WO2002098819A1 - Procede de production d'un materiau composite au carbure de silicium sic renforce de fibres sic - Google Patents

Procede de production d'un materiau composite au carbure de silicium sic renforce de fibres sic Download PDF

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Publication number
WO2002098819A1
WO2002098819A1 PCT/JP2001/009365 JP0109365W WO02098819A1 WO 2002098819 A1 WO2002098819 A1 WO 2002098819A1 JP 0109365 W JP0109365 W JP 0109365W WO 02098819 A1 WO02098819 A1 WO 02098819A1
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Prior art keywords
sic
sic fiber
composite material
fiber
slurry
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PCT/JP2001/009365
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English (en)
French (fr)
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WO2002098819A8 (fr
Inventor
Akira Kohyama
Yutai Katoh
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Japan Science And Technology Corporation
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Priority to CA002444963A priority Critical patent/CA2444963C/en
Priority to EP01980904A priority patent/EP1391442B1/en
Priority to US10/478,797 priority patent/US7318906B2/en
Priority to DE60141985T priority patent/DE60141985D1/de
Publication of WO2002098819A1 publication Critical patent/WO2002098819A1/ja
Publication of WO2002098819A8 publication Critical patent/WO2002098819A8/ja

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Definitions

  • the present invention is suitable as a structural material that is subjected to a high heat load and exposed to a harsh environment, such as power generation equipment, aerospace equipment, nuclear power and nuclear fusion equipment.
  • the present invention relates to a method for producing a SiC composite material. Background art
  • Structural materials used in aviation 'space equipment, nuclear power' nuclear fusion facilities, power generation facilities using fossil fuels, etc. are exposed to harsh environments subject to high heat loads.
  • Materials used in such environments include SiC, which has excellent heat resistance, chemical stability, and mechanical properties.
  • Si 3 N4, etc. various ceramic materials have been developed. Ceramic materials are also used as members exposed to severe conditions such as heat exchangers and mechanical seals. Among them, SiC is a material with excellent heat resistance, mechanical strength, abrasion resistance, and corrosion resistance, and is chemically stable, so it can be used in a wide range of fields from aviation and space use to nuclear power and nuclear power generation. Promising in.
  • SiC has an excellent melting point of 2600 ° C and excellent high-temperature properties, it is a brittle material by itself. Therefore, composite materials reinforced with SiC fibers have been proposed, and various manufacturing processes such as hot pressing and liquid phase sintering have been studied [A ⁇ acombe and C. Bonnet,
  • SiC fiber reinforced SiC composite material in which a highly crystalline SiC fiber having a composition close to stoichiometric and excellent in heat resistance is used as a reinforcing material and a matrix is formed by a liquid phase sintering method.
  • the manufactured SiC fiber-reinforced SiC composite material exhibits excellent thermal properties at high density, but it is still unresolved to achieve both high fracture strength and high toughness. Disclosure of the invention
  • the present invention solves this problem by using SiC fibers coated with carbon, boron nitride, etc., as a reinforcing material, so that high-density and high-strength SiC fibers can be provided by one hot press.
  • the purpose is to obtain a mold SiC composite material.
  • a slurry in which SiC fine powder and a sintering aid are dispersed is prepared and coated with one or more of carbon, boron nitride, and silicon carbide. It is characterized in that a slurry is impregnated into SiC fibers to form a preform, and the preform is hot-pressed.
  • the sintering aid, AI2O3, ⁇ 2 ⁇ 3, Si0 2 , 1 kind selected from CaO or the two or more kinds are used.
  • the slurry may further include a silicon-based polymer such as polycarbosilane, polyvinylsilane, and polymethylsilane.
  • Figure 1 is a micrograph showing the effect of C coating on the reaction between the SiC fiber and the matrix of the SiC fiber-reinforced SiC composite sintered body.
  • FIG. 2 is a stress-strain diagram illustrating that the strength of a SiC fiber-reinforced SiC composite material using C-coated SiC fibers as a reinforcing material is significantly improved.
  • SiC fiber reinforced SiC composite materials exposed to the extreme environment have low impurity content such as oxygen, close to the stoichiometric composition, and are required to have high crystalline SiC fiber.
