WO2024252896A1 - Procédé de production d'un corps fritté, feuille verte et corps fritté - Google Patents

Procédé de production d'un corps fritté, feuille verte et corps fritté Download PDF

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Publication number
WO2024252896A1
WO2024252896A1 PCT/JP2024/018301 JP2024018301W WO2024252896A1 WO 2024252896 A1 WO2024252896 A1 WO 2024252896A1 JP 2024018301 W JP2024018301 W JP 2024018301W WO 2024252896 A1 WO2024252896 A1 WO 2024252896A1
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Prior art keywords
sintered body
less
mass
producing
sheet
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PCT/JP2024/018301
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English (en)
Japanese (ja)
Inventor
真美 生田目
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AGC Inc
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Asahi Glass Co Ltd
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Priority to JP2025526033A priority Critical patent/JPWO2024252896A1/ja
Publication of WO2024252896A1 publication Critical patent/WO2024252896A1/fr
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/30—Producing shaped prefabricated articles from the material by applying the material on to a core or other moulding surface to form a layer thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/12—Apparatus or processes for treating or working the shaped or preshaped articles for removing parts of the articles by cutting
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • 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

Definitions

  • the present invention relates to a method for producing a sintered body, a green sheet, and a sintered body.
  • Quartz glass has high purity and excellent optical properties, and is used in many industrial fields, including the semiconductor industry.
  • Known methods for manufacturing quartz glass include the fusion method, in which silica melted at high temperatures is cooled (e.g., Patent Document 1), and the sol-gel method, in which silica gel prepared in a solution is dried and then heated (e.g., Patent Document 2).
  • an object of the present invention is to provide a method for easily producing a sintered body of thin plate-thickness quartz glass or the like.
  • the present inventors focused on a method of producing a sintered body of quartz glass or the like by firing a slurry containing silica powder.
  • a sintered body of quartz glass or the like having a thin plate thickness can be easily produced by a method of forming a green sheet using a slurry composition in which the ratio of silica powder in the inorganic powder is equal to or higher than a predetermined value, cutting the green sheet, and firing the resulting sheet molded body.
  • a sintered body such as a thin quartz glass plate can be easily manufactured by using a green sheet having a specific thickness and containing an inorganic powder having a silica powder ratio equal to or greater than a predetermined value, the silica powder containing spherical particles of a specific particle size.
  • one embodiment of the present invention relates to a method for producing a sintered body, the method including: preparing a slurry composition containing an inorganic powder, in which the proportion of silica powder in the inorganic powder is more than 85 mass %; forming the slurry composition into a green sheet having a thickness of 1.5 mm or less; cutting the green sheet to a desired size to obtain a sheet-shaped body; and sintering the sheet-shaped body to obtain a sintered body, wherein the sintered body has a plate thickness of 0.003 mm or more and 1 mm or less.
  • Another embodiment of the present invention relates to a green sheet and a sintered body thereof, which include an inorganic powder having a ratio of silica powder exceeding 85% by mass, the silica powder having a volume-based 50% particle diameter D50 in a cumulative particle size distribution of 80 nm or more and 15 ⁇ m or less, a ratio of a volume-based 10% particle diameter D10 in a cumulative particle size distribution of 0.2 or more and 1.0 or less, and a ratio of a volume-based 90% particle diameter D90 in a cumulative particle size distribution of 1.0 or more and 3.0 or less, and have a thickness of 1.5 mm or less.
  • the present invention makes it possible to easily manufacture sintered bodies such as thin-walled quartz glass.
  • FIG. 1 is a schematic diagram showing a case where a sheet compact 10 is placed on a lower sintering setter 11b and sintered.
  • FIG. 2 is a schematic diagram showing a case where firing is performed with a gap provided between the lower sintering setter 11b and the sheet compact 10.
  • a method for producing a sintered body includes preparing a slurry composition containing an inorganic powder, in which the proportion of silica powder in the inorganic powder is greater than 85% by mass; forming the slurry composition into a green sheet having a thickness of 1.5 mm or less; cutting the green sheet to a desired size to obtain a sheet-shaped body; and sintering the sheet-shaped body to obtain a sintered body, wherein the sintered body has a plate thickness of 0.003 mm or more and 1 mm or less.
  • a slurry composition is first prepared.
  • the slurry composition contains an inorganic powder, and is prepared so that the ratio of silica powder in the inorganic powder is more than 85% by mass.
  • the ratio of silica powder in the inorganic powder is preferably 90% by mass or more, more preferably 95% by mass or more, particularly preferably 99% by mass or more, and is usually 100% by mass or less.
