JPH0536384B2 - - Google Patents
Info
- Publication number
- JPH0536384B2 JPH0536384B2 JP59050365A JP5036584A JPH0536384B2 JP H0536384 B2 JPH0536384 B2 JP H0536384B2 JP 59050365 A JP59050365 A JP 59050365A JP 5036584 A JP5036584 A JP 5036584A JP H0536384 B2 JPH0536384 B2 JP H0536384B2
- Authority
- JP
- Japan
- Prior art keywords
- sic
- strength
- weight
- fibers
- matrix
- 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 - Lifetime
Links
- 239000000835 fiber Substances 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000001746 injection moulding Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical group [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910052644 β-spodumene Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 13
- 238000005245 sintering Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000462 isostatic pressing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052670 petalite Inorganic materials 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 239000003733 fiber-reinforced composite Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Description
本発明はセラミツクをSiC繊維で強化して強度
向上、脆性改善を計つた繊維で強化された複合セ
ラミツクスの製造法に関するものである。
従来、原料のガラス粉末とSiC繊維との混合泥
漿からグリーンシートを成形し、そのシートを積
層接着後、ホツトプレスで焼成し再処理によりマ
トリツクスの結晶化を行つたβ−スポジユメン−
SiC繊維系の公知技術がある。
また、SiC繊維でプリフオーム体を形成し、こ
れにSiC泥漿を含浸させて成形する方法やまた
は、これらの泥漿を鋳込み成形や、これらの混練
物を押出し成形したものをホツトプレスもしくは
反応焼結により焼成したSiC−SiC繊維系の公知
技術がある。
以上のいずれの公知技術ともホツトプレスを用
いる場合は、複数形状品の対応には不適であり、
また前者技術ではホツトプレスで焼成後再処理の
結晶化工程を別に必要とするために製造原価が高
くなる。また後者の反応焼結の場合はその焼結体
の耐熱強度が弱い問題点がある。
本発明は以上の問題点を解決し、ホツトプレス
や結晶化のための熱処理工程を必要としない、生
産性にすぐれた複合セラミツクスの製造法によつ
て、強度向上と脆性改善を計り、利用分野への適
用を拡大したものである。その要旨は、ペタライ
ト、リチウム長石等の結晶質原料粉末にSiC繊維
を10〜50重量％含有した素地を混練し、押出また
は射出成形法にて成形後、樹脂抜きして、更にア
イソスタテイツクプレス後に、1250〜1350℃の非
酸化雰囲気中にて焼結し、マトリツクスの主たる
結晶相がβ−スポジユメンより成ることを特徴と
する繊維で強化された複合セラミツクスの製造法
を提供するものである。
以下、本発明につき詳細に解説する。
SiC繊維を10〜50重量％の含有範囲に限定した
理由は、10重量％以下では抗折強度が所期する
900Kg／cm2以上を確保することが出来ず、強化へ
の効果が少ないためであり、50重量％以上では添
加量のわりには強度が向上せず、またSiC繊維が
高価でコスト高となる。また成形性や焼結後の外
観が悪くなるためである。
また、押出成形法と射出成形法を採用した理由
は、プレス成形では繊維含有のため成形ギレが多
発し、鋳込み成形では寸法精度および生産性に劣
るためであり、グリーンシート積層法では目的形
状への成形が困難である。その点押出成形では単
純形状品の成形性や生産性が良好であり、射出成
形では複雑形状品の成形性や生産性に優れるため
である。
成形体の樹脂抜き後更にアイソスタテイツクプ
レスを採用した理由は、従来技術では焼結後の密
度を上げるためにホツトプレスを採用している
が、これは上記した如く単純形状品だけに適用出
来て複雑形状品には無理である。その点、押出や
射出成形後樹脂抜きして、更にアイソスタテイツ
クプレスによりグリーン密度を向上したのち、非
加圧焼結することにより、焼結後の密度を所望の
レベルに確保し、強度を向上させることができ
る。このアイソスタテイツクプレスは、複雑形状
品において特に好ましく適用出来る。
非酸化雰囲気中での焼成を行なう理由として従
来技術は真空中またはアルゴン等不活性ガス中で
ホツトプレスしている。大気雰囲気中ではSiC繊
維が酸化分解し、ガスを発生し表面層に多量の気
泡が出来、強度が低下する。発泡しない程度の焼
成温度では強度向上が望めない。N2雰囲気中が
最も良好であり、真空中やアルゴンまたはH2お
よびこの混合雰囲気中でも可能である。
以上にて焼結したものは、マトリツクスの主た
る結晶相がβ−スポジユメンであるが、使用する
原料としては、Li2O・Al2O3・8SiO2の結晶組成
のペタライトが良好であり、その他にLi2O・
Al2O3・6SiO2の結晶組成のリチウム長石が使用
出来る。本願発明は、これらの結晶質原料粉末に
SiC繊維を含有させた素地を混練して用いるもの
である。
本発明の製造法で得られた複合セラミツクス
は、脆性が改善され抗折強度が910〜1940Kg／cm2
と大きく強化され、SiC繊維の無含有セラミツク
スは790Kg／cm2であつた。
本発明はデイーゼルエンジンのチヤンバーや一
般エンジンのポートライナー等の製造に利用する
ことが出来る。
以下、実施例につき具体的に述べる。
実施例
ペタライト粉末に日本カーボン製で商品名ニカ
ロンの径10〜20μｍ、長さ６mmのSiC繊維を０、
８、10、20、40、50、55重量％含有させる様調合
し、これら100重量部の各々に対してメチルセル
ローズを６重量％と水36重量％を添加して充分混
練後、押出成形機で径５mmφを押出し乾燥後、長
さ50mmに切断し、500℃中にて樹脂抜き後、ゴム
チユーブに入れ密閉して1500Kg／cm2でアイソスタ
テイツクプレスを行つた。これをN2雰囲気下の
1280℃中１時間加熱して焼結した。
これらの試料を三点曲げ試験機にて抗折強度を
測定し、また相対密度を繊維の密度2.55、マトリ
ツクスの密度2.365としてマトリツクス部のみの
算出を行い下表に示した。
また、粉末Ｘ線回折による同定の結果、主結晶
相はβスポジユメンとβ−SiCであつた。
The present invention relates to a method for producing fiber-reinforced composite ceramics in which ceramic is reinforced with SiC fibers to improve strength and brittleness. Conventionally, a green sheet was formed from a mixed slurry of raw material glass powder and SiC fibers, and the sheets were laminated and bonded, then fired in a hot press and reprocessed to crystallize the matrix.
There is a known technology based on SiC fibers. In addition, there is a method of forming a preform body from SiC fibers and impregnating it with SiC slurry and molding it, or casting the slurry, extrusion molding of the kneaded material, and firing it by hot pressing or reaction sintering. There is a known technology of SiC-SiC fiber system. When using a hot press with any of the above-mentioned known techniques, it is unsuitable for producing products with multiple shapes;
