO2020066152 A1 WO 2020066152A1 JP 2019023511 W JP2019023511 W JP 2019023511W WO 2020066152 A1 WO2020066152 A1 WO 2020066152A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particle powder
- particles
- mass
- coated
- silicon carbide
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62813—Alumina or aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62842—Metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/066—Treatment or coating resulting in a free metal containing surface-region
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5244—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5409—Particle size related information expressed by specific surface values
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/549—Particle size related information the particle size being expressed by crystallite size or primary particle size
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Definitions
- the present invention relates to a coated silicon carbide particle powder, a dispersion containing the same, a green sheet and a prepreg material, a sintered body of the coated silicon carbide particle powder, and a molded product containing the same.
- Silicon carbide is high in hardness, excellent in high-temperature heat resistance, mechanical strength, impact resistance, abrasion resistance, oxidation resistance and corrosion resistance, and has a small coefficient of thermal expansion. Applications in various applications, including high-temperature structural members, are expected.
- silicon carbide particles in forming a desired composition or material, silicon carbide particles (silicon carbide particles, SiC particles) may be dispersed in a dispersion medium or a medium of a polymer material and used, or ceramic particles may be used. It has been studied to use it in a mixture with other materials such as. Further, in order to improve the functions of a dispersion or a mixture containing silicon carbide particles, and a molded article formed therefrom, a compound capable of imparting a desired function is coordinated around the silicon carbide particles and dispersed. Mixing is being considered.
- Japanese Patent Application Laid-Open No. 2012-106888 discloses that the insulating property of silicon carbide particles is improved by coating the surface of silicon carbide particles with an oxide film such as alumina having a thickness of 10 nm to 500 nm provided by sintering. Is disclosed. Further, it is disclosed that by including such coated silicon carbide particles, heat resistance, high thermal conductivity, and high insulation of the composite composition can be realized.
- the present invention has been made in view of the above problems, and in a sintered body of a composition containing a sintering aid and silicon carbide particles and a molded body containing the same, the density and mechanical strength are improved. It is intended to provide a means that can be used.
- the above object of the present invention is solved by the following means; Silicon carbide particles, and a coating layer covering the silicon carbide particles, wherein the coating layer includes an aluminum element, and the mass of the aluminum element per unit surface area of the silicon carbide particles is 0.5 mg / m 2.
- the above is the coated silicon carbide particle powder.
- X to Y indicating a range means “X or more and Y or less”.
- the operation and measurement of physical properties and the like are performed under the conditions of room temperature (20 to 25 ° C.) / Relative humidity of 40 to 50% RH.
- One embodiment of the present invention includes a silicon carbide particle and a coating layer containing an aluminum element that coats the silicon carbide particle, wherein the coating layer contains an aluminum element, and the silicon carbide particles have a unit surface area per unit area.
- the present invention relates to a coated silicon carbide particle powder having a mass of aluminum element of 0.5 mg / m 2 or more.
- the present inventors presume the mechanism by which the above-mentioned problem is solved by the present invention as follows.
- an aluminum element-containing compound as a sintering aid during sintering of SiC particles, formation of a sintered body becomes easier.
- the amount of the sintering aid is small, the amount of the sintering aid present between the respective SiC particles is insufficient, and the SiC particles are fired in a state of being in direct contact with each other. May result in insufficient defect sites.
- Such a defective portion can be a starting point of destruction when stress is applied. For this reason, the mechanical strength of the sintered body having the defective portion is reduced.
- the mixing of the SiC particles and the sintering aid is insufficient, the number of the above-described defective sites in the sintered body and the manner of fusion between the SiC particles differ depending on the location, resulting in non-uniformity.
- stress concentration occurs at a specific location due to a difference in characteristics depending on the location, and the location can be a starting point of destruction. For this reason, in the case of a sintered body in which the number of defective sites generated and the manner of fusion are uneven, the mechanical strength is reduced.
- the coated SiC particle powder contains an aluminum element as a coating layer.
- the SiC particles and the sintering aid can be present in a more uniform dispersion state.
- the mass of the aluminum element per unit surface area of the SiC particles is 0.5 mg / m 2 or more, the amount of the sintering aid existing between the respective SiC particles is sufficient. Further, the dispersibility of the SiC particles and the sintering aid in the entire composition to be fired is also sufficient. As a result, the mechanical strength of the sintered body is improved, and the mechanical strength of the compact including the sintered body is also improved.
- coated SiC particles refers to coated particles having SiC particles and a coating layer that covers the SiC particles.
- the coated SiC particle may be a particle in which at least a part of the SiC particle is covered by the coating layer.
- coated SiC particle powder refers to an aggregate of particles including a plurality of coated SiC particles.
- the coated SiC particle powder may include components other than the coated SiC particles, but in this case, it is preferable that the other components are only unavoidable impurities in the coating process.
- the unavoidable impurities in the coating treatment include, for example, coating of raw material particles and raw materials of unreacted coating components, by-products, reagents used in reactions that can be added as necessary, impurities derived from raw materials, and the like.
- the inevitable impurities in the coating treatment do not include components that can be arbitrarily added for the purpose of developing functions during and after the manufacturing process.
- the coated SiC particle powder may be difficult to quantitatively and accurately analyze or remove the ratio of the coated SiC particles in the coated SiC particle powder depending on the type of other components contained therein. It is possible. In particular, when other components are unavoidable impurities in the coating process, the quantitative analysis of the ratio of the coated SiC particles in the coated SiC particle powder is accurately analyzed depending on the type because of the similarity in analytical characteristics. Or removal may be more difficult. However, even in this case, when the coated SiC particle powder is confirmed to contain the coated SiC particles by the analysis method described below, the coated SiC particle powder has a good dispersibility in a dispersion medium. And it has desired characteristics derived from the characteristics of the raw material particles and the coating component.
- the ratio of the coated SiC particles in the coated SiC particles is most preferably 100% by mass based on the total mass of the coated SiC particles.
- the ratio of the coated SiC particles in the coated SiC particle powder is preferably 50% by mass or more, more preferably 70% by mass or more, and is 90% by mass or more. More preferably, it is still more preferably 99% by mass or more, particularly preferably 99.9% by mass or more (upper limit 100% by mass).
- the term “powder” is used for convenience, but the term does not represent only a powdery (dry) substance, but exists in a dispersion medium in a dispersion medium, and A substance that can be obtained as a powder when the medium is volatilized is also represented. It is preferable that the coated SiC particle powder can maintain its form as coated SiC particles even when washed with a solvent such as water or in a state of being dispersed in a dispersion medium such as water.
- the mass of aluminum (Al) element per unit surface area of SiC particles of the coated SiC particle powder (hereinafter, also referred to as “mass of Al element per unit surface area of SiC”) is 0.5 mg / m 2 or more. If the mass of the Al element per unit surface area of SiC is less than 0.5 mg / m 2 , sintering does not sufficiently proceed in the sintered body of the coated SiC particle powder and the molded body containing the same, and the sintered body Has a non-uniform structure, resulting in insufficient density and mechanical strength.
- the mass of the Al element per unit surface area of SiC is preferably 1 mg / m 2 or more.
- the mass of the Al element per unit surface area of SiC is preferably 1.2 mg / m 2 or more. More preferably, it is more preferably 1.35 mg / m 2 or more. It should be noted that the color is related to the uniformity of the sintered body, and it is considered that the uniformity of the sintered body is improved as the uniformity of the color is improved.
- the upper limit of the mass of the Al element per unit surface area of the SiC is not particularly limited, but is preferably 30 mg / m 2 or less, more preferably 20 mg / m 2 or less, and more preferably 10 mg / m 2 or less. Is more preferable.
- the mass of the Al element per unit surface area of SiC can be measured as follows. First, the specific surface area of the SiC particles is measured using a specific surface area meter FlowSorb II manufactured by Micromeritics.
- the upper limit of the average secondary particle diameter of the coated SiC particle powder is not particularly limited, but is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, further preferably 2 ⁇ m or less, and still more preferably 1 ⁇ m or less. Is particularly preferred, and most preferably 0.5 ⁇ m or less. Within the above range, when the coated SiC particle powder is dispersed in a medium, the dispersibility is further improved. Further, the uniformity of a composition or a composite containing the coated SiC particle powder, the coated SiC particle powder such as a green sheet, a prepreg material, or the like is further improved.
- the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body including the same are further improved. This is presumed to be because when the average secondary particle size is small, the variation in the particle size of each coated SiC particle is small.
- the lower limit of the average secondary particle diameter of the coated SiC particle powder is not particularly limited, but is preferably 0.03 ⁇ m or more, more preferably more than 0.03 ⁇ m, and more preferably 0.05 ⁇ m or more. Is more preferably, more preferably more than 0.05 ⁇ m, particularly preferably not less than 0.1 ⁇ m, and most preferably more than 0.1 ⁇ m.
- the content is in the above range, when other particles described later are used in the dispersion, aggregation in the dispersion medium is more difficult to occur, and the dispersibility is further improved.
- a powder material containing the coated SiC particle powder a composition or a composite containing the coated SiC particle powder such as a green sheet, a prepreg material, and other particles described later, the uniformity is further improved. . Thereby, the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body containing the same are further improved.
- the value of the average secondary particle diameter of the coated SiC particle powder is a scattering particle manufactured by HORIBA, Ltd. in a dispersion obtained by dispersing the coated SiC particle powder in a dispersion medium so as to have an appropriate concentration for measurement. It can be measured by a diameter distribution measuring device LA-950.
- the lower limit of the isoelectric point pH of the coated SiC particle powder is not particularly limited, but is preferably 4.5 or more, more preferably 5 or more, still more preferably 5.5 or more, It is still more preferably 6 or more, particularly preferably 6.5 or more, and most preferably 7.5 or more.
- the upper limit of the isoelectric point pH of the coated SiC particle powder is not particularly limited, but is preferably 9 or less, and more preferably 8.5 or less.
- the uniformity is further improved.
- the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body containing the same are further improved.
- a zeta potential measurement solution having a pH of 1.0 in increments of 1.0, for example, a pH in the range of 3.0 to 10.0 in increments of 1.0 is prepared, the zeta potential is measured, and the zeta potential is measured. From the pH before and after the change of the sign and the zeta potential at the pH before and after the change, it can be calculated by the following equation.
- the pH can be measured with a pH meter (model number: F-71) manufactured by Horiba, Ltd.
- the zeta potential can be measured with a zeta potential measuring device (trade name “Zetasizer nano nano ZSP”) manufactured by Malvern Instruments.
- Silicon carbide particles have high hardness, are excellent in high-temperature heat resistance, mechanical strength, impact resistance, abrasion resistance, oxidation resistance and corrosion resistance, and have a small coefficient of thermal expansion. It can be used in various applications including high-temperature structural members.
- the upper limit of the average primary particle diameter of the SiC particles is not particularly limited, but is preferably less than 10 ⁇ m, more preferably less than 5 ⁇ m, still more preferably less than 2 ⁇ m, particularly preferably less than 1 ⁇ m, Most preferably, it is less than 0.5 ⁇ m.
