JPS6225628B2 - - Google Patents
Info
- Publication number
- JPS6225628B2 JPS6225628B2 JP56151236A JP15123681A JPS6225628B2 JP S6225628 B2 JPS6225628 B2 JP S6225628B2 JP 56151236 A JP56151236 A JP 56151236A JP 15123681 A JP15123681 A JP 15123681A JP S6225628 B2 JPS6225628 B2 JP S6225628B2
- Authority
- JP
- Japan
- Prior art keywords
- fibers
- sintered body
- fiber
- sic
- carbon
- 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
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- 239000000835 fiber Substances 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 17
- 229910010271 silicon carbide Inorganic materials 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000005489 elastic deformation Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
本発明は特定な方向にすぐれた抗張力を有する
炭化珪素焼結体の製造法に関する。
炭化珪素焼結体は低熱膨脹性で、機械強度や熱
伝導が大きく、耐酸化性も良好なことから、発熱
体やエンジン部品その他の耐熱構造材料として、
最近広範な用途が開けてきた材質であるが、金属
に比べ靭性が乏しく、特に抗脹力が弱いという難
点があつた。
本発明はこれを改良し、特定方向に著しく強い
抗脹力をもつSiC焼結体の製造法に関するもの
で、W繊維を1平面または1直線に実質的にほゞ
平行に配列し、炭素を含有する結合剤を加えて成
形し、非酸化性雰囲気中にて熱分解し溶融金属珪
素を滲透せしめて全体を繊維で強化されたSiCと
することを特徴とする繊維強化SiC焼結体の製造
法を提供するもので、SiCの反応焼結法の1種で
あるが、W(タングステン)繊維が実質的に平行
に配列されているため繊維の伸長方向に、著しく
強い抗張力を有し、また少量の金属珪素が残留す
るために、靭性の大きいものである。次にこれを
成形するには、W繊維を一平面上に不特定方向に
配置し結合すれば曲げや引張り応力に強い薄板が
得られ、放射状に配置すれば、半径方向の引張応
力即ち遠心力に特に強い薄板や羽根車が得られ、
円筒状や角筒状物の側面に捲回して結合すれば内
部で燃焼反応を起した時も、燃焼による気体の応
力や熱歪に著しく強い円筒や角筒を得ることがで
きる。また1直線に平行に配置し結合すればその
方向に特に強度のある線状体が得られこれを円
形、コイル状等に加工すればリングや耐熱性コイ
ルスプリング等に適したものとなり、従来のSiC
焼結体に比し著しく靭性の大きいものとなる。
次に炭素を含有する結合剤は、粘着性と炭素が
含まれることが必要で、ピツチ、タール、脂肪
酸、他特に熱可塑性または熱硬化性樹脂等が有効
に利用できる。これらはW繊維と混練しながら配
列してもよく、またW繊維を配列後液状の結合剤
に振動を加えながら、滲透せしめてもよく、何れ
の方法でも繊維の空隙を十分に埋めることが必要
でこれが不十分ならばそれに応じて焼結も不十分
となり、強度を低下するものである。
次にこれを熱分解して炭素を残留するには、非
酸化性雰囲気、具体的には真空、水素、アルゴ
ン、窒素等の雰囲気でよい。この時の分解残留炭
素はWの間隙を多孔質で活性の高い炭素の形で埋
め、溶融金属珪素の滲透を毛細管現象によつて容
易にし、1500℃付近で十分反応焼結を起す。これ
により、反応焼結SiCで結合したW繊維の焼結体
が得られると共に少量の珪素が残留するから、繊
維の方向に著しく抗脹力の大きく且つ靭性の高い
ものとなる。また炭化珪素は耐酸化性が大で、
種々燃焼機器に利用できる高強度部品となる。
以下実施例により一そう具体的に説明するが本
発明はこれにより拘束されるものではない。
実施例 1
市販のW繊維をメタクリル酸イソブチルエステ
ル、ニトロセルローズ,ジオクチルフタレートの
混合物に少量のトリクロ−ルエチレンを加えた液
に浸漬したのち、平行に堆積し、加圧して厚さ2
mm×巾10mm×長さ100mmのテストピースを作成し
乾燥後、N2雰囲気中で800℃に5時間加熱して有
機物の結合剤を熱分解し、W繊維を炭素で結合し
た物体を製作し、次にアルミナ製のサヤの中に金
属珪素の粉末を入れこのテストピースの一端を粉
末中に入れ、1430℃に真空中で昇温せしめ、金属
珪素を溶融せしめると共に焼結体中に滲透させ、
反応焼結を完了した。これをNo.1とする。次にポ
リウレタン樹脂の代りにピツチを用いる以外No.1
と同様にして製作しNo.2とした。また従来の周知
の反応焼結法によりNo.1と同形状のテストピース
を作成しNo.3Rとした。これの特性を表1に示
す。表1より、本発明のSiC焼結体は長さ方向の
抗脹力が従来の反応焼結SiCに比し、7割以上大
きく、抗折力が約4割大きかつた。これは耐熱構
造材料として利用範囲を拡大できるものである。
The present invention relates to a method for producing a silicon carbide sintered body having excellent tensile strength in a specific direction. Silicon carbide sintered bodies have low thermal expansion, high mechanical strength and thermal conductivity, and good oxidation resistance, so they are used as heat-resistant structural materials for heating elements, engine parts, and other parts.