  • the SiC fiber deteriorates due to the reaction with the matrix. Therefore, in the present invention, the surface of the SiC fiber is coated with one or more of carbon, boron nitride, and silicon carbide in order to suppress the reaction between the matrix and the SiC fiber.
  • Coatings such as C, BN, and SiC suppress the interdiffusion reaction between the matrix and the SiC fiber and protect the SiC fiber from damage during the manufacturing process.
  • the coating layer promotes the dispersion / bending of cracks and the pulling out of the SiC fiber in the covered portion at the time of fracture, and also has the effect of controlling the fracture strength. As a result, the molding pressure can be increased during hot pressing, and the density of the SiC fiber reinforced SiC composite material can be increased.
  • the slurry to be impregnated in SiC fiber in addition to the SiC powder to be Matrix components of the SiC fiber-reinforced SiC composite material, ⁇ 1 2 0 3, ⁇ 2 ⁇ 3, blended sintering aid such as Si0 2, CaO ing.
  • the sintering aid forms a transition liquid phase with SiC at a relatively low temperature of 1800 ° C or lower, and promotes sintering to increase the density of the SiC fiber-reinforced SiC composite.
  • the slurry may further contain a silicon-based polymer such as polycarbosilane, polybutylsilane, and polymethylsilane.
  • Silicon-based polymers are The density of SiC fiber reinforced SiC composite material is increased by penetrating into fine inter-fiber voids that are difficult to penetrate.
  • a SiC fiber reinforced SiC composite material is produced by hot pressing a preformed body in which slurry is impregnated with SiC fibers, but hot pressing can be performed at a sintering temperature of 1600 to 1800 ° C and a molding pressure of lOMPa or higher. I like it.
  • the higher the sintering temperature and molding pressure the higher the density of the SiC fiber reinforced SiC composite material.
  • the molding pressure exceeding 30 MPa also degrades the SiC fiber and decreases the strength of the obtained SiC fiber reinforced SiC composite material.
  • the sintering temperature is less than 1600 ° C, the sintering of the matrix becomes insufficient and the porosity of the molded body increases significantly. I can't get it. Also, at a molding pressure of less than lOMPa, the porosity of the obtained sintered body tends to increase even when sintering is performed at the upper limit of the sintering temperature of 1800 ° C.
  • the slurry to be impregnated into SiC fiber is ultra-fine ⁇ -SiC particles: average particle size 0.3 ⁇
  • Table 1 shows the characteristics of the obtained SiC fiber reinforced SiC composite sintered body. Table 1: Hot pressing conditions and physical properties of SiC fiber reinforced SiC composites
  • the SiC fiber-reinforced SiC composite material obtained by hot pressing a preformed body containing SiC fibers coated with C or BN at 1750 ° C and 15MPa is the same as sample No. l using uncoated SiC fibers. As is clear from the comparison, the strength and the bending fracture energy were remarkably improved.
  • each SiC fiber-reinforced SiC composite was observed with a scanning electron microscope to investigate the cause of the increase in bending characteristics depending on the presence or absence of the coating.
  • Fig. 1 in Sample No. 1 using SiC fibers without C coating, the reaction between the SiC fibers and the matrix progressed, and the soundness of the SiC fibers was impaired. .
  • samples Nos. 2 to 4 using C-coated SiC fibers the soundness of the SiC fibers was maintained, and it was found that the reaction between the SiC fibers and the matrix was completely suppressed.
  • a relatively large diameter ⁇ -SiC particle is used as the matrix material.
  • the ⁇ -SiC particles were not sufficiently filled between the SiC fibers, and pores were found in the matrix.
  • Figures 1 and 2 show the effectiveness of C-coating.When hot-pressing with BN-coated SiC fibers as a reinforcing material, the reaction between the SiC fibers and Matritus is suppressed, and A high strength SiC fiber reinforced SiC composite material was obtained. Industrial applicability
  • the SiC fiber used as the reinforcing material by coating the SiC fiber used as the reinforcing material with C or BN, the damage of the SiC fiber is almost completely suppressed in the sintering process, and the SiC fiber reinforced SiC composite Manufactures sintered bodies that exhibit excellent properties inherent in materials.
  • the suppression of SiC fiber damage enables hot pressing at higher sintering temperatures and molding pressures, further improving the properties of SiC fiber reinforced SiC composites.
  • the SiC fiber-reinforced SiC composite material obtained in this way makes use of its excellent high-temperature properties, and is used as a structural material exposed to the extreme atmospheres of aviation, space, nuclear reactors, fusion reactors, and power generation. used.

