JP3120884B2 - SiC coated C / C composite - Google Patents
SiC coated C / C compositeInfo
- Publication number
- JP3120884B2 JP3120884B2 JP03351272A JP35127291A JP3120884B2 JP 3120884 B2 JP3120884 B2 JP 3120884B2 JP 03351272 A JP03351272 A JP 03351272A JP 35127291 A JP35127291 A JP 35127291A JP 3120884 B2 JP3120884 B2 JP 3120884B2
- Authority
- JP
- Japan
- Prior art keywords
- sic
- layer
- composite
- coated
- reinforcing layer
- 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.)
- Expired - Fee Related
Links
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
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00862—Uses not provided for elsewhere in C04B2111/00 for nuclear applications, e.g. ray-absorbing concrete
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00982—Uses not provided for elsewhere in C04B2111/00 as construction elements for space vehicles or aeroplanes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、半導体製造工程で使用
されるサセプタ、ヒータ、ルツボ等や、核融合炉炉壁
材、タービンブレード、航空用ブレーキ材、宇宙航空機
体用ＳｉＣ複合材として用いられるＳｉＣ被覆Ｃ／Ｃ複
合材に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is used as a susceptor, a heater, a crucible, etc. used in a semiconductor manufacturing process, a fusion reactor furnace wall material, a turbine blade, an aircraft brake material, and a SiC composite material for a space aircraft body. The C / C composite material to be coated.
【０００２】[0002]
【従来の技術】従来、ＳｉＣ被覆Ｃ／Ｃ複合材が半導体
分野で広く用いられている。これは、Ｃ／Ｃ複合基材の
表面に、ＣＶＤ法等の気相成長法や、けい化法、塗布
法、含浸法等によってＳｉＣ層をコーティングしたもの
である。Ｃ／Ｃ複合基材は熱伝導性が良好で高周波誘導
加熱によって均一に加熱できると共に、耐熱衝撃性に優
れ、かつ高純度化が可能である。従って高温部材として
適している。しかし、Ｃ／Ｃ複合基材はガスを吸収し易
く加熱時にそれを放出するため、表面にＳｉＣ層を形成
してこれを防止している。2. Description of the Related Art Hitherto, SiC-coated C / C composites have been widely used in the field of semiconductors. In this method, the surface of a C / C composite substrate is coated with a SiC layer by a vapor phase growth method such as a CVD method, a silicification method, a coating method, an impregnation method, or the like. The C / C composite substrate has good thermal conductivity, can be uniformly heated by high-frequency induction heating, has excellent thermal shock resistance, and can be highly purified. Therefore, it is suitable as a high-temperature member. However, since the C / C composite base material easily absorbs gas and releases it upon heating, a SiC layer is formed on the surface to prevent this.
【０００３】しかしながら、ＳｉＣ被膜とＣ／Ｃ複合基
材は熱膨張係数が異なるため、急熱急冷を繰り返すヒー
トサイクルによって、ＳｉＣ被膜にクラックが生じたり
剥離する等の不都合が生じている。また、両者は機械的
性質も異なるので、全体的強度の点でもマイナスであ
る。However, since the SiC coating and the C / C composite base material have different coefficients of thermal expansion, inconveniences such as cracking and peeling of the SiC coating are caused by repeated heat cycles of rapid heating and quenching. Also, since both have different mechanical properties, they are also negative in terms of overall strength.
【０００４】ＳｉＣ被膜とＣ／Ｃ複合基材の熱膨張差を
吸収緩和するために、両者の間に中間層を形成すること
が試みられている。例えば、ＳｉＣ被膜をコーティング
する前にＣ／Ｃ複合基材にけい化処理を施し、その表層
部にけい化層を形成する。そして、けい化層の表面にＳ
ｉＣ被膜をコーティングするのである。In order to absorb and reduce the difference in thermal expansion between the SiC coating and the C / C composite substrate, an attempt has been made to form an intermediate layer between them. For example, before the SiC film is coated, the C / C composite substrate is subjected to a silicidation treatment, and a silicide layer is formed on the surface layer. Then, S on the surface of the silicide layer
The iC film is coated.
