JPH0481547B2 - - Google Patents
Info
- Publication number
- JPH0481547B2 JPH0481547B2 JP62157520A JP15752087A JPH0481547B2 JP H0481547 B2 JPH0481547 B2 JP H0481547B2 JP 62157520 A JP62157520 A JP 62157520A JP 15752087 A JP15752087 A JP 15752087A JP H0481547 B2 JPH0481547 B2 JP H0481547B2
- Authority
- JP
- Japan
- Prior art keywords
- sic
- whiskers
- thin film
- sic whiskers
- carbonaceous thin
- 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
- 239000010409 thin film Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000011226 reinforced ceramic Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 229920001187 thermosetting polymer Polymers 0.000 claims description 5
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 239000011224 oxide ceramic Substances 0.000 claims description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000010304 firing Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 239000005011 phenolic resin Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001568 phenolic resin Polymers 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Description
〔産業上の利用分野〕
本発明は、SiCウイスカーで複合強化したセラ
ミツクスの製造方法に関する。
〔従来の技術〕
耐熱性や耐食性に優れたセラミツクス材料は、
エンジンをはじめ高温下に用いられる各種構造部
材として有用されている。
一般にセラミツクス材料は、破壊靭性が充分で
なく、微小な傷や内部欠陥により応力の集中が生
じ易く破壊してしまう欠点がある。
近年この破壊靭性を向上させる方法が広く研究
されており、ウイスカーをセラミツクスに複合化
することにより靭性を向上させる試みも種々提案
されている。これは高弾性を有するウイスカーを
分散複合化することにより、セラミツクス中にお
けるクラツクの成長を停止あるいは抑制して、ク
ラツクの進行方向を屈曲させて応力集中を緩和
し、あるいはウイスカーの引き抜き効果により、
クラツク先端でのエネルギーを吸収して破壊靭性
の向上をはかるものである。
この場合、ウイスカーとセラミツクスとの界面
結合の状態が大きく影響し、界面結合が大きいと
上記破壊靭性向上効果が充分発揮されない。ま
た、界面結合が小さいとクラツク発生の起点とな
る欠点がある。
この改善策として、ウイスカーとセラミツクス
を複合化するに当り、SiCウイスカーの表面に
CVD法により炭素を被覆してからAl2O3と複合化
する方法が提案されている（第25回窯業基礎討論
会講演要旨集P41）が、この場合の炭素被覆層は
層膜が厚く（約450Å）不均一であるために、か
えつて強度、破壊靭性の低下を招く結果となつて
いる。
このように高温耐食性構造部材用として、セラ
ミツクス材料の破壊靭性を向上させることは極め
て重要な課題であるにも拘わらず、有効な改善手
段は見出されていない。
〔発明が解決しようとする問題点〕
本発明は、上記問題点を解決するために、SiC
ウイスカーとセラミツクスとの界面結合を制御す
ることにより、破壊靭性の大きいSiCウイスカー
強化セラミツクスの製造方法を提供するものであ
る。
〔問題点を解決するための手段〕
すなわち本発明は、SiCウイスカーの表面に炭
素質薄膜を形成被着した後、炭化物、窒化物、酸
化物系セラミツク粉末と混合し、不活性雰囲気も
しくは真空中で焼結することを特徴とするSiCウ
イスカー強化セラミツクスの製造方法である。
SiCウイスカーは直径0.1〜1μm、長さ30〜
100μmの針状単結晶から成るものであり、強度特
性が大きく補強材として有用されている。この
SiCウイスカーをセラミツクス材料に分散複合化
して靭性の向上をはかる場合、SiOウイスカーは
セラミツクス材料との界面において密に結合する
ために、ウイスカーの引き抜き効果が充分発揮さ
れず、破壊靭性の向上をはかることが難しい。
本発明は、SiCウイスカーの表面に単分子膜に
相当する程度の炭素質薄膜を形成被着して、ウイ
スカーとセラミツクスとの界面結合を調節するこ
とにより、破壊靭性の向上をはかることができる
ことを知見して完成したものである。
SiCウイスカー表面に炭素質薄膜を形成被着さ
せるためには、まず熱硬化性樹脂を有機溶媒に溶
解して0.5％以下の希薄溶液に調製する。次いで
長時間、例えば数日間放置して、熱硬化性樹脂の
高分子中に有機溶媒が無制限に混ざる状態、すな