- the dispersibility is further improved.
- the uniformity of a composition or a composite containing the coated SiC particle powder, the coated SiC particle powder such as a green sheet, a prepreg material, or the like is further improved. Then, the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body including the same are further improved.
- the lower limit of the average primary particle diameter of the SiC particles is not particularly limited, but is preferably 0.03 ⁇ m or more, more preferably 0.05 ⁇ m or more, and further preferably 0.1 ⁇ m or more. Within the above range, the function of the formed coated SiC particles can be further improved.
- the value of the average primary particle diameter of the SiC particles was determined by taking an image using SEM @ SU8000 manufactured by Hitachi High-Technologies Corporation, and using the image analysis type particle size distribution software MacView manufactured by Mountech Co., Ltd. to obtain 100 volume average particles. It can be calculated as a diameter.
- the upper limit of the average secondary particle size of the SiC particles is not particularly limited, but is preferably less than 10 ⁇ m, more preferably less than 5 ⁇ m, further preferably less than 2 ⁇ m, and particularly preferably less than 1 ⁇ m. Preferably, it is most preferably less than 0.5 ⁇ m.
- the dispersibility is further improved.
- the uniformity of a composition or a composite containing the coated SiC particle powder, the coated SiC particle powder such as a green sheet, a prepreg material, or the like is further improved. Then, the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body including the same are further improved.
- the lower limit of the average secondary particle size of the SiC particles is not particularly limited, but is preferably 0.03 ⁇ m or more, more preferably 0.05 ⁇ m or more, and further preferably 0.1 ⁇ m or more. .
- the content is in the above range, when other particles described later are used in the dispersion, aggregation in the dispersion medium is more difficult to occur, and the dispersibility is further improved.
- a powder material containing the coated SiC particle powder a composition or a composite containing the coated SiC particle powder such as a green sheet, a prepreg material, and other particles described later, the uniformity is further improved. .
- the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body containing the same are further improved. Moreover, when it is in the above range, the coating of the SiC particles can be performed more efficiently.
- the value of the average secondary particle size of the SiC particles can be measured by a scattering type particle size distribution measuring device LA-950 manufactured by Horiba, Ltd.
- SiC particles a commercially available product or a synthetic product may be used. Although it does not specifically limit as a commercial item, For example, GC # 40000, GC8000S, etc. made by Fujimi Incorporated can be used.
- the SiC particles may be used alone or in combination of two or more.
- the coating layer of the coated SiC particles contains an aluminum element.
- the coating layer has a function of imparting insulating properties to the SiC particles, a function as a sintering aid when producing a molded article, and a function of improving polishing characteristics when used in a polishing composition. Can be provided.
- the aluminum element in the coating layer is preferably contained in the form of an aluminum compound.
- the aluminum compound is not particularly limited, and a known compound can be appropriately employed.
- an aluminum oxide precursor is particularly preferable. That is, the coating layer according to a preferred embodiment of the present invention includes an aluminum oxide precursor, and the aluminum oxide precursor includes an aluminum element.
- the aluminum oxide precursor in the coating layer changes to aluminum oxide when the coated SiC particle powder is fired. Aluminum oxide functions as a good sintering aid. Then, by using a method in which the aluminum oxide precursor in the coating layer is changed to aluminum oxide during the firing of the coated SiC particle powder, the density of the sintered body of the coated SiC particle powder, The mechanical strength is further improved.
- the coated SiC particle powder preferably changes the coating layer to aluminum oxide by firing, the coating layer preferably does not substantially contain aluminum oxide.
- substantially free of aluminum oxide means that in the EELS (Electron Energy Loss Spectroscopy) analysis of the coated SiC particle powder, a spectrum shape specific to the EELS standard spectrum of aluminum oxide is not clearly observed. It represents that.
- the EELS analysis can be performed using TITAN80-300 manufactured by FEI.
- Examples of the aluminum compound that can be used as the aluminum oxide precursor include, but are not particularly limited to, aluminum hydroxide; aluminum hydroxide hydroxide, aluminum nitrate, aluminum chloride, aluminum acetate, aluminum sulfate, aluminum alum, aluminum formate, aluminum benzoate, Aluminum salts such as aluminum linoleate, aluminum oleate, aluminum palmitate, aluminum salicylate, and aluminum gallate; aluminum alkoxides such as trimethoxyaluminum, triethoxyaluminum, triisopropoxyaluminum, and tributoxyaluminum; triethylaluminum, triisobutylaluminum , Diethylaluminum chloride, ethylaluminum sesquichloride Ethylaluminum dichloride, an organic aluminum compound such as tri -n- octyl aluminum and the like.
- the coating layer preferably contains aluminum hydroxide.
- Coated SiC particles having a coating layer containing aluminum hydroxide (hereinafter, also simply referred to as “aluminum hydroxide coated SiC particles”) disperse the coated SiC particle powder in a medium while having a function derived from an aluminum compound. In this case, higher dispersibility can be obtained.
- a higher uniformity can be obtained in a composition and a composite including a coated SiC particle powder, a coated sheet such as a green sheet and a prepreg material, and a sintered body of the coated SiC particle powder.
- Higher density and higher mechanical strength can be obtained in a molded body containing the same.
- the coating layer may contain other components as long as the effects of the present invention are not impaired.
- the coating layer contains an aluminum element can be confirmed by observing the coated SiC particles by SEM (Scanning Electron Microscope) -EDX (Energy Dispersive X-ray Spectroscopy) and EELS (Electron Energy Analysis). The details of the measurement method will be described in Examples.
- the thickness of the coating layer may be difficult to measure directly due to a change in the presence state of the particles due to the coating, but can be determined from the mass of the aluminum element per unit surface area of the SiC particles.
- the isoelectric point of the zeta potential tends to increase as the film thickness of the coating layer increases. Therefore, the preferable film thickness of the coating layer means that the coated SiC particles are preferable. It can also be determined from having a value within the range of the point.
- the method for producing the coated SiC particle powder includes, when the aluminum element in the coating layer is contained in the form of an aluminum compound, a dispersion comprising SiC particles, the aluminum compound or its precursor contained in the coating layer, and a dispersion medium. It is preferable that the coating be carried out in a body state.
- the coating is performed after controlling the pH of the dispersion containing the SiC particles, the aluminum compound or its precursor contained in the coating layer, and the dispersion medium (pH at the coating stage) to a value within a predetermined range. It is preferable to carry out this by maintaining for a certain period.
- the lower limit of the pH range in the coating step is not particularly limited, but is preferably more than 7.0, more preferably 9.0 or more, and further preferably 10.0 or more. Within the above range, the occurrence of aggregation of the SiC particles can be suppressed, and the coating can be advanced while maintaining the dispersibility of the SiC particles more favorably.
- the upper limit of the pH range in the coating step is not particularly limited, but is preferably 12.0 or less, more preferably 11.5 or less, and even more preferably 11.0 or less. Within the above range, the generation of unavoidable impurities in the coating treatment is further reduced, and the purity of the coated SiC particle powder to be produced is further increased.
- the pH in the coating step can be controlled with a known pH adjuster.
- acids or alkalis are preferable.
- the acid include, but are not particularly limited to, inorganic acids such as nitric acid, sulfuric acid, phosphoric acid, and hydrochloric acid (particularly, strong inorganic acids such as nitric acid, sulfuric acid, and hydrochloric acid), acetic acid, citric acid, lactic acid, oxalic acid, and phthalic acid. And organic acids.
- inorganic acids such as nitric acid, sulfuric acid, and hydrochloric acid
- acetic acid citric acid
- lactic acid lactic acid
- oxalic acid phthalic acid
- organic acids it is preferable to use an inorganic strong acid from the viewpoint that the objective can be achieved with a smaller amount of addition, and a high-purity product having a low possibility of mixing other elements is easily available.
- nitric acid sulfuric acid and hydrochloric acid. These acids may be used alone or in combination of two or more.
- alkali include, but are not particularly limited to, for example, ammonia, potassium hydroxide, sodium hydroxide, ammonium hydrogen carbonate, ammonium carbonate, potassium hydrogen carbonate, potassium carbonate, sodium hydrogen carbonate, sodium carbonate, tetramethyl ammonium hydroxide, Tetraethylammonium hydroxide, tetrabutylammonium hydroxide, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N- ( ⁇ -aminoethyl) ethanolamine, hexamethylenediamine, diethylenetriamine, triethylene Tetramine, anhydrous piperazine, piperazine hexahydrate, 1- (2-aminoethyl) piperazine, N-methylpiperazine, guan
- the precursor of the aluminum compound contained in the coating layer is sodium aluminate
- sodium hydroxide is preferable from the viewpoint that the generation of unavoidable impurities in the coating treatment is small.
- alkalis can be used alone or in combination of two or more.
- the coated SiC particle powder according to a preferred embodiment of the present invention is an aluminum hydroxide-coated SiC particle powder as described above, and the production method is not particularly limited, but includes SiC particles, alkali and water, a step (A) of preparing a raw material dispersion (1) having a pH of 9.0 or more and 12.0 or less and a raw material solution (2) containing sodium aluminate and water; ), The raw material solution (2) and an acid are added to maintain the pH in the range of 9.0 to 12.0, and a coating having a coating layer containing aluminum hydroxide on the surface of the SiC particles. And a step (B) of forming particles.
- the manufactured aluminum hydroxide-coated SiC particle powder may be manufactured in a state of being dispersed in a dispersion medium, or may be manufactured through a step of removing the dispersion medium thereafter.
- the method for producing the aluminum hydroxide-coated SiC particle powder includes a raw material dispersion (1) containing SiC particles, an alkali and water, and having a pH of 9.0 or more and 12.0 or less; And a raw material solution (2) containing sodium acid and water.
- the method for preparing the raw material dispersion (1) is not particularly limited, and examples thereof include a method in which SiC particles are dispersed in a dispersion medium containing water and an alkali is added.
- the procedure and method for dispersing the SiC particles in a dispersion medium containing water and adding an alkali are not particularly limited, and known procedures and methods can be used.
- a method in which an alkali is added to an aqueous dispersion of SiC particles (a dispersion containing water as a dispersion medium, preferably an aqueous dispersion) may be used.
- the aqueous dispersion of SiC particles may be a commercial product or a synthetic product.
- a procedure or method of mixing or dispersing or dissolving each component with water using an organic solvent without mixing with water may be employed.
- the content of the SiC particles in the raw material dispersion (1) is not particularly limited, but from the viewpoint of productivity, the total mass of the raw material dispersion (1) is It is preferably at least 8% by mass, more preferably at least 10% by mass.
- the content of the SiC particles in the raw material dispersion (1) is not particularly limited, but is preferably 50% by mass or less based on the total mass of the raw material dispersion (1) from the viewpoint of dispersibility. , 40% by mass or less, more preferably 30% by mass or less.