【０００５】[0005]
【発明が解決しようとする課題】しかし、このようにし
てＳｉＣ被膜とＣ／Ｃ複合基材の間に形成した従来のけ
い化層は、表層部が炭素繊維の中心部まで１００％また
はそれに近い比率でけい化されている。このため、緩衝
層として充分に機能せず、他方では機械的強度の低下も
生じている。このため、依然として、ＳｉＣ被膜の剥離
等の問題が生じ、充分な製品寿命が得られていない状況
にある。However, the conventional silicide layer formed between the SiC coating and the C / C composite substrate in this manner has a surface layer portion of 100% or close to the center of the carbon fiber. It is silicified in proportion. For this reason, it does not function sufficiently as a buffer layer, and on the other hand, the mechanical strength is reduced. For this reason, problems such as peeling of the SiC film still occur, and a sufficient product life has not been obtained.
【０００６】本発明は、Ｃ／Ｃ複合基材とＳｉＣ被膜の
熱的及び機械的マッチングを良好に行い、耐熱衝撃性に
優れ機械的強度も充分に高く、製品としての耐用寿命が
長いＳｉＣ被覆Ｃ／Ｃ複合材を提供することを目的とし
ている。The present invention provides a SiC coating having good thermal and mechanical matching between a C / C composite base material and a SiC coating, excellent thermal shock resistance, sufficiently high mechanical strength, and a long service life as a product. It is intended to provide a C / C composite.
【０００７】[0007]
【課題を解決するための手段】この発明は、Ｃ繊維を含
むＣ／Ｃ複合基材にＳｉＣ層を被覆したＳｉＣ被覆Ｃ／
Ｃ複合材において、Ｃ／Ｃ複合基材とＳｉＣ層の間に強
化層を設け、強化層がＣ／Ｃ複合基材を部分的にけい化
処理することによって構成されていて、強化層の厚さが
ＳｉＣ層の厚さの７／１０〜１０／７倍でありかつＣ繊
維直径の１０〜３０倍であって、強化層におけるけい化
部分の総断面積がけい化されていないＣ繊維の総断面積
の１／９〜１倍であることを特徴とするＳｉＣ被覆Ｃ／
Ｃ複合材を要旨としている。SUMMARY OF THE INVENTION The present invention relates to a SiC-coated C / C composite in which a C / C composite substrate containing C fibers is coated with a SiC layer.
In the C composite material, a reinforcing layer is provided between the C / C composite substrate and the SiC layer, and the reinforcing layer is formed by partially silicifying the C / C composite substrate. Is 7/10 to 10/7 times the thickness of the SiC layer and 10 to 30 times the diameter of the C fiber, and the total cross-sectional area of the silicided portion of the reinforcing layer SiC coated C /, characterized in that it is 1/9 to 1 times the total cross-sectional area
The gist is C composite material.
【０００８】[0008]
【作用】Ｃ／Ｃ複合基材とＳｉＣ層の間に形成された強
化層は、熱的及び機械的にＣ／Ｃ複合基材とＳｉＣ層の
中間的性質を有する。従って、Ｃ／Ｃ複合基材とＳｉＣ
層を熱的及び機械的に良好にマッチングすることができ
る。The reinforcing layer formed between the C / C composite substrate and the SiC layer has properties intermediate between the C / C composite substrate and the SiC layer both thermally and mechanically. Therefore, C / C composite substrate and SiC
The layers can be well matched thermally and mechanically.
【０００９】[0009]
【実施例】強化層の厚さをＳｉＣ層の厚さの７／１０〜
１０／７倍にしたのは、これが７／１０倍未満であると
Ｃ／Ｃ複合基材とＳｉＣ層の熱膨張差を充分に吸収でき
ないからである。また、１０／７倍を超えると強化層が
厚くなりすぎて、けい化処理の段階で強化層の外側部分
のけい化が進みすぎてけい化度１００％の層が形成され
る可能性があるからである。DESCRIPTION OF THE PREFERRED EMBODIMENTS The thickness of the reinforcing layer was set to 7/10 of the thickness of the SiC layer.
