JP2001348288A - Particle-dispersed silicon material and method of producing the same - Google Patents

Particle-dispersed silicon material and method of producing the same

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Publication number
JP2001348288A
JP2001348288A JP2000166972A JP2000166972A JP2001348288A JP 2001348288 A JP2001348288 A JP 2001348288A JP 2000166972 A JP2000166972 A JP 2000166972A JP 2000166972 A JP2000166972 A JP 2000166972A JP 2001348288 A JP2001348288 A JP 2001348288A
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JP
Japan
Prior art keywords
silicon
dispersed
particle
silicon material
pressure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2000166972A
Other languages
Japanese (ja)
Other versions
JP3830733B2 (en
Inventor
Akiko Suyama
章子 須山
Yoshiyasu Ito
義康 伊藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toshiba Corp
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Toshiba Corp
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Priority to JP2000166972A priority Critical patent/JP3830733B2/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5093—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with elements other than metals or carbon
    • C04B41/5096—Silicon

Abstract

PROBLEM TO BE SOLVED: To obtain a silicon material having reliability and durability by improving the mechanical characteristics of a ceramic or MMC. SOLUTION: A reinforcing base material is obtained by using silicon carbide having an average particle size of 0.1 to 10 μm. The particle-dispersed silicon material is composed of the reinforcing base material and a silicon matrix infiltrated into the reinforcing base material.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明はシリコン材料の機械
的特性である強度、靭性を向上する材料に係り、特に、
高温域で用いられるガスタービンの構造部品、あるい
は、半導体部品に適用される粒子分散シリコン材料に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a material for improving strength and toughness which are mechanical properties of a silicon material.
The present invention relates to a particle-dispersed silicon material applied to a structural component of a gas turbine used in a high temperature range or a semiconductor component.

【０００２】[0002]

【従来の技術】一般にセラミックスの一つであるシリコ
ン材料は、金属材料に比べて、強度および靭性等の機械
的特性が低く、破壊しやすいことから耐久性の面で問題
がある。そのため、上述の技術分野等の製品歩留まりの
向上、高信頼性が要求される部品や製品へのシリコン材
料の適用を可能にするため、高強度化および高靭性化を
図ったシリコン材料が求められている。この材料とし
て、炭化ケイ素セラミックスや金属基複合材料（ＭＭ
Ｃ：Metal Matrix Composite）が検討され、特に高温域
で使用されるガスタービンの構造部材である燃焼器や、
半導体部品やその関連製品であるヒートシンク、製造治
具、ダミーウエハへの適用が期待されている。2. Description of the Related Art In general, a silicon material, which is one of ceramics, has low mechanical properties such as strength and toughness as compared with a metal material and is easily broken, and thus has a problem in durability. Therefore, in order to improve the product yield in the above-mentioned technical fields and to apply the silicon material to parts and products requiring high reliability, a silicon material with high strength and high toughness is required. ing. Such materials include silicon carbide ceramics and metal matrix composite materials (MM
C: Metal Matrix Composite) has been studied, and in particular, combustors that are structural members of gas turbines used in high-temperature regions,
It is expected to be applied to semiconductor components and related products such as heat sinks, manufacturing jigs, and dummy wafers.

【０００３】[0003]

【発明が解決しようとする課題】しかしながら、機械的
特性の低い既存のセラミックスやＭＭＣによる材料を適
用した場合は強度を確保することで部品が大きな形状と
なり、また、耐久性が低いためコスト高となる。コスト
減の観点から、機器およびシステム全体をコンパクトに
するため、機器を構成する部品等の材料特性の見直しが
要請されているのが最近の傾向でもある。However, when using existing ceramics or MMC materials having low mechanical properties, parts are formed in a large shape by securing strength, and cost is increased due to low durability. Become. From the viewpoint of cost reduction, it is a recent trend that a review of the material characteristics of components and the like constituting the device is demanded in order to make the device and the whole system compact.

