WO2023171181A1 - セラミック焼結体形成用分散体、セラミック焼結体形成用グリーンシート、セラミック焼結体形成用プリプレグ材、およびセラミック焼結体 - Google Patents

セラミック焼結体形成用分散体、セラミック焼結体形成用グリーンシート、セラミック焼結体形成用プリプレグ材、およびセラミック焼結体 Download PDF

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Publication number
WO2023171181A1
WO2023171181A1 PCT/JP2023/003069 JP2023003069W WO2023171181A1 WO 2023171181 A1 WO2023171181 A1 WO 2023171181A1 JP 2023003069 W JP2023003069 W JP 2023003069W WO 2023171181 A1 WO2023171181 A1 WO 2023171181A1
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Prior art keywords
dispersion
component
sintered body
forming
ceramic
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Ceased
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PCT/JP2023/003069
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English (en)
French (fr)
Japanese (ja)
Inventor
雄己 藤本
創万 田口
友昭 中村
直也 三輪
圭史 芦▲高▼
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Fujimi Inc
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Fujimi Inc
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Priority to JP2024505946A priority Critical patent/JPWO2023171181A1/ja
Priority to EP23766361.2A priority patent/EP4491665A4/en
Priority to US18/844,351 priority patent/US20250197301A1/en
Publication of WO2023171181A1 publication Critical patent/WO2023171181A1/ja
Anticipated expiration legal-status Critical
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    • C04B2235/522—Oxidic
    • C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6025—Tape casting, e.g. with a doctor blade
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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    • 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
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    • 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

Definitions

  • the present invention relates to a dispersion for forming a ceramic sintered body, a green sheet for forming a ceramic sintered body, a prepreg material for forming a ceramic sintered body, and a ceramic sintered body.
  • ceramic materials have advantages such as excellent hardness, mechanical strength, heat resistance, impact resistance, abrasion resistance, oxidation resistance or corrosion resistance, or a small coefficient of thermal expansion. There is. For this reason, ceramic materials are expected to be used in various applications such as electronic components and high-temperature structural members. Furthermore, composite materials containing ceramics are being considered for the purpose of further improving functionality and/or improving production efficiency. Examples of the composite material containing ceramic include a composite material of a plurality of ceramics, a composite material of a ceramic and another material, and the like. Such ceramic materials include those formed using ceramic-containing dispersions.
  • a fiber made of an oxide or a composite oxide and a matrix made of an oxide or a composite oxide are combined.
  • An oxide group composite material obtained by oxidation is disclosed.
  • a method for manufacturing the composite material it is disclosed that a fiber sheet is impregnated with a dispersion in which powder of a matrix component is dispersed, and then dried and fired.
  • Japanese Patent Application Publication No. 2008-024585 discloses a mullite-alumina ceramic comprising a ceramic powder mixture having mullite-alumina powder and an alumina precursor solution.
  • a substrate is disclosed.
  • oxide-based ceramic matrix composites obtained by impregnating ceramic fibers with a ceramic powder matrix.
  • JP 2017-222544A discloses a ceramic matrix composite material that includes an aggregate made of mullite fibers and a matrix made of mullite filled between the mullite fibers. Further, as a method for manufacturing a ceramic matrix composite material, a method is disclosed which includes impregnating mullite fibers constituting aggregate with a mullite precursor solution and filling a matrix made of mullite between the mullite fibers. There is.
  • the method for producing a ceramic material involves forming a ceramic sintered body using a dispersion containing ceramic or a dispersion containing a ceramic precursor. It has been found that there is a problem in that some components bleed out during the process, resulting in non-uniformity of the components.
  • the present invention provides a means for suppressing the occurrence of bleed-out of some components during the formation of a ceramic sintered body in a dispersion for forming a ceramic sintered body containing ceramic particles, a resin, and a plasticizer. With the goal.
  • One embodiment of the present invention that can solve the above problems is a dispersion for forming a ceramic sintered body, which contains the following components (A) to (D) and has a pH of 4.0 or more at 25°C: (A) Component: ceramic particles, (B) Component: resin, (C) Component: plasticizer, (D) Component: water, Regarding.
  • One embodiment of the present invention is a dispersion for forming a ceramic sintered body, which contains the following components (A) to (D) and has a pH of 4.0 or more at 25°C: Component (A): ceramic particles, Component (B): resin, Component (C): plasticizer, Component (D): water, Regarding. That is, this embodiment relates to a dispersion for forming a ceramic sintered body, which contains ceramic particles, a resin, a plasticizer, and water, and has a pH of 4.0 or more at 25°C.
  • a means for suppressing the occurrence of bleed-out of some components during the formation of a ceramic sintered body can be provided.
  • the present inventors estimate the mechanism by which the above-mentioned problems are solved by the present invention as follows.
  • the dispersion contains ceramic particles, a resin, and a plasticizer
  • the pH is below a certain level
  • the resin decomposes in the dispersion, resulting in lower molecular weight.
  • an unsintered intermediate material such as a green sheet or prepreg material formed using this dispersion
  • the three-dimensional network of the resin is easily dissolved.
  • the effect of the resin on suppressing the diffusion of other additive components is weakened, and at least the diffusion of the plasticizer becomes more likely to occur, making bleed-out more likely to occur.
  • the dispersion for forming a ceramic sintered body according to one embodiment of the present invention includes ceramic particles, a resin, a plasticizer, and water, and its pH at 25° C. is limited to 4.0 or higher. .
  • decomposition of the resin becomes less likely to occur, and the three-dimensional network of the resin is better maintained, so bleed-out is suppressed.
  • Component (A): Ceramic particles A dispersion for forming a ceramic sintered body according to an embodiment of the present invention contains ceramic particles as the component (A).
  • ceramic particles refer to particles containing ceramic.
  • Component (A) constitutes at least a portion of the ceramic sintered body formed using the dispersion for forming a ceramic sintered body.
  • the content of ceramic based on the total mass of ceramic particles that can be used as component (A) is not particularly limited, but is preferably 50% by mass or more, more preferably 70% by mass or more, and 90% by mass or more. It is more preferable (upper limit: 100% by mass).
  • the ceramic content can be evaluated by weight change by thermogravimetric analysis.
  • the ceramic contained in the ceramic particles that can be used as component (A) is not particularly limited.
  • the ceramic contained in the ceramic particles include compounds consisting only of carbon, oxides, hydroxides, carbides, carbonates, nitrides, halides, phosphates, borides, and the like.
  • the oxide include, but are not limited to, silicon oxide, aluminum oxide (alumina, Al 2 O 3 ), mullite, copper oxide, iron oxide, nickel oxide, tin oxide, cadmium oxide, zinc oxide, zirconium oxide, etc.
  • the hydroxide include, but are not particularly limited to, aluminum hydroxide (Al(OH) 3 ).
  • Examples of the carbide include, but are not limited to, silicon carbide (SiC), boron carbide, and the like.
  • Examples of the nitride include, but are not limited to, silicon nitride, gallium nitride, titanium nitride, lithium nitride, and the like.
  • examples of the ceramic included in the ceramic particles include oxides or composite oxides of Si, Ti, Zr, Mg, Hf, Al, and rare earth elements described in International Publication No. 2012/077787. The ceramic particles may contain one of these ceramics, or may contain two or more of them in combination.
  • component (A) includes ceramic particles containing at least one selected from the group consisting of oxides, carbides, nitrides, and borides.
  • the content ratio of ceramic particles containing at least one selected from the group consisting of oxides, carbides, nitrides, and borides to the total mass of component (A) is preferably 50% by mass or more. , more preferably 90% by mass or more (upper limit: 100% by mass). It is more preferable that the ceramic particles as component (A) are ceramic particles containing at least one selected from the group consisting of oxides, carbides, nitrides, and borides.
  • component (A) includes ceramic particles containing at least one selected from the group consisting of oxides and carbides.
  • the content ratio of ceramic particles containing at least one selected from the group consisting of oxides and carbides to the total mass of component (A) is 50% by mass or more based on the total mass of component (A).
  • the content is preferably 90% by mass or more (upper limit: 100% by mass).
  • the ceramic particles serving as component (A) are ceramic particles containing at least one selected from the group consisting of oxides and carbides.