The reason for increasing the ratio by 10/7 is that if the ratio is less than 7/10, the difference in thermal expansion between the C / C composite base material and the SiC layer cannot be sufficiently absorbed. On the other hand, if the ratio exceeds 10/7, the reinforcing layer becomes too thick, and the silicidation of the outer portion of the reinforcing layer proceeds excessively at the stage of the silicification treatment, so that a layer having a degree of silicidation of 100% may be formed. Because.
【００１０】強化層の厚さをＣ繊維の直径の１０〜３０
倍に設定したのは、これが１０倍未満であると強化層の
厚さが不充分となり、熱膨張差を充分に吸収できないか
らである。また３０倍を超えると、強化層が厚くなりす
ぎて、前述したように、けい化処理によって部分的にけ
い化度１００％の層が形成される恐れがあるからであ
る。The thickness of the reinforcing layer is set to be 10 to 30 times the diameter of the C fiber.
The reason for setting the ratio to twice is that if the ratio is less than ten times, the thickness of the reinforcing layer becomes insufficient, and the difference in thermal expansion cannot be sufficiently absorbed. On the other hand, if it exceeds 30 times, the reinforcing layer becomes too thick, and as described above, there is a possibility that a layer having a degree of silicidation of 100% may be partially formed by the silicification treatment.
【００１１】所定位置で断面をとった場合に、強化層に
おけるけい化部分の総断面積がけい化されていないＣ繊
維の総断面積の１／９〜１倍になるように設定したの
は、この範囲内であると、強化層の熱的及び機械的性質
がＣ／Ｃ複合基材とＳｉＣ層の性質の中間的値を有し、
良好なマッチングが可能になるからである。The reason for setting the total cross-sectional area of the silicided portion in the reinforcing layer to be 1/9 to 1 times the total cross-sectional area of the non-silicified C fiber when a cross section is taken at a predetermined position is as follows. Within this range, the thermal and mechanical properties of the reinforcing layer have intermediate values between the properties of the C / C composite substrate and the SiC layer,
This is because good matching becomes possible.
【００１２】ＳｉＣ被覆Ｃ／Ｃ複合材の製造方法を簡単
に説明する。まず、Ｃ／Ｃ複合基材の表面に多孔性のＳ
ｉＣ被膜を形成する。被覆はＣＶＤ法や他の気相成長
法、または塗布法によって行ってもよい。次に、多孔性
ＳｉＣ被膜の上からけい化処理を行って、強化層を形成
する。最後に、強化層の表面に緻密なＳｉＣ被膜を形成
する。緻密ＳｉＣ被膜はＣＶＤ法によってＳｉＣ柱状結
晶となるように形成するのが望ましい。A method for producing a SiC-coated C / C composite will be briefly described. First, porous S
An iC coating is formed. The coating may be performed by a CVD method, another vapor deposition method, or a coating method. Next, a siliconization treatment is performed on the porous SiC film to form a reinforcing layer. Finally, a dense SiC film is formed on the surface of the reinforcing layer. The dense SiC film is desirably formed by CVD to form SiC columnar crystals.
【００１３】多孔性ＳｉＣ被膜の膜厚は５〜５０μｍに
設定するのが望ましい。この範囲の膜厚ならば、けい化
処理の際に適度な浸透が得られるからである。また、多
孔性ＳｉＣ被覆の孔径は、１〜５０μｍが望ましい。孔
径が１μｍ未満であると、この孔を通してのＣ／Ｃ複合
基材のけい化が行われにくくなる。５０μｍを超える
と、この孔を通してのＣ／Ｃ複合基材の表層部のけい化
が過度に進行し、けい化度が１００％の層が形成される
可能性がある。さらに望ましくは１０〜３０μｍに設定
する。The thickness of the porous SiC film is desirably set to 5 to 50 μm. If the film thickness is in this range, appropriate penetration can be obtained during the silicidation treatment. Further, the pore diameter of the porous SiC coating is desirably 1 to 50 μm. When the pore size is less than 1 μm, it becomes difficult to silicate the C / C composite base material through the pores. If it exceeds 50 μm, the surface of the C / C composite base material through the pores may be excessively silicided, and a layer having a silicidation degree of 100% may be formed. More preferably, it is set to 10 to 30 μm.