【０００４】本発明の目的は、セラミックスやＭＭＣの
機械的特性を向上することにより、信頼性と耐久性を確
保したシリコン材料を得ることにある。[0004] It is an object of the present invention to obtain a silicon material having improved reliability and durability by improving the mechanical properties of ceramics and MMC.

【０００５】[0005]

【課題を解決するための手段】本発明の粒子分散シリコ
ン材料は、平均粒径０．１〜１０μｍの炭化ケイ素を用
いることにより得られた強化素材と、この強化素材に溶
浸されたシリコンマトリックスとからなることを特徴と
する。The particle-dispersed silicon material of the present invention comprises a reinforcing material obtained by using silicon carbide having an average particle size of 0.1 to 10 μm, and a silicon matrix infiltrated into the reinforcing material. And characterized by the following.

【０００６】本発明の粒子分散シリコン材料の製造方法
は、平均粒径０．１〜１０μｍの炭化ケイ素粉末と平均
粒径０．０３〜３μｍのカーボン粉末とを溶媒に分散す
ることによりのスラリーを得る第一工程と、このスラリ
ーを０．１〜１０ＭＰａの圧力で加圧した後に乾燥させ
る第二工程と、ここで乾燥した成形体を６００〜８００
℃の不活性な雰囲気中で一定時間保持し成形助剤を脱脂
する第三工程と、ここで脱脂した成形体を減圧下または
不活性な雰囲気中で１４００℃以上に加熱し、これにシ
リコンを溶浸させる第四工程とを備えたことを特徴とす
る。The method for producing a particle-dispersed silicon material according to the present invention is characterized in that a slurry obtained by dispersing silicon carbide powder having an average particle diameter of 0.1 to 10 μm and carbon powder having an average particle diameter of 0.03 to 3 μm in a solvent is used. A first step of obtaining the slurry; a second step of drying the slurry after pressurizing the slurry at a pressure of 0.1 to 10 MPa;
A third step of degreasing the molding aid by holding the molding aid in an inert atmosphere at a constant temperature of 1 ° C., and heating the degreased molded body to 1400 ° C. or more under reduced pressure or in an inert atmosphere, and silicon is added thereto. And a fourth step of infiltrating.

【０００７】また、本発明の粒子分散シリコン材料は、
上述の製法により作製された粒子分散シリコン材料であ
って、分散粒子である炭化ケイ素の含有量を含浸させる
シリコンに対して５０〜９５重量％としたことを特徴と
する。[0007] The particle-dispersed silicon material of the present invention comprises:
A particle-dispersed silicon material produced by the above-mentioned method, wherein the content of silicon carbide as dispersed particles is set to 50 to 95% by weight based on silicon to be impregnated.

【０００８】まず、第二工程でスラリーを０．１〜１０
ＭＰａの圧力で加圧するのは大きく複雑な形状のものま
で均質に高速に成形するためでである。そして、脱脂し
た成形体の加熱温度を１４００℃以上としたのは、シリ
コンが溶融し成形体に均質に溶浸できるためである。First, in the second step, the slurry is 0.1 to 10%.
The reason why the pressure is applied at the pressure of MPa is to uniformly and rapidly form a large and complicated shape. The reason why the heating temperature of the degreased molded body is set to 1400 ° C. or higher is that silicon can be melted and uniformly infiltrated into the molded body.

【０００９】次に、分散粒子である炭化ケイ素の含有量
が５０重量％未満である場合は、十分な機械的特性が得
られず、逆に、９５重量％を超える場合は機械的特性が
向上する反面、製造プロセス上、粒子の適正な分散が望
めないことから所定の値の範囲にしている。この範囲と
することで、粒子間の平均距離が２μｍという概ね均質
に分散したシリコン材料を得ることができる。Next, when the content of the silicon carbide particles as the dispersed particles is less than 50% by weight, sufficient mechanical properties cannot be obtained. Conversely, when the content exceeds 95% by weight, the mechanical properties are improved. On the other hand, since the dispersion of the particles cannot be expected due to the production process, the range is set to a predetermined value. Within this range, it is possible to obtain a substantially homogeneously dispersed silicon material having an average distance between particles of 2 μm.