  • the ceramic particles containing carbide include ceramic particles containing silicon carbide.
  • the content ratio of ceramic particles containing silicon carbide to the total mass of ceramic particles containing carbide is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit 100% by mass).
  • the carbide-containing ceramic particles in component (A) are more preferably silicon carbide-containing ceramic particles.
  • the ceramic particles containing an oxide include ceramic particles containing at least one selected from the group consisting of alumina and mullite.
  • the content ratio of ceramic particles containing at least one selected from the group consisting of alumina and mullite to the total mass of ceramic particles containing oxides is preferably 50% by mass or more, and preferably 90% by mass or more. It is more preferable that it exists (upper limit: 100% by mass).
  • the oxide-containing ceramic particles in component (A) are ceramic particles containing at least one selected from the group consisting of alumina and mullite.
  • the ceramic particles that can be used as component (A) may be uncoated particles, particles coated with a coating layer (coated particles), or a combination thereof.
  • covered means that at least a portion of the particle is covered with a coating layer.
  • the coating layer is not particularly limited, but a coating layer containing aluminum hydroxide is preferred.
  • the coating method is not particularly limited, and any known method may be used. Silicon carbide particles coated with a coating layer containing aluminum hydroxide are not particularly limited, but can be manufactured by appropriately adopting known methods and conditions described in International Publication No. 2019/065956, etc. can.
  • composition and structure of the coated particles can be determined by, for example, SEM (Scanning Electron Microscope)-EDX (Energy Dispersive X-ray Spectroscopy) observation, TEM (Transmission Electron Microscope) tron Microscope)-EDX (Energy Dispersive X-ray Spectroscopy) observation, EELS ( Analysis can be performed by combining multiple measurements as necessary, such as by Electron Energy Loss Spectroscopy analysis.
  • the ceramic particles that can be used as component (A) may be surface-treated.
  • the type, method, etc. of surface treatment are not particularly limited, and known types, methods, etc. of surface treatment can be appropriately employed.
  • component (A) include oxide particles, carbide particles, oxide particles covered with a coating layer, carbide particles covered with a coating layer, and the like. Specific examples include, but are not limited to, silicon oxide particles, mullite particles, alumina particles, copper oxide particles, iron oxide particles, nickel oxide particles, tin oxide particles, cadmium oxide particles, zinc oxide particles, zirconium oxide particles, Examples include silicon carbide particles, boron carbide particles, and particles thereof coated with a coating layer. Among these, mullite particles, alumina particles, silicon carbide particles, and silicon carbide particles coated with a coating layer containing aluminum hydroxide (aluminum hydroxide-coated SiC particles) are more preferable.
  • silicon carbide particles coated with a coating layer containing alumina particles, silicon carbide particles, and aluminum hydroxide are more preferable.
  • alumina particles are particularly preferred.
  • aluminum hydroxide-coated SiC particles are particularly preferred.
  • the shape of the ceramic particles that can be used as component (A) is not particularly limited, and may be spherical or non-spherical.
  • specific examples of non-spherical shapes include polygonal prisms such as triangular prisms and square prisms, cylindrical shapes, bale-like shapes where the center of the cylinder bulges out more than the ends, donut-like shapes where the center of a disk penetrates through, plate-like shapes, The so-called cocoon-shaped shape with a constriction in the center, the so-called associative spherical shape where multiple particles are integrated, the bead-shaped shape where multiple particles are connected in almost a line, the so-called confetti-shaped shape with multiple protrusions on the surface, and rugby.
  • Various shapes can be mentioned, such as a ball shape, a needle shape that is thinner than a rugby ball shape, and the shape is not particularly limited.
  • the average primary particle diameter of the ceramic particles that can be used as component (A) is not particularly limited, but is preferably 0.001 ⁇ m or more, more preferably 0.005 ⁇ m or more, and 0.01 ⁇ m or more. is even more preferable. Within these ranges, agglomeration of ceramic particles is further suppressed, and a dispersion with higher dispersibility can be obtained.
  • the average primary particle diameter of the ceramic particles that can be used as component (A) is not particularly limited, but is preferably 2.0 ⁇ m or less, more preferably 1.5 ⁇ m or less, and 1.0 ⁇ m or less. is more preferable, and particularly preferably 0.5 ⁇ m or less.
  • the average primary particle diameter of the ceramic particles is determined based on the average value of the specific surface area (SA) of the ceramic particles calculated from the values measured three times in a row using the BET method, using the value of the true density of the ceramic particles, and determining the shape of the ceramic particles. It can be calculated assuming that is a true sphere.
  • SA specific surface area
  • the specific surface area of the ceramic particles can be measured using, for example, Flow Sorb II 2300 manufactured by Micromeritex.
  • examples of the average primary particle size range of ceramic particles that can be used as component (A) are 0.001 ⁇ m or more and 2.0 ⁇ m or less, 0.005 ⁇ m or more and 1.5 ⁇ m or less, and 0.01 ⁇ m or more and 1.5 ⁇ m or less. Examples include, but are not limited to, .0 ⁇ m or less, 0.01 ⁇ m or more and 0.5 ⁇ m or less. Therefore, in a preferred embodiment of the present invention, component (A) is a ceramic particle having an average primary particle size within the above range.
  • the average secondary particle diameter of the ceramic particles that can be used as component (A) is not particularly limited, but is preferably 0.01 ⁇ m or more, more preferably 0.03 ⁇ m or more, and 0.05 ⁇ m or more. It is even more preferable that the thickness be 0.1 ⁇ m or more. Within these ranges, the possibility of excessive thickening of the dispersion is further reduced, and a dispersion more suitable for coating or impregnation can be obtained.
  • the average secondary particle diameter of the ceramic particles that can be used as component (A) is not particularly limited, but is preferably 3 ⁇ m or less, more preferably 2 ⁇ m or less, and even more preferably 1.5 ⁇ m or less. , 1 ⁇ m or less is particularly preferable.
  • component (A) is a ceramic particle having an average secondary particle diameter within the above range.
  • Component (A) may be a commercially available product or a synthetic product.
  • the pre-coated particles that are the raw material for the coated particles may also be commercially available products or synthetic products.
  • Commercially available products include, but are not particularly limited to, product names such as WA#30000 and GC#40000 manufactured by Fujimi Incorporated.
  • one type of ceramic particles may be used alone, or two or more types of ceramic particles may be used in combination.
  • the content of component (A) in the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 0.1% by mass or more based on the total mass of the dispersion for forming a ceramic sintered body. , more preferably 1% by mass or more, and still more preferably 10% by mass or more. Within this range, the amount of other components removed during drying, degreasing, etc. will be smaller, resulting in a dispersion that is more excellent in terms of manufacturing cost.
  • the content of component (A) in the dispersion for forming a ceramic sintered body is not particularly limited, but it is preferably 90% by mass or less, and 80% by mass or less based on the total mass of the dispersion for forming a ceramic sintered body.
  • an example of the range of the content of component (A) in the dispersion for forming a ceramic sintered body is 0.1% by mass or more based on the total mass of the dispersion for forming a ceramic sintered body. Examples include, but are not limited to, 90% by mass or less, 1% by mass or more and 80% by mass or less, 10% by mass or more and 75% by mass or less.
  • the dispersion for forming a ceramic sintered body may contain particles containing boron nitride (BN), but may not substantially contain particles containing BN, or may contain no particles containing BN at all.
  • substantially not containing particles containing BN means that the content of particles containing BN in the dispersion for forming a ceramic sintered body is such that the total mass of the dispersion for forming a ceramic sintered body is It represents less than 0.1% by mass.
  • the dispersion for forming a ceramic sintered body may contain particles containing silicon carbide (SiC), but may not substantially contain particles containing SiC, or may not contain particles containing SiC at all.
  • substantially not containing particles containing SiC means that the content of particles containing SiC in the dispersion for forming a ceramic sintered body is such that the total mass of the dispersion for forming a ceramic sintered body is It represents less than 0.1% by mass.
  • the dispersion for forming a ceramic sintered body may contain aluminum hydroxide-coated SiC particles, but it may not contain substantially aluminum hydroxide-coated SiC particles, or it may not contain aluminum hydroxide-coated SiC particles at all. good.