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  • Organic Chemistry (AREA)
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  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)

Description

明 細 書
SiC繊維強化型 SiC複合材料の製造方法 技術分野
本発明は、 発電設備， 航空 ·宇宙機器， 原子力，核融合設備等、 高い熱負荷を受 け過酷な環境に曝される構造材料として好適で、 高温特性、 機械的強度に優れた SiC繊維強化型 SiC複合材料を製造する方法に関する。 背景技術
航空'宇宙機器， 原子力'核融合設備， 化石燃料を使用した発電設備等に使用さ れる構造材料は、 高い熱負荷を受ける過酷な環境に曝される。 このような環境下 で使用される材料として、 耐熱性， 化学的安定性， 機械的特性に優れた SiC，
Si3N4等、 種々のセラミックス材料が開発されてきた。 セラミックス材料は、 熱 交換器， メカニカルシール等の過酷な条件に曝される部材としても使用されてい る。 なかでも、 SiCは、 耐熱性， 機械的強度， 耐摩耗性， 耐食性に優れ、 しかも 化学的に安定な材料であるため、 航空'宇宙用途から原子力'核融合， 発電等にわ たる広範囲な分野で有望視されている。
SiC は、 融点が 2600°Cと高温特性に優れているが、 それ自体では脆い材料で ある。 そこで、 SiC繊維で強化した複合材料が提案され、 ホッ トプレス法， 液相 焼結法等、 種々の製造プロセスが検討されている [A丄 acombe and C.Bonnet,
2nd Int.Aerospace Planes Conf.Proc.AIAA-90-5208(l990), C. W. Hollenberg et al" J. Nucl. Mat, 219, (1995)70-86参照]。
何れの製法によっても、 高い熱伝導特性や高い密度、 更には高い強度特性、 優 れた破壊挙動特性を有する S i C繊維/ S i C複合材料を得ることは容易でなく、 同一プロセスの繰返し等によって特性の向上を図っている。 プロセスの繰返しは、 製造プロセスの複雑化を意味し、 製造コストを上昇させる原因となる。 また、 製 造上の問題から製品形状に制約が加わり、 複雑形状の部品等の製造が困難となる。 煩雑な製造プロセスや製品形状に加わる制約は、 SiC繊維強化型 SiC 複合材料 を実用材料として普及させる上でのネックとなる。
他方、 化学量論に近い組成をもち耐熱性に優れた高結晶性の SiC 繊維を強化 材に使用し、 液相焼結法でマトリックスを成形する SiC繊維強化型 SiC複合材 料の製造方法も知られている。 製造された SiC繊維強化型 SiC複合材料は、 高 密度で優れた熱特性を発現するが、 破壊強度及び靭性を高レベルで両立させるこ とに関しては依然として未解決である。 発明の開示
本発明は、 このような問題を解消すべく、 炭素， 窒化ホウ素等で被覆した SiC 繊維を強化材として使用することにより、 1回のホットプレスで高密度， 高強度 が付与された SiC繊維強化型 SiC複合材料を得ることを目的とする。
本発明の製造方法は、 その目的を達成するため、 SiC微粉末及び焼結助剤を分 散させたスラリーを用意し、 炭素， 窒化ホウ素， 炭化ケィ素の 1種又は 2種以上 で被覆した SiC 繊維にスラリーを含浸させて予備成形体とし、 該予備成形体を ホットプレスすることを特徴とする。
焼結助剤としては、 AI2O3, Υ2θ3, Si02， CaO から選ばれた 1種又は 2種以 上が使用される。 スラリーは、 更にポリカルボシラン， ポリ ビニルシラン， ポリ メチルシラン等のケィ素系ポリマ一を含むことができる。
SiC繊維にスラリ一を含浸させることによつて調製した予備成形体を焼結温度 1600〜1800°C, 圧力 lOMPa 以上でホッ トプレスするとき、 液相焼結反応によ つて高密度， 高靭性の SiC繊維強化型 SiC複合材料が得られる。 図面の簡単な説明
図 1は、 SiC繊維強化型 SiC複合材料焼結体の SiC繊維とマトリ ックスとの 反応に及ぼす C被覆の影響を説明するための組織写真
図 2は、 C被覆した SiC繊維を強化材とした SiC繊維強化型 SiC複合材料の 強度が格段に向上することを説明する応力一歪線図 発明を実施するための最良の形態
極限環境に曝される SiC繊維強化型 SiC複合材料では、 酸素等の不純物含有 量が低く化学量論組成に近レ、高結晶性の SiC繊維が必要とされる力 SiC繊維 に SiC微粉末を配合した予備成形体を焼結する際、 マトリックスとの反応によ つて SiC繊維が劣化 '破壊されやすレ、。 そこで、 本発明では、 マトリックスと SiC繊維との反応を抑制するため、 SiC繊維の表面を炭素， 窒化ホウ素， 炭化ケ ィ素の 1種又は 2種以上で被覆している。
C， BN, SiC等の被覆は、 マトリ ックスと SiC繊維との相互拡散反応を抑え、 製造過程における SiC繊維を損傷から保護する。 被覆層は、 破壊時において被 覆部分で亀裂の分散 ·屈曲， SiC繊維の引き抜け等を助長し、 破壊強度を制御す る作用も呈する。 その結果、 ホットプレス時に成形圧力の向上が可能となり、 SiC繊維強化型 SiC複合材料を高密度化できる。