- the alkali is not particularly limited, and for example, those mentioned as the pH adjuster used for controlling the pH in the coating step can be used.
- the amount of the alkali used is not particularly limited, and may be adjusted so that the pH of the raw material dispersion (1) is not less than 9.0 and not more than 12.0.
- the raw material dispersion (1) contains water as a dispersion medium.
- the water is preferably free from impurities as much as possible.
- water having a total content of transition metal ions of 100 ppb or less is preferable.
- the purity of water can be increased by operations such as removal of impurity ions using an ion exchange resin, removal of foreign substances by a filter, and distillation.
- the content of water in the raw material dispersion (1) is not particularly limited, but from the viewpoint of promoting the coating of the SiC particles with aluminum hydroxide more favorably, the total mass of the raw material dispersion (1). Is preferably 50% by mass or more, more preferably 60% by mass or more, and still more preferably 70% by mass or more (up to less than 100% by mass).
- the dispersion medium may contain a solvent other than water, and the solvent other than water is preferably an organic solvent.
- the organic solvent include water-miscible organic solvents such as acetone, acetonitrile, ethanol, methanol, isopropanol, glycerin, ethylene glycol, and propylene glycol. These organic solvents can be used alone or in combination of two or more.
- the method for preparing the raw material solution (2) is not particularly limited, and examples thereof include a method of adding sodium aluminate to water.
- the procedure and method for dispersing sodium aluminate in water and the procedure and method for adding an alkali are not particularly limited, and known procedures and methods can be used.
- the content of sodium aluminate in the raw material solution (2) is not particularly limited, but is preferably from 10% by mass to 50% by mass, and more preferably from 20% by mass to 40% by mass with respect to the total mass of the raw material solution (2). It is more preferable that the content is not more than mass%.
- Step (B) In the method for producing the aluminum hydroxide-coated SiC particle powder according to the preferred embodiment, a raw material solution (2) and an acid are added to the raw material dispersion (1) prepared in the step (A). a step (B) of maintaining the pH in the range of 9.0 to 12.0 and forming coated particles having a coating layer containing aluminum hydroxide on the surface of the SiC particles. In this step (B), SiC particles coated with aluminum hydroxide are produced.
- the method of adding the raw material solution (2) and the acid to the raw material dispersion (1) is such that the pH can be maintained at 9.0 or more and 12.0 or less (that is, unless the concentration of aluminate ions becomes excessive).
- a method in which the raw material solution (2) and the acid are added simultaneously, a method in which the raw material solution (2) and the acid are added little by little alternately, and the like can be mentioned.
- the addition amount of the raw material solution (2) is not particularly limited because it varies depending on the content of sodium aluminate in the raw material solution (2), but the addition amount of sodium aluminate to 100 parts by mass of the SiC particles is 7 parts by mass or more.
- the amount is preferably 20 parts by mass or more, more preferably 22 parts by mass or more. That is, the lower limit of the preferable range of the addition amount of sodium aluminate with respect to 100 parts by mass of the SiC particles is the above-described value.
- the SiC particles can be sufficiently coated with aluminum hydroxide (Al (OH) 3 ), and the function derived from aluminum hydroxide is further improved.
- the amount of the raw material solution (2) to be added is not particularly limited because it varies depending on the content of sodium aluminate in the raw material solution (2).
- the content of sodium aluminate relative to 100 parts by mass of the SiC particles is 800 parts by mass or less.
- the amount is preferably 400 parts by mass or less, more preferably 100 parts by mass or less, even more preferably 100 parts by mass or less, and particularly preferably 50 parts by mass or less. . That is, the upper limit of the preferable range of the addition amount of sodium aluminate with respect to 100 parts by mass of the SiC particles is the above-described value. If the coating proceeds to some extent, the effect obtained by the coating becomes constant, so that the economical efficiency and the production efficiency are further improved by controlling the amount of the raw material solution (2) to a predetermined amount or less.
- the amount of the acid used is not particularly limited, and may be adjusted so that the pH of the raw material dispersion (1) is not less than 9.0 and not more than 12.0.
- the acid is preferably added in the form of an aqueous solution, and the concentration of the acid in the aqueous solution is not particularly limited, but is not less than 1.0% by mass based on the total mass of the aqueous solution containing the acid. Is preferably 1.5% by mass or more, more preferably 2.0% by mass or more.
- the amount can be reduced from the addition amount of the aqueous solution containing an acid, and the productivity is further improved.
- the concentration of the acid in the aqueous solution is not particularly limited, but is preferably 30% by mass or less, more preferably 20% by mass or less, and more preferably 10% by mass or less, based on the total mass of the aqueous solution containing the acid. It is more preferred that: When the content is in the above range, the corrosiveness is lower and the equipment load is lower.
- the rate at which the raw material solution (2) and the acid are added is not particularly limited, and is appropriately in a range of pH 9.0 or more and 12.0 or less, and appropriately maintained thereafter. Adjust it.
- the maintenance time of the state in which the pH is in the range of 9.0 to 12.0 in the step (B) is not particularly limited, but is preferably 1 minute or more, more preferably 30 minutes or more, and 50 minutes or more. Minutes or more, more preferably 60 minutes or more.
- the SiC particles can be more sufficiently covered with aluminum hydroxide, and the function derived from aluminum hydroxide is further improved. Further, when the content is in the above range, when other particles described later are used in the dispersion, aggregation in the dispersion medium becomes more difficult to occur, and the dispersibility is further improved.
- the uniformity is further improved.
- the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body containing the same are further improved.
- the maintenance time of the state in which the pH is in the range of 9.0 or more and 12.0 or less in step (B) is not particularly limited, but is preferably 200 minutes or less, and more preferably 150 minutes or less. , 120 minutes or less, particularly preferably 90 minutes or less. If the coating progresses to some extent, the effect obtained by the coating will be constant, and if the maintenance time is within this range, the economic efficiency and the production efficiency will be further improved.
- step (B) is the same as the pH range in the coating step described above.
- the aluminum hydroxide-coated SiC particle powder is produced in the form of a dispersion containing the aluminum hydroxide-coated SiC particle powder and the dispersion medium.
- the aluminum hydroxide-coated SiC particle powder is produced in a state of being dispersed in the dispersion medium. It is also an example of a body manufacturing method.
- the dispersion medium, impurities, and the like may be removed using a known procedure and method.
- the above-described method for producing the aluminum hydroxide-coated SiC particle powder may further include a step other than the step (A) and the step (B). May further be provided.
- the solution or dispersion used in each step may contain other components as long as the effects of the present invention are not impaired.
- a dispersion including the above-described coated SiC particle powder and a dispersion medium.
- the dispersion has high dispersibility, for example, a powder material containing coated SiC particles having high uniformity, a green sheet, a prepreg material, or the like, a composition or a composite containing coated SiC particles powder. It can be preferably used as a raw material for the body. Further, it can be preferably used as a raw material for a sintered body of coated SiC particle powder and a molded body containing the same. As a result, higher density and higher mechanical strength can be obtained in the sintered body of the coated SiC particle powder and the molded body including the same by the dispersion. Further, the dispersion can be preferably used as a polishing composition having high polishing characteristics. However, the use of the dispersion is not limited to these.
- a dispersion according to one embodiment of the present invention includes a dispersion medium.
- the dispersion medium has a function of dispersing or dissolving each component.
- the dispersion medium may be a dispersion medium that is present immediately after the coating treatment in the production of the coated SiC particle powder, or may be a dispersion medium that has been replaced by a subsequent step of replacing the dispersion medium. Good.
- the dispersion medium preferably contains water, and more preferably only water. The water is preferably free from impurities as much as possible. For example, water having a total content of transition metal ions of 100 ppb or less is preferable.
- the purity of water can be increased by operations such as removal of impurity ions using an ion exchange resin, removal of foreign substances by a filter, and distillation.
- the dispersion medium may contain a solvent other than water, and the solvent other than water is preferably an organic solvent.
- the organic solvent include water-miscible organic solvents such as acetone, acetonitrile, ethanol, methanol, isopropanol, glycerin, ethylene glycol, and propylene glycol.
- the dispersion medium may be a mixed solvent of water and an organic solvent. These organic solvents can be used alone or in combination of two or more.
- the dispersion according to one embodiment of the present invention may contain other components as long as the effects of the present invention are not impaired.
- Other components are not particularly limited, but are particularly preferably other particles or a pH adjuster.
- the other particles do not include unavoidable impurities in the coating treatment.
- Other particles are not particularly limited, but particles having a lower limit of the isoelectric point pH of 5 or more are preferable.
- the other particles are not particularly limited, but particles having an upper limit of the isoelectric point pH of 11 or less are preferable.
- the uniformity is further improved. .
- the density and mechanical strength of the sintered body of the coated SiC particle powder and the molded body containing the same are further improved.
- the absolute value of the difference between the pH of the isoelectric point of the other particles and the pH of the isoelectric point of the coated SiC particle powder is preferably as small as possible, more preferably 2 or less, and preferably 1.5 or less. More preferably, it is still more preferably 1 or less (lower limit 0). This is because particles having a similar isoelectric point pH are less likely to aggregate.
- the particles having an isoelectric point pH of 5 or more and 11 or less are not particularly limited, and examples thereof include alumina, copper oxide, iron oxide, nickel oxide, tin oxide, cadmium oxide, zinc oxide, and zirconium oxide. Can be
- the pH adjuster is not particularly limited as long as a desired pH can be achieved, and a known pH adjuster may be appropriately used. Among these, it is preferable to use known acids, bases, salts, amines, chelating agents and the like.
- the pH of the dispersion according to one embodiment of the present invention is not particularly limited. From the viewpoint of achieving higher dispersibility, the pH of the dispersion is preferably a value that falls within the preferable pH range of the isoelectric point of the coated SiC particle powder.
- the method for producing a coated SiC particle powder when the coated SiC particle powder is produced in the form of a dispersion containing the coated SiC particle powder and a dispersion medium, the method is directly applied to the dispersion according to one embodiment of the present invention. It may be a manufacturing method. Further, in the method for producing the coated SiC particle powder, the target dispersion may be produced by replacing the dispersion medium present immediately after the coating treatment with another dispersion medium. For example, the coated SiC particles may be dispersed in the dispersion medium after removing the dispersion medium, impurities, and the like from the manufactured dispersion using known procedures and methods to take out the coated SiC particle powder.
- the procedure and method for dispersing the coated SiC particle powder in the dispersion medium are not particularly limited, and known procedures and methods can be used.
- the desired dispersion may be produced by adding the above-mentioned other components to the dispersion produced by these methods, if necessary.
- Green sheet> Another embodiment of the present invention relates to a green sheet including the coated SiC particle powder and a resin. Since the above-mentioned coated SiC particle powder has high dispersibility, the green sheet containing the same has the coated SiC particle powder present at high density and uniform inside thereof, resin is hardly separated, and voids are formed. Few. Therefore, by using the green sheet, it is possible to manufacture a high-density and high-strength compact including a sintered body of the coated SiC particle powder described later.