  • examples of inorganic powders contained in the slurry composition include, in addition to silica powder , B2O3 , P2O5 , CaO, MgO, BaO , Li2O , Na2O , K2O , MgCO3 , CaCO3 , SrCO3, BaCO3 , and Na2CO3 .
  • the volume solid content of the inorganic powder containing more than 85 mass% of silica powder is preferably 12 vol% or more and less than 60 vol%.
  • the volume solid content of the inorganic powder can be easily adjusted to 30 vol% or more.
  • the volume solids content of the inorganic powder is more preferably 13 vol % or more, further preferably 20 vol % or more, and particularly preferably 30 vol % or more.
  • the slurry composition has a volume solid fraction of the inorganic powder of less than 60 vol.%, as described below, in a green sheet obtained by drying the slurry composition, the volume solid fraction of the inorganic powder can be easily adjusted to less than 93 vol.%, and chipping of the green sheet due to impact can be suppressed.
  • the volume solids content of the inorganic powder is more preferably 45 vol % or less, further preferably 40 vol % or less, and particularly preferably 35 vol % or less.
  • the type of silica powder is not particularly limited, and examples thereof include silica sand, quartz powder, cristobalite powder, amorphous silica powder, spherical silica powder, etc.
  • the silica powder may be used alone or in combination of two or more kinds.
  • the shape of the silica powder may be spherical or may be non-spherical such as amorphous or crushed, but from the viewpoint of packing density, it is preferable that it is spherical.
  • the silica powder may be subjected to any surface treatment.
  • Examples of the surface treatment include treatment of adding a methacryl group, a vinyl group, a phenyl group, a trimethylsilyl group, a phenylamino group, an epoxy group, or the like to the surface of the silica powder.
  • the purity of the silica powder is preferably 99.0% or more, more preferably 99.5% or more, and even more preferably 99.8% or more.
  • the D50 of the silica powder is preferably 80 nm or more and 15 ⁇ m or less.
  • the D50 of the silica powder is 80 nm or more, it is easy to adjust the silica solid content of the green sheet to 30 vol% or more.
  • the D50 of the silica powder is 15 ⁇ m or less, the firing temperature can be suppressed from increasing, and a sintered body such as quartz glass can be produced by sintering.
  • the D50 of the silica powder is more preferably 120 nm or more, even more preferably 150 nm or more, particularly preferably 300 nm or more, most preferably 500 nm or more, more preferably 10 ⁇ m or less, even more preferably 5 ⁇ m or less, particularly preferably 2 ⁇ m or less, and most preferably 1 ⁇ m or less.
  • the silica powder preferably contains spherical particles with a ratio of D10 to D50 ( D10 / D50 ) of 0.2 or more and 1.0 or less.
  • D10 / D50 is more preferably 0.3 or more, even more preferably 0.4 or more, particularly preferably 0.5 or more, and more preferably 0.9 or less, and even more preferably 0.8 or less.
  • the silica powder preferably contains spherical particles having a ratio of D90 to D50 ( D90 / D50 ) of 1.0 to 3.0.
  • D90 / D50 is more preferably 1.2 or more, even more preferably 1.5 or more, and particularly preferably 1.7 or more, and more preferably 2.8 or less, even more preferably 2.5 or less, and particularly preferably 2.0 or less.
  • D50 , D10 , and D90 of the silica powder refer to particle sizes at 50%, 10%, and 90% cumulative values in the particle size distribution determined by a laser diffraction/scattering method, respectively, and can be measured, for example, using a laser diffraction/scattering particle size analyzer MT-3000 manufactured by Nikkiso Co., Ltd.
  • D50 , D10 , and D90 can be calculated by determining the size distribution of the silica powder from image analysis of an optical microscope image or an electron microscope image of the green sheet.
  • the slurry composition may contain a binder.
  • the type of binder is not particularly limited, and examples thereof include polyvinyl alcohol-based resins such as polyvinyl alcohol, butyral-based resins such as polyvinyl butyral, cellulose-based resins such as methyl cellulose, ethyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and cellulose acetate phthalate, acrylic resins such as poly(meth)acrylic acid ester, nitrile resins such as polyacrylonitrile and polymethacrylonitrile, urethane resins such as polyurethane, vinyl resins such as polyethylene, polypropylene, polyvinylidene fluoride, polyvinylidene chloride, polyvinyl fluoride, and vinyl acetate, rubber resins such as styrene butadiene rubber, and epoxy resins.
  • the binder may be used alone
  • the slurry composition is preferably prepared so that the binder content relative to the silica powder is 5% by mass or more, more preferably 10% by mass or more, and particularly preferably 15% by mass or more.