SiC繊維に含浸させるスラリーとしては、 SiC繊維強化型 SiC複合材料のマト リ ックス成分となる SiC微粉末の他に、 Α1203, Υ2θ3， Si02， CaO等の焼結助 剤を配合している。 焼結助剤は、 1800°C以下の比較的低い温度において SiC と 共に遷移液相を形成し、 焼結を促進させて SiC繊維強化型 SiC複合材料を高密 度化する。
スラリーは、 更にポリカルボシラン， ポリ ビュルシラン， ポリメチルシラン等 のケィ素系ポリマーを含むことができる。 ケィ素系ポリマーは、 スラリー中の粒 子が浸透し難い微細な繊維間空隙に浸透することにより、 SiC 繊維強化型 SiC 複合材料を高密度化する。
SiC 繊維にスラリーを含浸させた予備成形体をホッ トプレスすることにより SiC繊維強化型 SiC複合材料が作製されるが、 焼結温度 1600〜1800°C， 成形圧 力 lOMPa以上でホットプレスすることが好ましレ、。 SiC繊維強化型 SiC複合材 料は、 焼結温度及び成形圧力が高いほど高密度化する。 しかし、 1800°Cを超え る高温で焼結すると、 成形圧力の下限 lOMPaにおいても SiC繊維が著しく劣化 する。 30MPaを超える成形圧力も SiC繊維を劣化させ、 得られた SiC繊維強化 型 SiC 複合材料の強度が低下する。 他方、 1600°C未満の焼結温度では、 マトリ ックスの焼結が不十分となって成形体の空隙率が著しく上昇するため、 要求特性 を満足する SiC繊維強化型 SiC複合材料焼結体が得られない。 また、 lOMPa未 満の成形圧力では、 焼結温度の上限 1800°Cで焼結しても得られた焼結体の空隙 率が高くなりやすい。
次いで、 図面を参照しながら、 実施例によって本発明を具体的に説明する。 化学量論に近い組成をもつ高結晶性の SiC繊維 （TVrannoTM— SA繊維；宇部 興産株式会社製） を使用し、 CVD 法によって熱分解炭素及び窒化ホウ素を SiC 繊維表面に析出させることにより、 膜厚約 Ι μπιの C又は ΒΝ被覆層を SiC繊維 の表面に形成した。
SiC繊維に含浸させるスラリ一は、 極微細 β— SiC粒子：平均粒径 0.3 μιηの
Α12θ3 (焼結助剤） ：ポリカルボシラン = 4.5： 0.5： 5 (質量比） でへキサン （溶 剤） に分散させることにより調製した。 真空吸引によって SiC繊維にスラリー を含浸させることにより、 SiC繊維：マトリ ックス原料 =4： 6 (質量比） の予 備成形体を作製した。
予備成形体をホッ トプレス機にセットし、 表 1に示す条件下でホットプレス した。 得られた SiC繊維強化型 SiC複合材料焼結体の特性を表 1に併せ示す。 表 1：ホットプレス条件及び SiC繊維強化型 SiC複合材料の物性
Figure imgf000007_0001
C又は BN被覆した SiC繊維を配合した予備成形体を 1750°C, 15MPaでホ ットプレスすることにより得られた SiC繊維強化型 SiC複合材料は、 無被覆の SiC繊維を用いた試料 No.lとの対比から明らかなように、 強度及び曲げ破壊ェ ネルギ一が飛躍的に向上していた。
被覆の有無によって曲げ特性が大きくことなる原因を調査するため、 各 SiC 繊維強化型 SiC複合材料の組織を走査型電子顕微鏡で観察した。 図 1の観察結 果にみられるように、 C被覆を施していない SiC繊維を使用した試料 No.lでは、 SiC繊維とマトリックスとの反応が進行し、 SiC繊維の健全性が損なわれていた。 他方、 C被覆した SiC繊維を使用した試料 No.2〜4は、 何れも SiC繊維の健全 性が維持されており、 SiC繊維とマトリックスとの反応が完全に抑制されている ことが判る。 ただし、 マトリ ックス材料として比較的大径の β— SiC粒子を用い た試料 No.4では、 SiC繊維間に β— SiC粒子が十分に充填されず、 マトリック スにポアが散見された。
各資料 No. l〜4 を 3点曲げ試験に供し、 応力一歪曲線 （図 2) を求めた。 試 料 No. l との対比から明らかなように、 C被覆 SiC繊維を使用した試料 No.2〜4 の SiC繊維強化型 SiC複合材料は、 何れも弾性限界を超えて最大荷重が得られ ており、 最大荷重点以降の伸びも確保されていた。 このことからも、 擬延性的破 壊挙動を C'被覆が有効に制御していることが窺われる。
図 1, 2は、 C被覆の有効性を示すデータであるが、 BN被覆した SiC繊維を 強化材に用いてホットプレスした場合にも、 SiC繊維とマトリッタスとの反応が 抑制され、 同様に機械強度の高い SiC繊維強化型 SiC複合材料が得られた。 産業上の利用可能性
以上に説明したように、 本発明で、 強化材として使用される SiC繊維を Cや BNで被覆することにより、 焼結工程において SiC繊維の損傷をほぼ完全に抑止 し、 SiC 繊維強化型 SiC 複合材料本来の優れた特性を呈する焼結体を製造して いる。 SiC繊維の損傷が抑制されることは、 より高い焼結温度や成形圧力でのホ ットプレスを可能とし、 SiC 繊維強化型 SiC 複合材料の特性が更に向上する。 このようにして得られた SiC繊維強化型 SiC複合材料は、 優れた高温特性を活 用し、 航空，宇宙， 原子炉 ·核融合炉， 発電等の極限雰囲気に曝される構造材料と して使用される。