- the resin has a function as a binder.
- the resin used is not particularly limited, and a resin used for a known green sheet can be appropriately adopted.
- a butyral resin such as polyvinyl butyral, a polyacrylate resin, and a polymethacrylate resin are preferable, a butyral resin is more preferable, and polyvinyl butyral is more preferable.
- These resins may be used alone or in combination of two or more.
- the lower limit of the content of the resin in the green sheet is not particularly limited, but is preferably at least 1 part by mass, more preferably at least 10 parts by mass, based on 100 parts by mass of the coated SiC particle powder. More preferably, the amount is at least part by mass. Within the above range, a sheet containing the coated SiC particles can be formed more favorably.
- the upper limit of the content of the resin in the green sheet is not particularly limited, but is preferably 1,000 parts by mass or less, more preferably 500 parts by mass or less, based on 100 parts by mass of the coated SiC particle powder. , 200 parts by mass or less. When the content is in the above range, the amount of the resin component removed in the firing step is reduced, so that the economy and production efficiency are further improved.
- the green sheet according to one embodiment of the present invention preferably contains a plasticizer from the viewpoint of improving workability and flexibility.
- the plasticizer used is not particularly limited, and a known plasticizer used for a green sheet can be appropriately employed.
- a plasticizer glycerin, polyethylene glycol, dibutyl phthalate, di-2-ethylhexyl phthalate (dioctyl phthalate), and diisononyl phthalate are preferable, and glycerin is more preferable. These resins may be used alone or in combination of two or more.
- the lower limit of the content of the plasticizer in the green sheet is not particularly limited, but is preferably 1 part by mass or more, more preferably 5 parts by mass or more, based on 100 parts by mass of the coated SiC particle powder. More preferably, the amount is 10 parts by mass or more. Within the above range, the flexibility of the green sheet is further improved.
- the upper limit of the content of the plasticizer in the green sheet is not particularly limited, but is preferably 300 parts by mass or less, more preferably 200 parts by mass or less, based on 100 parts by mass of the coated SiC particle powder. More preferably, the amount is 100 parts by mass or less. Within the above range, the uniformity of the components in the green sheet is further improved.
- the green sheet according to one embodiment of the present invention may further include other green sheet forming components such as the other particles and the pH adjuster described in the section of the dispersion.
- the method for manufacturing the green sheet is not particularly limited, and a known procedure and method can be appropriately adopted.
- a coating liquid for forming a green sheet (dispersion for forming a green sheet) containing the above-mentioned coated SiC particle powder and a dispersion medium is prepared on a substrate, and the coating liquid for forming a green sheet is prepared.
- a method of forming a sheet by coating may be used.
- the application method is not particularly limited, and known procedures and methods can be appropriately adopted.
- an applicator coating method a bar coating method, a die coating method, a comma coating method, a gravure roll coating method, a blade coating method, a spray coating method, an air knife coating method, a dip coating method, a transfer method and the like can be mentioned.
- the dispersion medium of the coating liquid for forming a green sheet is not particularly limited, and examples thereof include the dispersion medium described in the section of the dispersion.
- the method of preparing the coating liquid for forming a green sheet is not particularly limited, and a known procedure and method can be appropriately employed. Among these, it is more preferable to mix each component of the green sheet forming dispersion under vacuum from the viewpoint of suppressing the mixing of impurities and unintended reactions to further improve the uniformity of the green sheet.
- the substrate is not particularly limited, for example, a resin film such as a polyolefin film (eg, a polyethylene film, a polypropylene film, etc.), a polyester film (eg, a polyethylene terephthalate (PET) film, a polyethylene naphthalate film, etc.), and polyvinyl chloride And the like are preferably used.
- a resin film such as a polyolefin film (eg, a polyethylene film, a polypropylene film, etc.), a polyester film (eg, a polyethylene terephthalate (PET) film, a polyethylene naphthalate film, etc.), and polyvinyl chloride And the like are preferably used.
- the thickness of the substrate is not particularly limited, but is preferably from 10 to 300 ⁇ m, more preferably from 20 to 150 ⁇ m.
- the method for producing a green sheet preferably includes a drying treatment of a coating film of a coating liquid for forming a green sheet.
- the drying temperature is not particularly limited, but is preferably from 25 ° C to 200 ° C, and more preferably from 25 ° C to 100 ° C.
- the drying time is not particularly limited, but is preferably 10 minutes or more and 3 hours or less.
- the coating film thickness (wet film thickness) of the coating liquid for forming a green sheet is not particularly limited, but is preferably 100 to 2000 ⁇ m from the viewpoint of productivity and suppression of cracking.
- a molded body including a sintered body of coated SiC particle powder described below can be manufactured.
- the molded article becomes a high-density and high-strength molded article.
- a prepreg material including a fiber base material, the above-described coated SiC particle powder and resin, or the above-described green sheet.
- the prepreg material is a semi-cured composite material produced by impregnating a fiber base material (fiber woven fabric) such as glass cloth, SiC fiber, or carbon fiber with a dispersion containing a resin and drying. .
- the above-mentioned coated SiC particle powder has high dispersibility.
- the prepreg material containing the coated SiC particle powder the coated SiC particle powder is present at a high density and uniform inside thereof, the resin is hardly separated, and there are few voids. Thereby, the prepreg material can produce a high-density and high-strength compact including a sintered body of the coated SiC particle powder described later.
- the method for producing the prepreg material is not particularly limited, and known procedures and methods can be appropriately adopted.
- a method of producing a prepreg material for example, a fiber substrate is impregnated with a prepreg material-forming dispersion containing the above-described coated SiC particle powder, a resin, and a dispersion medium, and the solvent is evaporated in a drying step. There is a method of removing. At this time, the impregnation may be performed by dipping, coating, or the like, and the operation may be repeated a plurality of times as necessary.
- the prepreg material forming dispersion for example, the same dispersion as the green sheet forming dispersion described above can be used.
- a method for producing the prepreg material for example, a method of laminating a sheet-like green sheet with a fiber base material can be used. Further, as a method of manufacturing the prepreg material, for example, a method of combining these two methods may be used.
- the prepreg material according to one embodiment of the present invention can produce a molded body including a sintered body of coated SiC particle powder described below by firing.
- the molded article becomes a high-density and high-strength molded article.
- ⁇ Sintered body> Another embodiment of the present invention relates to a sintered body of the coated SiC particle powder.
- the sintered body has high uniformity because the coated SiC particle powder as a raw material has high dispersibility. Then, high uniformity is realized also in a molded body including a sintered body of the coated SiC particle powder, such as a molded body obtained by firing a composition such as a green sheet or a prepreg material or a composite.
- the sintered body has a high density and a high strength
- a molded body including the same also has a high density and a high strength.
- the method for producing the sintered body is not particularly limited, and a known procedure and method can be appropriately employed.
- a method for producing a sintered body for example, a method of obtaining a dried powder of the coated SiC particle powder from the dispersion containing the above-mentioned coated SiC particle powder and a dispersion medium, followed by baking while applying pressure, and the like Is mentioned.
- the dispersion is filtered, washed, dried to obtain a dry powder, and then filled with a dry powder in a mold, and baked while uniaxially pressing, to form a molded article of a specific shape.
- the procedures and methods of filtration, washing and drying are not particularly limited, and known procedures and methods can be used.
- the filtration method and the washing method are not particularly limited, and examples thereof include a method of adding pure water to the dried powder of the coated SiC particle powder after the suction filtration, and repeating the suction filtration again.
- the mold for filling the dry powder at the time of sintering is not particularly limited, and examples thereof include a carbon mold having excellent heat resistance.
- Examples of the method for producing a sintered body include a method in which the green sheet and the prepreg material are fired while being pressed. As an example of the method, there is a method in which the green sheet and the prepreg material are fired while being uniaxially pressed to produce a sintered body in a state of a molded body having a specific shape.
- the procedure and method of uniaxial pressing are not particularly limited, and known procedures and methods can be used.
- the pressure device is not particularly limited, and for example, a commercially available vacuum hot press machine or the like can be used.
- the lower limit of the pressure during firing is not particularly limited, but is preferably 0.1 MPa or more, more preferably 1 MPa or more, and even more preferably 5 MPa or more.
- the sintering of the coated SiC particle powder can be further advanced.
- the upper limit of the firing pressure is not particularly limited, but is preferably 50 MPa or less, more preferably 40 MPa or less, and even more preferably 30 Pa or less.
- the load on the device is further reduced, and the economy is further improved.
- the firing time is preferably determined as a firing keep time.
- the firing keep time refers to the time from when the firing temperature is higher than the target temperature to when the temperature is lower than the firing temperature.
- the temperature can be measured using, for example, a thermocouple thermometer.
- the lower limit of the firing keep time is not particularly limited, but is preferably 1 minute or more, more preferably 5 minutes or more, further preferably 10 minutes or more, and particularly preferably 60 minutes or more. .
- the sintering of the coated SiC particle powder can be further advanced. As a result, the density of the sintered body is further improved, the uniformity is further improved, and the mechanical strength of the sintered body and the molded body including the same are further improved.
- the upper limit of the firing keep time is that when the firing keep time is equal to or more than a certain value, sintering proceeds sufficiently, and since the composition and structure of the sintered body become constant, from the viewpoint of density, uniformity, and mechanical strength.
- the firing keep time is preferably 600 minutes or less, more preferably 480 minutes or less, and even more preferably 300 minutes or less, from the viewpoint of economy and production efficiency. When it is in the above range, economic efficiency and production efficiency are further improved.
- sintering conditions are employed such that there are two or more time zones in which the sintering temperature is equal to or higher than the target sintering temperature, it is preferable that each sintering keep time satisfies the above range.
- the firing temperature is preferably determined as a firing keep temperature.
- the firing keep temperature means an average temperature during the firing keep time.
- the average temperature can be calculated as the average of the values measured at two-second intervals.
- the temperature can be measured using, for example, a thermocouple thermometer.
- the lower limit of the firing keep temperature is not particularly limited, but is preferably 1000 ° C. or higher, more preferably 1100 ° C. or higher, further preferably 1200 ° C. or higher, and particularly preferably 1400 ° C. or higher. . Within the above range, the sintering of the coated SiC particle powder can be further advanced.
- the density of the sintered body is further improved, the uniformity is improved, and the mechanical strength of the sintered body and the molded body including the same are further improved.
- the upper limit of the firing keep temperature the sintering proceeds sufficiently when the firing keep temperature is above a certain level, the composition and structure of the sintered body become constant, from the viewpoint of density, uniformity, mechanical strength Is not particularly limited.
- the firing keep temperature is preferably 2400 ° C. or lower, more preferably 2200 ° C. or lower, and further preferably 2000 ° C. or lower, from the viewpoint of economy and production efficiency. When the content is in the above range, economy and productivity are further improved.