  • the binder content relative to the silica powder is preferably prepared so that it is 60% by mass or less, more preferably 45% by mass or less, and particularly preferably 30% by mass or less.
  • the slurry composition may contain an organic solvent.
  • the organic solvent is selected taking into consideration the compatibility with the binder, dispersants and plasticizers described below, the desired properties of the green sheet, the process load that can be tolerated, and the like.
  • organic solvents include hydrocarbons such as toluene, xylene, methylcyclohexane, and terpineol; alcohols such as ethanol, n-propanol, isopropanol, and n-butanol; ketones such as acetone, methyl ethyl ketone, and methyl isobutyl ketone; ethers such as ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, and propylene glycol monomethyl ether; esters such as ethyl acetate, butyl acetate, isobutyl acetate, and propylene glycol monomethyl ether acetate, and the like.
  • the organic solvents can
  • the slurry composition is preferably prepared so that the organic solvent content is 30% by mass or more, more preferably 40% by mass or more, and even more preferably 45% by mass or more.
  • the slurry composition is preferably prepared so that the organic solvent content is 90% by mass or less, more preferably 80% by mass or less, and even more preferably 70% by mass or less.
  • the slurry composition may be prepared so as to contain, as other components, a dispersant, a plasticizer, an antifoaming agent, a rheology control agent, a wetting agent, and the like.
  • a dispersant include surfactant-type dispersants, polymer dispersants, etc.
  • the dispersants may be used alone or in combination of two or more.
  • surfactant-type dispersants include alkylamine salts, aliphatic or aromatic quaternary ammonium salts, heterocyclic quaternary ammonium salts such as pyridinium and imidazolium, aliphatic or heterocyclic phosphonium or sulfonium salts, and acetylene glycol.
  • polymer dispersant examples include a polymer having a primary to tertiary amine, a quaternary ammonium base, a quaternary phosphonium base, a carboxylic acid group, a hydrochloric acid group, a phosphoric acid group, or the like in the polymer main chain or side chain; a homopolymer of acrylic acid or a salt thereof; or an aminocarboxylic acid-based, polyamine-based, polyurethane-based, or polyacrylate-based homopolymer, copolymer, or block copolymer.
  • the dispersant commercially available products may be used.
  • the slurry composition is prepared so that the dispersant is 1% by mass or more relative to the inorganic powder containing more than 85% by mass of silica powder, more preferably 2% by mass or more, and even more preferably 4% by mass or more.
  • the content of the dispersant is 1% by mass or more, the dispersibility of the powder is improved, and it is easy to adjust the volumetric solid content of the inorganic powder to 30 vol% or more in the final green sheet.
  • the slurry composition is prepared so that the content of the dispersant is 15% by mass or less relative to the inorganic powder, more preferably 12% by mass or less, and even more preferably 10% by mass or less. When the content of the dispersant is 15% by mass or less, it is possible to suppress the aggregation of the powder, and it is easy to adjust the volumetric solid content of the inorganic powder to 30 vol% or more in the green sheet.
  • plasticizers examples include adipic acid-based, adipic acid ether ester-based, phthalic acid-based, terephthalic acid ester-based, triethylene glycol diester-based, polyether ester-based, and epoxy-based plasticizers.
  • the slurry composition is preferably prepared so that the plasticizer content relative to the silica powder is 1% by mass or more, more preferably 5% by mass or more, and even more preferably 7% by mass or more.
  • the plasticizer content relative to the silica powder is 15% by mass or less, more preferably 10% by mass or less.
  • the phenomenon of the plasticizer bleeding out from the green sheet can be suppressed.
  • the prepared slurry composition is formed into a green sheet having a thickness of 1.5 mm or less.
  • the prepared slurry composition is applied onto a support in the form of a sheet to form a green sheet.
  • the support may be, for example, a resin film.
  • a resin film a thermoplastic resin film is usually used, and specifically, polyethylene terephthalate film, polypropylene film, polyethylene film, polycarbonate film, polyethylene naphthalate film, polyarylate film, nylon film, etc. are mentioned.
  • polyethylene terephthalate film and polyethylene naphthalate film are preferred from the viewpoints of heat resistance, chemical resistance, peelability after lamination, etc.
  • the thickness of the support is not particularly limited, but from the viewpoint of workability and the like, it is usually 10 to 200 ⁇ m, preferably 30 to 150 ⁇ m, and more preferably 50 to 120 ⁇ m.
  • the method for applying the slurry composition onto the support in the form of a sheet can be a known wet coating method, such as spin coating, doctor blade, reverse roll coater, spray coating, dip coating, die coating, curtain coating, screen coating, inkjet, flow coating, gravure coating, bar coating, flexo coating, slit coating, roll coating, sponge roll coating, squeegee coating, etc.