【００１４】強化層の厚さは前述の条件を満し、しかも
５０〜１５０μｍにするのが望ましい。It is desirable that the thickness of the reinforcing layer satisfies the above-mentioned conditions, and that the thickness be 50 to 150 μm.
【００１５】Ｃ繊維の直径が５〜１０μｍで、ＳｉＣ層
の厚みが５０〜２００μｍが好ましい。The diameter of the C fiber is preferably 5 to 10 μm, and the thickness of the SiC layer is preferably 50 to 200 μm.
【００１６】Ｃ／Ｃ複合基材は、ＰＡＮ系、ピッチ系、
セルロール系のＣファイバーがフィラーで、ピッチ含
浸、焼成、ＣＶＩによりカーボンを含浸したマトリック
スからなる材料である。Ｃ／Ｃ複合基材の種類は製品の
用途に合せて適当に選択する。例えば、半導体製造具と
しては密度が１．６０〜１．８５ｇ／ｃｍ3 で２次元材
または短繊維系のものが用いられ、また、航空宇宙用耐
熱材としては密度が１．７０〜１．８５ｇ／ｃｍ3 で１
次元の積層構造のものが用いられる。Ｃ／Ｃ複合基材の
厚さは半導体用が１０〜３０ｍｍで、航空用が１〜１０
ｍｍであることが望ましい。The C / C composite base material includes PAN-based, pitch-based,
Cellulol-based C fiber is a filler and is a material composed of a matrix impregnated with carbon by pitch impregnation, firing and CVI. The type of C / C composite substrate is appropriately selected according to the use of the product. For example, a two-dimensional material or a short fiber material having a density of 1.60 to 1.85 g / cm 3 is used as a semiconductor manufacturing tool, and a density of 1.70 to 1.85 is used as a heat-resistant material for aerospace. 1 at 85 g / cm 3
A one-dimensional laminated structure is used. The thickness of the C / C composite substrate is 10 to 30 mm for semiconductors and 1 to 10 for aviation.
mm.
【００１７】緻密なＳｉＣ被膜の厚さは２０〜２０００
μｍが望ましい。２０μ未満であると表面の被覆が不充
分で耐酸化性に劣ってしまう。また２０００μｍを超え
ると使用に際しＳｉＣ被覆の歪が大きくなり、クラッ
ク、剥離を生じ易い。より望ましくは４０〜１２０μｍ
である。The thickness of the dense SiC film is 20 to 2000.
μm is desirable. If it is less than 20 μm, the coating on the surface is insufficient and the oxidation resistance is poor. On the other hand, if it exceeds 2000 μm, the strain of the SiC coating increases during use, and cracks and peeling are likely to occur. More preferably, 40 to 120 μm
It is.
【００１８】図示例 以下、図面を参照して本発明の実施例を詳細に説明す
る。The illustrated embodiment will now be described in detail embodiments of the present invention with reference to the drawings.
【００１９】密度１．８ｇ／ｃｍ3 、ＰＡＮ系２次元の
黒鉛繊維を含有するＣ／Ｃ複合基材５（２×５×３０ｍ
ｍ）を反応炉内に設置し、反応温度１５００℃で反応ガ
スとしてＳｉＣｌ4 ，ＣＨ4 及びＨ2 を流し、蒸着スピ
ード１〜１０μｍ／ｈｒでＣＶＤ反応を行い、厚さ２０
μｍ、孔径１〜５０μｍの多孔性のＳｉＣ被膜３を形成
した。A C / C composite substrate 5 (2 × 5 × 30 m) having a density of 1.8 g / cm 3 and containing PAN-based two-dimensional graphite fibers
m) was placed in a reaction furnace, SiCl 4 , CH 4, and H 2 were passed as reaction gases at a reaction temperature of 1500 ° C., and a CVD reaction was performed at a deposition speed of 1 to 10 μm / hr.
A porous SiC coating 3 having a thickness of 1 μm and a pore size of 1 to 50 μm was formed.