わち微視的に均一に一相化することが必要であ
る。
熱硬化性樹脂としては炭化率の大きいフエノー
ル系やフラン系樹脂が、有機溶媒としてはエタノ
ール、アセトン、ベンゼン、トルエンなどが好ま
しく用いられる。
このように有機溶媒が連続相となつた溶液中に
SiCウイスカーを50〜200ｇ／ｌ程度の濃度に分
散させ、過乾燥して有機溶媒を除去し、加熱硬
化した後、非酸化性雰囲気中800〜1200℃で焼成
炭化して炭素質の薄膜を被着させる。このように
して単分子膜に近い７〜20Å程度の非常に薄い炭
素質被膜相が形成される。この場合過はできる
だけ緩やかに行い、加熱硬化および焼成炭化処理
も緩徐に行うことが好ましい。
炭素質薄膜を形成被着したSiCウイスカーは、
次いでセラミツクス粉末およびY2O3などの焼結
助剤と水中で混合分散させ、過乾燥して均一な
混合粉末とした後、常法に従つて不活性雰囲気も
しくは真空中でホツトプレスにより焼結して、
SiCウイスカー強化セラミツクス材料を得る。こ
の際、マトリツクス材となるセラミツクスとして
は、SiC，TiC，Si3N4，Al2O3などの各種炭化
物、窒化物、酸化物系セラミツクスの粉末が用い
られる。
〔作用〕
上記構成に基づき、SiCウイスカー表面に単分
子膜に相当する程度の炭素質薄膜を形成被着する
ことにより、セラミツクス粉末との界面結合力を
適度に調節することができ、引き抜き効果による
破壊靭性および強度の増大化を可能とする。更に
炭素質薄膜は界面における衝撃を和らげるクツシ
ヨン的機能を有するので靭性破壊の鋭敏性を低下
する作用を営む。
〔実施例〕
(1) フエノール樹脂（群栄化学製レジトツプ
PGA−4508）14.4ｇをエタノール4780ml中に
溶解（濃度0.3wt％）した後７日間静置して、
フエノール樹脂の高分子鎖がエタノール中に均
一相に分散する溶液を調製した。
この溶液中にSiCウイスカー（直径0.1〜
1μm、長さ30〜100μm）480ｇを攪拌混合して
充分に分散させた後過し、風乾してエタノー
ルを揮散除去した。SiCウイスカーに付着した
フエノール樹脂は2.4ｇであつた。次いで170℃
で２時間加熱してフエノール樹脂を硬化した
後、高周波炉にてアルゴン雰囲気1000℃の温度
で４時間焼成炭化した。
このようにして得られた炭素質薄膜を形成被
着したSiCウイスカーの表面を透過型電子顕微
鏡写真（TEM）で観察した。写真観察の結果
から炭素質薄膜の厚さは約15Åであつた。
フエノール樹脂96ｇをエタノール4700ml中に
溶解（濃度2wt％）し、７日間静置して調製し
た溶液を使用した以外は、同一の方法で処理し
たSiCウイスカー表面に被着した炭素質薄膜の
厚さは約100Åであつた。
(2) この炭素質薄膜を被着したSiCウイスカーと
Si3N4粉末（粒度0.2μm）とを所定の割合で水
中に分散させ、過乾燥して均一な混合粉末を
得た。なお、焼結助剤として、Y2O3をSi3N4粉
末に10wt％の割合で添加した。この混合粉体
を真空中、1800℃、35MPaの条件でホツトプ
レスして直径40mm、厚さ５mmのセラミツクス焼
結体を得た。このセラミツクス焼結体の破壊靭
性、曲げ強度特性を測定して表−１に示した。
なお、比較のための炭素質薄膜を被着しない
SiCウイスカーについても実施し、同表中に併
記した。
表−１の結果から、炭素質薄膜とくに15Å程
度の薄膜を形成被着することによつて、破壊靭
性や強度の向上をはかることができる。
[Industrial Application Field] The present invention relates to a method for producing ceramics compositely reinforced with SiC whiskers. [Conventional technology] Ceramic materials with excellent heat resistance and corrosion resistance are
It is useful as a variety of structural members used at high temperatures, including engines. Ceramic materials generally have the disadvantage that they do not have sufficient fracture toughness and are prone to stress concentration due to minute scratches or internal defects, resulting in fracture. In recent years, methods for improving fracture toughness have been widely studied, and various attempts have been made to improve toughness by compounding whiskers with ceramics. This is achieved by dispersing and compounding highly elastic whiskers, stopping or suppressing the growth of cracks in ceramics, bending the direction of propagation of cracks to alleviate stress concentration, or by pulling out the whiskers.
