WO2014208460A1 - 炭化ケイ素粉体 - Google Patents
炭化ケイ素粉体 Download PDFInfo
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- WO2014208460A1 WO2014208460A1 PCT/JP2014/066404 JP2014066404W WO2014208460A1 WO 2014208460 A1 WO2014208460 A1 WO 2014208460A1 JP 2014066404 W JP2014066404 W JP 2014066404W WO 2014208460 A1 WO2014208460 A1 WO 2014208460A1
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- silicon carbide
- carbide powder
- particle size
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- silicon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/977—Preparation from organic compounds containing silicon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/575—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- 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
- C04B2235/5463—Particle size distributions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Definitions
- the present invention relates to silicon carbide powder.
- a silicon source that is liquid at room temperature specifically, ethyl silicate
- a carbon source that is liquid at room temperature specifically, a phenol resin
- a catalyst that specifically dissolves the carbon source specifically, maleic acid
- the content of sulfur contained in the silicon carbide powder is smaller than in the case where toluenesulfonic acid is used as the catalyst. Therefore, by using maleic acid as a catalyst, a silicon carbide powder suitable for the semiconductor field in which sulfur is an impurity can be produced.
- the pulverized silicon carbide powder (hereinafter, pulverized powder) is accommodated in a sintered body mold, and the pulverized powder accommodated in the sintered body mold is sintered. By doing so, a silicon carbide sintered body is manufactured.
- a silicon carbide sintered body As the silicon carbide sintered body, a high-strength silicon carbide sintered body is required.
- the present invention has been made to solve the above-described problems, and an object thereof is to provide a silicon carbide powder suitable for producing a high-strength silicon carbide sintered body.
- the ratio of the carbon contained in the mixture composed of the silicon source, the carbon source and the catalyst to the silicon contained in the mixture is 2.5 or more in molar ratio.
- the average particle size of the silicon carbide powder is 10 ⁇ m or more and 25 ⁇ m or less.
- the particle size when the particle size reaches 90% is greater than 25 ⁇ m and 50 ⁇ m or less.
- the silicon source is methyl silicate.
- a silicon carbide powder suitable for producing a high-strength silicon carbide sintered body can be provided.
- FIG. 1 is a flowchart showing a method for producing silicon carbide powder according to the first embodiment.
- FIG. 2 is a view showing a particle size distribution of the silicon carbide powder according to the first embodiment.
- FIG. 3 is a diagram showing experimental results.
- the ratio of the carbon contained in the mixture composed of the silicon source, the carbon source, and the catalyst to the silicon contained in the mixture is 2.5 or more in molar ratio.
- the average particle size of the silicon carbide powder is 10 ⁇ m or more and 25 ⁇ m or less.
- the ratio of carbon to silicon (C / Si) in the mixture is 2.5 or more in terms of molar ratio, and the average particle size of the silicon carbide powder is 10 ⁇ m or more and 25 ⁇ m or less.
- FIG. 1 is a flowchart showing a method for producing silicon carbide powder according to the first embodiment. As FIG. 1 shows, the manufacturing method of the silicon carbide powder which concerns on 1st Embodiment has mixing process S10 and baking process S20.
- a silicon source that is liquid at normal temperature, a carbon source that is liquid at normal temperature, and a catalyst (polymerization catalyst or crosslinking catalyst) that is solubilized in the carbon source are mixed to generate a mixture containing the silicon source, the carbon source, and the catalyst. It is a process.
- the silicon source examples include methyl silicate (that is, tetramethoxysilane).
- a monomer of methyl silicate may be used, or a polymer of methyl silicate (for example, a low molecular weight polymer (oligomer) of methyl silicate) may be used.
- the oligomer is a polymer having a degree of polymerization of about 2 to 15.
- methyl silicate it is preferable to use methyl silicate having a purity determined according to the use of the silicon carbide powder.
- the initial impurity content of methyl silicate is preferably 20 ppm or less, and more preferably 5 ppm or less.
- the carbon source is selected from coal tar pitch, phenol resin, furan resin, epoxy resin, phenoxy resin, monosaccharides such as glucose, oligosaccharides such as sucrose, polysaccharides such as cellulose and starch as the carbon source. It is preferable.