- sintering conditions are employed such that there are two or more time zones in which the sintering temperature is equal to or higher than the target sintering temperature, it is preferable that each sintering keep time satisfies the above range.
- the atmosphere during firing is not particularly limited, and includes, for example, air or an inert gas atmosphere.
- an inert atmosphere is used.
- the atmosphere is more preferably a gas atmosphere, more preferably a nitrogen atmosphere or an argon atmosphere, and particularly preferably an argon atmosphere.
- the strength of the sintered body can be determined by the bending strength of the formed body composed of only the sintered body.
- the strength of the sintered body is preferably as high as possible, more preferably 250 MPa or more, further preferably 300 MPa or more, particularly preferably 350 MPa or more, and most preferably 400 MPa or more.
- the upper limit of the strength of the sintered body is not particularly limited because it varies depending on the type and size of the SiC particles, the composition and thickness of the coating layer, firing conditions, and the like.
- the strength of the sintered body can be measured by a four-point bending test of a test piece having a length of 25 mm, a width of 2 mm, and a thickness of 1.5 mm using an electromechanical universal testing machine manufactured by Instron. The details of the measurement method will be described in Examples.
- the uniformity of the sintered body can be determined based on the density of a formed body composed of only the sintered body.
- the lower limit of the density of the sintered body is preferably 2.80 g / cm 3 or more, more preferably 2.85 g / cm 3 or more, further preferably 2.90 g / cm 3 or more.
- the upper limit of the density of the sintered body is preferably 3.90 g / cm 3 or less, more preferably 3.60 g / cm 3 or less, still be at 3.40 g / cm 3 or less preferable.
- the density of the sintered body can be measured by an Archimedes density measurement method using an analytical balance HR-250AZ manufactured by A & D Corporation and a specific gravity measurement kit AD-1654.
- ⁇ Molded body> Another embodiment of the present invention relates to a formed body including the above sintered body.
- the molded body has high uniformity, high density and high strength because the coated SiC particle powder as a raw material has high dispersibility.
- the method for producing the molded article according to one embodiment of the present invention is not particularly limited, but as described above, the coated SiC particle powder alone is fired, or the green sheet or the prepreg material containing the same is used. And a method of firing the composition and the composite. And as a preferable example of the manufacturing method of the molded article, the method for manufacturing the coated SiC particle powder includes SiC particles and a coating layer for coating the SiC particles, wherein the coating layer contains an aluminum element. A production step of producing coated SiC particle powder, and a composition or a composite containing the coated SiC particle powder, or the coated green sheet or the prepreg material containing the coated SiC particle powder such as the prepreg material.
- the control means for controlling the mass of the aluminum element per unit surface area of the SiC particles to 0.5 mg / m 2 or more is the same as that described in the method for producing coated SiC particles. The same is true.
- Example 1> (Production of powder 1) After preparing a 20% by mass aqueous dispersion of SiC particles (GC # 40000, average secondary particle diameter 0.36 ⁇ m, manufactured by Fujimi Incorporated), a 1M aqueous solution of NaOH was adjusted to pH 10.0 with a 1M NaOH aqueous solution. It was added to the aqueous dispersion of the particles to obtain a raw material dispersion (1). Next, a 30% by mass aqueous dispersion of sodium aluminate (raw material solution (2)) was prepared.
- GC # 40000 average secondary particle diameter 0.36 ⁇ m, manufactured by Fujimi Incorporated
- an aqueous dispersion of sodium aluminate (raw material solution (2)) in an amount of 8.9 parts by mass (in terms of solid content) of sodium aluminate with respect to 100 parts by mass of SiC particles, and 9.9 parts by mass % Nitric acid aqueous solution is added to the raw material dispersion (1) over 45 minutes with stirring so that the pH is maintained in the range of 9.0 to 11.0, and the dispersion (3-1) is added. Obtained. Then, the obtained dispersion liquid (3-1) was further stirred for 45 minutes.
- a 9.9% by mass aqueous solution of nitric acid was added over 10 minutes while stirring so as to have a pH of 10.5 to obtain a dispersion (3-2). .
- a 9.9% by mass aqueous nitric acid solution is further added to the obtained dispersion (3-2) so as to have a pH of 3.0 over 5 minutes to obtain a dispersion containing the powder 1.
- powder 1 was prepared.
- the maintenance time for maintaining the pH in the range of 9.0 or more and 11.0 or less is more than 100 minutes and less than 105 minutes. Met.
- Example 2> (Production of powder 2) Except that the amount of the aqueous dispersion of sodium aluminate was changed to 14.5 parts by mass of sodium aluminate (in terms of solid content) with respect to 100 parts by mass of SiC particles in the production of the powder 1. Prepared powder 2 in the same manner.
- Example 3 (Production of powder 3) Except that the amount of the aqueous dispersion of sodium aluminate was changed to 19.0 parts by mass of sodium aluminate (in terms of solid content) with respect to 100 parts by mass of SiC particles in the production of the powder 1. In the same manner, powder 3 was prepared.
- Example 4> (Production of powder 4) Except that the amount of the aqueous dispersion of sodium aluminate was changed to 23.0 parts by mass of sodium aluminate (in terms of solid content) with respect to 100 parts by mass of SiC particles in the production of the powder 1. Prepared powder 4 in the same manner.
- Example 5 (Production of powder 5) Except that in the production of the powder 1, the amount of the aqueous dispersion of sodium aluminate was changed so that 42.0 parts by mass (in terms of solid content) of sodium aluminate was added to 100 parts by mass of the SiC particles. In the same manner, powder 5 was prepared.
- the firing conditions were a firing temperature of 1400 ° C. or more, a pressure of 5 MPa or more, a firing time of 60 minutes or more, and an argon atmosphere.
- the temperature was measured at 2-second intervals using a thermocouple thermometer attached to the apparatus.
- the specific surface area of the raw material SiC particles used for producing the powders 1 to 7 was measured using a specific surface area meter (Flowsorb II, manufactured by Micromeritics). The specific surface area of the SiC particles was 32.3 m 2 / g.
- each dried powder was collected on a carbon tape and subjected to EELS (Electron Energy Loss Spectroscopy) analysis using TITAN80-300 manufactured by FEI.
- EELS Electro Energy Loss Spectroscopy
- the observed EELS spectrum is a spectrum shape specific to the EELS standard spectrum of aluminum hydroxide (Al (OH) 3 ) (the spectrum of Al and other compounds containing Al and O). Therefore, it was determined that the components containing Al and O in the coating layer of each powder included those existing in the state of Al (OH) 3 .
- Powders 1 to 7 were coated SiC particle powders containing SiC particles and a coating layer containing an aluminum element for coating the SiC particles.
- the density (g / cm 3 ) of each of the obtained sintered bodies was measured using Archimedes density measurement method.
- the measuring instrument used was an electronic balance for analysis HR-250AZ (manufactured by A & D Corporation) and a specific gravity measurement kit AD-1654 (manufactured by A & D Corporation).
- the bending strength (MPa) of each of the obtained sintered bodies was measured by a four-point bending test using an electromechanical universal testing machine (manufactured by Instron).
- the test piece shape was 25 mm in length, 2 mm in width, and 1.5 mm in thickness, the support span was 20 mm, the loading span was 10 mm, and the crosshead speed was 0.1 mm / min.
- Table 1 shows the mass of aluminum element per unit surface area of SiC particles in powder (mass of Al element per unit surface area of SiC), and the evaluation results of density, bending strength and color of the sintered body.
- the sintered body manufactured using the coated SiC particle powder according to Examples 1 to 5 wherein the mass of the aluminum element per unit surface area of the SiC particle is 0.5 mg / m 2 or more. It was confirmed that the molded article made of was high in density and bending strength, uniform and excellent in mechanical strength.
- the mixing mass ratio of the finally obtained coating liquid for forming a green sheet is 3: 3: 1 coated SiC particle powder: resin: plasticizer.
- These green sheet forming coating liquids 1 to 7 are applied to a PET film (thickness: 100 ⁇ m) with a wet film thickness of 1000 ⁇ m using an applicator having a 1000 ⁇ m gap to form a green sheet. 1 to 7 were obtained.
- the prepreg materials 1 to 7 were obtained by laminating the obtained green sheets 1 to 7 with SiC fiber woven fabrics, respectively.
- each green sheet and each prepreg material obtained above are fired while being uniaxially pressed by a vacuum hot press machine (manufactured by Fuji Denki Kogyo Co., Ltd.) to fire each coated SiC particle powder contained therein.
- a molded body including each sintered body of each coated SiC particle powder was manufactured.
- the firing conditions were a firing temperature of 1400 ° C. or more, a pressure of 5 MPa or more, a firing time of 60 minutes or more, and an argon atmosphere. During firing, the temperature was measured at 2-second intervals using a thermocouple thermometer attached to the apparatus.
- the bending strength of each of the obtained compacts was measured in the same manner as above, and the order of the strength (order) was the order of the bending strength of the compact, which was a sintered body of each powder contained therein. (Order).