Although this material has recently found wide range of uses, it suffers from the disadvantage that it has poor toughness compared to metals, and in particular has weak bulging strength. The present invention improves this and relates to a method for manufacturing a SiC sintered body that has extremely strong bulging strength in a specific direction, in which W fibers are arranged substantially parallel to each other in one plane or in one straight line, and carbon is Manufacture of a fiber-reinforced SiC sintered body, which is characterized by adding a binder contained therein, molding it, thermally decomposing it in a non-oxidizing atmosphere, allowing molten metal silicon to seep through, and making the entire fiber-reinforced SiC. This is a type of reaction sintering method for SiC, but because the W (tungsten) fibers are arranged substantially parallel, it has extremely strong tensile strength in the fiber elongation direction. It has high toughness because a small amount of metallic silicon remains. Next, to form this, if the W fibers are arranged in an unspecified direction on one plane and bonded, a thin plate that is strong against bending and tensile stress can be obtained, and if they are arranged radially, radial tensile stress, that is, centrifugal force It is possible to obtain thin plates and impellers that are particularly strong against
By winding and bonding it to the side surface of a cylindrical or rectangular tube, it is possible to obtain a cylinder or rectangular tube that is extremely resistant to gas stress and thermal strain caused by combustion, even when a combustion reaction occurs inside. Also, if they are arranged parallel to a straight line and joined together, a linear body that is particularly strong in that direction can be obtained, and if this is processed into a circular or coiled shape, it becomes suitable for rings, heat-resistant coil springs, etc. SiC
It has significantly greater toughness than a sintered body. Next, the carbon-containing binder must be adhesive and contain carbon, and pitch, tar, fatty acids, and especially thermoplastic or thermosetting resins can be effectively used. These may be arranged while being kneaded with the W fibers, or after the W fibers are arranged, they may be permeated by applying vibration to the liquid binder. In either method, it is necessary to sufficiently fill the voids between the fibers. If this is insufficient, the sintering will also be insufficient, resulting in a decrease in strength. Next, in order to thermally decompose this and leave carbon behind, a non-oxidizing atmosphere, specifically, a vacuum, hydrogen, argon, nitrogen or the like atmosphere may be used. The decomposed residual carbon at this time fills the gaps in the W in the form of porous and highly active carbon, making it easier for molten metal silicon to permeate through capillary action, and reaction sintering occurs sufficiently at around 1500°C. As a result, a sintered body of W fibers bonded by reactive sintered SiC is obtained, and since a small amount of silicon remains, the body has a significantly large swelling resistance in the direction of the fibers and has high toughness. Silicon carbide also has great oxidation resistance,
It is a high-strength component that can be used in various combustion equipment. The present invention will be explained in more detail below with reference to Examples, but the present invention is not limited thereto. Example 1 Commercially available W fibers were immersed in a mixture of isobutyl methacrylate, nitrocellulose, and dioctyl phthalate to which a small amount of trichlorethylene was added, then piled up in parallel and pressed to a thickness of 2.