【００１０】一方、分散粒子の平均粒径が０．１μｍ未
満である場合は、製造プロセスにおいて、分散粒子が凝
集し易いため適正な分散が望めず、逆に、１０μｍを超
えると機械的特性である強度、靭性の向上が十分に発現
しないことから所定の値の範囲にしている。この範囲と
することで、粒子間の平均距離が２μｍという概ね均質
に分散したシリコン材料を得ることができる。On the other hand, when the average particle size of the dispersed particles is less than 0.1 μm, proper dispersion cannot be expected because the dispersed particles are easily aggregated in the manufacturing process. Since a certain improvement in strength and toughness is not sufficiently exhibited, the range is set to a predetermined value. Within this range, it is possible to obtain a substantially homogeneously dispersed silicon material having an average distance between particles of 2 μm.

【００１１】また、本発明による粒子分散シリコン材料
は、シリコンおよび炭化ケイ素に含有する不純物の量を
０．００１〜２重量％以下の範囲とする。これは、不純
物の含有量が０．００１重量％未満である場合、分散粒
子である炭化ケイ素とマトリックスのシリコンとのぬれ
性が向上し、安定した機械的特性が得られる。逆に、２
重量％を超えると機械的特性等の低下をきたす。In the particle-dispersed silicon material according to the present invention, the amount of impurities contained in silicon and silicon carbide is in the range of 0.001 to 2% by weight or less. When the content of the impurities is less than 0.001% by weight, the wettability between silicon carbide as the dispersed particles and silicon as the matrix is improved, and stable mechanical properties are obtained. Conversely, 2
If the content exceeds% by weight, mechanical properties and the like will be reduced.

【００１２】さらにまた、本発明による粒子分散シリコ
ン材料は、開気孔率を３％以下とする。これは、開気孔
率が３％を超えると、強度のバラツキが生じるためであ
り、３％以下とすることで、強度低下の原因となる欠陥
の数や大きさを減らすことで、所望の機械的特性を備え
たシリコン材料を得ることができる。Further, the particle-dispersed silicon material according to the present invention has an open porosity of 3% or less. This is because if the open porosity exceeds 3%, there is a variation in strength. By setting the porosity to 3% or less, the number and size of defects that cause a decrease in strength can be reduced, and the desired mechanical strength can be reduced. A silicon material having a characteristic characteristic can be obtained.

【００１３】ここで、分散粒子間の平均距離の測定は以
下のように行う。得られたシリコン材料を減圧下１８７
３Ｋに加熱してシリコンを除去した後、水銀圧入法を用
いて気孔径を測定し、平均気孔径を分散粒子間の平均距
離とした。気孔径（Ｄ）は、気孔に水銀を圧入する圧力
Ｐ、水銀と試料の接触角（θ）を１３０゜、水銀の表面
張力（γ）を０．４８Ｎ／ｍとして式（１）を用いて計
算した。Here, the average distance between the dispersed particles is measured as follows. The obtained silicon material was removed under reduced pressure for 187 minutes.
After heating to 3K to remove silicon, the pore size was measured using a mercury intrusion method, and the average pore size was taken as the average distance between dispersed particles. The pore diameter (D) is obtained by using the formula (1), where the pressure P at which mercury is injected into the pores, the contact angle (θ) between mercury and the sample is 130 °, and the surface tension (γ) of mercury is 0.48 N / m. Calculated.

【００１４】〔数１〕 Ｄ＝−４・γ・ｃｏｓθ／Ｐ (１) そして、全気孔体積のｄ５０値の気孔径を平均気孔径と
した。[Equation 1] D = −4 · γ · cos θ / P (1) Then, the pore diameter of the d50 value of the total pore volume was defined as the average pore diameter.

【００１５】[0015]

【発明の実施の形態】以下、本発明の実施の形態につい
て図面を参照して説明する。図１は本発明に係る粒子分
散シリコン材料１の組成を拡大して示す断面図である。
表１に、以下に示す実施例および比較例の一覧を示す。Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an enlarged sectional view showing the composition of the particle-dispersed silicon material 1 according to the present invention.
Table 1 shows a list of the following examples and comparative examples.