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
炭化珪素粒子と、前記炭化珪素粒子を被覆する被覆層と、を含み、前記被覆層は、アルミニウム元素を含み、前記炭化珪素粒子の単位表面積当たりの前記アルミニウム元素の質量が0.5mg/m2以上である、被覆炭化珪素粒子粉体。
本発明の一形態は、炭化珪素粒子と、前記炭化珪素粒子を被覆するアルミニウム元素を含む被覆層と、を含み、前記被覆層は、アルミニウム元素を含み、前記炭化珪素粒子の単位表面積当たりの前記アルミニウム元素の質量が0.5mg/m2以上である、被覆炭化珪素粒子粉体に関する。本発明の一形態によれば、焼結助剤と、炭化珪素粒子とを含む組成物の焼結体およびこれを含む成形体において、密度および機械的強度を向上させうる手段が提供される。
被覆SiC粒子粉体のSiC粒子の単位表面積あたりのアルミニウム(Al)元素の質量(以下、「SiC単位表面積あたりのAl元素の質量」とも称する)は0.5mg/m2以上である。SiC単位表面積あたりのAl元素の質量が0.5mg/m2未満であると、被覆SiC粒子粉体の焼結体およびこれを含む成形体において、焼結が十分に進行せず、焼結体が不均一な構造となり、密度および機械的強度が不十分となる。同様の観点から、SiC単位表面積あたりのAl元素の質量は、1mg/m2以上であることが好ましい。さらに得られる焼結体およびこれを含む成形体に色味の均一性を向上させるとの観点も加味すると、SiC単位表面積あたりのAl元素の質量は、1.2mg/m2以上であることがより好ましく、1.35mg/m2以上であることがさらに好ましい。なお、色味は焼結体の均一性と関連しており、色味の均一性が向上すると、焼結体の均一性も向上すると考えられる。また、SiC単位表面積あたりのAl元素の質量の上限は、特に制限されないが、30mg/m2以下であることが好ましく、20mg/m2以下であることがより好ましく、10mg/m2以下であることがさらに好ましい。上記範囲であると、焼結体およびこれを含む成形体におけるSiC粒子に由来する機能がより向上する。SiC単位表面積あたりのAl元素の質量は、以下のように測定することができる。まず、SiC粒子の比表面積をMicromeritics社製の比表面積測定計FlowSorb IIを用いて測定する。次いで、株式会社島津製作所製の蛍光X線分析装置 XRF-1700を用いて、被覆SiC粒子粉体(乾燥粉体)100質量部および四ホウ酸リチウム10質量部からなるバルク体のAl元素とSi元素との重量比α(α=Al/Si)を測定する。続いて、SiC単位表面積あたりのAl元素の質量を、αと、SiC粒子の比表面積と、Si原子量およびSiC分子量とを用いて算出する。なお、測定方法、算出方法の詳細は実施例に記載する。
被覆SiC粒子粉体の平均二次粒子径の上限は、特に制限されないが、10μm以下であることが好ましく、5μm以下であることがより好ましく、2μm以下であることがさらに好ましく、1μm以下であることが特に好ましく、0.5μm以下であることが最も好ましい。上記範囲であると、被覆SiC粒子粉体を媒体に分散させた際に、分散性がより向上する。また、被覆SiC粒子粉体や、グリーンシート、プリプレグ材等の被覆SiC粒子粉体を含む組成物や複合体の均一性がより向上する。そして、被覆SiC粒子粉体の焼結体、およびこれを含む成形体の密度および機械的強度がより向上する。この理由は、平均二次粒子径が小さい場合、個々の被覆SiC粒子の粒子径のバラツキも小さいからであると推定される。また、被覆SiC粒子粉体の平均二次粒子径の下限は、特に制限されないが、0.03μm以上であることが好ましく、0.03μm超であることがより好ましく、0.05μm以上であることがさらに好ましく、0.05μm超であることがよりさらに好ましく、0.1μm以上であることが特に好ましく、0.1μm超であることが最も好ましい。上記範囲であると、分散体において後述する他の粒子を併用する場合、分散媒中における凝集がより生じ難くなり、分散性がより向上する。また、被覆SiC粒子粉体を含む粉体材料、グリーンシート、プリプレグ材等の被覆SiC粒子粉体を含む組成物や複合体において、後述する他の粒子を併用する場合、均一性がより向上する。これより、被覆SiC粒子粉体の焼結体、およびこれを含む成形体の密度および機械的強度がより向上する。この理由は、粒子径が大きくなると、同一質量における被覆SiC粒子の数が減少することから、被覆SiC粒子と、他の粒子との間で生じる粒子凝集の頻度をより低減させることができるからと推定される。ここで、被覆SiC粒子粉体の平均二次粒子径の値は、測定の適正濃度となるよう被覆SiC粒子粉体を分散媒に分散させた分散体において、株式会社堀場製作所製の散乱式粒子径分布測定装置LA-950により測定することができる。
被覆SiC粒子粉体の等電点のpHの下限は、特に制限されないが、4.5以上であることが好ましく、5以上であることがより好ましく、5.5以上であることがさらに好ましく、6以上であることがよりさらに好ましく、6.5以上であることが特に好ましく、7.5以上であることが最も好ましい。また、被覆SiC粒子粉体の等電点のpHの上限は、特に制限されないが、9以下であることが好ましく、8.5以下であることがより好ましい。上記範囲であると、分散体において後述する他の粒子を併用する場合、分散媒中における凝集がより生じ難くなり、分散性がより向上する。また、被覆SiC粒子粉体を含む粉体材料、グリーンシート、プリプレグ材等の被覆SiC粒子粉体を含む組成物や複合体において、後述する他の粒子を併用する場合、均一性がより向上する。これより、被覆SiC粒子粉体の焼結体、およびこれを含む成形体の密度および機械的強度がより向上する。等電点のpHは、1.0刻みのpH、例えば、1.0刻みのpH3.0~10.0の範囲のpHのゼータ電位測定液を調製してゼータ電位を測定し、ゼータ電位の符号が変化した前後のpHと、前後のpHにおけるゼータ電位から、以下の式により算出することができる。
炭化珪素(SiC)粒子は、高硬度であり、高温耐熱性、機械的強度、耐衝撃性、耐摩耗性、耐酸化性および耐食性に優れ、熱膨張係数が小さいことから、研磨用組成物や、高温構造部材をはじめとして、種々の用途で用いられうる。
被覆SiC粒子の被覆層は、アルミニウム元素を含む。当該被覆層は、SiC粒子に対して、絶縁性を付与する機能や、成形体を製造する際の焼結助剤としての機能や、研磨用組成物に使用した際の研磨特性を向上させる機能を付与することができる。
被覆SiC粒子粉体の製造方法は、被覆層中のアルミニウム元素がアルミニウム化合物の形で含有される場合、SiC粒子と、被覆層に含まれるアルミニウム化合物またはその前駆体と、分散媒とを含む分散体の状態で被覆を進行させる方法であることが好ましい。
上記の好ましい一形態に係る水酸化アルミニウム被覆SiC粒子粉体の製造方法は、SiC粒子、アルカリおよび水を含み、pHが9.0以上12.0以下である原料分散体(1)と、アルミン酸ナトリウムおよび水を含む原料溶液(2)と、をそれぞれ準備する工程(A)を有する。
上記の好ましい一形態に係る水酸化アルミニウム被覆SiC粒子粉体の製造方法は、工程(A)で準備された原料分散体(1)に、原料溶液(2)と、酸とを添加して、pHを9.0以上12.0以下の範囲に維持し、前記SiC粒子の表面に水酸化アルミニウムを含む被覆層を有する被覆粒子を形成する工程(B)を有する。本工程(B)では、水酸化アルミニウム被覆SiC粒子が製造される。
上記の水酸化アルミニウム被覆SiC粒子粉体の製造方法では、工程(A)および工程(B)以外の他の工程をさらに有していてもよく、工程(A)および工程(B)において、他の操作に係る段階をさらに有していてもよい。
本発明の他の一形態は、上記の被覆SiC粒子粉体と、分散媒とを含む、分散体に関する。当該分散体は、高い分散性を有することから、例えば、高い均一性を有する被覆SiC粒子粉体を含む粉体材料、グリーンシート、プリプレグ材等の、被覆SiC粒子粉体を含む組成物や複合体の原料として好ましく用いられうる。また、被覆SiC粒子粉体の焼結体、およびこれを含む成形体の原料として好ましく用いられうる。これより、当該分散体によって、被覆SiC粒子粉体の焼結体、およびこれを含む成形体において、より高い密度およびより高い機械的強度が得られる。また、当該分散体は、高い研磨特性を有する研磨用組成物として好ましく用いられうる。ただし、分散体の用途はこれらに限定されるものではない。
本発明の一形態に係る分散体は、分散媒を含む。分散媒は、各成分を分散または溶解させる機能を有する。分散媒は、上記の被覆SiC粒子粉体の製造における被覆処理の直後に存在する分散媒であってもよく、その後、当該分散媒を置換する工程、操作によって置換された分散媒であってもよい。分散媒は、水を含むことが好ましく、水のみであることがより好ましい。水は、不純物をできる限り含有しない水が好ましい。例えば、遷移金属イオンの合計含有量が100ppb以下である水が好ましい。ここで、水の純度は、例えば、イオン交換樹脂を用いる不純物イオンの除去、フィルタによる異物の除去、蒸留等の操作によって高めることができる。具体的には、水としては、例えば、脱イオン水(イオン交換水)、純水、超純水、蒸留水などを用いることが好ましい。また、分散媒は、水以外の溶剤を含んでいてもよく、水以外の溶剤は有機溶剤であることが好ましい。有機溶媒としては、例えば、アセトン、アセトニトリル、エタノール、メタノール、イソプロパノール、グリセリン、エチレングリコール、プロピレングリコール等の水と混和する有機溶媒が挙げられる。分散媒は、水と有機溶媒との混合溶媒であってもよい。これら有機溶媒は、単独でもまたは2種以上組み合わせても用いられうる。
本発明の一形態に係る分散体は、本発明の効果を損なわない限り、他の成分を含んでいてもよい。他の成分は、特に制限されないが、他の粒子またはpH調整剤であることが特に好ましい。ここで、他の粒子には、被覆処理における不可避不純物は含まない。
本発明の一形態に係る分散体のpHは、特に制限されない。より高い分散性を実現するとの観点から、分散体のpHは、上記の被覆SiC粒子粉体の好ましい等電点のpHの範囲内となる値であることが好ましい。
被覆SiC粒子粉体の製造方法において、被覆SiC粒子粉体および分散媒を含む分散体の形態で被覆SiC粒子粉体が製造される場合、当該方法をそのまま本発明の一形態に係る分散体の製造方法としてもよい。また、被覆SiC粒子粉体の製造方法における、被覆処理の直後に存在する分散媒を、他の分散媒へと置換することによって目的の分散体を製造してもよい。例えば、製造される分散体から公知の手順、方法を用いて分散媒や不純物等を除去して被覆SiC粒子粉体を取り出した後、分散媒に、被覆SiC粒子を分散させてもよい。分散媒に、被覆SiC粒子粉体を分散させる手順、方法としては、特に制限されず、公知の手順、方法が用いられうる。なお、これらの方法により製造される分散体に、必要に応じて上記他の成分を添加して目的の分散体を製造してもよい。
本発明の他の一形態は、上記の被覆SiC粒子粉体と、樹脂とを含む、グリーンシートに関する。上記の被覆SiC粒子粉体は、高い分散性を有することから、これを含むグリーンシートは、その内部において被覆SiC粒子粉体が高密度で均一に存在し、樹脂の分離が生じにくく、空隙が少ない。よって、当該グリーンシートを用いることにより、後述する被覆SiC粒子粉体の焼結体を含む、高密度かつ高強度の成形体を製造することができる。
本発明の他の一形態は、繊維基材と、上記の被覆SiC粒子粉体および樹脂、または上記グリーンシートとを含む、プリプレグ材に関する。プリプレグ材とは、ガラスクロス、SiC繊維、炭素繊維等の繊維基材(繊維織布)に樹脂を含んだ分散体を含浸させ、乾燥させることで作製した半硬化状態の複合材料のことである。上記の被覆SiC粒子粉体は、高い分散性を有する。そして、当該被覆SiC粒子粉体を含むプリプレグ材は、その内部において被覆SiC粒子粉体が高密度で均一に存在し、樹脂の分離が生じにくく、空隙が少ない。これより、当該プリプレグ材は、後述する被覆SiC粒子粉体の焼結体を含む、高密度かつ高強度の成形体を製造することができる。
本発明の他の一形態は、上記の被覆SiC粒子粉体の焼結体に関する。当該焼結体は、原料となる被覆SiC粒子粉体が高い分散性を有することから、高い均一性を有する。そして、グリーンシート、プリプレグ材等の組成物や複合体等を焼成して得られる成形体等の、当該被覆SiC粒子粉体の焼結体を含む成形体においても高い均一性が実現される。これより、当該焼結体は高密度かつ高強度であり、これを含む成形体も高密度かつ高強度となる。
本発明の他の一形態は、上記の焼結体を含む、成形体に関する。当該成形体は、原料となる被覆SiC粒子粉体が高い分散性を有することから、高い均一性を有し、高密度かつ高強度である。
(粉体1の製造)
SiC粒子(GC#40000、平均二次粒子径0.36μm、株式会社フジミインコーポレーテッド製、粉体)の20質量%水分散液を準備した後、1M NaOH水溶液をpH10.0となるよう前記SiC粒子の水分散液に添加して、原料分散体(1)を得た。次いで、アルミン酸ナトリウムの30質量%水分散液(原料溶液(2))を準備した。続いて、SiC粒子100質量部に対してアルミン酸ナトリウムが8.9質量部(固形分換算)となる量の前記アルミン酸ナトリウムの水分散液(原料溶液(2))と、9.9質量%硝酸水溶液とを、pHが9.0以上11.0以下の範囲を保持するように、撹拌しながら45分間かけて、原料分散体(1)に添加して分散体(3-1)を得た。そして、得られた分散液(3-1)をさらに45分間撹拌した。その後、攪拌後の分散体(3-1)に対して、pH10.5となるよう9.9質量%硝酸水溶液を撹拌しながら10分間かけて添加して分散体(3-2)を得た。そして、得られた分散液(3-2)に対して、pH3.0となるように9.9質量%硝酸水溶液をさらに5分間かけて添加して、粉体1を含む分散液を得ることで、粉体1を調製した。ここで、原料分散体(1)に原料溶液(2)と、酸とを添加してから、pHを9.0以上11.0以下の範囲に維持する維持時間は、100分超105分未満であった。