- the carbon source is liquid at room temperature.
- the carbon source may be a substance that dissolves in a solvent, and may be a substance that has thermoplasticity or heat solubility and is softened or liquefied by heating.
- a carbon source it is preferable to use the compound comprised only from a hydrogen atom and a carbon atom from a viewpoint of a residual carbon ratio, heat polymerization, or heat bridge
- the carbon source is preferably selected from phenol resin, polyvinyl alcohol, and polyvinyl acetate.
- the catalyst is preferably selected from, for example, saturated carboxylic acids, unsaturated carboxylic acids, dicarboxylic acids, and aromatic carboxylic acids.
- the catalyst is preferably selected from saturated aliphatic dicarboxylic acids, unsaturated aliphatic carboxylic acids, and derivatives thereof.
- the catalyst is preferably selected from maleic acid and derivatives thereof from the viewpoint of solubility in water.
- maleic acid derivatives include maleic anhydride.
- the catalyst is preferably a compound composed only of carbon atoms, hydrogen atoms and oxygen atoms. Since such a catalyst is composed of only carbon atoms, hydrogen atoms, and oxygen atoms, it does not contain sulfur like toluenesulfonic acid (C 7 H 8 O 3 S) used as a general-purpose catalyst in the prior art. Therefore, no harmful sulfur compounds are generated in the firing step.
- the catalyst preferably has at least good homogeneity so as to uniformly dissolve with the carbon source that reacts with the catalyst.
- the catalyst is preferably a compound containing a carboxyl group.
- “good homogeneity” means that the catalyst is uniformly diffused into the carbon source at the molecular level by mixing the carbon source and the catalyst.
- maleic acid has the necessary acid strength
- maleic acid contains both unsaturated bonds and carboxyl groups in the molecule, it has an affinity between the hydrophobic part and the hydrophilic part, and it is easy to mix the methyl silicate and the carbon source uniformly.
- maleic acid Since a strong exothermic reaction is not caused, the curing reaction is slow, and the reaction rate can be easily controlled by the amount of catalyst added. From such a viewpoint, it is preferable to use maleic acid as a catalyst.
- the ratio of carbon contained in the mixture of carbon source, methyl silicate and catalyst to silicon contained in the mixture (hereinafter referred to as C / Si) is preferably 2.5 or more in molar ratio.
- the C / Si of the mixture is adjusted by the amount of methyl silicate, carbon source and catalyst.
- the C / Si of the mixture can be defined by elemental analysis of a carbonized intermediate obtained by carbonizing the mixture.
- the compounding ratio of methyl silicate, carbon source and catalyst for example, when methyl silicate is 100% by weight, the carbon source is preferably 40 to 60% by weight and the catalyst is preferably 5 to 10% by weight.
- the catalyst may be mixed with methyl silicate and a carbon source in a state dissolved in a solvent not containing impurities.
- the catalyst may be used in a state saturated with a solvent such as water or acetone (saturated solution).
- a surfactant may be appropriately added to the mixture depending on the homogeneity of the mixture.
- the surfactant Span 20 or Tween 20 (trade name, manufactured by Kanto Chemical Co., Inc.) can be used.
- the addition amount of the surfactant is preferably 5 to 10% by weight when the mixture is 100% by weight.
- methyl silicate, a carbon source, and a catalyst are mixed. Specifically, it is preferable to add the catalyst after sufficiently stirring and mixing the methyl silicate and the carbon source.
- the mixture of methyl silicate, carbon source and catalyst solidifies. The mixture is preferably solidified in a gel form.
- the mixture may be heated after adding the catalyst to methyl silicate and carbon source.
- the mixture may be carbonized by heating the mixture at a temperature of 800 ° C. to 1000 ° C. for 30 to 120 minutes. Such heating is performed in a temperature range lower than that in the firing step S20 and should be considered as pretreatment.
- Firing step S20 is a step of producing silicon carbide powder by heating a mixture of methyl silicate, a carbon source and a catalyst in a non-oxidizing atmosphere.