【００１６】［実施例１〜４］平均粒径１〜３μｍの炭
化ケイ素粉末１００重量部（昭和電工（株）製グリーン
デンシックＧＣ粉末）とカーボン粉末１０〜５０重量部
（三菱化成（株）製カーボンブラック）を、溶媒中に分
散して、低粘度のスラリーを作製した。次に、このスラ
リーを圧力鋳込み成形機を用いて、成形型に加圧しなが
ら充填した。成形圧力を０.１〜１０ＭＰａの間で変化
させて、成形体密度の異なる４種類の成形体を作製し
た。さらに自然乾燥した後に、不活性な雰囲気である窒
素ガス中、温度６００〜８００℃で２時間保持し、成形
助剤として添加した有機物を脱脂した後に、減圧下また
は不活性雰囲気中において温度１４００℃以上に加熱
し、成形体中にシリコンを溶浸させた。こうして得られ
た焼結体は表面加工を施して、それぞれ実施例１〜４と
して粒子分散強化シリコン材料１を製造した。この実施
例１〜４の材料組成比（シリコン：分散粒子）は、実施
例１が４５：５５〜５０：５０、実施例２が３０：７０
〜３５：６５、実施例３が１５：８５〜２０：８０、実
施例４は５：９５〜１０：９０である。この材料組成比
は、出発原料に添加するカーボン粉末の量と、スラリー
から作製した成形体密度によって、調整可能である。Examples 1 to 4 100 parts by weight of silicon carbide powder having an average particle diameter of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (Mitsubishi Chemical Corporation) Carbon black) was dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. By changing the molding pressure between 0.1 and 10 MPa, four types of molded bodies having different molded body densities were produced. Further, after natural drying, the mixture is kept at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas which is an inert atmosphere, and after degreased organic substances added as a molding aid, the temperature is reduced to 1400 ° C. under reduced pressure or in an inert atmosphere. The above heating was performed to infiltrate silicon into the molded body. The sintered body thus obtained was subjected to surface processing to produce a particle dispersion strengthened silicon material 1 as Examples 1 to 4, respectively. The material composition ratio (silicon: dispersed particles) of Examples 1 to 4 was 45:55 to 50:50 in Example 1, and 30:70 in Example 2.
35:65, Example 3 is 15:85 to 20:80, and Example 4 is 5:95 to 10:90. This material composition ratio can be adjusted by the amount of the carbon powder added to the starting material and the density of the compact formed from the slurry.

【００１７】［実施例５〜６］平均粒径０.２〜０.５μ
ｍ、または６〜９μｍの炭化ケイ素粉末１００重量部
（昭和電工（株）製グリーンデンシックＧＣ粉末）とカ
ーボン粉末１０〜５０重量部（三菱化成（株）製カーボ
ンブラック）を、溶媒中に分散して、低粘度のスラリー
を作製した。次に、このスラリーを圧力鋳込み成形機を
用いて、成形型に加圧しながら充填した。成形圧力を
０.１〜１０ＭＰａの間で変化させて、成形体密度の異
なる２種類の成形体を作製した。さらに自然乾燥した後
に、窒素ガス雰囲気中温度６００〜８００℃で２時間保
持し、成形助剤として添加した有機物を脱脂した後に、
減圧下または不活性雰囲気中において温度１４００℃以
上に加熱し、成形体中にシリコンを溶浸させた。こうし
て得られた焼結体は表面加工を施し、それぞれ実施例５
〜６として粒子分散シリコン材料１を製造した。[Examples 5 and 6] Average particle size 0.2 to 0.5 µm
m or 6 to 9 μm of silicon carbide powder (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (Mitsubishi Chemical Corporation carbon black) are dispersed in a solvent. Thus, a slurry having a low viscosity was produced. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. By changing the molding pressure between 0.1 and 10 MPa, two types of molded bodies having different molded body densities were produced. After further air drying, the mixture was held at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas atmosphere to degrease organic substances added as a molding aid.
Heating was performed at a temperature of 1400 ° C. or higher under reduced pressure or in an inert atmosphere to infiltrate silicon into the molded body. The sintered body thus obtained was subjected to a surface treatment, and the sintered body was obtained in Example 5
As No.-6, the particle-dispersed silicon material 1 was produced.