(粉体2の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 14.5質量部(固形分換算)となるように変更したこと以外は同様にして、粉体2を調製した。
(粉体3の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 19.0質量部(固形分換算)となるように変更したこと以外は同様にして、粉体3を調製した。
(粉体4の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 23.0質量部(固形分換算)となるように変更したこと以外は同様にして、粉体4を調製した。
(粉体5の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 42.0質量部(固形分換算)となるように変更したこと以外は同様にして、粉体5を調製した。
(粉体6の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 3.5質量部(固形分換算)となるように変更したこと以外は同様にして、粉体6を調製した。
(粉体7の製造)
上記粉体1の製造において、アルミン酸ナトリウムの水分散液の添加量を、SiC粒子1 100質量部に対してアルミン酸ナトリウム 5.9質量部(固形分換算)となるように変更したこと以外は同様にして、粉体7を調製した。
上記得られた粉体1~7を含む各分散液300gをろ紙(5A)を用いて吸引ろ過した後、純水50gを加えて吸引ろ過を再度行う洗浄工程を3回行い、ろ紙上の粉体の湿潤物を回収し乾固することで、各乾燥粉体を得た。次いで、カーボン製の幅40mm×奥行40mm×高さ30mmの直方体状の型に得られた各乾燥粉体を充填し、真空ホットプレス機(富士電波工業株式会社製)にて一軸加圧しながら焼成することで、各焼結体からなる成形体を製造した。ここで、焼成条件は、焼成キープ温度が1400℃以上、圧力が5MPa以上、焼成キープ時間が60分以上、アルゴン雰囲気下の条件であった。焼成中は、装置付随の熱電対式温度計を用いて、2秒間隔で温度測定を行った。
(平均一次粒子径の測定)
粉体1~7の製造に用いた原料SiC粒子について、SEM(株式会社日立ハイテクノロジーズ製、SU8000)撮影を行い、画像解析式粒度分布ソフトウェア(株式会社マウンテック製、MacView)を用いて、粒子100個の体積平均粒子径より平均一次粒子径を測定した。SiC粒子の平均一次粒子径は0.30μmであった。
粉体1~7の製造に用いた原料SiC粒子について比表面積測定計(Micromeritics社製、FlowSorb II)を用いて比表面積を測定した。SiC粒子の比表面積は32.3m2/gであった。
上記得られた粉体1~7を含む各分散体を約2mL採取し、フィルタ(ニュークリポア 5μm)(WHATMAN製)上に滴下した。続いて、吸引濾過を行い、その後、純水10mL用いてフィルタ上で粉体を洗浄し、乾燥させることで、各乾燥粉体を得た。そして、各乾燥粉体をSiウエーハ上に採取して、株式会社日立ハイテクノロジーズ製走査型電子顕微鏡SU-8000を用いて、SEM(Scanning Electron Microscope)-EDX(Energy Dispersive X-ray Spectroscopy)観察を行った。
上記焼結体の製造と同様の手順にて、実施例および比較例に係る各粉体を含む分散液より各乾燥粉体を得た。この乾燥粉体10gに対し、四ホウ酸リチウム1gを加え、加圧成型することでバルク体を形成し、蛍光X線分析装置 XRF-1700(株式会社島津製作所製)にてAl元素とSi元素との重量比α(α=Al/Si)を測定した。前記αとSiC原料(SiC粒子)の比表面積より、下記式を用いて、SiC粒子の単位表面積あたりのアルミニウム元素の質量γ(g)を算出した。なお、下記式において、SiC原料の比表面積とは、粉体の製造において原料として用いた、SiC粒子の比表面積を表す。
上記得られた各焼結体について、アルキメデス密度測定法を用いて密度(g/cm3)測定を行った。測定機は、分析用電子天秤 HR-250AZ(株式会社エー・アンド・ディ製)および比重測定キット AD-1654(株式会社エー・アンド・ディ製)を用いた。
上記得られた各焼結体について、電気機械式万能試験機(インストロン社製)を用いて、4点曲げ試験により曲げ強度(MPa)を測定した。試験片形状は長さ25mm、幅2mm、厚さ1.5mmとし、サポートスパンは20mm、ローディングスパンは10mm、クロスヘッドスピードは0.1mm/minの条件にて実施した。
上記得られた各焼結体について、目視にて色味を確認し、以下の基準に従って評価を行った。なお、色味は均一であることがより望ましいが、外周部にのみ変色が確認された場合であっても実用上許容され得る範囲とする:
A:全体で色味は均一であった;
B:外周部にのみ変色が確認された。
上記得られた粉体1~7を含む各分散液に対し、可塑剤であるグリセリン(和光純薬工業株式会社製)を混合し、真空下で15分混練して分散体を得た(ハイビスミックス2P-03型、プライミクス株式会社製使用)。その後、得られた分散体に対して、20質量%PVB(ポリビニルブチラール、製品名KW-1、積水マテリアルソリューションズ株式会社製)水溶液を投入し、真空下で30分混練して、グリーンシート形成用塗工液(グリーンシート形成用分散体)1~7を得た。最終的に得られたグリーンシート形成用塗工液の混合質量比は、被覆SiC粒子粉体:樹脂:可塑剤が3:3:1である。これらのグリーンシート形成用塗工液1~7を、1000μmギャップのアプリケーターを用いて、湿潤膜厚1000μmとして、PETフィルム(厚さ:100μm)上に塗布してシート成形を行うことで、グリーンシート1~7を得た。
上記得られたグリーンシート1~7を、それぞれSiC繊維織布と積層することでプリプレグ材1~7を得た。
上記得られた各グリーンシートおよび各プリプレグ材を、それぞれ真空ホットプレス機(富士電波工業株式会社製)にて一軸加圧しながら焼成することで、これらに含まれる各被覆SiC粒子粉体を焼成し、各被覆SiC粒子粉体の各焼結体を含む成形体を製造した。ここで、焼成条件は、焼成キープ温度が1400℃以上、圧力が5MPa以上、焼成キープ時間が60分以上、アルゴン雰囲気下の条件であった。焼成中は、装置付随の熱電対式温度計を用いて、2秒間隔で温度測定を行った。
Claims (8)
- 炭化珪素粒子と、前記炭化珪素粒子を被覆する被覆層とを含み、前記被覆層は、アルミニウム元素を含み、前記炭化珪素粒子の単位表面積当たりの前記アルミニウム元素の質量が0.5mg/m2以上である、被覆炭化珪素粒子粉体。
- 前記被覆層は、酸化アルミニウム前駆体を含み、前記酸化アルミニウム前駆体は、前記アルミニウム元素を含む、請求項1に記載の被覆炭化珪素粒子粉体。
- 前記酸化アルミニウム前駆体は、水酸化アルミニウムを含む、請求項2に記載の被覆炭化珪素粒子粉体。
- 請求項1~3のいずれか1項に記載の被覆炭化珪素粒子粉体と、分散媒とを含む、分散体。
- 請求項1~3のいずれか1項に記載の被覆炭化珪素粒子粉体と、樹脂とを含む、グリーンシート。
- 繊維基材と、請求項1~3のいずれか1項に記載の被覆炭化珪素粒子粉体および樹脂、または請求項5に記載のグリーンシートとを含む、プリプレグ材。
- 請求項1~3のいずれか1項に記載の被覆炭化珪素粒子粉体の焼結体。
- 請求項7に記載の焼結体を含む、成形体。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19865314.9A EP3858802A4 (en) | 2018-09-28 | 2019-06-13 | COATED SILICON CARBIDE PARTICLE POWDER |
CA3113924A CA3113924A1 (en) | 2018-09-28 | 2019-06-13 | Coated silicon carbide particle powder |
US17/280,648 US20210380813A1 (en) | 2018-09-28 | 2019-06-13 | Coated silicon carbide particle powder |
CN201980061962.9A CN112739664B (zh) | 2018-09-28 | 2019-06-13 | 覆盖碳化硅颗粒粉体 |
JP2020547971A JP7466871B2 (ja) | 2018-09-28 | 2019-06-13 | 被覆炭化珪素粒子粉体 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2018183284 | 2018-09-28 | ||
JP2018-183284 | 2018-09-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2020066152A1 true WO2020066152A1 (ja) | 2020-04-02 |
Family
ID=69952557
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2019/023511 WO2020066152A1 (ja) | 2018-09-28 | 2019-06-13 | 被覆炭化珪素粒子粉体 |
Country Status (6)
Country | Link |
---|---|
US (1) | US20210380813A1 (ja) |
EP (1) | EP3858802A4 (ja) |
JP (1) | JP7466871B2 (ja) |
CN (1) | CN112739664B (ja) |
CA (1) | CA3113924A1 (ja) |
WO (1) | WO2020066152A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112479729A (zh) * | 2021-01-05 | 2021-03-12 | 中钢南京环境工程技术研究院有限公司 | 一种高强碳化硅-氧化物复合材料及其制备方法 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113912399B (zh) * | 2021-12-15 | 2022-02-25 | 山东金鸿新材料股份有限公司 | 一种高密度无压烧结碳化硅陶瓷的制备方法 |
CN117658642B (zh) * | 2023-11-30 | 2024-05-28 | 东莞傲众磨具制品有限公司 | 一种高耐磨的研磨材料及其制备方法 |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5771868A (en) * | 1980-10-22 | 1982-05-04 | Hitachi Chemical Co Ltd | Manufacture of silicon carbide powder clad with aluminum fine powder |
JPS62138362A (ja) * | 1985-12-13 | 1987-06-22 | 新日本製鐵株式会社 | 炭化珪素質焼結原料の製造方法 |
JPH02267167A (ja) * | 1989-04-10 | 1990-10-31 | Teijin Ltd | 複合セラミックスシート状成形物及びその製造方法 |
JPH0912373A (ja) * | 1995-06-27 | 1997-01-14 | Ishikawajima Harima Heavy Ind Co Ltd | 界面制御セラミックスの製造方法 |
JP2001284509A (ja) * | 2000-03-30 | 2001-10-12 | Hitachi Metals Ltd | Al−SiC複合体 |
JP2012106888A (ja) | 2010-11-18 | 2012-06-07 | Shinano Denki Seiren Kk | 高絶縁性炭化ケイ素粉体及び該粉体を含有する組成物 |
JP2018183284A (ja) | 2017-04-24 | 2018-11-22 | 株式会社オリンピア | 遊技機 |
WO2019049784A1 (ja) * | 2017-09-08 | 2019-03-14 | 国立研究開発法人物質・材料研究機構 | 被覆SiCナノ粒子を用いたSiCセラミックス及びその製造方法 |
Family Cites Families (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5165996A (en) * | 1990-05-08 | 1992-11-24 | E. I. Du Pont De Nemours And Company | Coated refractory compositions and method for preparing the same |
JP2671945B2 (ja) * | 1995-03-03 | 1997-11-05 | 科学技術庁無機材質研究所長 | 超塑性炭化ケイ素焼結体とその製造方法 |