In addition, the former technique requires a separate crystallization step of reprocessing after firing in hot pressing, which increases manufacturing costs. In addition, in the case of the latter reaction sintering, there is a problem that the heat resistance strength of the sintered body is low. The present invention solves the above problems and improves strength and brittleness through a highly productive method for manufacturing composite ceramics that does not require hot pressing or heat treatment for crystallization, and is applicable to the field of application. This is an expanded application of . The gist is that a base material containing 10 to 50% by weight of SiC fibers is kneaded with crystalline raw material powder such as petalite or lithium feldspar, molded by extrusion or injection molding, resin removed, and then isostatically pressed. The present invention is then sintered in a non-oxidizing atmosphere at 1250 to 1350 DEG C., and provides a method for producing fiber-reinforced composite ceramics characterized in that the main crystal phase of the matrix is composed of .beta.-spodium. The present invention will be explained in detail below. The reason for limiting the SiC fiber content to 10 to 50% by weight is that below 10% by weight, the bending strength is lower than expected.
This is because it is not possible to secure a content of 900 Kg/cm 2 or more, and the effect on reinforcement is small. If the content is more than 50% by weight, the strength will not improve despite the amount added, and the SiC fiber will be expensive. This is also because moldability and appearance after sintering deteriorate. In addition, the reason why we adopted extrusion molding and injection molding is that press molding often suffers from molding glitches due to the fiber content, and cast molding is inferior in dimensional accuracy and productivity, while green sheet lamination is not suitable for achieving the desired shape. It is difficult to mold. In this respect, extrusion molding has good moldability and productivity for products with simple shapes, while injection molding has excellent moldability and productivity for products with complex shapes. The reason why we adopted isostatic press after resin removal from the molded body is that in conventional technology, hot press is used to increase the density after sintering, but as mentioned above, this can only be applied to products with simple shapes. This is not possible for products with complex shapes. In this regard, by removing the resin after extrusion or injection molding, improving the green density by isostatic pressing, and then performing non-pressure sintering, we can ensure the density after sintering at the desired level and increase the strength. can be improved. This isostatic press can be particularly preferably applied to products with complex shapes. The reason for firing in a non-oxidizing atmosphere is that in the prior art, hot pressing is carried out in vacuum or in an inert gas such as argon. In the air, SiC fibers oxidize and decompose, producing gas and forming a large number of bubbles in the surface layer, reducing its strength. No improvement in strength can be expected at firing temperatures that do not cause foaming. N 2 atmosphere is best, vacuum and argon or H 2 and mixtures thereof are also possible. The main crystalline phase of the matrix of the sintered product above is β-spodumene, but petalite with a crystal composition of Li 2 O, Al 2 O 3 , 8SiO 2 is good as a raw material, and other to Li 2 O・
Lithium feldspar with a crystal composition of Al 2 O 3 6SiO 2 can be used. The present invention applies to these crystalline raw material powders.