【００１８】［実施例７］平均粒径１〜３μｍの炭化ケ
イ素粉末１００重量部（昭和電工（株）製グリーンデン
シックＧＣ粉末）とカーボン粉末１０〜５０重量部（三
菱化成（株）製カーボンブラック）を酸洗いによる純化
処理をした後、溶媒中に分散して、低粘度のスラリーを
作製した。次に、このスラリーを圧力鋳込み成形機を用
いて、成形型に加圧しながら充填した。成形圧力は０.
１〜１０ＭＰａの間で、成形体を作製した。さらに自然
乾燥した後に、窒素ガス雰囲気中温度６００〜８００℃
で２時間保持し、成形助剤として添加した有機物を脱脂
した後に、塩素ガス雰囲気で加熱処理による純化処理を
施した。そして、減圧下または不活性雰囲気中において
温度１４００℃以上に加熱し、成形体中にシリコンを溶
浸させた。こうして得られた焼結体は表面加工を施し、
実施例７として粒子分散シリコン材料１を製造した。Example 7 100 parts by weight of silicon carbide powder having an average particle diameter of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (carbon manufactured by Mitsubishi Kasei KK) Black) was subjected to a purification treatment by pickling, and then dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. The molding pressure is 0.
A molded body was prepared at a pressure of 1 to 10 MPa. After further air drying, the temperature in a nitrogen gas atmosphere is 600 to 800 ° C.
For 2 hours, and degreased organic matter added as a molding aid, and then subjected to a purification treatment by a heat treatment in a chlorine gas atmosphere. Then, it was heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere to infiltrate the molded body with silicon. The sintered body thus obtained is subjected to surface processing,
Example 7 A particle-dispersed silicon material 1 was produced.

【００１９】［実施例８］平均粒径１〜３μｍの炭化ケ
イ素粉末１００重量部（昭和電工（株）製グリーンデン
シックＧＣ粉末）とカーボン粉末１０〜５０重量部（三
菱化成（株）製カーボンブラック）後、溶媒中に分散し
て、低粘度のスラリーを作製した。次に、このスラリー
を圧力鋳込み成形機を用いて、成形型に加圧しながら充
填した。成形圧力は０.１〜１０ＭＰａの間で、成形体
を作製した。さらに自然乾燥した後に、窒素ガス雰囲気
中温度６００〜８００℃で２時間保持し、成形助剤とし
て添加した有機物を脱脂した後に、減圧下または不活性
雰囲気中において温度１４００℃以上に加熱し、成形体
中にシリコン（実施例１〜４に用いたものより若干純度
の低いもの）を溶浸させた。こうして得られた焼結体は
表面加工を施し、実施例８として粒子分散シリコン材料
１を製造した。Example 8 100 parts by weight of silicon carbide powder having an average particle diameter of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (carbon manufactured by Mitsubishi Kasei KK) Black), and then dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. A molding was produced at a molding pressure of 0.1 to 10 MPa. After natural drying, the mixture was kept at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas atmosphere to degrease organic substances added as a molding aid, and then heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere to form The body was infiltrated with silicon (those having a slightly lower purity than those used in Examples 1 to 4). The sintered body thus obtained was subjected to surface processing, and as Example 8, a particle-dispersed silicon material 1 was produced.