【００２０】ついで、反応温度１５００℃で反応ガスと
してＳｉＯガスを流し、Ｃ／Ｃ複合基材１の表層部にけ
い化処理を施し、厚さ２００μｍの強化層４を形成し
た。このけい化処理に際し、多孔性のＳｉＣ被膜３はマ
スクとして機能する。多孔性ＳｉＣ被膜３によって強化
層４の表層部におけるけい化が適度に抑制され、けい化
度１００％の領域は形成されず、Ｃ／Ｃ複合基材の表層
部が選択的に深部までけい化される。図１では強化層４
におけるけい化部分を符号９で示した。また、反応等は
未だ充分解明されていないが、Ｃ充填物の方が繊維より
選択的にけい化され、繊維８のけい化はその表層部でわ
ずかに表面にとどまり、中心部までには達していない。
けい化部は０．０５〜０．１μｍのＳｉＣ微結晶層とな
る。強化層４では、けい化部分９の総断面積がけい化さ
れていないＣ繊維８の総断面積の約１倍になっている。
また、強化層４の厚さはＳｉＣ層２の厚さの約８〜１０
倍、Ｃ繊維１０の直径の約１０倍になっている。図１の
例では強化層４とＣ／Ｃ複合基材５の境界が平面になっ
ているが、実際には図２に示すように凹凸になる。Then, SiO gas was flowed as a reaction gas at a reaction temperature of 1500 ° C., and the surface layer of the C / C composite base material 1 was subjected to a silicidation treatment to form a 200 μm thick reinforcing layer 4. During this silicidation treatment, the porous SiC film 3 functions as a mask. By the porous SiC coating 3, silicidation in the surface layer of the reinforcing layer 4 is appropriately suppressed, a region having a degree of silicidation of 100% is not formed, and the surface layer of the C / C composite base material is selectively silicified to a deep portion. Is done. In FIG. 1, the reinforcing layer 4
The symbol 9 represents the silicidized portion in. Further, although the reaction and the like have not been sufficiently elucidated, the C-filled material is selectively silicified rather than the fiber, and the silicidation of the fiber 8 slightly remains on the surface at the surface layer and reaches the center. Not.
The silicified portion becomes a SiC microcrystal layer of 0.05 to 0.1 μm. In the reinforced layer 4, the total cross-sectional area of the silicided portion 9 is about one times the total cross-sectional area of the unsilicided C fibers 8.
The thickness of the reinforcing layer 4 is about 8 to 10 times the thickness of the SiC layer 2.
Twice as large as the diameter of the C fiber 10. In the example of FIG. 1, the boundary between the reinforcing layer 4 and the C / C composite base material 5 is a flat surface, but in reality, it becomes uneven as shown in FIG. 2.
【００２１】上記けい化処理後、反応温度１３００℃で
反応ガスとしてメチルトリクロロシラン（ＭＴＣＳ）と
Ｈ2 を流し、蒸着スピード５〜１０μｍ／ｈｒでＣＶＤ
反応を行い、厚さ８０μｍの緻密なＳｉＣ柱状結晶から
なる被膜２を形成した。柱状結晶の径は５μｍである。
このＳｉＣ被膜２は、表層部のけい化層及び多孔性のＳ
ｉＣ被膜３と一体となっている。After the above-mentioned silicidation treatment, methyltrichlorosilane (MTCS) and H 2 are passed as reaction gases at a reaction temperature of 1300 ° C., and CVD is performed at a deposition speed of 5 to 10 μm / hr.
The reaction was performed to form a coating 2 made of dense SiC columnar crystals having a thickness of 80 μm. The diameter of the columnar crystal is 5 μm.
The SiC film 2 has a silicide layer on the surface and a porous S
It is integrated with the iC coating 3.
【００２２】得られたＳｉＣ被覆Ｃ／Ｃ複合材は、以下
に述べるヒートサイクルテストを施したがマイクロクラ
ックは全く発生せず、また剥離も生じなかった。The obtained SiC-coated C / C composite material was subjected to the heat cycle test described below. As a result, no microcracks occurred and no peeling occurred.