A test piece measuring mm x width 10 mm x length 100 mm was created, dried, and heated to 800°C for 5 hours in an N 2 atmosphere to thermally decompose the organic binder and create an object in which W fibers were bonded with carbon. Next, a metal silicon powder was placed in an alumina pod, one end of the test piece was placed in the powder, and the temperature was raised to 1430°C in a vacuum to melt the metal silicon and permeate it into the sintered body. ,
Reaction sintering was completed. Let this be No.1. Next, No. 1 except using Pitch instead of polyurethane resin.
It was made in the same manner as No. 2. In addition, a test piece with the same shape as No. 1 was prepared using a conventional well-known reaction sintering method and designated as No. 3R. The characteristics of this are shown in Table 1. Table 1 shows that the SiC sintered body of the present invention had a longitudinal bulge strength that was 70% greater and a transverse rupture strength that was about 40% greater than conventional reaction sintered SiC. This can expand the scope of its use as a heat-resistant structural material.
【表】
実施例 2
市販のW繊維を一平面上に平行に1mmの厚さに
並べ、炭素粉末を混ぜたタールを含浸させた後、
上記繊維と直角方向に1mmの厚さに並べ、同じく
炭素粉末を混ぜたタールを含浸させ、プレスして
厚さ2mmの平板とし、直径60mmの円板に切断した
後は、実施例1のNo.2と同様にして反応焼結SiC
としNo.4とした。また別に従来の反応焼結法によ
り、同形状の円板を得、これをNo.5Rとしこれら
を第1図に側面図を示す如くピストンの上面に設
置した。図中1はアルミニウム合金製ピストン、
2はSiC焼結体である。これを気筒容積1200c.c.の
内燃機関に取付け、100時間運転したところ、No.
5Rは5個中4個破損したが、No.4は5個中1個
も破損を起さなかつた。
実施例 3
市販のW繊維を溶融ピツチに浸漬し、直径100
mmの円筒の側面に捲回し、厚さ3mmとし、冷却し
て内径100mm、外径106mm、長さ300mmの円筒を成
形した。この後、実施例2と同条件にて反応焼結
SiCとし、No.6とする。次に従来の周知の反応焼
結法にて同形状の円筒を製作しNo.7Rとした。こ
れの内部にて都市ガスを燃焼させ、内部温度を3
分で600℃、700℃、800℃、900℃と上昇させるテ
ストを行つた処、No.7Rは600℃の時に破壊したの
に対し、No.6は900℃迄上昇させても破壊せず、
急熱に著しく強いことが判つた。
実施例 4
市販のW繊維を直径2mmのひも状にし、糖密液
に浸して半乾燥状態にし、直径50mmの円筒の表面
にピツチ10mmのらせん状に捲回して軸方向の長さ
100mmのコイルスプリングとし、実施例2と同様
にして、反応焼結SiCとしNo.8とした。また、従
来の反応焼結法にて同形状のSiCコイルスプリン
グを製作しNo.9Rとし、1000℃の炉中で軸方向に
圧縮し破壊に至る迄の弾性変形量を調べたが、No.
9Rは5mm変形できるのに対して本発明のNo.8は
9mm変形でき、スプリングとして利用価値を大き
く改善できた。
以上の如く本発明によるW焼結体は特定方向に
抗張力大きく、振動衝撃に強く、熱衝撃にも強く
暖性変形も大きくでき強靭で産業上利用価値の大
きい耐熱部品の製造法を提供できるものである。[Table] Example 2 Commercially available W fibers were arranged in parallel on one plane to a thickness of 1 mm, and after impregnated with tar mixed with carbon powder,
The fibers were arranged perpendicularly to the above fibers to a thickness of 1 mm, impregnated with tar mixed with carbon powder, pressed to form a flat plate with a thickness of 2 mm, and cut into disks with a diameter of 60 mm. Reactive sintered SiC in the same manner as in .2.
It was set as No.4. Separately, a disk of the same shape was obtained by a conventional reaction sintering method, and this was designated as No. 5R, and these were placed on the upper surface of the piston as shown in the side view in FIG. 1 in the figure is an aluminum alloy piston,
2 is a SiC sintered body. When this was installed in an internal combustion engine with a cylinder capacity of 1200 c.c. and operated for 100 hours, it achieved No.
5R had 4 out of 5 pieces damaged, but No. 4 didn't have 1 out of 5 breakage. Example 3 Commercially available W fibers were immersed in a molten pitch, and the diameter was 100 mm.