  • substantially not containing aluminum hydroxide-coated SiC particles means that the content of aluminum hydroxide-coated SiC particles in the dispersion for forming a ceramic sintered body is It represents less than 0.1% by mass based on the total mass of the body.
  • the dispersion for forming a ceramic sintered body according to one embodiment of the present invention contains a resin as the component (B).
  • Component (B) constitutes a binder (binder resin) of a green sheet formed using the dispersion for forming a ceramic sintered body, and can improve the formability of the green sheet.
  • the component (B) constitutes a part of the prepreg material formed using the dispersion for forming a ceramic sintered body, and can improve the handling properties of the prepreg material.
  • Component (B) is not particularly limited, and known resins can be used. Among these, resins with hydroxyl groups (hereinafter also referred to as component (B1)) are used from the viewpoint of being able to obtain excellent dispersibility and high stability over time under conditions where the pH at 25°C is 4.0 or higher. ) is preferred.
  • Components include polyvinyl alcohol (PVA); modified polyvinyl alcohol (modified PVA) such as polyvinyl butyral (PVB), polyvinyl propyral, polyvinyl acetal, and polyvinyl formal; hydroxyl group-containing glyoxal resin; hydroxyl group-containing acrylic resin; phenol resin Preferred examples include, but are not limited to, hydroxyl group-containing polyvinylpyrrolidone (PVP); hydroxyl group-containing polyester; hydroxyl group-containing silicone; hydroxyl group-containing polycarboxylic acid.
  • PVA polyvinyl alcohol
  • modified PVA such as polyvinyl butyral (PVB), polyvinyl propyral, polyvinyl acetal, and polyvinyl formal
  • hydroxyl group-containing glyoxal resin hydroxyl group-containing acrylic resin
  • phenol resin Preferred examples include, but are not limited to, hydroxyl group-containing polyvinylpyrrolidone (PVP);
  • polyvinyl alcohol and modified polyvinyl alcohol are more preferred, polyvinyl alcohol, polyvinyl butyral, and polyvinyl acetal are even more preferred, and polyvinyl acetal is particularly preferred.
  • component (B) includes component (B1): a resin having a hydroxyl group.
  • the content ratio of component (B1) to the total mass of component (B) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit: 100% by mass).
  • the resin that is component (B) is more preferably component (B1).
  • component (B1) resin having a hydroxyl group is polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polyvinyl propyral, polyvinyl acetal, polyvinyl formal, hydroxyl group-containing glyoxal resin, hydroxyl group-containing resin.
  • the content ratio of component (B2) to the total mass of component (B1) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit: 100% by mass).
  • Component (B1) in component (B) The resin having a hydroxyl group is more preferably component (B2).
  • the resin that is the component (B) is particularly preferably the component (B2).
  • the weight average molecular weight of the resin that can be used as component (B) is not particularly limited, but is preferably 1,000 or more, more preferably 2,000 or more, and even more preferably 5,000 or more. preferable. Within these ranges, a dispersion with better moldability for green sheets, prepreg materials, etc. can be obtained.
  • the weight average molecular weight of the resin that can be used as component (B) is not particularly limited, but is preferably 500,000 or less, more preferably 100,000 or less, and even more preferably 50,000 or less. preferable. Within these ranges, the possibility of excessive thickening of the dispersion is further reduced, and a dispersion more suitable for coating or impregnation can be obtained.
  • the value of the weight average molecular weight of the resin can be measured by gel permeation chromatography (GPC), and specifically, it can be measured by the method described in Examples. Based on these, examples of the weight average molecular weight range of the resin that can be used as component (B) are 1,000 to 500,000, 2,000 to 100,000, and 5,000 to 50,000. Examples include, but are not limited to, the following. Therefore, in a preferred embodiment of the present invention, component (B) is a resin having a weight average molecular weight within the above range.
  • Component (B) may be a commercially available product or a synthetic product.
  • Commercially available products are not particularly limited, but include, for example, S-LEC (registered trademark) KW-3 manufactured by Sekisui Chemical Co., Ltd.
  • one type of resin may be used alone, or two or more types of resin may be used in combination.
  • the content of component (B) in the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 0.01% by mass or more based on the total mass of the dispersion for forming a ceramic sintered body. , more preferably 0.1% by mass or more, and still more preferably 1% by mass or more. Within this range, a dispersion with excellent green sheet formability can be obtained.
  • the content of component (B) in the dispersion for forming a ceramic sintered body is not particularly limited, but it is preferably 50% by mass or less, and 30% by mass or less based on the total mass of the dispersion for forming a ceramic sintered body. It is more preferably at most 20% by mass, even more preferably at most 20% by mass.
  • an example of the range of the content of component (B) in the dispersion for forming a ceramic sintered body is 0.01% by mass or more based on the total mass of the dispersion for forming a ceramic sintered body. 50% by mass or less, 0.1% by mass or more and 30% by mass or less, 1% by mass Examples include, but are not limited to, 20% by mass or less.
  • the content ratio of component (A) and component (B) described below is not particularly limited.
  • the content of component (B) is preferably 0.1 part by mass or more, more preferably 1 part by mass or more, and 2.5 parts by mass or more based on 100 parts by mass of component (A). It is more preferable that the amount is 5 parts by mass or more, and particularly preferably 5 parts by mass or more. Within this range, a dispersion with excellent moldability for green sheets, prepreg materials, etc. can be obtained.
  • the content of component (B) is preferably 1,000 parts by mass or less, more preferably 100 parts by mass or less, and 50 parts by mass or less based on 100 parts by mass of component (A). is even more preferable.
  • component (B) is 0.1 part by mass or more and 1,000 parts by mass or less, 1 part by mass or more and 100 parts by mass or less, 2.5 parts by mass or more, per 100 parts by mass of component (A). Examples include, but are not limited to, 5 parts by mass or more and 50 parts by mass or less, and 5 parts by mass or more and 50 parts by mass or less.
  • Component (C) Plasticizer
  • the dispersion for forming a ceramic sintered body according to one embodiment of the present invention contains a plasticizer as the component (C).
  • Component (C) constitutes a part of the green sheet, prepreg material, etc. formed using the dispersion for forming a ceramic sintered body, and can improve the flexibility of the green sheet, prepreg material, etc.
  • a plasticizer refers to a compound that has the function of increasing the flexibility of an unsintered intermediate material such as a green sheet or prepreg material formed using a dispersion for forming a ceramic sintered body.
  • the compound be a compound that can be made difficult to cause destruction.
  • the bending angle is not particularly limited as long as the difference in flexibility can be confirmed.
  • a plasticizer it is used as a plasticizer in cases where a green sheet that does not contain the compound used as a plasticizer breaks when the green sheet is bent at an angle of 170° or more (for example, 170°). It is particularly preferred that the green sheet containing the compound can be prevented from breaking.
  • the bending position can be performed, for example, by bending the center position of the long side of the green sheet, but is not limited to this position.
  • the green sheet used for folding may be, for example, a green sheet with a long side of 5 cm x a short side of 1.5 cm x a thickness of 150 ⁇ m, but is not limited to this size.
  • Component (C) is not particularly limited, and any known plasticizer can be used. Among these, from the viewpoint of the dispersibility of the plasticizer in the dispersion, component (C) includes water-soluble plasticizers such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerin, triethanolamine, and phthalate. Preferred examples include, but are not limited to, plasticizers that are insoluble in water and transfer to emulsions, such as phthalate ester plasticizers such as dibutyl acid.
  • water-soluble plasticizers such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerin, triethanolamine, and phthalate.
  • plasticizers that are insoluble in water and transfer to emulsions such as phthalate ester plasticizers such as dibutyl acid.
  • a water-soluble plasticizer is more preferable, a water-soluble plasticizer that is a multimer is even more preferable, diethylene glycol, triethylene glycol, and polyethylene glycol are even more preferable, and polyethylene glycol is particularly preferable.
  • Diethylene glycol, triethylene glycol, and polyethylene glycol are multimers of two, three, and four or more ethylene glycols, respectively.
  • component (C) is at least one compound selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerin, triethanolamine, and dibutyl phthalate (hereinafter referred to as , (also referred to as component (C1)).
  • the content ratio of component (C1) to the total mass of component (C) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit 100% by mass).
  • the plasticizer that is component (C) is more preferably component (C1).