- silicon carbide powder can be obtained by heating the mixture produced by the mixing step S10 at 1350 ° C. to 2000 ° C. for about 30 minutes to 3 hours in an argon atmosphere.
- Non-oxidizing atmosphere means an atmosphere in which no oxidizing gas exists.
- the non-oxidizing atmosphere may be an inert atmosphere (a rare gas such as helium or argon, nitrogen, or the like) or a vacuum atmosphere.
- the carbon contained in the mixture becomes a reducing agent, and a reaction of “SiO 2 + C ⁇ SiC” occurs.
- the decarburization treatment may be performed by heating the silicon carbide powder in an atmospheric furnace.
- the heating temperature of the silicon carbide powder in the decarburization process is 700 ° C., for example.
- the average particle diameter of the silicon carbide powder is 10 ⁇ m or more and 25 ⁇ m or less.
- the heating temperature and the heating time are determined so that the average particle diameter of the silicon carbide powder is 10 ⁇ m or more and 25 ⁇ m or less.
- FIG. 2 is a diagram showing the particle size distribution of the silicon carbide powder.
- the vertical axis represents weight
- the horizontal axis represents particle size.
- the “average particle size” is the particle size (D50) when the particle size distribution of the silicon carbide powder reaches the weight of 50% of the whole by accumulating from the smaller particle size. .
- the particle size (D10) when the particle size is accumulated from the smaller one and reaches the weight of 10% of the whole is the first particle size, which is 90% of the whole.
- the particle size (D90) when reaching weight is the second particle size.
- the second particle diameter when the particle diameter reaches 90% is greater than 25 ⁇ m and 50 ⁇ m or less.
- the upper limit of the second particle size is preferably smaller than 40 ⁇ m.
- the particle size distribution of the silicon carbide powder can be obtained by sieving the silicon carbide powder using a plurality of types of sieves.
- C / Si of a mixture is 2.5 or more by molar ratio, and the average particle diameter of silicon carbide powder is 10 micrometers or more and 25 micrometers or less, and manufactures a high intensity
- “Sinterability” is an evaluation related to the sintering of the sample, “ ⁇ ” indicates that the entire sample was sintered satisfactorily, and “ ⁇ ” indicates that only a part of the sample was sintered. The “x” indicates that the sample was hardly sintered. “Density” is an evaluation related to the density of the sample after sintering. “Visual confirmation result” is an evaluation related to chipping generated in the polishing process, “ ⁇ ” indicates that no chipping was observed, and “ ⁇ ” indicates that almost no chipping was observed. “X” indicates that chipping was observed. Note that “ ⁇ ” indicates that the sample could not be evaluated because it was not sintered.
- Example 1-3 where C / Si of the mixture is 2.5 or more in molar ratio and the particle size (D50), that is, the average particle size is 10 ⁇ m or more and 25 ⁇ m or less, the polishing step It was confirmed that a high-strength silicon carbide sintered body can be produced by using the silicon carbide powder according to Example 1-3.
- Example 1-3 in which the mixture had a C / Si molar ratio of 2.5 or more and a particle size (D90) of more than 25 ⁇ m and 50 ⁇ m or less, almost no chipping was observed in the polishing step. It was confirmed that a high-strength silicon carbide sintered body can be produced by using the silicon carbide powder according to Example 1-3. Further, it was confirmed that in Examples 2 and 3 in which the particle size (D90) was larger than 25 ⁇ m and smaller than 40 ⁇ m, chipping was further reduced as compared with Example 1.
- a silicon carbide powder suitable for producing a high-strength silicon carbide sintered body can be provided.