It is used by kneading a base material containing SiC fibers. The composite ceramics obtained by the production method of the present invention have improved brittleness and a bending strength of 910 to 1940 Kg/cm 2
The strength of the SiC fiber-free ceramics was 790 kg/cm 2 . The present invention can be used to manufacture chambers for diesel engines, port liners for general engines, and the like. Examples will be described in detail below. Example: Petalite powder was coated with SiC fibers manufactured by Nippon Carbon under the trade name Nicalon with a diameter of 10 to 20 μm and a length of 6 mm.
8, 10, 20, 40, 50, and 55 parts by weight.To each of these 100 parts by weight, 6% by weight of methylcellulose and 36% by weight of water were added, and after thorough kneading, the extrusion molding machine was used. After drying and extruding a piece with a diameter of 5 mmφ, it was cut into pieces of 50 mm in length, and after the resin was removed at 500°C, it was placed in a rubber tube and sealed, followed by isostatic pressing at 1500 kg/cm 2 . This is done under N2 atmosphere.
It was sintered by heating at 1280°C for 1 hour. The bending strength of these samples was measured using a three-point bending tester, and the relative densities were calculated for the matrix portion only, with the fiber density of 2.55 and the matrix density of 2.365, as shown in the table below. Further, as a result of identification by powder X-ray diffraction, the main crystal phases were β-spodumene and β-SiC.
【表】
以上の特性調査の外に、射出成形機を用いて繊
維含有量20、50％のものにつきターボチヤジヤロ
ーターの成形と樹脂抜き後のアイソスタテイツク
プレスおよび焼結テストを行つたところ、外観に
ついては良好な結果を得ることが出来た。
本発明は上記の如く、単純形状品から複雑形状
品の作成に適し、かつ脆性の改善と強度向上によ
り、その適用を拡大したもので今後の利用への期
待は大きい。[Table] In addition to the above characteristics investigation, turbocharger rotors were molded using an injection molding machine with fiber content of 20% and 50%, and isostatic pressing and sintering tests were conducted after resin removal. Good results were obtained regarding the appearance. As described above, the present invention is suitable for producing products with simple shapes to complex shapes, and its application has been expanded by improving brittleness and increasing strength, and there are high expectations for its future use.
Claims (1)
有した素地を混練し、押出または射出成形法にて
成形後、樹脂抜きして、更にアイソスタテイツク
プレス後に、1250〜1350℃の非酸化雰囲気中にて
焼結し、マトリツクスの主たる結晶相がβ−スポ
ジユメンより成ることを特徴とする繊維で強化さ
れた複合セラミツクスの製造法。1. A base material containing 10 to 50% by weight of SiC fibers is kneaded with crystalline raw material powder, molded by extrusion or injection molding, resin removed, and isostatically pressed to form a non-oxidized material at 1250 to 1350°C. A method for producing composite ceramics reinforced with fibers, characterized in that the main crystalline phase of the matrix is β-spodumene, which is sintered in an atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59050365A JPS60195064A (en) | 1984-03-15 | 1984-03-15 | Fiber reinforced composite ceramics and manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59050365A JPS60195064A (en) | 1984-03-15 | 1984-03-15 | Fiber reinforced composite ceramics and manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60195064A JPS60195064A (en) | 1985-10-03 |
| JPH0536384B2 true JPH0536384B2 (en) | 1993-05-28 |
Family
ID=12856860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59050365A Granted JPS60195064A (en) | 1984-03-15 | 1984-03-15 | Fiber reinforced composite ceramics and manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60195064A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4769346A (en) * | 1986-10-24 | 1988-09-06 | Corning Glass Works | Whisker composite ceramics for metal extrusion or the like |
| JPH11240749A (en) * | 1998-02-27 | 1999-09-07 | Taiheiyo Cement Corp | Ceramic reinforced with fiber and its production |
| JP4540239B2 (en) * | 2001-01-31 | 2010-09-08 | 京セラ株式会社 | Aluminosilicate sintered body and stress relieving member using the same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5520259A (en) * | 1978-07-28 | 1980-02-13 | Ngk Spark Plug Co | Production of high density sintered body |
| JPS56109186A (en) * | 1980-02-04 | 1981-08-29 | Mitsubishi Heavy Ind Ltd | Monitoring method for shielding gas for welding |
| JPS56169186A (en) * | 1980-02-13 | 1981-12-25 | United Technologies Corp | Silicon carbide fiber reinforced ceramic composite material |
| JPS57160974A (en) * | 1981-03-10 | 1982-10-04 | Asea Ab | Manufacture of ceramic products |
-
1984
- 1984-03-15 JP JP59050365A patent/JPS60195064A/en active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5520259A (en) * | 1978-07-28 | 1980-02-13 | Ngk Spark Plug Co | Production of high density sintered body |
| JPS56109186A (en) * | 1980-02-04 | 1981-08-29 | Mitsubishi Heavy Ind Ltd | Monitoring method for shielding gas for welding |
| JPS56169186A (en) * | 1980-02-13 | 1981-12-25 | United Technologies Corp | Silicon carbide fiber reinforced ceramic composite material |
| JPS57160974A (en) * | 1981-03-10 | 1982-10-04 | Asea Ab | Manufacture of ceramic products |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60195064A (en) | 1985-10-03 |
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