【００２０】［比較例１〜２］平均粒径１〜３μｍの炭
化ケイ素粉末１００重量部（昭和電工（株）製グリーン
デンシックＧＣ粉末）とカーボン粉末１０〜５０重量部
（三菱化成（株）製カーボンブラック）を、溶媒中に分
散して、低粘度のスラリーを作製した。次に、このスラ
リーを圧力鋳込み成形機を用いて、成形型に加圧しなが
ら充填した。成形圧力を０.１〜１０ＭＰａの間で変化
させて、成形体密度の異なる２種類の成形体を作製し
た。さらに自然乾燥した後に、窒素ガス雰囲気中温度６
００〜８００℃で２時間保持し、成形助剤として添加し
た有機物を脱脂した後に、減圧下または不活性雰囲気中
において温度１４００℃以上に加熱し、成形体中に溶融
したシリコンを含浸させた。こうして得られた焼結体は
表面加工を施し、それぞれ比較例１〜２として粒子分散
シリコン材料を製造した。比較例１〜２の材料組成比
（シリコン：分散粒子）は、比較例１が５０：５０〜６
０：４０、比較例２が＜５：＞９５である。この材料組
成比は、出発原料に添加するカーボン粉末の量と、スラ
リーから作製した成形体密度によって、調整可能であ
る。特に、比較例２は出発原料として添加したカーボン
粉末が分散粒子へ転化せずにそのままの状態で残る場合
がある。Comparative Examples 1 and 2 100 parts by weight of silicon carbide powder having an average particle diameter of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (Mitsubishi Chemical Corporation) Carbon black) was dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. By changing the molding pressure between 0.1 and 10 MPa, two types of molded bodies having different molded body densities were produced. After air drying, the temperature in the nitrogen gas atmosphere
After holding at 00 to 800 ° C. for 2 hours to degrease organic substances added as a molding aid, the molded body was heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere to impregnate molten silicon into the molded body. The sintered body thus obtained was subjected to surface processing to produce particle-dispersed silicon materials as Comparative Examples 1 and 2, respectively. The material composition ratio (silicon: dispersed particles) of Comparative Examples 1 and 2 is 50:50 to 6 in Comparative Example 1.
0:40, Comparative Example 2 <5:> 95. This material composition ratio can be adjusted by the amount of the carbon powder added to the starting material and the density of the compact formed from the slurry. In particular, in Comparative Example 2, the carbon powder added as a starting material sometimes remains as it is without being converted into dispersed particles.

【００２１】［比較例３〜４］平均粒径２０μｍ、また
は４０μｍの炭化ケイ素粉末１００重量部（昭和電工
（株）製グリーンデンシックＧＣ粉末）とカーボン粉末
１０〜５０重量部（三菱化成（株）製カーボンブラッ
ク）を、溶媒中に分散して、低粘度のスラリーを作製し
た。次に、このスラリーを圧力鋳込み成形機を用いて、
成形型に加圧しながら充填した。成形圧力を０.１〜１
０ＭＰａの間で変化させて、成形体密度の異なる２種類
の成形体を作製した。さらに自然乾燥した後に、窒素ガ
ス雰囲気中温度６００〜８００℃で２時間保持し、成形
助剤として添加した有機物を脱脂した後に、減圧下また
は不活性雰囲気中において温度１４００℃以上に加熱
し、成形体中にシリコンを溶浸させた。こうして得られ
た焼結体は表面加工を施し、それぞれ比較例３〜４とし
て粒子分散シリコン材料を製造した。Comparative Examples 3 and 4 100 parts by weight of silicon carbide powder having an average particle diameter of 20 μm or 40 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (Mitsubishi Chemical Corporation) ) Produced carbon black) was dispersed in a solvent to prepare a low viscosity slurry. Next, using a pressure casting molding machine, this slurry,
The mold was filled under pressure. Molding pressure is 0.1 ~ 1
By changing the pressure between 0 MPa, two types of compacts having different compact densities were produced. After natural drying, the mixture was kept at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas atmosphere to degrease organic substances added as a molding aid, and then heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere to form Silicon was infiltrated into the body. The sintered body thus obtained was subjected to surface processing to produce particle-dispersed silicon materials as Comparative Examples 3 and 4, respectively.