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Abstract
Description
実施形態に係る炭化ケイ素粉体において、ケイ素源、炭素源及び触媒によって構成される混合物に含まれる炭素と前記混合物に含まれるケイ素との比率はモル比で2.5以上である。炭化ケイ素粉体の平均粒径は10μm以上25μm以下である。
実施形態では、混合物の炭素とケイ素との比率(C/Si)がモル比で2.5以上であり、炭化ケイ素粉体の平均粒径が10μm以上25μm以下であることによって、高強度の炭化ケイ素焼結体を製造するための炭化ケイ素粉体が得られる。
(炭化ケイ素粉体の製造方法)
第1実施形態に係る炭化ケイ素粉体の製造方法について説明する。図1は、第1実施形態に係る炭化ケイ素粉体の製造方法を示すフロー図である。図1に示されるように、第1実施形態に係る炭化ケイ素粉体の製造方法は、混合工程S10と焼成工程S20とを有する。
混合工程S10は、常温で液状のケイ素源と常温で液状の炭素源と炭素源に溶化する触媒(重合触媒又は架橋触媒)とを混合し、ケイ素源、炭素源及び触媒を含む混合物を生成する工程である。
焼成工程S20は、非酸化雰囲気下において、メチルシリケート、炭素源及び触媒の混合物を加熱することによって、炭化ケイ素粉体を生成する工程である。例えば、アルゴン雰囲気中において、1350℃~2000℃で、約30分~3時間に亘って、混合工程S10によって生成された混合物を加熱することによって、炭化ケイ素粉体が得られる。
第1実施形態では、混合物のC/Siがモル比で2.5以上であり、炭化ケイ素粉体の平均粒径が10μm以上25μm以下であることによって、高強度の炭化ケイ素焼結体を製造するための炭化ケイ素粉体が得られる。
以下において、評価結果について説明する。評価では、比較例1-4及び実施例1-3に係るサンプル(炭化ケイ素粉体)を準備した。これらのサンプルの組成及び粒径は、図3に示す通りである。また、評価では2280℃の温度条件、500kgf/cm2の圧力条件、9時間の時間条件において、これらのサンプルを焼結することによって、インゴッドを製造するとともに、インゴッドを研磨した。このように製造されたインゴッドについて、「焼結性」、「密度(g/cm3)」、「目視確認結果」について評価した。
本発明は上述した実施形態によって説明したが、この開示の一部をなす論述及び図面は、この発明を限定するものであると理解すべきではない。この開示から当業者には様々な代替実施形態、実施例及び運用技術が明らかとなろう。
Claims (3)
- ケイ素源、炭素源及び触媒によって構成される混合物に含まれる炭素と前記混合物に含まれるケイ素との比率がモル比で2.5以上であり、
炭化ケイ素粉体の平均粒径が10μm以上25μm以下であることを特徴とする炭化ケイ素粉体。 - 前記炭化ケイ素粉体の粒度分布において、粒径が小さい方から累積した場合において、粒径が90%に達するときの粒径が25μmよりも大きく50μm以下であることを特徴とする請求項1に記載の炭化ケイ素粉体。
- 前記ケイ素源がメチルシリケートであることを特徴とする請求項1に記載の炭化ケイ素粉体。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US14/900,800 US9630854B2 (en) | 2013-06-26 | 2014-06-20 | Silicon carbide powder |
JP2015524023A JP6423341B2 (ja) | 2013-06-26 | 2014-06-20 | 炭化ケイ素粉体の製造方法 |
EP14816624.2A EP3015427A4 (en) | 2013-06-26 | 2014-06-20 | silicon carbide powder |
CN201480035422.0A CN105324332B (zh) | 2013-06-26 | 2014-06-20 | 碳化硅粉体 |
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JP2013133921 | 2013-06-26 | ||
JP2013-133921 | 2013-06-26 |
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US (1) | US9630854B2 (ja) |
EP (1) | EP3015427A4 (ja) |
JP (1) | JP6423341B2 (ja) |
CN (1) | CN105324332B (ja) |
TW (1) | TWI555703B (ja) |
WO (1) | WO2014208460A1 (ja) |
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JP2021155236A (ja) * | 2020-03-25 | 2021-10-07 | 日本碍子株式会社 | 炭化珪素含有ハニカム構造体の製造方法 |
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DE102018127877A1 (de) * | 2018-11-08 | 2020-05-14 | Psc Technologies Gmbh | Präkursormaterial für die Herstellung siliciumcarbidhaltiger Materialien |
JP7442288B2 (ja) * | 2019-09-30 | 2024-03-04 | 株式会社フジミインコーポレーテッド | セラミックス粉末 |
US11685662B2 (en) * | 2020-06-17 | 2023-06-27 | Touchstone Research Laboratory, Ltd. | Coal based silicon carbide foam |