  • component (C) contains a water-soluble plasticizer that is a multimer.
  • the content ratio of the multimeric water-soluble plasticizer to the total mass of component (C) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit: 100% by mass).
  • the plasticizer as component (C) is more preferably a multimeric water-soluble plasticizer.
  • component (C) contains at least one compound selected from the group consisting of diethylene glycol, triethylene glycol, and polyethylene glycol.
  • the content of at least one compound selected from the group consisting of diethylene glycol, triethylene glycol, and polyethylene glycol relative to the total mass of component (C) is preferably 50% by mass or more, and preferably 90% by mass or more. More preferably (upper limit: 100% by mass).
  • the plasticizer as component (C) is at least one compound selected from the group consisting of diethylene glycol, triethylene glycol, and polyethylene glycol.
  • the molecular weight of the plasticizer that can be used as component (C) is not particularly limited, but is preferably smaller than the molecular weight of the resin.
  • the total atomic weight of the plasticizers is preferably less than 1,000.
  • the average molecular weight calculated from the hydroxyl value measurement results of the plasticizer by neutralization titration is preferably less than 1,000.
  • the average molecular weight calculated from the hydroxyl value measurement results of the plasticizer by neutralization titration can be calculated based on JIS K 0070:1992. Within these ranges, the effect of the plasticizer is further improved.
  • the (B) component: resin is a resin having a weight average molecular weight of 1,000 or more
  • the (C) component: plasticizer is calculated from the results of hydroxyl value measurement by neutralization titration method. It is preferable that the plasticizer has an average molecular weight of less than 1,000.
  • the plasticizer that can be used as component (C) may be a commercially available product or a synthetic product.
  • Commercially available products include, but are not particularly limited to, polyethylene glycol 200 manufactured by Fuji Film Wako Pure Chemical Industries, Ltd., for example.
  • one type of plasticizer may be used alone, or two or more types of plasticizers may be used in combination.
  • the content of component (C) in the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 0.01% by mass or more based on the total mass of the dispersion for forming a ceramic sintered body. , more preferably 0.1% by mass or more, and still more preferably 1% by mass or more. Within this range, green sheets, prepreg materials, etc. have excellent flexibility.
  • the content of component (C) in the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 50% by mass or less, based on the total mass of the dispersion for forming a ceramic sintered body, and is preferably 25% by mass or less. It is more preferably at most 10% by mass, even more preferably at most 10% by mass.
  • the content of component (C) in the dispersion for forming a ceramic sintered body is 0.01% by mass or more and 50% by mass or less, based on the total mass of the dispersion for forming a ceramic sintered body, Examples include, but are not limited to, 0.1% by mass to 25% by mass, 1% by mass to 10% by mass, and the like.
  • the content ratio of component (C) and component (A) is not particularly limited.
  • the content of component (C) is preferably 0.1 part by mass or more, more preferably 1 part by mass or more, and 2.5 parts by mass or more based on 100 parts by mass of component (A). It is even more preferable that there be. Within this range, green sheets, prepreg materials, etc. have excellent flexibility.
  • the content of component (C) is preferably 1,000 parts by mass or less, more preferably 100 parts by mass or less, and 50 parts by mass or less based on 100 parts by mass of component (A). is even more preferable. Within this range, the amount of plasticizer component removed during degreasing becomes smaller, resulting in a dispersion that is more excellent in terms of manufacturing cost.
  • component (C) is 0.1 parts by mass or more and 1,000 parts by mass or less, 1 part by mass or more and 100 parts by mass or less, and 2.5 parts by mass or more, per 100 parts by mass of component (A).
  • Examples include, but are not limited to, 50 parts by mass or more and 50 parts by mass or less.
  • the dispersion for forming a ceramic sintered body according to an embodiment of the present invention contains water as the component (D).
  • Component (D) is preferably water containing as few impurities as possible. For example, water with a total content of transition metal ions of 100 ppb or less is preferred.
  • the purity of water that can be used as component (D) can be increased by, for example, removing impurity ions using an ion exchange resin, removing foreign substances using a filter, distilling, or the like.
  • component (D) it is preferable to use, for example, deionized water (ion-exchanged water), pure water, ultrapure water, distilled water, or the like.
  • Component (E) acid
  • the dispersion for forming a ceramic sintered body according to one embodiment of the present invention may further contain an acid as the component (E).
  • Component (E) is preferably used as a pH adjuster, and component (E) can further lower the pH of the dispersion.
  • Component (E) is not particularly limited, and any known acid can be used.
  • Component (E) includes organic acids and inorganic acids.
  • the acid is a non-multimeric acid.
  • the non-multimeric acid is a compound having a total atomic weight of less than 1,000.
  • organic acids include, but are not limited to, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, and 4-methylpentane.
  • Acid n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, Pimelic acid, maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, methoxy
  • carboxylic acids such as acetic acid, methoxyphenylacetic acid, and phenoxyacetic acid
  • organic sulfuric acids such as methanesulfonic acid, ethanesulfonic acid, and isethionic acid; and the like.
  • inorganic acids include, but are not limited to, carbonic acid, hydrochloric acid, nitric acid, phosphoric acid, hypophosphorous acid, phosphorous acid, phosphonic acid, sulfuric acid, boric acid, hydrofluoric acid, orthophosphoric acid, pyrophosphoric acid, and polyphosphoric acid.
  • examples include acids, metaphosphoric acid, hexametaphosphoric acid, and the like.
  • inorganic acids are preferred, nitric acid, sulfuric acid, and hydrochloric acid are more preferred, nitric acid and hydrochloric acid are even more preferred, and hydrochloric acid is particularly preferred.
  • the acid that can be used as component (E) includes an inorganic acid.
  • the content ratio of the inorganic acid to the total mass of component (E) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit: 100% by mass). It is more preferable that the acid as component (E) is an inorganic acid.
  • component (E) includes carbonic acid, hydrochloric acid, nitric acid, phosphoric acid, hypophosphorous acid, phosphorous acid, phosphonic acid, sulfuric acid, boric acid, hydrofluoric acid, orthophosphoric acid, It contains at least one acid (hereinafter also referred to as component (E1)) selected from the group consisting of pyrophosphoric acid, polyphosphoric acid, metaphosphoric acid, and hexametaphosphoric acid.
  • the content ratio of component (E1) to the total mass of component (E) is preferably 50% by mass or more, more preferably 90% by mass or more (upper limit: 100% by mass).
  • the acid that is component (E) is more preferably component (E1).
  • component (E) a commercially available product or a synthetic product may be used.
  • one type of acid may be used alone, or two or more types of acids may be used in combination.
  • the content of component (E) in the dispersion for forming a ceramic sintered body is not particularly limited, but the pH at 25°C of the dispersion for forming a ceramic sintered body is within the preferred pH range at 25°C described below. It is preferable that the amount is within the range.
  • the dispersion for forming a ceramic sintered body according to one embodiment of the present invention may further contain a thickener as the component (F).
  • the viscosity of the dispersion for forming a ceramic sintered body can be adjusted by the component (F).
  • the thickener refers to a compound that has the function of increasing the viscosity of the dispersion for forming a ceramic sintered body.
  • the thickener is preferably a compound that can increase the viscosity at 25° C. to 1 Pa ⁇ s or more in a thickening effect test. Further, in the thickening effect test, it is more preferable that the compound is capable of increasing the viscosity at 25°C to 5 Pa ⁇ s or more, and the compound is capable of increasing the viscosity at 25°C to 10 Pa ⁇ s or more. is even more preferable.
  • Component (F) preferably contains the compounds listed above. It is preferable that the compound serving as the component (B) and the compound serving as the component (C) each have a viscosity of less than 1 Pa ⁇ s at 25°C in a thickening effect test. However, the compound serving as component (B) and the compound serving as component (C) are not limited to such compounds.
  • the thickening effect test is performed as follows. First, an aqueous dispersion (alumina particles and water 100 g of this aqueous dispersion with an alumina particle concentration of 25% by mass is added to 5 g of an aqueous hydrochloric acid solution with a concentration of 2.5% by mass with stirring. Next, the compound to be tested is added to the obtained aqueous dispersion (aqueous dispersion containing alumina particles and hydrochloric acid) in an amount of 4 parts by mass or less based on 100 parts by mass of alumina particles. Then, the viscosity at 25° C. of the aqueous dispersion of alumina particles after adding the compound to be tested is measured.