【００２３】ヒートサイクルテストは、試験片を１２０
０℃まで昇温した炉内に挿入し、２分間保持した後、炉
外（室温約２５℃）へ取り出す操作を繰り返し行うもの
で、５回おきにその表面状態を目視により観察し、５０
回まで行った。In the heat cycle test, the test piece was
After inserting into a furnace heated to 0 ° C., holding for 2 minutes, and taking it out of the furnace (room temperature of about 25 ° C.), the surface state is visually observed every 5 times,
I went up to times.
【００２４】また、曲げ強度を測定したところ、６５Ｍ
Ｐａであった。When the bending strength was measured, it was found to be 65M
Pa.
【００２５】比較例 実験例と同様のＣ／Ｃ複合基材を反応炉内に納置し、反
応温度１５００℃で反応ガスとしてＳｉＯガスを流し、
Ｃ／Ｃ複合基材の表層部にけい化処理を施し、厚さ２０
０μｍのけい化層を形成した。このけい化処理によっ
て、けい化度１００％領域が表面から８０〜１２０μｍ
の深さで全面に亘って形成された。 Comparative Example A C / C composite base material similar to that of the experimental example was placed in a reaction furnace, and SiO gas was flowed as a reaction gas at a reaction temperature of 1500 ° C.
The surface layer of the C / C composite substrate is silicided to a thickness of 20
A silicide layer of 0 μm was formed. By this silicidation treatment, the region with a degree of silicidation of 100% is 80 to 120 μm from the surface.
Formed over the entire surface at a depth of.
【００２６】ついで、反応温度１３００℃で反応ガスと
してＭＴＣＳ＋Ｈ2を流し、蒸着スピード５〜１０μｍ
／ｈｒでＣＶＤ反応を行い、厚さ８０μｍの緻密なＳｉ
Ｃ被膜を形成した。Then, MTCS + H 2 is flowed as a reaction gas at a reaction temperature of 1300 ° C., and a vapor deposition speed of 5 to 10 μm
/ Hr CVD reaction and a dense 80 μm thick Si
A C film was formed.
【００２７】得られたＳｉＣ被覆Ｃ／Ｃ複合体は、５回
のヒートサイクルテストでマイクロクラックが多数発生
し、ＳｉＣ被膜が剥離した。また、曲げ強度を測定した
ところ、３５ＭＰａであった。In the obtained SiC-coated C / C composite, a number of microcracks occurred in five heat cycle tests, and the SiC coating was peeled off. The flexural strength measured was 35 MPa.
【００２８】従って、本発明に係る実施例によるもの
は、耐熱衝撃性に優れていると共に、強度も優れている
ことがわかる。Therefore, it can be seen that the embodiment according to the present invention is excellent not only in thermal shock resistance but also in strength.
【００２９】[0029]
【発明の効果】本発明のＳｉＣ被覆Ｃ／Ｃ複合材におい
ては、強化層によってＣ／Ｃ複合基材とＳｉＣ被膜のマ
ッチングが良好に行われているので、耐熱衝撃性に優
れ、機械的強度も充分に高い。従って、本発明のＳｉＣ
被覆Ｃ／Ｃ複合材は従来品にくらべて高品質であって耐
用寿命が飛躍的に長い。According to the SiC-coated C / C composite material of the present invention, since the C / C composite base material and the SiC coating are well matched by the reinforcing layer, the thermal shock resistance is excellent and the mechanical strength is excellent. Is also high enough. Therefore, the SiC of the present invention
The coated C / C composite is of higher quality and has a significantly longer useful life than conventional products.
【図１】本発明のＳｉＣ被覆Ｃ／Ｃ複合材の実施例を模
式的に示した断面図。FIG. 1 is a cross-sectional view schematically showing an embodiment of a SiC-coated C / C composite material of the present invention.
【図２】本発明のＳｉＣ被覆Ｃ／Ｃ複合材の実施例を示
す断面図。FIG. 2 is a sectional view showing an embodiment of the SiC-coated C / C composite material of the present invention.