【００２２】［比較例５］平均粒径１〜３μｍの炭化ケ
イ素粉末１００重量部（昭和電工（株）製グリーンデン
シックＧＣ粉末）とカーボン粉末１０〜５０重量部（三
菱化成（株）製カーボンブラック）を、溶媒中に分散し
て、低粘度のスラリーを作製した。次に、このスラリー
を圧力鋳込み成形機を用いて、成形型に加圧しながら充
填した。成形圧力は０.１〜１０ＭＰａの間で、成形体
を作製した。さらに自然乾燥した後に、窒素ガス雰囲気
中温度６００〜８００℃で２時間保持し、成形助剤とし
て添加した有機物を脱脂した後に、減圧下または不活性
雰囲気中において温度１４００℃以上に加熱し、成形体
中にシリコン（実施例８で用いたシリコンよりさらに純
度の低いもの）を溶浸させた。こうして得られた焼結体
は表面加工を施し、比較例５として粒子分散シリコン材
料を製造した。Comparative Example 5 100 parts by weight of silicon carbide powder having an average particle size of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (carbon manufactured by Mitsubishi Chemical Corporation) Black) was dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. A molding was produced at a molding pressure of 0.1 to 10 MPa. After natural drying, the mixture was kept at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas atmosphere to degrease organic substances added as a molding aid, and then heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere to form The body was infiltrated with silicon (which had a lower purity than the silicon used in Example 8). The sintered body thus obtained was subjected to surface processing to produce a particle-dispersed silicon material as Comparative Example 5.

【００２３】［比較例６］平均粒径１〜３μｍの炭化ケ
イ素粉末１００重量部（昭和電工（株）製グリーンデン
シックＧＣ粉末）とカーボン粉末１０〜５０重量部（三
菱化成（株）製カーボンブラック）と、シリコン粉末１
０〜１００重量部（（株）高純度化学研究所）を、溶媒
中に分散して、低粘度のスラリーを作製した。次に、こ
のスラリーを圧力鋳込み成形機を用いて、成形型に加圧
しながら充填した。成形圧力は０.１〜１０ＭＰａの間
で、成形体を作製した。さらに自然乾燥した後に、窒素
ガス雰囲気中温度６００〜８００℃で２時間保持し、成
形助剤として添加した有機物を脱脂した後に、減圧下ま
たは不活性雰囲気中において温度１４００℃以上に加熱
した。得られた焼結体は表面加工を施し、比較例６とし
て粒子分散シリコン材料を製造した。Comparative Example 6 100 parts by weight of silicon carbide powder having an average particle diameter of 1 to 3 μm (Green Densic GC powder manufactured by Showa Denko KK) and 10 to 50 parts by weight of carbon powder (carbon manufactured by Mitsubishi Chemical Corporation) Black) and silicon powder 1
0 to 100 parts by weight (manufactured by Kojundo Chemical Laboratory Co., Ltd.) was dispersed in a solvent to prepare a low-viscosity slurry. Next, this slurry was filled into a molding die while applying pressure using a pressure casting molding machine. A molding was produced at a molding pressure of 0.1 to 10 MPa. After air drying, the mixture was held at a temperature of 600 to 800 ° C. for 2 hours in a nitrogen gas atmosphere to degrease organic substances added as a molding aid, and then heated to a temperature of 1400 ° C. or more under reduced pressure or in an inert atmosphere. The obtained sintered body was subjected to surface processing to produce a particle-dispersed silicon material as Comparative Example 6.

【００２４】[0024]

【表１】 [Table 1]

【００２５】[0025]

【発明の効果】本発明によれば、シリコンマトリックス
に炭化ケイ素を適正に分散させ、セラミックスやＭＭＣ
の機械的特性を向上することにより、信頼性と耐久性を
確保した粒子分散シリコン材料が提供できる。According to the present invention, silicon carbide is appropriately dispersed in a silicon matrix, and ceramics and MMC are dispersed.
By improving the mechanical properties of the particles, it is possible to provide a particle-dispersed silicon material that ensures reliability and durability.