  • Component (F) is particularly preferably used in a dispersion for forming a ceramic sintered body used for forming a green sheet, since it can further improve the formability of the green sheet.
  • the uses of the dispersion for forming a ceramic sintered body containing the component (F) are not limited to these.
  • Component (F) is not particularly limited, and any known thickener can be used.
  • the thickener that can be used as component (F) may be an ionic thickener or a nonionic thickener.
  • the ionic thickener may be an anionic thickener or a cationic thickener.
  • the thickener is preferably an ionic thickener, more preferably a cationic thickener, and a cationic thickener containing a polymer having a (meth)acryloyl group.
  • a W/O emulsion containing a poly(meth)acrylic acid ester-based cationic polymer for example, a cationic polymer containing a (meth)acrylic acid ester structural unit.
  • a W/O emulsion containing an acid ester-based cationic polymer for example, a cationic polymer containing a methacrylic acid ester structural unit
  • Component (F) preferably contains a thickener such as those listed above.
  • the (meth)acryloyl group represents a general term for an acryloyl group and a methacryloyl group.
  • (Meth)acrylic ester is a general term for acrylic ester and methacrylic ester.
  • component (F) a commercially available product or a synthetic product may be used.
  • Commercially available products include, but are not particularly limited to, Senka Actogel AP200, Senka Actogel NS100, Senka Actogel CM100, and Senka Actogel CD100 manufactured by Senka Co., Ltd., for example.
  • one type of thickener may be used alone, or two or more types of thickeners may be used in combination.
  • the content of component (F) in the dispersion for forming a ceramic sintered body is not particularly limited, but the viscosity of the dispersion for forming a ceramic sintered body at 25°C is within the range of the viscosity at 25°C described below. It is preferable that the amount is as follows.
  • the dispersion for forming a ceramic sintered body further includes component (E): an acid, and component (F): a thickener.
  • the dispersion for forming a ceramic sintered body according to an embodiment of the present invention may further contain components other than the above-mentioned components (A) to (F) as the component (G), as long as the effects of the present invention are not impaired. good.
  • Component (G) is not particularly limited, but includes, for example, bases (basic compounds, alkalis), salts, chelating agents, antifoaming agents, organic solvents, and the like.
  • component (G) is not particularly limited as long as the effects of the present invention can be obtained, but it is preferably less than 10% by mass based on the total mass of the dispersion for forming a ceramic sintered body, It is more preferably less than 5% by mass, and even more preferably 0% by mass.
  • the pH of the dispersion for forming a ceramic sintered body according to one embodiment of the present invention at 25° C. is 4.0 or more. If the pH at 25° C. is less than 4.0, some components may bleed out during the formation of the ceramic sintered body, resulting in non-uniformity of the components.
  • the pH of the dispersion for forming a ceramic sintered body at 25° C. is more preferably over 4.0, and even more preferably 4.1 or higher. Within these ranges, it is possible to further suppress the occurrence of bleed-out of some components during the formation of the ceramic sintered body.
  • the pH of the dispersion for forming a ceramic sintered body at 25° C. can be measured using a pH meter, and specifically, can be measured by the method described in Examples.
  • the pH of the dispersion for forming a ceramic sintered body at 25°C is 4.0 or more and 12.0 or less, 4.0 or more and 7.0 or less, 4.0 or more and 6.0 or less, and 4. Examples include, but are not limited to, 1 or more and 5.5 or less.
  • the viscosity at 25°C of the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 0.01 Pa ⁇ s or more, more preferably 0.05 Pa ⁇ s or more, and 0.1 Pa ⁇ s. It is more preferable that it is s or more. Within these ranges, the formability of the green sheet formed using the dispersion for forming a ceramic sintered body can be further improved.
  • the viscosity at 25°C of the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 100 Pa ⁇ s or less, more preferably 50 Pa ⁇ s or less, and preferably 30 Pa ⁇ s or less. More preferred.
  • the coating properties of the ceramic sintered body-forming dispersion are improved, and the ceramic fibers can be more easily impregnated with the ceramic sintered body-forming dispersion.
  • the viscosity at 25° C. of the dispersion for forming a ceramic sintered body can be measured using a B-type viscometer, and specifically, can be measured by the method described in Examples. Examples of the range of the viscosity at 25°C of the dispersion for forming a ceramic sintered body are 0.01 Pa.s or more and 100 Pa.s or less, 0.05 Pa.s or more and 50 Pa.s or less, and 0.1 Pa.s or more and 30 Pa. Examples include, but are not limited to, s or less.
  • the viscosity at 25° C. of the dispersion for forming a ceramic sintered body may be, for example, 15 Pa ⁇ s or more and 25 Pa ⁇ s or less, or 20 Pa ⁇ s or more and 25 Pa ⁇ s or less.
  • a method for producing a dispersion for forming a ceramic sintered body is to mix component (A): ceramic particles, component (B): resin, component (C): plasticizer, and component (D): water. including.
  • Another embodiment of the present invention includes mixing (A) component: ceramic particles, (B) component: resin, (C) component: plasticizer, and (D) component: water. It can also be said that this is a method for producing a dispersion having a pH of 4.0 or higher at °C.
  • the method for producing a dispersion for forming a ceramic sintered body further includes mixing other components (for example, the above-mentioned (E) component, (F) component, and (G) component) as necessary. You can stay there.
  • Component (A) is preferably added as a dispersion containing component (A) and component (D).
  • Component (B) is preferably added as a dispersion or solution containing component (B) and component (D).
  • the method for producing a dispersion for forming a ceramic sintered body includes a dispersion containing the (A) component and the (D) component, and a dispersion or solution containing the (B) component and the (D) component. It is preferable to include mixing the component (C) with at least one selected from the group consisting of component (C), a solution containing this, and a dispersion containing this.
  • a preferred embodiment of the present invention includes a dispersion containing component (A) and component (D), a dispersion or solution containing component (B) and component (D), and component (C) or It can also be said that it is a method for producing a dispersion having a pH of 4.0 or more at 25° C., which includes mixing the solution or the dispersion (the dispersion).
  • the content (concentration) of component (A) in the dispersion is not particularly limited; It is preferably at least 20% by mass, more preferably at least 20% by mass, even more preferably at least 40% by mass.
  • the content (concentration) of component (A) in the dispersion is not particularly limited, but is 90% of the total mass of the dispersion. It is preferably at most 85% by mass, even more preferably at most 80% by mass, particularly preferably at most 75% by mass.
  • examples include 5% by mass or more and 90% by mass or less, 20% by mass or more and 85% by mass or less, 40% by mass or more and 80% by mass or less, 40% by mass or more and 75% by mass or less. However, it is not limited to these.
  • the content (concentration) of component (B) in the dispersion or solution is not particularly limited; It is preferably 1% by mass or more, more preferably 5% by mass or more, and even more preferably 10% by mass or more, based on the total mass of.
  • the content (concentration) of component (B) in the dispersion or solution is not particularly limited, but the total amount of the dispersion or solution is It is preferably 60% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less.
  • examples of the content (concentration) range of component (B) in a dispersion or solution containing component (B) and component (D) include component (B) and component (D).
  • examples include, but are not limited to, 1% by mass to 60% by mass, 5% by mass to 40% by mass, 10% by mass to 30% by mass, etc., based on the total mass of the dispersion or solution containing the components. Not done.
  • the dispersion containing the component (A) and the component (D), and the dispersion or solution containing the component (B) and the component (D) may be prepared by adding other components (for example, the above-mentioned (E) component, (F) component, (G) component).
  • the dispersion containing component (A) and component (D) further contains component (E): an acid.
  • Component (E) is preferably added as a solution (aqueous acid solution) containing component (E) and component (D) to a dispersion containing component (A) and component (D). .
  • the content (concentration) of component (E) in the acid aqueous solution is not particularly limited.
  • the content of component (E) in the acid aqueous solution is preferably 0.00001% by mass or more, more preferably 0.00005% by mass or more, and 0.0001% by mass or more, based on the total mass of the acid aqueous solution. More preferably, it is at least % by mass.