  • the slurry composition is applied in sheet form onto the support so that the thickness of the green sheet obtained after drying, etc., as described below, is 1.5 mm or less.
  • the thickness of the sheet-like slurry composition applied onto the support is preferably 0.005 mm or more and 3.0 mm or less, more preferably 0.05 mm or more and 2.0 mm or less, and even more preferably 0.09 mm or more and 1.0 mm or less.
  • the slurry composition After the slurry composition is applied in sheet form on the support, it may be dried to form a green sheet. By drying, the organic solvent and the like are removed from the slurry composition applied in sheet form on the support.
  • the drying conditions are set appropriately depending on the type and amount of the organic solvent used, and can be set, for example, at 60 to 150°C and for 0.5 to 5 hours.
  • a green sheet with a thickness of 1.5 mm or less is formed.
  • the green sheet is preferably formed to a thickness of 0.003 mm to 0.7 mm or less.
  • the green sheet is more preferably formed to a thickness of 0.5 mm or less, and particularly preferably to a thickness of 0.3 mm or less, and may also be formed to a thickness of, for example, 0.005 mm or more.
  • the volume solid content of the inorganic powder in the green sheet containing more than 85% by mass of silica powder is preferably 30 vol% or more and less than 93 vol%.
  • the volume solid content of the inorganic powder is more preferably 40 vol% or more, and even more preferably 45 vol% or more.
  • the volume solid content of the inorganic powder containing more than 85 mass% of silica powder in the green sheet is less than 93 vol%, chipping of the green sheet due to impact is suppressed, and the handling property is excellent.
  • the volume solid content of the inorganic powder is more preferably 90 vol% or less, further preferably 88 vol% or less, and particularly preferably 85 vol% or less.
  • the volumetric solid content of the inorganic powder containing more than 85 mass% silica powder in the green sheet means the proportion (by volume) of the inorganic powder containing more than 85 mass% silica powder among all the components of the above-mentioned slurry composition excluding the solvent component.
  • the width of the green sheet is preferably 1 cm or more, more preferably 10 cm or more, even more preferably 15 cm or more, and particularly preferably 20 cm or more. When the width of the green sheet is 1 cm or more, productivity can be improved, and when the width of the green sheet is 10 cm or more, productivity can be further improved.
  • the width of the green sheet is preferably 200 cm or less, more preferably 150 cm or less, and even more preferably 130 cm or less. When the width of the green sheet is 200 cm or less, it is easy to obtain a green sheet with a uniform thickness.
  • the length in the width direction of the green sheet means the length in the direction perpendicular to the longitudinal direction of the green sheet.
  • the length of the green sheet in the long axis direction is preferably 1 cm or more, more preferably 10 cm or more, even more preferably 100 cm or more, particularly preferably 200 cm or more, and most preferably 300 cm or more.
  • the length of the green sheet in the long axis direction is preferably 8000 cm or less, more preferably 7000 cm or less, and even more preferably 5000 cm or less. When the length of the green sheet in the long axis direction is 8000 cm or less, handling becomes easy.
  • one embodiment of the present invention is a green sheet comprising an inorganic powder having a ratio of silica powder exceeding 85 mass%, the silica powder including spherical particles having a D50 , which is a 50% particle diameter on a volume basis in a cumulative particle size distribution, of 80 nm or more and 15 ⁇ m or less, a ratio ( D10 / D50 ) of D10, which is a 10% particle diameter on a volume basis in the cumulative particle size distribution, to the D50 , of 0.2 or more and 1.0 or less, and a ratio ( D90 / D50 ) of D90, which is a 90% particle diameter on a volume basis in the cumulative particle size distribution, to the D50 , of 1.0 or more and 3.0 or less, and having a thickness of 1.5 mm or less.
  • a D50 which is a 50% particle diameter on a volume basis in a cumulative particle size distribution, of 80 nm or more and 15 ⁇ m or less
  • the green sheet of this embodiment can suppress devitrification because the proportion of silica powder in the inorganic powder contained in the green sheet is more than 85 mass%.
  • the proportion of silica powder in the inorganic powder is preferably 90 mass% or more, more preferably 95 mass% or more, particularly preferably 99 mass% or more, and is usually 100 mass% or less.
  • the D50 of the silica powder is 80 nm or more, it is easy to adjust the silica solid content of the green sheet to 30 vol% or more, and the shrinkage rate during firing described below is suppressed to 33% or less, making it possible to control the shape of the resulting sintered body.
  • the D50 of the silica powder is 15 ⁇ m or less, it is possible to suppress the firing temperature from becoming high, and it is possible to produce a sintered body such as quartz glass by sintering.