US11685661B2 (en) * | 2020-06-17 | 2023-06-27 | Touchstone Research Laboratory, Ltd. | Carbon foam based silicon carbide |
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JPH10120411A (ja) | 1996-08-26 | 1998-05-12 | Bridgestone Corp | 炭化ケイ素粉体の製造方法 |
JP2001130972A (ja) * | 1999-08-24 | 2001-05-15 | Bridgestone Corp | 炭化ケイ素粉末、グリーン体の製造方法、及び炭化ケイ素焼結体の製造方法 |
JP2009173501A (ja) | 2008-01-28 | 2009-08-06 | Bridgestone Corp | 炭化ケイ素単結晶製造用高純度炭化ケイ素粉体の製造方法及び炭化ケイ素単結晶 |
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US6251353B1 (en) * | 1996-08-26 | 2001-06-26 | Bridgestone Corporation | Production method of silicon carbide particles |
JP2000351614A (ja) * | 1999-06-10 | 2000-12-19 | Bridgestone Corp | 炭化ケイ素粉体、及びその製造方法 |
JP5630333B2 (ja) | 2011-03-08 | 2014-11-26 | 信越化学工業株式会社 | 易焼結性炭化ケイ素粉末及び炭化ケイ素セラミックス焼結体 |
JP2012240869A (ja) | 2011-05-18 | 2012-12-10 | Sumitomo Electric Ind Ltd | 炭化珪素粉末および炭化珪素粉末の製造方法 |
CN103060890B (zh) * | 2013-01-22 | 2015-07-01 | 华南理工大学 | 一种合成纳米碳化硅晶须的方法 |
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- 2014-06-20 EP EP14816624.2A patent/EP3015427A4/en not_active Ceased
- 2014-06-20 CN CN201480035422.0A patent/CN105324332B/zh not_active Expired - Fee Related
- 2014-06-20 US US14/900,800 patent/US9630854B2/en not_active Expired - Fee Related
- 2014-06-20 WO PCT/JP2014/066404 patent/WO2014208460A1/ja active Application Filing
- 2014-06-20 JP JP2015524023A patent/JP6423341B2/ja not_active Expired - Fee Related
- 2014-06-24 TW TW103121648A patent/TWI555703B/zh not_active IP Right Cessation
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JPH10120411A (ja) | 1996-08-26 | 1998-05-12 | Bridgestone Corp | 炭化ケイ素粉体の製造方法 |
JP2001130972A (ja) * | 1999-08-24 | 2001-05-15 | Bridgestone Corp | 炭化ケイ素粉末、グリーン体の製造方法、及び炭化ケイ素焼結体の製造方法 |
JP2009173501A (ja) | 2008-01-28 | 2009-08-06 | Bridgestone Corp | 炭化ケイ素単結晶製造用高純度炭化ケイ素粉体の製造方法及び炭化ケイ素単結晶 |
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Cited By (2)
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JP2021155236A (ja) * | 2020-03-25 | 2021-10-07 | 日本碍子株式会社 | 炭化珪素含有ハニカム構造体の製造方法 |
JP7153684B2 (ja) | 2020-03-25 | 2022-10-14 | 日本碍子株式会社 | 炭化珪素含有ハニカム構造体の製造方法 |
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TWI555703B (zh) | 2016-11-01 |
US20160137513A1 (en) | 2016-05-19 |
US9630854B2 (en) | 2017-04-25 |
EP3015427A1 (en) | 2016-05-04 |
EP3015427A4 (en) | 2016-05-04 |
JPWO2014208460A1 (ja) | 2017-02-23 |
TW201500279A (zh) | 2015-01-01 |
JP6423341B2 (ja) | 2018-11-14 |
CN105324332B (zh) | 2018-08-03 |
CN105324332A (zh) | 2016-02-10 |
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