１ ＳｉＣ被覆Ｃ／Ｃ複合材 ２ ＳｉＣ柱状結晶被膜 ３ 多孔質ＳｉＣ被膜 ４ 強化層 ５ Ｃ／Ｃ複合基材 ６ ＳｉＣ柱状結晶 ８ 表層のみがけい化されたＣ繊維 ９ けい化部 １０ Ｃ繊維 １１ 境界 DESCRIPTION OF SYMBOLS 1 SiC coating C / C composite material 2 SiC columnar crystal coating 3 Porous SiC coating 4 Reinforcement layer 5 C / C composite base material 6 SiC columnar crystal 8 C fiber with only surface layer silicided 9 Silicified portion 10 C fiber 11 boundary
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｃ０４Ｂ 35/83 Ｃ０４Ｂ 35/80 Ｂ (72)発明者 菅井 照夫 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (72)発明者 小池 弘明 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (72)発明者 保立 四郎 東京都新宿区西新宿１―26―２ 東芝セ ラミックス株式会社内 (58)調査した分野(Int.Cl.7，ＤＢ名) C04B 41/80 - 41/91 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification code FI C04B 35/83 C04B 35/80 B (72) Inventor Teruo Suga 378 Oguni-cho, Oguni-cho, Oguni-machi, Nishiokitama-gun, Yamagata Toshiba Ceramics Corporation Oguni Works (72) Inventor Hiroaki Koike 378 Ogunimachi, Oguni-machi, Oguni-machi, Nishiokitama-gun, Yamagata Toshiba Ceramics Co., Ltd.Oguni Works (72) Inventor Shiro Hotate 1-26-2 Nishishinjuku, Shinjuku-ku, Tokyo Toshiba Sera (58) Investigated field (Int. Cl. 7 , DB name) C04B 41/80-41/91
Claims (1)
を被覆したＳｉＣ被覆Ｃ／Ｃ複合材において、Ｃ／Ｃ複
合基材とＳｉＣ層の間に強化層を設け、強化層がＣ／Ｃ
複合基材を部分的にけい化処理することによって構成さ
れていて、強化層の厚さがＳｉＣ層の厚さの７／１０〜
１０／７倍でありかつＣ繊維直径の１０〜３０倍であっ
て、強化層におけるけい化部分の総断面積がけい化され
ていないＣ繊維の総断面積の１／９〜１倍であることを
特徴とするＳｉＣ被覆Ｃ／Ｃ複合材。In a SiC-coated C / C composite material in which a C / C composite substrate containing a C fiber is coated with a SiC layer, a reinforcing layer is provided between the C / C composite substrate and the SiC layer. C / C
It is constituted by partially silicifying the composite substrate, and the thickness of the reinforcing layer is 7/10 to the thickness of the SiC layer.
It is 10/7 times and 10 to 30 times the diameter of the C fiber, and the total cross-sectional area of the silicided portion in the reinforcing layer is 1/9 to 1 times the total cross-sectional area of the unsilicided C fiber. A SiC-coated C / C composite material, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03351272A JP3120884B2 (en) | 1991-12-13 | 1991-12-13 | SiC coated C / C composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03351272A JP3120884B2 (en) | 1991-12-13 | 1991-12-13 | SiC coated C / C composite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05163086A JPH05163086A (en) | 1993-06-29 |
| JP3120884B2 true JP3120884B2 (en) | 2000-12-25 |
Family
ID=18416196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03351272A Expired - Fee Related JP3120884B2 (en) | 1991-12-13 | 1991-12-13 | SiC coated C / C composite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3120884B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1306890A2 (en) * | 2001-10-25 | 2003-05-02 | Matsushita Electric Industrial Co., Ltd. | Semiconductor substrate and device comprising SiC and method for fabricating the same |
| EP2471764B1 (en) * | 2010-12-28 | 2016-05-11 | SGL Carbon SE | Process for producing friction disks having a structured ceramic friction Layer |
| CN105645966B (en) * | 2015-12-30 | 2018-02-23 | 南京航空航天大学 | A kind of preparation method of C/C SiC ceramic matrix composite materials vacuum insulation panel |
-
1991
- 1991-12-13 JP JP03351272A patent/JP3120884B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05163086A (en) | 1993-06-29 |
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