  • the D50 of the silica powder is more preferably 120 nm or more, even more preferably 150 nm or more, particularly preferably 300 nm or more, most preferably 500 nm or more, more preferably 10 ⁇ m or less, even more preferably 5 ⁇ m or less, particularly preferably 2 ⁇ m or less, and most preferably 1 ⁇ m or less.
  • the silica powder contains spherical particles having a D10 / D50 in the above range, the silica solid content of the green sheet can be easily adjusted to 30 vol% or more, and a green sheet with a uniform thickness can be easily obtained.
  • D10 / D50 is more preferably 0.3 or more, even more preferably 0.4 or more, and particularly preferably 0.5 or more, and is more preferably 0.9 or less, and even more preferably 0.8 or less.
  • the silica powder contains spherical particles having a D90 / D50 in the above range, the silica solid content of the green sheet can be easily adjusted to 30 vol% or more, and a green sheet with a uniform thickness can be easily obtained.
  • D90 / D50 is more preferably 1.2 or more, even more preferably 1.5 or more, and particularly preferably 1.7 or more, and is more preferably 3.0 or less, even more preferably 2.5 or less, and particularly preferably 2.0 or less.
  • a green sheet with a stable film thickness can be obtained.
  • the thickness of the green sheet is preferably 0.003 mm or more and 0.7 mm or less, more preferably 0.5 mm or less, and particularly preferably 0.3 mm or less, and may be, for example, 0.005 mm or more.
  • the formed green sheet is cut to a desired size to obtain a sheet body.
  • the molded green sheet is preferably cut to any length in the width direction within a range of 1000 mm or less, more preferably cut to any length in the range of 500 mm or less, even more preferably cut to any length in the range of 300 mm or less, and may also be cut to any length in the range of 100 mm or more.
  • the molded green sheet is preferably cut to any length in the long axis direction within a range of 1000 mm or less, more preferably cut to any length in the range of 500 mm or less, even more preferably cut to any length in the range of 300 mm or less, and may also be cut to any length in the range of 100 mm or more.
  • the formed green sheet can be cut to any length within the above range to facilitate handling in subsequent steps.
  • the method for cutting the molded green sheet is not particularly limited, and examples include dicing, vertical cutting, ultrasonic cutting, laser cutting, shearing, and cutting using a rotary cutter, slide cutter, and disc cutter.
  • the sheet molded body Before firing the produced sheet molded body, the sheet molded body may be subjected to a degreasing treatment.
  • the degreasing treatment is carried out, for example, by burning organic components of the sheet molded body.
  • the degreasing treatment is preferably carried out using a heating furnace such as an electric furnace at a temperature of 400 to 800°C for 0.5 to 80 hours.
  • the degreasing treatment may be carried out using a sintering setter used in firing the sheet molded body described later, so that the degreasing treatment and firing of the sheet molded body may be carried out continuously.
  • a sintered body can be obtained by firing the sheet compact.
  • the sheet compact may be fired in air, vacuum, or in an inert gas atmosphere.
  • the sintering temperature is preferably 1000° C. or higher, more preferably 1050° C. or higher, and even more preferably 1100° C. or higher. By setting the sintering temperature at 1000° C. or higher, a high-density sintered body such as quartz glass can be obtained.
  • the sintering temperature is preferably 1500° C. or lower, more preferably 1450° C. or lower, and even more preferably 1350° C. or lower. By setting the sintering temperature at 1500° C. or lower, cracking of the sintered body due to crystal precipitation can be suppressed.
  • the sintering time is, for example, 0.03 to 5 hours, may be 5 to 30 hours, or may be 30 to 100 hours.
  • the firing temperature is preferably 1300° C. or higher, more preferably 1350° C. or higher, and even more preferably 1400° C. or higher.
  • the firing temperature is preferably 1600° C. or less, more preferably 1550° C. or less, and even more preferably 1500° C. or less.
  • the sintering time is, for example, 0.01 to 10 hours, may be 0.03 to 5 hours, or may be 0.05 to 2 hours.
  • the sheet molded body can be fired using a sintering setter, or a roll-to-roll method without using a setter, in which the sheet is sintered while tension is applied to the sheet.
  • a sintering setter In consideration of the simplicity of the manufacturing equipment, the method using a sintering setter is preferable.
  • the sheet molded body is preferably fired using a sintering setter having a thermal conductivity of 2.0 W/m ⁇ K or more. By firing the sheet molded body using the sintering setter, it is possible to suppress firing unevenness and deformation.