Claims

請求の範囲
1. SiC 微粉末及び焼結助剤を分散させたスラリーを用意し、 炭素， 窒化ホウ素， 炭化ケィ素の 1種又は 2種以上で被覆した SiC繊維に前記スラリーを含浸さ せて予備成形体とし、 該予備成形体をホッ トプレスすることを特徴とする SiC繊維強化型 SiC複合材料の製造方法。
2. AI2O3, Υ2Ο3, Si02, CaOから選ばれた 1種又は 2種以上を焼結助剤に使 用する請求項 1記載の製造方法。
3. ポリカルボシラン， ポリビュルシラン， ポリメチルシランから選ばれた 1種 又は 2種以上のケィ素系ポリマーを含むスラリーを使用する請求項 1記載の 製造方法。
4. 焼結温度 1600〜1800°C, 圧力 lOMPa以上でホットプレスする請求項 1記 載の製造方法。
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EP1391442A1 (en) 2004-02-25
US7318906B2 (en) 2008-01-15
US20050001361A1 (en) 2005-01-06
WO2002098819A8 (fr) 2003-03-06
CA2444963C (en) 2009-06-30
JP2002356381A (ja) 2002-12-13
EP1391442B1 (en) 2010-04-28
EP1391442A4 (en) 2006-05-17
DE60141985D1 (de) 2010-06-10
CA2444963A1 (en) 2002-12-12
JP3971903B2 (ja) 2007-09-05

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