【図面の簡単な説明】[Brief description of the drawings]

【図１】本発明に係る粒子分散シリコン材料１の組成を
拡大して示す断面図である。FIG. 1 is an enlarged sectional view showing the composition of a particle-dispersed silicon material 1 according to the present invention.

【符号の説明】[Explanation of symbols]

１…粒子分散シリコン材料、２…シリコン、３…炭化ケ
イ素強化素材。1 ... particle-dispersed silicon material, 2 ... silicon, 3 ... silicon carbide reinforced material.

Claims (7)

【特許請求の範囲】[Claims] 【請求項１】 平均粒径０．１〜１０μｍの炭化ケイ素
を用いることにより得られた強化素材と、この強化素材
に溶浸されたシリコンマトリックスとからなることを特
徴とする粒子分散シリコン材料。1. A particle-dispersed silicon material comprising a reinforcing material obtained by using silicon carbide having an average particle size of 0.1 to 10 μm, and a silicon matrix infiltrated into the reinforcing material. 【請求項２】 請求項１に記載の粒子分散シリコン材料
であって、分散粒子である炭化ケイ素の含有量を含浸さ
せるシリコンに対して５０〜９５重量％としたことを特
徴とする粒子分散シリコン材料。2. The particle-dispersed silicon material according to claim 1, wherein the content of silicon carbide as the dispersed particles is 50 to 95% by weight based on silicon to be impregnated. material. 【請求項３】 請求項１に記載の粒子分散シリコン材料
であって、その室温における３点曲げ強度が５００〜１
３００ＭＰａであることを特徴とする粒子分散シリコン
材料。3. The particle-dispersed silicon material according to claim 1, wherein the three-point bending strength at room temperature is 500 to 1.
A particle-dispersed silicon material having a pressure of 300 MPa. 【請求項４】 請求項１に記載の粒子分散シリコン材料
であって、その室温における熱伝導率が１００〜２００
Ｗ／ｍ・Ｋであることを特徴とする粒子分散シリコン材
料。4. The particle-dispersed silicon material according to claim 1, which has a thermal conductivity of 100 to 200 at room temperature.
A particle-dispersed silicon material having a W / m · K ratio. 【請求項５】 請求項１に記載の粒子分散シリコン材料
であって、その破壊靭性値が２〜４ＭＰａｍ1/2である
ことを特徴とする粒子分散シリコン材料。5. The particle-dispersed silicon material according to claim 1, wherein the fracture toughness value is 2 to 4 MPam 1/2 . 【請求項６】 請求項１に記載の製法により作製された
粒子分散シリコン材料であって、そのビッカース硬さ
（Ｈｖ）が１３００〜２０００であることを特徴とする
粒子分散シリコン材料。6. A particle-dispersed silicon material produced by the method according to claim 1, wherein the Vickers hardness (Hv) is 1300 to 2000. 【請求項７】 平均粒径０．１〜１０μｍの炭化ケイ素
粉末と平均粒径０．０３〜３μｍのカーボン粉末とを水
または有機溶媒に分散することによりスラリーを得る第
一工程と、このスラリーを０．１〜１０ＭＰａの圧力で
加圧した後に乾燥させる第二工程と、ここで乾燥した成
形体を６００〜８００℃の不活性な雰囲気中で一定時間
保持して脱脂する第三工程と、ここで脱脂した成形体を
減圧下または不活性な雰囲気中で１４００℃以上に加熱
して、これにシリコンを溶浸させる第四工程とを備えた
ことを特徴とする粒子分散シリコン材料の製造方法。7. A first step of obtaining a slurry by dispersing a silicon carbide powder having an average particle size of 0.1 to 10 μm and a carbon powder having an average particle size of 0.03 to 3 μm in water or an organic solvent; A second step of drying after pressing at a pressure of 0.1 to 10 MPa, and a third step of degreasing by holding the dried body here for a certain time in an inert atmosphere at 600 to 800 ° C. Heating the degreased molded body to 1400 ° C. or more under reduced pressure or in an inert atmosphere, and infiltrating silicon into the molded body. .
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