  • the thermal conductivity of the sintering setter is preferably 2.0 W/m ⁇ K or more, more preferably 10.0 W/m ⁇ K or more, even more preferably 80.0 W/m ⁇ K or more, and may be 1000.0 W/m ⁇ K or less.
  • the sintering setter preferably contains a material such as carbon, SiC, Si-impregnated SiC, BN, alumina, or mullite. By containing the above-mentioned material, the sintering setter can increase the thermal conductivity.
  • the sintering setter may contain one type of the above-mentioned material alone, or may contain two or more types of the above-mentioned material.
  • the sheet molded body When firing the sheet molded body, for example, as shown in FIG. 1, it is preferable to place sintering setters 11 above and below the sheet molded body 10 and fire the sheet molded body. In other words, it is preferable to fire the sheet molded body 10 in a state in which the sheet molded body 10 is placed between the upper sintering setter 11a and the lower sintering setter 11b.
  • the gap between the upper sintering setter 11a and the sheet molding 10 is preferably 1 mm or less. By keeping the gap within the above range, it is possible to suppress deformation due to uneven sintering.
  • the gap is more preferably 0.5 mm or less, even more preferably 0.2 mm or less, and may be 0.01 mm or more.
  • the sheet molded body 10 When firing the sheet molded body, as shown in FIG. 1, the sheet molded body 10 may be placed on the lower sintering setter 11b and fired, or as shown in FIG. 2, a gap may be provided between the lower sintering setter 11b and the sheet molded body 10 by providing an optional pedestal (not shown) on the lower sintering setter 11b.
  • the gap may be, for example, within 1 mm.
  • the sheet molded body 10 may also be sandwiched between the sintering setters with no gap between them.
  • the temperature difference between the upper surface of the sintering setter (upper sintering setter 11a) installed on the upper part of the sheet molded body and the upper surface of the sintering setter (lower sintering setter 11b) installed on the lower part of the sheet molded body is preferably within 5°C. By keeping the temperature difference within 5°C, it is possible to suppress uneven firing and deformation.
  • the temperature difference is preferably within 5°C, more preferably within 4°C, and even more preferably within 3°C, and may be 1°C or more.
  • the temperature of the upper surface of the upper sintering setter 11a and the temperature of the upper surface of the lower sintering setter 11b can be measured by inserting a thermocouple. If it is not possible to insert a thermocouple, the temperature difference can be estimated by using a material with a known shrinkage rate at a certain temperature, such as Referthermo.
  • the flatness Ra of the upper surface of the sintering setter installed under the sheet molded body i.e., the flatness Ra of the main surface of the lower sintering setter 11b on which the sheet molded body is placed, is preferably 0.1 mm or less.
  • the flatness Ra is preferably 0.05 mm or less, more preferably 0.01 mm or less, even more preferably 0.001 mm or less, and may be 0.0001 mm or more.
  • the flatness Ra means the arithmetic mean roughness Ra, and can be measured based on JIS B 0601:2013, for example, by a SURFCOM1400D manufactured by Tokyo Seimitsu Co., Ltd.
  • the sintered body obtained by firing the sheet molded body has a thickness of 0.003 mm or more and 1 mm or less.
  • a thickness of 0.003 mm or more can suppress cracking during handling.
  • a thickness of 1 mm or less can minimize grinding processing, allowing a thin substrate such as quartz glass to be obtained.
  • the thickness of the sintered body is preferably 0.01 mm or more, more preferably 0.02 mm or more, and preferably 0.5 mm or less, more preferably 0.3 mm or less, and even more preferably 0.2 mm or less.
  • the shrinkage rate during sintering is preferably 33% or less, more preferably 25% or less, and even more preferably 20% or less. By making the shrinkage rate during sintering 33% or less, shape control becomes easier.
  • the sintered body obtained by firing the sheet molded body preferably contains more than 10 ppm by mass and less than 5000 ppm by mass of Zr.
  • the sintered body contains more than 10 ppm by mass of Zr, it is easy to obtain a sintered body from the sheet molded body. Also, when the sintered body contains less than 5000 ppm by mass of Zr, cracks due to crystal precipitation during firing of the sheet molded body can be suppressed.
  • the sintered body preferably contains 20 ppm by mass or more of Zr, even more preferably 50 ppm by mass or more, and particularly preferably 70 ppm by mass or more, and more preferably contains less than 4000 ppm by mass of Zr, even more preferably contains less than 3000 ppm by mass, particularly preferably contains less than 1000 ppm by mass, and most preferably contains less than 500 ppm by mass.
  • Zr the amount of mixed-in ball material and the like from the mixing process is taken into consideration, and the shortage is adjusted with the raw materials.