  • the content of component (E) in the acid aqueous solution is preferably 10% by mass or less, more preferably 5% by mass or less, and 2.5% by mass or less based on the total mass of the acid aqueous solution. It is even more preferable that there be.
  • examples of the range of the content of component (E) in the acid aqueous solution are 0.00001% by mass or more and 10% by mass or less, 0.00005% by mass or more and 5% by mass or less, based on the total mass of the acid aqueous solution.
  • examples include, but are not limited to, 0.0001% by mass and 2.5% by mass, and the like.
  • the content (concentration) of component (E) in the acid aqueous solution is not particularly limited, but it is preferably an amount such that the resulting dispersion for forming a ceramic sintered body has a pH of 4.0 or more at 25°C. Further, it is more preferable that the amount is such that the pH of the obtained dispersion for forming a ceramic sintered body at 25° C. falls within the above-mentioned preferable range.
  • the means for mixing each component in the production of the dispersion for forming a ceramic sintered body there are no particular restrictions on the means for mixing each component in the production of the dispersion for forming a ceramic sintered body.
  • the mixing means include known kneading and stirring machines such as an autorotation mixer (rotation/revolution mixer) and a planetary mixer.
  • an autorotation mixer rotating/revolution mixer
  • a planetary mixer As a commercially available product, for example, Awatori Rentaro ARE-310 manufactured by Thinky Co., Ltd. can be used.
  • the conditions for mixing each component in the production of the dispersion for forming a ceramic sintered body are not particularly limited.
  • the mixing temperature is not particularly limited, and may be, for example, 10° C. or higher and 40° C. or lower, but heating may be used to increase the mixing speed.
  • the mixing time is not particularly limited, but preferably 10 seconds or more and 60 minutes or less, more preferably 30 seconds or more and 10 minutes or less. From the viewpoint of suppressing bubble generation during mixing, mixing may be performed under vacuum.
  • Green sheet for forming ceramic sintered bodies Another aspect of the present invention relates to a green sheet for forming a ceramic sintered body (hereinafter also simply referred to as a "green sheet") formed from the above dispersion for forming a ceramic sintered body. That is, the green sheet according to this embodiment is characterized in that it is formed from the above-mentioned dispersion for forming a ceramic sintered body having a pH of 4.0 or more at 25°C.
  • the above-mentioned dispersion for forming a ceramic sintered body has a pH at 25°C of 4.0 or more (preferably in the above-mentioned preferred pH range at 25°C).
  • examples include a green sheet formed from a body and containing (A) component: ceramic particles, (B) component: resin, and (C) component: plasticizer.
  • the green sheet according to a more preferred embodiment of the present invention has a pH at 25°C of 4.0 or more (preferably in the above-mentioned preferred pH range at 25°C), and has a pH at 25°C as described above.
  • Examples include a green sheet formed from a dispersion for forming a ceramic sintered body having a viscosity within a range, and containing (A) component: ceramic particles, (B) component: resin, and (C) component: plasticizer. .
  • the green sheet may further contain other components (for example, the above-mentioned (E) component, (F) component, and (G) component) as necessary.
  • (A) component, (B) component, (C) component, and other components are for forming the above-mentioned ceramic sintered body. As per the dispersion.
  • the content ratio of component (A) to component (B) in the green sheet and the content ratio of component (A) to component (C) in the green sheet are not particularly limited, but are preferable.
  • the ranges are the same as those described above for the dispersion for forming a ceramic sintered body.
  • the film thickness (dry film thickness) of the green sheet is not particularly limited, but is preferably 1 ⁇ m or more and 500 ⁇ m or less, more preferably 10 ⁇ m or more and 450 ⁇ m or less, and even more preferably 20 ⁇ m or more and 300 ⁇ m or less.
  • the method for producing the green sheet is not particularly limited, and any known method can be used. Among these, the coating method is preferred.
  • a method including a step of applying the above dispersion for forming a ceramic sintered body preferably a step of applying the above dispersion for forming a ceramic sintered body to a base material
  • a step of obtaining a dispersion for forming a ceramic sintered body by a dispersion manufacturing method preferably, a step of applying the obtained dispersion for forming a ceramic sintered body.
  • Examples include a method including a step of coating the base material.
  • the coating method is not limited, and any known method can be used. Examples include an applicator coating method, a bar coating method, a die coater method, a comma coating method, a gravure roll coater method, a blade coater method, a spray coater method, an air knife coating method, a dip coating method, a transfer method, and the like.
  • the coating film thickness (wet film thickness) of the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 10 ⁇ m or more, more preferably 50 ⁇ m or more, and even more preferably 100 ⁇ m or more.
  • the coating film thickness (wet film thickness) of the dispersion for forming a ceramic sintered body is not particularly limited, but is preferably 2000 ⁇ m or less, more preferably 1800 ⁇ m or less, and even more preferably 1500 ⁇ m or less. Within these ranges, a dispersion that requires less load in the drying process and can be manufactured at low cost can be obtained.
  • examples of the range of the coating film thickness (wet film thickness) of the dispersion for forming a ceramic sintered body include 10 ⁇ m or more and 2000 ⁇ m or less, 50 ⁇ m or more and 1800 ⁇ m or less, and 100 ⁇ m or more and 1500 ⁇ m or less. but not limited to.
  • the application is preferably performed by applying the dispersion for forming a ceramic sintered body onto the base material.
  • the base material is not particularly limited, but for example, resin films such as polyolefin films (polyethylene films, polypropylene films, etc.), polyester films (polyethylene terephthalate (PET) films, polyethylene naphthalate films, etc.), polyvinyl chloride films are preferably used. It will be done.
  • the base material may be used only for producing the green sheet, or after production, it may be used, for example, as a support for improving handling properties, a protective film, etc.
  • the film thickness of the base material is not particularly limited, but is preferably 10 ⁇ m or more, more preferably 20 ⁇ m or more.
  • the thickness of the base material is not particularly limited, but is preferably 300 ⁇ m or less, more preferably 150 ⁇ m or less. Within these ranges, the supportability of the green sheet, the windability into a roll, etc. are further improved. For these reasons, examples of the range of the film thickness of the base material include, but are not limited to, 10 ⁇ m or more and 300 ⁇ m or less, 20 ⁇ m or more and 150 ⁇ m or less, and the like.
  • drying conditions are not particularly limited, and any suitable conditions can be adopted as appropriate.
  • Prepreg material for forming ceramic sintered bodies Another aspect of the present invention relates to a prepreg material for forming a ceramic sintered body (hereinafter also simply referred to as "prepreg material"), which is formed using the above dispersion for forming a ceramic sintered body.
  • the prepreg material refers to a semi-cured composite material made by impregnating ceramic fibers with a resin or a resin-containing composition.
  • the prepreg material may be a semi-cured composite material produced by impregnating it with a resin or a resin-containing composition and then further drying it if necessary.
  • the prepreg material is formed from ceramic fibers and the above-mentioned dispersion for forming a ceramic sintered body having a pH at 25°C of 4.0 or more (preferably in the above-mentioned preferred pH range at 25°C). It is preferable to include a resin-containing composition comprising (A) component: ceramic particles, (B) component: resin, and (C) component: plasticizer.
  • the prepreg material includes ceramic fibers, a ceramic sintered material having a pH at 25°C of 4.0 or more (preferably in the above preferred pH range at 25°C), and a viscosity in the above preferred range at 25°C.
  • a resin-containing composition formed from the body-forming dispersion which includes (A) component: ceramic particles, (B) component: resin, and (C) component: plasticizer.
  • the resin-containing composition may further contain other components (for example, the above-mentioned components (E), (F), and (G)) as necessary.
  • (A) component, (B) component, (C) component, and other components are for forming the above-mentioned ceramic sintered body. As per the dispersion.
  • the content ratio of component (A) and component (B) in the resin-containing composition and the content ratio of component (A) and component (C) in the resin-containing composition are each subject to particular restrictions. However, the preferred ranges are the same as those described above for the dispersion for forming a ceramic sintered body.
  • the ceramic fiber is not particularly limited as long as it is a fiber made essentially of ceramic.
  • the content of ceramic in the ceramic fiber is preferably 80% by mass or more, more preferably 90% by mass or more, and preferably 100% by mass, based on the total mass of the ceramic fiber. More preferred (upper limit: 100% by mass).