It was wound around the side of a 3 mm cylinder to a thickness of 3 mm, and then cooled to form a cylinder with an inner diameter of 100 mm, an outer diameter of 106 mm, and a length of 300 mm. After this, reaction sintering was carried out under the same conditions as in Example 2.
It will be SiC and number 6. Next, a cylinder with the same shape was manufactured using the conventional well-known reaction sintering method and named No. 7R. City gas is combusted inside this to raise the internal temperature to 3.
In a test where the temperature was raised to 600℃, 700℃, 800℃, and 900℃ in minutes, No. 7R broke down at 600℃, while No. 6 did not break even when the temperature rose to 900℃. ,
It was found to be extremely resistant to sudden heat. Example 4 A commercially available W fiber was made into a string with a diameter of 2 mm, immersed in a molasses solution to make it semi-dry, and wound into a spiral shape with a pitch of 10 mm on the surface of a cylinder with a diameter of 50 mm.
A coil spring of 100 mm was used, and No. 8 was made of reactive sintered SiC in the same manner as in Example 2. In addition, we fabricated a SiC coil spring with the same shape using the conventional reaction sintering method, named No. 9R, and compressed it in the axial direction in a 1000°C furnace to examine the amount of elastic deformation until fracture.
While 9R can be deformed by 5 mm, No. 8 of the present invention can be deformed by 9 mm, greatly improving its utility as a spring. As described above, the W sintered body according to the present invention has high tensile strength in a specific direction, is strong against vibration shock, is strong against thermal shock, and has large warm deformation, and can provide a method for manufacturing heat-resistant parts that are strong and have great industrial utility value. It is.
第1図は本発明の実施例2の試料No.4の繊維強
化SiC焼結体を装着したピストンの側面図。
FIG. 1 is a side view of a piston equipped with a fiber-reinforced SiC sintered body of sample No. 4 of Example 2 of the present invention.
Claims (1)
形し、非酸化性雰囲気中にて結合剤を熱分解し、
溶融金属珪素を滲透して全体を繊維で強化された
SiCとすることを特徴とする繊維強化SiC焼結体
の製造法。 2 W繊維が1平面に実質的に平行に配列した特
許請求の範囲第1項記載の繊維強化SiC焼結体の
製造法。 3 W繊維が1直線に実質的に平行に配列した特
許請求の範囲第1項記載の繊維強化SiC焼結体の
製造法。 4 炭素を含有する結合剤が有機質の樹脂である
特許請求の範囲第1項記載の繊維強化SiC焼結体
の製造法。[Claims] 1 W fibers are molded with a carbon-containing binder, and the binder is thermally decomposed in a non-oxidizing atmosphere;
Penetrated through molten metal silicon and reinforced with fiber throughout
A method for producing a fiber-reinforced SiC sintered body, characterized in that it is made of SiC. 2. The method for producing a fiber-reinforced SiC sintered body according to claim 1, wherein the W fibers are arranged substantially parallel to one plane. 3. The method for producing a fiber-reinforced SiC sintered body according to claim 1, wherein the W fibers are arranged substantially parallel to each other in a straight line. 4. The method for producing a fiber-reinforced SiC sintered body according to claim 1, wherein the carbon-containing binder is an organic resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56151236A JPS5855380A (en) | 1981-09-24 | 1981-09-24 | Manufacture of fiber reinforced sic sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56151236A JPS5855380A (en) | 1981-09-24 | 1981-09-24 | Manufacture of fiber reinforced sic sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5855380A JPS5855380A (en) | 1983-04-01 |
| JPS6225628B2 true JPS6225628B2 (en) | 1987-06-04 |
Family
ID=15514220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56151236A Granted JPS5855380A (en) | 1981-09-24 | 1981-09-24 | Manufacture of fiber reinforced sic sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5855380A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1282943C (en) * | 1985-01-17 | 1991-04-16 | George A. Rossetti, Jr. | Fiber-reinforced ceramic and process therefor |
| JPH09519U (en) * | 1991-12-10 | 1997-10-07 | シンプソン インダストリーズ インコーポレイテッド | Crankshaft vibration damper |
| DE4430393C5 (en) * | 1994-08-26 | 2011-06-30 | Carl Freudenberg KG, 69469 | Torsionally flexible coupling with integrated torsional vibration damper |
-
1981
- 1981-09-24 JP JP56151236A patent/JPS5855380A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5855380A (en) | 1983-04-01 |
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