  • the sintered body obtained by firing the sheet molded body preferably contains more than 1 ppm by mass and less than 5000 ppm by mass of Al.
  • the sintered body contains more than 1 ppm by mass of Al, it is easy to obtain a sintered body from the sheet molded body.
  • the sintered body contains less than 5000 ppm by mass of Al, cracks due to crystal precipitation during firing of the sheet molded body can be suppressed.
  • the sintered body preferably contains 5 ppm by mass or more of Al, even more preferably 10 ppm by mass or more, and particularly preferably 20 ppm by mass or more, and more preferably contains less than 500 ppm by mass of Al, even more preferably contains less than 400 ppm by mass, and particularly preferably contains less than 300 ppm by mass.
  • the Zr and Al contents in the above sintered body can be measured using an ICP mass spectrometer (Agilent 8800) manufactured by Agilent Technologies.
  • the sintered body obtained by firing the sheet molded body preferably has a relative density of 99% or more.
  • a sintered body without bubbles can be obtained by having a relative density of 99% or more.
  • the relative density of the sintered body is more preferably 99.1% or more, even more preferably 99.5% or more, particularly preferably 99.6% or more, and may be 99.9% or less.
  • the relative density of the sintered body can be measured by the Archimedes method.
  • the present specification discloses the following: [1] Preparing a slurry composition containing an inorganic powder, in which the proportion of silica powder in the inorganic powder is more than 85% by mass; forming the slurry composition into a green sheet having a thickness of 1.5 mm or less; Cutting the green sheet to a desired size to obtain a sheet molded body; and and sintering the sheet compact to obtain a sintered body.
  • the method for producing a sintered body wherein the sintered body has a plate thickness of 0.003 mm or more and 1 mm or less.
  • An inorganic powder containing more than 85% by mass of silica powder The silica powder includes spherical particles having a D50 , which is a 50% particle diameter on a volume basis in a cumulative particle size distribution, of 80 nm or more and 15 ⁇ m or less, a ratio of a D10, which is a 10% particle diameter on a volume basis in a cumulative particle size distribution, to the D50 , of 0.2 or more and 1.0 or less, and a ratio of a D90 , which is a 90% particle diameter on a volume basis in a cumulative particle size distribution, to the D50 , of 1.0 or more and 3.0 or less, The thickness is 1.5 mm or less.
  • Green sheet [20] The green sheet according to the above [19], having a width of 1 cm or more and a length of 1 cm or more in the major axis direction. [21] The green sheet according to [19] or [20] above, having a thickness of 0.003 mm or more and 0.7 mm or less. [22] A sintered body of the green sheet according to any one of [19] to [21] above.
  • Example 1 A spherical silica powder having a volume-based 50% particle diameter D50 of 150 nm in the cumulative particle size distribution, a volume-based 10% particle diameter D10 of 110 nm in the cumulative particle size distribution, and a volume-based 90% particle diameter D90 of 270 nm in the cumulative particle size distribution was prepared, and propylene glycol monomethyl ether acetate was weighed out as an organic solvent in a ratio of 45 mass %, 2-butanol 30 mass %, and isopropyl alcohol 25 mass %, and a dispersant (a polymer dispersant having an ammonium base on the polymer side chain) was added thereto in an amount of 8 mass % relative to the silica powder, and a plasticizer (a commercially available triethylene glycol diester-based product) was added thereto in an amount of 7.5 mass % relative to the silica powder, and the mixture was mixed in a ball mill using zirconia media.
  • a dispersant a polymer dispersant
  • a solution containing resin 1 (a low molecular weight acrylic resin binder) and resin 2 (a high molecular weight acrylic resin binder) in a mass ratio of 95:5 was prepared as a binder with a component ratio of 25% by mass, and was weighed out to be 30% by mass relative to the silica powder, and added to the ball mill container.
  • the solvent of the binder was the same as the solvent composition of the dispersion slurry.
  • the amount of silica in the inorganic powder of the obtained slurry was 100% by mass.
  • the volumetric solid content of the inorganic powder containing the silica powder in the obtained slurry was 17.2 vol%.
  • the amount of Zr and Al was adjusted with raw materials to make up for the shortage, taking into account the amount of contamination from the process such as ball materials during mixing.
  • the obtained slurry was degassed under reduced pressure and coated on a PET film by a doctor blade method to form a green sheet having a thickness of 0.40 mm.
  • the volume solid content of the inorganic powder including the silica powder in the obtained green sheet was 56 vol %.
  • the obtained green sheet was dried at 60° C. for 4 hours and cut to a width of 40 mm and a length of 40 mm using a disk cutter to obtain a sheet molded body.