EP0792853B1 (en) * | 1996-02-29 | 2001-04-25 | Bridgestone Corporation | Process for making a silicon carbide sintered body |
JPH1017365A (ja) * | 1996-05-01 | 1998-01-20 | Mitsubishi Heavy Ind Ltd | 炭化珪素質焼結体およびその製造方法 |
JPH1179843A (ja) * | 1997-08-27 | 1999-03-23 | Bridgestone Corp | 炭化ケイ素構造体の製造方法および該製造方法による炭化ケイ素構造体 |
RU2404021C2 (ru) * | 2004-09-23 | 2010-11-20 | Элемент Сикс (Пти) Лтд. | Поликристаллические абразивные материалы и способ их изготовления |
JP4951753B2 (ja) * | 2005-01-25 | 2012-06-13 | 国立大学法人 鹿児島大学 | 炭化ケイ素焼結体の製造方法 |
FR2918982B1 (fr) * | 2007-07-19 | 2010-10-22 | Sicat | Support de catalyseur a base de beta-sic avec une couche d'alumine |
JP2010189203A (ja) * | 2009-02-16 | 2010-09-02 | Sumitomo Osaka Cement Co Ltd | SiC系耐摩耗材料およびその製造方法 |
JP5706671B2 (ja) * | 2010-11-15 | 2015-04-22 | 独立行政法人産業技術総合研究所 | 昇華再結晶法による炭化ケイ素単結晶製造用炭化ケイ素粉体及びその製造方法 |
CN103011822B (zh) * | 2011-09-28 | 2015-03-11 | 深圳光启高等理工研究院 | 一种超材料的介质基板材料及其制备方法 |
FR2989970A1 (fr) * | 2012-04-27 | 2013-11-01 | Saint Gobain Ct Recherches | Produit en carbure de silicium dense |
EP2861546B1 (en) * | 2012-06-15 | 2022-08-31 | Saint-Gobain Ceramics & Plastics Inc. | Method of forming a ceramic body comprising silicon carbide, and armor component comprising said ceramic body |
KR102090984B1 (ko) * | 2015-03-31 | 2020-03-19 | 니끼 쇼꾸바이 카세이 가부시키가이샤 | 실리카계 복합 미립자 분산액, 그의 제조 방법 및 실리카계 복합 미립자 분산액을 포함하는 연마용 슬러리 |
KR102384719B1 (ko) * | 2016-06-22 | 2022-04-08 | 우니베르시태트 바이로이트 | 세라믹 복합 재료 및 이의 제조 방법 |
CN107500772A (zh) * | 2017-07-27 | 2017-12-22 | 苏州诺瑞达新材料科技有限公司 | 一种碳化硅陶瓷预制体、铝基碳化硅陶瓷材料及其制备方法 |
CA3074410C (en) | 2017-09-28 | 2022-06-21 | Fujimi Incorporated | Method for producing aluminum hydroxide-coated silicon carbide particle powder and method for producing dispersion containing the same powder and dispersing medium |
CN108249925B (zh) * | 2017-12-20 | 2021-01-05 | 中核北方核燃料元件有限公司 | 一种全陶瓷微封装燃料芯块的制备方法 |
JP7252941B2 (ja) * | 2018-03-30 | 2023-04-05 | 株式会社フジミインコーポレーテッド | 炭化ケイ素焼結体用分散体、これを用いた炭化ケイ素焼結体用グリーンシートおよび炭化ケイ素焼結体用プリプレグ材、ならびにその製造方法 |
-
2019
- 2019-06-13 EP EP19865314.9A patent/EP3858802A4/en active Pending
- 2019-06-13 US US17/280,648 patent/US20210380813A1/en active Pending
- 2019-06-13 CA CA3113924A patent/CA3113924A1/en active Pending
- 2019-06-13 JP JP2020547971A patent/JP7466871B2/ja active Active
- 2019-06-13 CN CN201980061962.9A patent/CN112739664B/zh active Active
- 2019-06-13 WO PCT/JP2019/023511 patent/WO2020066152A1/ja unknown
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5771868A (en) * | 1980-10-22 | 1982-05-04 | Hitachi Chemical Co Ltd | Manufacture of silicon carbide powder clad with aluminum fine powder |
JPS62138362A (ja) * | 1985-12-13 | 1987-06-22 | 新日本製鐵株式会社 | 炭化珪素質焼結原料の製造方法 |
JPH02267167A (ja) * | 1989-04-10 | 1990-10-31 | Teijin Ltd | 複合セラミックスシート状成形物及びその製造方法 |
JPH0912373A (ja) * | 1995-06-27 | 1997-01-14 | Ishikawajima Harima Heavy Ind Co Ltd | 界面制御セラミックスの製造方法 |
JP2001284509A (ja) * | 2000-03-30 | 2001-10-12 | Hitachi Metals Ltd | Al−SiC複合体 |
JP2012106888A (ja) | 2010-11-18 | 2012-06-07 | Shinano Denki Seiren Kk | 高絶縁性炭化ケイ素粉体及び該粉体を含有する組成物 |
JP2018183284A (ja) | 2017-04-24 | 2018-11-22 | 株式会社オリンピア | 遊技機 |
WO2019049784A1 (ja) * | 2017-09-08 | 2019-03-14 | 国立研究開発法人物質・材料研究機構 | 被覆SiCナノ粒子を用いたSiCセラミックス及びその製造方法 |
Non-Patent Citations (1)
Title |
---|
See also references of EP3858802A4 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112479729A (zh) * | 2021-01-05 | 2021-03-12 | 中钢南京环境工程技术研究院有限公司 | 一种高强碳化硅-氧化物复合材料及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN112739664B (zh) | 2023-07-21 |
EP3858802A4 (en) | 2021-11-10 |
US20210380813A1 (en) | 2021-12-09 |
EP3858802A1 (en) | 2021-08-04 |
CN112739664A (zh) | 2021-04-30 |
JP7466871B2 (ja) | 2024-04-15 |
CA3113924A1 (en) | 2020-04-02 |
JPWO2020066152A1 (ja) | 2021-08-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP2409952B1 (en) | Zinc oxide particle, heat conductive filler, heat conductive resin composition, heat conductive grease and heat conductive coating composition | |
JP7466871B2 (ja) | 被覆炭化珪素粒子粉体 | |
US8399092B2 (en) | Zinc oxide particle having high bulk density, method for producing it, exoergic filler, exoergic resin composition, exoergic grease and exoergic coating composition | |
JP6404503B2 (ja) | アルミナおよびこれを含有するスラリー、ならびにこれを用いたアルミナ多孔膜、積層セパレータ、非水電解液二次電池および非水電解液二次電池の製造方法 | |
EP2455339B1 (en) | Magnesium oxide particles, method for producing same, heat dissipating filler, resin composition, heat dissipating grease, and heat dissipating coating composition | |
CN111132931B (zh) | 覆氢氧化铝的碳化硅颗粒粉体的制造方法、以及包含该粉体和分散介质的分散体的制造方法 | |
US20110081548A1 (en) | Zinc oxide particle, method for producing it, exoergic filler, exoergic resin composition, exoergic grease and exoergic coating composition | |
CN113365964B (zh) | 覆盖颗粒、包含其的分散液和成型体、以及使用其而形成的烧结体 | |
EP2565160B1 (en) | Filler particles, resin composition, grease, and coating composition | |
KR20140063691A (ko) | 옥살산바륨티타닐의 제조 방법 및 티탄산바륨의 제조 방법 | |
WO2019189254A1 (ja) | 炭化ケイ素焼結体用分散体、これを用いた炭化ケイ素焼結体用グリーンシートおよび炭化ケイ素焼結体用プリプレグ材、ならびにその製造方法 | |
JP6317536B1 (ja) | アルミナおよびこれを含有するスラリー、ならびにこれを用いたアルミナ多孔膜、積層セパレータ、非水電解液二次電池および非水電解液二次電池の製造方法 | |
JP5974683B2 (ja) | 粒子内部に空隙を有する粒子及びその製造方法 | |
WO2021145288A1 (ja) | 酸化物焼結体および酸化物焼結体の製造方法 | |
CN109906202A (zh) | 微粒复合金属氢氧化物、其烧制物、其制造方法及其树脂组合物 | |
KR102288642B1 (ko) | 복합 코팅액, 이를 이용하여 제조된 금속 기판 구조체, 및 그 제조 방법 | |
WO2021100617A1 (ja) | 六方晶窒化ホウ素粉末 | |
JP6028420B2 (ja) | 中空粒子及びその製造方法 | |
JP2021024778A (ja) | 表面3次元ナノ構造粉体、その緻密体及びそれらの製造方法 | |
CN110734292A (zh) | 一种CuO与陶瓷粉体均匀混合的方法 | |
CN110461505A (zh) | 金属粉末的制造方法 | |
TWI538941B (zh) | 填料粒子、樹脂組成物、潤滑脂及塗料組成物 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 19865314 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 2020547971 Country of ref document: JP Kind code of ref document: A |
|
ENP | Entry into the national phase |
Ref document number: 3113924 Country of ref document: CA |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 2019865314 Country of ref document: EP Effective date: 20210428 |