  • the content ratio of ceramic in the ceramic fiber can be evaluated by weight change etc. by thermogravimetric analysis.
  • the ceramic constituting the ceramic fiber is not particularly limited, and may include materials used for known ceramic fibers. Examples include glass, silicon carbide, alumina, silica, mullite, and carbon. Further, examples thereof include oxides or composite oxides of Si, Ti, Zr, Mg, Hf, Al, and rare earth elements described in International Publication No. 2012/077787.
  • the ceramics constituting the ceramic fibers may be used alone or in combination of two or more.
  • the ceramic fiber is a fiber base material.
  • glass cloth alumina fiber base material, SiC fiber base material, carbon fiber base material, and fiber base materials containing alumina and SiC are preferred.
  • the ceramic fiber As the ceramic fiber, a commercially available product or a manufactured product may be used. Commercially available products include, but are not particularly limited to, product name: Nextel (registered trademark) 720 woven fabric type EF-11 manufactured by 3M Company.
  • Ceramic fibers may be used alone or in combination of two or more.
  • a preferred embodiment of the present invention is formed using the above green sheet for forming a ceramic sintered body (a green sheet for forming a ceramic sintered body formed from the above dispersion for forming a ceramic sintered body).
  • a prepreg material for forming a ceramic sintered body relates to a prepreg material for forming a ceramic sintered body. That is, the prepreg material according to this aspect is characterized in that it is formed using a green sheet formed using the above dispersion for forming a ceramic sintered body having a pH of 4.0 or more at 25°C. do.
  • the prepreg material according to this embodiment is preferably formed using a green sheet and ceramic fibers.
  • the green sheet constitutes the resin-containing composition.
  • the method for manufacturing the prepreg material according to this embodiment is not particularly limited, and any known method can be used.
  • a method including a step of laminating a fiber base material and the above green sheet, a step of obtaining a green sheet by the above green sheet manufacturing method, and a step of laminating a fiber base material and the obtained green sheet examples include methods including the following.
  • a method including a step of laminating a fiber base material and the above green sheet under heat and pressure a step of obtaining a green sheet by the above green sheet manufacturing method, a fiber base material and the obtained green sheet.
  • Examples include a method including a step of laminating under heat and pressure.
  • the green sheet may be laminated with heat and pressure from one side of the fiber base material, or may be laminated with heat and pressure from both sides of the fiber base material.
  • Another preferred embodiment of the present invention relates to a prepreg material for forming a ceramic sintered body, which is formed by impregnating ceramic fibers with the above dispersion for forming a ceramic sintered body. That is, the prepreg material according to this aspect is characterized in that it is formed by impregnating ceramic fibers with the above dispersion for forming a ceramic sintered body having a pH of 4.0 or more at 25°C.
  • the method for manufacturing the prepreg material according to this embodiment is not particularly limited, and any known method can be used.
  • the method includes a step of impregnating ceramic fibers with the obtained dispersion for forming a ceramic sintered body and removing the solvent.
  • the impregnation method is not particularly limited, but can be performed by, for example, dipping, coating, etc., and may be repeated multiple times as necessary.
  • the method for removing the solvent is not particularly limited, but it can be carried out, for example, by evaporating the solvent by a known drying process.
  • the manufacturing method of prepreg material includes the steps of laminating a fiber base material and a green sheet under heat and pressure, impregnating ceramic fibers with a dispersion for forming a ceramic sintered body, and removing the solvent by evaporation in a drying step.
  • the method may also include a step.
  • the prepreg material may further include other members.
  • ⁇ Ceramic sintered body> Another aspect of the present invention relates to a ceramic sintered body formed using the above dispersion for forming a ceramic sintered body.
  • a preferred embodiment of the present invention relates to a ceramic sintered body formed from the above prepreg agent for forming a ceramic sintered body.
  • the method for manufacturing the ceramic sintered body is not particularly limited, but includes, for example, a method including a step of sintering the prepreg material described above, a step of obtaining a prepreg material by the method for manufacturing the prepreg material described above, and a method including the step of producing a prepreg material using the obtained prepreg material.
  • Examples include a method including a step of sintering.
  • the resin having a hydroxyl group includes polyvinyl alcohol (PVA), polyvinyl butyral (PVB), polyvinyl propyral, polyvinyl acetal, polyvinyl formal, hydroxyl group-containing glyoxal resin, hydroxyl group-containing acrylic resin, phenol resin, hydroxyl group-containing polyvinylpyrrolidone (The dispersion for forming a ceramic sintered body according to [5], comprising at least one resin selected from the group consisting of PVP), hydroxyl group-containing polyester, hydroxyl group-containing silicone, and hydroxyl group-containing polycarboxylic acid.
  • PVA polyvinyl alcohol
  • PVB polyvinyl butyral
  • polyvinyl propyral polyvinyl acetal
  • polyvinyl formal hydroxyl group-containing glyoxal resin
  • acrylic resin phenol resin
  • phenol resin hydroxyl group-containing polyvinylpyrrolidone
  • the component (C) contains at least one compound selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerin, triethanolamine, and dibutyl phthalate, [1] The dispersion for forming a ceramic sintered body according to any one of [6]. [8] The dispersion for forming a ceramic sintered body according to any one of [1] to [7], further comprising component (E): an acid, and component (F): a thickener. [9] A green sheet for forming a ceramic sintered body, which is formed from the dispersion for forming a ceramic sintered body according to any one of [1] to [8].
  • a prepreg material for forming a ceramic sintered body which is formed using the green sheet for forming a ceramic sintered body according to [9].
  • a prepreg material for forming a ceramic sintered body which is formed by impregnating ceramic fiber with the dispersion for forming a ceramic sintered body according to any one of [1] to [8].
  • alumina particles 1 As alumina particles 1, alumina particles (product name: WA#30000, manufactured by Fujimi Inc., powder) having an average secondary particle diameter of 0.3 ⁇ m were prepared.
  • alumina particles 2 As alumina particles 2, alumina particles (powder) having an average secondary particle diameter of 0.4 ⁇ m were prepared.
  • SiC particles A 20% by mass aqueous dispersion of silicon carbide (SiC) particles (product name: GC#40000, average secondary particle diameter 0.36 ⁇ m, manufactured by Fujimi Incorporated, powder) was prepared, and a 1M NaOH aqueous solution was adjusted to pH 10. It was added so that it became 0. Next, a 30% by mass aqueous dispersion of sodium aluminate was prepared, and the sodium aluminate aqueous dispersion was added in an amount such that the amount of sodium aluminate was 25 parts by mass per 100 parts by mass of SiC particles, and 9.9% by mass hydrochloric acid.
  • the aqueous solution was added over 45 minutes with stirring so that the pH was maintained in the range of 9.0 to 11.0. Thereafter, after further stirring for 45 minutes, a 9.9% by mass aqueous hydrochloric acid solution was added to adjust the pH to 10.5, thereby preparing an aqueous dispersion containing particles. Thereafter, a 9.9% by mass aqueous hydrochloric acid solution was added to adjust the pH to 3.0, and the mixture was concentrated by suction filtration. An aqueous dispersion 4a having a concentration of 50% by mass of secondary particles having a diameter of 0.48 ⁇ m was obtained. Note that the pH was measured at 25° C. using a pH meter (model number: F-71) manufactured by Horiba, Ltd.
  • aqueous dispersion 4a obtained above was collected and dropped onto a filter (Nuclipore 5 ⁇ m) (manufactured by WHATMAN). Subsequently, suction filtration was performed, and then the powder was washed on the filter using 10 mL of pure water, and the particles were dried. Then, the dried particles were collected on a Si wafer and analyzed using a scanning electron microscope SU-8000 manufactured by Hitachi High-Technologies Corporation. y) Observation went.
  • the dried particles were collected on a carbon tape and subjected to EELS (Electron Energy Loss Spectroscopy) analysis using TITAN 80-300 manufactured by FEI.
  • EELS Electro Energy Loss Spectroscopy
  • C, Al, and O are selected as the elements to be observed, and the EDX spectrum of Al is observed, and the positions where the EDX spectra of C, Al, and O are observed, and the SEM observation.
  • the SiC particle was coated with a component containing Al and O.