  • the sheet molded body was peeled off from the PET film and degreased at 550° C.
  • Example 14 the raw materials were adjusted so that the Al content was 8100 ppm by mass, and as a result, cracks were observed.
  • Example 15 the raw materials were adjusted so that the Zr content was 8000 ppm by mass, and as a result, cracks were observed.
  • Example 16 Sintered bodies were produced in the same manner as in Example 1, except for the points shown in Tables 1 and 2 and the fact that a solution containing a polyvinyl butyral resin with a component ratio of 25 mass % was used as the binder.
  • Sheet molded body 11 Sintering setter 11a Upper sintering setter 11b Lower sintering setter

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  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
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Abstract

La présente invention concerne un procédé de production d'un corps fritté, le procédé comprenant : la préparation d'une composition de bouillie qui contient une poudre inorganique dans laquelle la proportion d'une poudre de silice est supérieure à 85% en masse ; le moulage de la composition de bouillie en une feuille verte qui a une épaisseur de 1,5 mm ou moins ; la découpe de la feuille verte à une taille arbitraire de façon à obtenir un corps moulé en feuille ; et le frittage du corps moulé en feuille de façon à obtenir un corps fritté. Dans ce procédé de production d'un corps fritté, l'épaisseur du corps fritté est de 0,003 mm à 1 mm inclus.
PCT/JP2024/018301 2023-06-09 2024-05-17 Procédé de production d'un corps fritté, feuille verte et corps fritté Pending WO2024252896A1 (fr)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01320269A (ja) * 1988-06-20 1989-12-26 Fujitsu Ltd 窒化アルミニウム焼結体の製造方法
JPH0254597A (ja) * 1988-08-18 1990-02-23 Fujitsu Ltd 窒化アルミニウム基板の製造方法
JPH03187933A (ja) * 1989-12-15 1991-08-15 Toshiba Ceramics Co Ltd シリカガラスの製造方法
JPH0832238A (ja) * 1994-05-13 1996-02-02 Nec Corp 多層配線基板とその製造方法、及びそれに用いるシリカ焼結体の製造方法
JPH09100154A (ja) * 1995-07-25 1997-04-15 Nec Corp 低温焼結石英基板の製造方法
JP2004075399A (ja) * 2002-08-09 2004-03-11 Ngk Insulators Ltd セラミックス電子部品焼成用セッター
JP2008001558A (ja) * 2006-06-22 2008-01-10 Sumitomo Metal Electronics Devices Inc 窒化アルミニウム成形体の焼成方法と焼成用治具
JP2009120444A (ja) * 2007-11-14 2009-06-04 Kyushu Univ ガラス用グリーンシート及びこのガラス用グリーンシートを焼成してなるガラス
WO2022039072A1 (fr) * 2020-08-21 2022-02-24 Ａｇｃ株式会社 Verre chimiquement renforcé et verre cristallisé et procédés de fabrication associés
WO2023248932A1 (fr) * 2022-06-24 2023-12-28 Ａｇｃ株式会社 Feuille verte et comprimé fritté, et procédés de production de ceux-ci

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01320269A (ja) * 1988-06-20 1989-12-26 Fujitsu Ltd 窒化アルミニウム焼結体の製造方法
JPH0254597A (ja) * 1988-08-18 1990-02-23 Fujitsu Ltd 窒化アルミニウム基板の製造方法
JPH03187933A (ja) * 1989-12-15 1991-08-15 Toshiba Ceramics Co Ltd シリカガラスの製造方法
JPH0832238A (ja) * 1994-05-13 1996-02-02 Nec Corp 多層配線基板とその製造方法、及びそれに用いるシリカ焼結体の製造方法
JPH09100154A (ja) * 1995-07-25 1997-04-15 Nec Corp 低温焼結石英基板の製造方法
JP2004075399A (ja) * 2002-08-09 2004-03-11 Ngk Insulators Ltd セラミックス電子部品焼成用セッター
JP2008001558A (ja) * 2006-06-22 2008-01-10 Sumitomo Metal Electronics Devices Inc 窒化アルミニウム成形体の焼成方法と焼成用治具
JP2009120444A (ja) * 2007-11-14 2009-06-04 Kyushu Univ ガラス用グリーンシート及びこのガラス用グリーンシートを焼成してなるガラス
WO2022039072A1 (fr) * 2020-08-21 2022-02-24 Ａｇｃ株式会社 Verre chimiquement renforcé et verre cristallisé et procédés de fabrication associés
WO2023248932A1 (fr) * 2022-06-24 2023-12-28 Ａｇｃ株式会社 Feuille verte et comprimé fritté, et procédés de production de ceux-ci

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