It aims to improve fracture toughness by absorbing energy at the tip of the crack. In this case, the state of interfacial bonding between the whiskers and the ceramics has a large effect, and if the interfacial bonding is large, the above-mentioned effect of improving fracture toughness will not be sufficiently exhibited. In addition, if the interfacial bond is small, there is a drawback that it becomes a starting point for crack generation. As a measure to improve this, when combining whiskers and ceramics, the surface of SiC whiskers is
A method has been proposed in which carbon is coated using the CVD method and then composited with Al 2 O 3 (P41 of the 25th Ceramics Basics Conference Lecture Abstracts), but the carbon coating layer in this case is thick ( The non-uniformity (approximately 450 Å) results in a decrease in strength and fracture toughness. Although it is an extremely important issue to improve the fracture toughness of ceramic materials for use in high-temperature corrosion-resistant structural members, no effective means of improvement has yet been found. [Problems to be Solved by the Invention] In order to solve the above problems, the present invention
The present invention provides a method for producing SiC whisker-reinforced ceramics with high fracture toughness by controlling the interfacial bonding between whiskers and ceramics. [Means for solving the problem] That is, the present invention forms and deposits a carbonaceous thin film on the surface of SiC whiskers, mixes it with carbide, nitride, and oxide ceramic powder, and then heats it in an inert atmosphere or vacuum. This is a method for producing SiC whisker-reinforced ceramics, which is characterized by sintering. SiC whiskers have a diameter of 0.1~1μm and a length of 30~
It is made of a 100μm needle-shaped single crystal, and has great strength properties, making it useful as a reinforcing material. this
When trying to improve toughness by dispersing and compounding SiC whiskers into ceramic materials, the SiO whiskers are tightly bonded at the interface with the ceramic material, so the whisker pullout effect is not sufficiently exerted, making it difficult to improve fracture toughness. is difficult. The present invention shows that fracture toughness can be improved by forming and depositing a thin carbon film equivalent to a monomolecular film on the surface of SiC whiskers and adjusting the interfacial bond between the whiskers and ceramics. This is what I learned and completed. In order to form and adhere a carbonaceous thin film to the surface of SiC whiskers, first, a thermosetting resin is dissolved in an organic solvent to prepare a dilute solution of 0.5% or less. It is then necessary to leave it for a long period of time, for example, several days, so that the organic solvent is mixed in the polymer of the thermosetting resin without restriction, that is, it is microscopically uniform and becomes one phase. As the thermosetting resin, phenolic or furan resins having a high carbonization rate are preferably used, and as the organic solvent, ethanol, acetone, benzene, toluene, etc. are preferably used. In this way, in a solution where the organic solvent is the continuous phase,
SiC whiskers are dispersed at a concentration of about 50 to 200 g/l, overdried to remove the organic solvent, heated and hardened, and then fired and carbonized at 800 to 1200°C in a non-oxidizing atmosphere to form a carbonaceous thin film. Let them wear it. In this way, a very thin carbonaceous film phase of about 7 to 20 Å, close to a monomolecular film, is formed. In this case, it is preferable to carry out the filtration as slowly as possible, and also to carry out heat curing and calcination carbonization slowly. SiC whiskers coated with a carbonaceous thin film are
Next, the ceramic powder and a sintering aid such as Y 2 O 3 are mixed and dispersed in water, overdried to form a uniform mixed powder, and then sintered using a hot press in an inert atmosphere or vacuum according to a conventional method. hand,
Obtain SiC whisker-reinforced ceramic material. At this time, the ceramics used as the matrix material include powders of various carbide, nitride, and oxide ceramics such as SiC, TiC, Si 3 N 4 , and Al 2 O 3 . [Function] Based on the above structure, by forming and depositing a carbonaceous thin film equivalent to a monomolecular film on the SiC whisker surface, the interfacial bonding force with the ceramic powder can be adjusted appropriately, and the Enables increase in fracture toughness and strength. Furthermore, since the carbonaceous thin film has a cushion-like function that cushions the impact at the interface, it acts to reduce the sensitivity of toughness fracture. [Example] (1) Phenol resin (Gunei Chemical Resistop)
PGA-4508) 14.4g was dissolved in 4780ml of ethanol (concentration 0.3wt%) and left to stand for 7 days.