  • the observed EELS spectrum has a spectral shape unique to the EELS standard spectrum of aluminum hydroxide (Al(OH) 3 ) (different from the spectra of Al and other Al- and O-containing compounds). shape), it was determined that the component containing Al and O contained Al(OH) 3 .
  • Dispersion 1 Prepare an aqueous dispersion containing the above alumina particles 1 with a concentration of 55% by mass, and add 100g of the aqueous dispersion containing alumina particles 1 with a concentration of 55% by mass to 10g of an aqueous hydrochloric acid solution with a concentration of 2.5% by mass while stirring. In this way, an aqueous dispersion 1a of alumina particles was obtained.
  • Dispersion medium 2 In the preparation of Dispersion 1, the alumina particles used were changed from alumina particles 1 to the above-mentioned alumina particles 2, and the aqueous hydrochloric acid solution used and its amount were changed from 10 g of an aqueous hydrochloric acid solution with a concentration of 2.5% by mass to 0.5% by mass. Dispersion 2 having a pH of 5.5 was obtained in the same manner except that 10 g of a mass % hydrochloric acid aqueous solution was used.
  • Dispersion 3 having a pH of 4.7 was obtained in the same manner as in the preparation of Dispersion 2, except that the amount of the aqueous hydrochloric acid solution used was increased.
  • Dispersion 4 having a pH of 4.4 was obtained in the same manner as in the preparation of Dispersion 1, except that water dispersion 4a obtained above was used instead of water dispersion 1a.
  • Dispersion 5 having a pH of 3.4 was obtained in the same manner as in the preparation of Dispersion 1 except that the amount of the aqueous hydrochloric acid solution used was increased.
  • Dispersion 6 having a pH of 3.2 was obtained in the same manner as in the preparation of Dispersion 1 except that the amount of the aqueous hydrochloric acid solution used was increased.
  • Dispersion 7 having a pH of 3.6 was obtained in the same manner as in the preparation of Dispersion 2, except that the amount of the aqueous hydrochloric acid solution used was increased.
  • Dispersion 8 having a pH of 3.0 was obtained in the same manner as in the preparation of Dispersion 2, except that the amount of the aqueous hydrochloric acid solution used was increased.
  • Dispersion 9 In the preparation of dispersion 4, after further adding an aqueous hydrochloric acid solution with a concentration of 2.5% by mass to the aqueous dispersion 4a, the resulting aqueous dispersion and a polyvinyl acetal aqueous solution with a concentration of 20% by mass as a resin (product name Dispersion 9 with a pH of 3.9 was prepared in the same manner except that S-LEC (registered trademark) KW-3, manufactured by Sekisui Chemical Co., Ltd., weight average molecular weight 13,000) and polyethylene glycol as a plasticizer were mixed. Obtained.
  • S-LEC registered trademark
  • KW-3 manufactured by Sekisui Chemical Co., Ltd., weight average molecular weight 13,000
  • the obtained dispersions 1 to 9 are (A) component: ceramic particles (alumina particles 1, alumina particles 2, or aluminum hydroxide coated SiC particles), (B) component: polyvinyl acetal, (C) component: polyethylene glycol , component (D): water, and component (E): hydrochloric acid.
  • the weight average molecular weight of the resin used in the preparation of the above dispersion was measured as a value in terms of polyethylene oxide by gel permeation chromatography (GPC) under the following measurement conditions: ⁇ GPC measurement conditions ⁇ Sample concentration: 0.1% by mass Column: “TSKgel GMPWXL” manufactured by Tosoh Corporation Detector: Differential refractometer Eluent: 100mM sodium nitrate aqueous solution Flow rate: 1mL/min Measurement temperature: 40°C Sample injection volume: 200 ⁇ L Measuring device: “HLC-8320GPC” manufactured by Tosoh Corporation.
  • each dispersion was adjusted by kneading the mixture for 2 minutes using a 300-ml (Sinky-310, manufactured by Shinky Co., Ltd.), leaving it to stand at room temperature for 24 hours, and then kneading it again for 4 minutes. Then, by forming a sheet of each dispersion after adjusting the viscosity onto a PET film (thickness: 100 ⁇ m) using an applicator with a 900 ⁇ m gap, green Sheets 1 to 9 were obtained.
  • a 300-ml Tinky-310, manufactured by Shinky Co., Ltd.
  • aqueous dispersion from alumina particles and water
  • alumina particles product name: WA#30000, manufactured by Fujimi Incorporated, average secondary particle diameter 0.3 ⁇ m
  • a dispersion was prepared.
  • 100 g of the aqueous dispersion of alumina particles having a concentration of 25% by mass was added to 5g of an aqueous hydrochloric acid solution having a concentration of 2.5% by mass with stirring.
  • a dispersion was prepared in the same manner as Dispersion 1 except that polyethylene glycol was not added. Using this prepared dispersion, a green sheet was manufactured by a method similar to the method for manufacturing the green sheet described above so that the thickness of the obtained green sheet was 150 ⁇ m. The green sheet was manufactured as a laminate of a PET film and a green sheet. By cutting the obtained laminate of the PET film and the green sheet and peeling off the PET film, a green sheet for testing with a length of 5 cm on the long side x 1.5 cm on the short side x 150 ⁇ m in thickness was prepared. A bending test was conducted in which the sheet was bent at the center of the long side.
  • the obtained green sheet had low flexibility and could not be bent at an angle of 170° while maintaining its structure.
  • a green sheet was manufactured using a method similar to the method for manufacturing the green sheet described above so that the thickness of the obtained green sheet was 150 ⁇ m.
  • the produced green sheet was subjected to a bending test in the same manner, it was possible to bend it at an angle of 170° while maintaining the structure. From this, it was confirmed that in the green sheet 1 for forming a ceramic sintered body formed from the dispersion 1, polyethylene glycol improves the flexibility of the green sheet and functions as a plasticizer.
  • a dispersion 10 having a pH of 3.5 was prepared in the same manner except that the amount of polyethylene glycol as a plasticizer was changed to 0 g, and using this dispersion 10, A green sheet 10 was manufactured in the same manner as the green sheet 5 described above.
  • the green sheet 10 was evaluated for the presence or absence of bleed-out in the same manner as above, and the evaluation was "A", with no bleed-out observed. From this result, it is considered that the bleed-out component in the above evaluation is mainly polyethylene glycol, which is a plasticizer. Note that when a bending test was conducted using the dispersion 10 in the same manner as above, the green sheet formed from the dispersion 10 could not be bent at an angle of 170° while maintaining its structure.
  • Prepreg material 1-1 A laminate of the PET film and green sheet 1 obtained above, and a ceramic fiber (manufactured by 3M Company, product name: Nextel (registered trademark) 720 fabric type EF-11) were added to the green sheet 1 and the ceramic fiber.
  • a prepreg material 1-1 with a PET film was obtained by laminating the fibers so that they were in contact with each other.
  • prepreg material 5 In the production of prepreg material 1-1, PET film was produced in the same manner except that the laminate of PET film and green sheet 1 used was changed to a laminate of the PET film obtained above and green sheet 5. A prepreg material 5 in a state of being attached was obtained.
  • Prepreg material 1-2 After impregnating a ceramic fiber (manufactured by 3M Company, product name: Nextel (registered trademark) 720 fabric type EF-11) with the above dispersion 1, the surplus material is removed by passing the ceramic fiber between two bar coaters. The dispersion was removed and dried to obtain prepreg material 1-2.
  • a ceramic fiber manufactured by 3M Company, product name: Nextel (registered trademark) 720 fabric type EF-11
  • a sintered body 5 was obtained in the same manner as in the production of the sintered body 1-1, except that the prepreg material 1-1 with the PET film was changed to the prepreg material 5 with the PET film attached.
  • sintered body 1-2 In the production of sintered body 1-1, the same except that prepreg material 1-1 with PET film was changed to prepreg material 1-2 without PET film, and the PET film was not peeled off. Then, a sintered body 1-2 was obtained.

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PCT/JP2023/003069 2022-03-11 2023-01-31 セラミック焼結体形成用分散体、セラミック焼結体形成用グリーンシート、セラミック焼結体形成用プリプレグ材、およびセラミック焼結体 Ceased WO2023171181A1 (ja)

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