A solution in which the polymer chains of phenolic resin were dispersed in a homogeneous phase in ethanol was prepared. SiC whiskers (diameter 0.1~
1 μm, length 30 to 100 μm) were stirred and mixed to sufficiently disperse them, filtered, and air-dried to volatilize and remove ethanol. The amount of phenolic resin attached to the SiC whiskers was 2.4 g. Then 170℃
After curing the phenolic resin by heating for 2 hours, it was fired and carbonized in a high frequency furnace at a temperature of 1000°C in an argon atmosphere for 4 hours. The surface of the SiC whiskers on which the carbonaceous thin film thus obtained was formed and adhered was observed using a transmission electron micrograph (TEM). From the results of photographic observation, the thickness of the carbonaceous thin film was approximately 15 Å. Thickness of carbonaceous thin film deposited on the surface of SiC whiskers treated in the same manner except that a solution prepared by dissolving 96 g of phenolic resin in 4700 ml of ethanol (concentration 2 wt%) and allowing it to stand for 7 days was used. was approximately 100 Å. (2) SiC whiskers coated with this carbonaceous thin film and
Si 3 N 4 powder (particle size: 0.2 μm) was dispersed in water at a predetermined ratio and overdried to obtain a uniform mixed powder. Note that Y 2 O 3 was added to the Si 3 N 4 powder at a rate of 10 wt% as a sintering aid. This mixed powder was hot pressed in a vacuum at 1800° C. and 35 MPa to obtain a ceramic sintered body having a diameter of 40 mm and a thickness of 5 mm. The fracture toughness and bending strength characteristics of this ceramic sintered body were measured and shown in Table 1.
For comparison, a carbonaceous thin film was not applied.
The test was also conducted for SiC whiskers and is also listed in the same table. From the results in Table 1, it is possible to improve fracture toughness and strength by forming and depositing a carbonaceous thin film, especially a thin film of about 15 Å.
【表】【table】
上記説明で明らかなように、本発明の手法によ
るSiCウイスカーの複合強化により、高温構造部
材として有用な破壊靭性、曲げ強度の大きなセラ
ミツクス材料の製造が可能となる。
As is clear from the above description, composite reinforcement of SiC whiskers by the method of the present invention makes it possible to produce ceramic materials with high fracture toughness and bending strength useful as high-temperature structural members.
Claims (1)
着した後、炭化物、窒化物、酸化物系セラミツク
粉末と混合し、不活性雰囲気もしくは真空中で焼
結することを特徴とするSiCウイスカー強化セラ
ミツクスの製造方法。 ２ 熱硬化性樹脂を有機溶媒に溶解し、充分に均
相化させた溶液中にSiCウイスカーを分散させ、
過乾燥して有機溶媒を除去し、次いで加熱して
熱硬化性樹脂を硬化した後、非酸化性雰囲気中で
800〜1200℃に焼成炭化してSiCウイスカーの表
面に７〜20Åの炭素質薄膜を形成被着する特許請
求の範囲第１項記載のSiCウイスカー強化セラミ
ツクスの製造方法。[Claims] 1. A carbonaceous thin film is formed and deposited on the surface of SiC whiskers, then mixed with carbide, nitride, or oxide ceramic powder, and sintered in an inert atmosphere or vacuum. A method for producing SiC whisker-reinforced ceramics. 2. Dissolve the thermosetting resin in an organic solvent, disperse SiC whiskers in the sufficiently homogenized solution,
After over-drying to remove the organic solvent and then heating to cure the thermosetting resin, in a non-oxidizing atmosphere.
2. The method for producing SiC whisker-reinforced ceramics according to claim 1, which comprises firing and carbonizing the SiC whiskers at 800 to 1,200°C to form a carbonaceous thin film of 7 to 20 Å on the surface of the SiC whiskers.
Priority Applications (8)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62157520A JPS643081A (en) | 1987-06-26 | 1987-06-26 | Production of sic whisker reinforced ceramic |
| GB8812149A GB2206572B (en) | 1987-06-26 | 1988-05-23 | Surface-coated sic whiskers, processes for preparing the same, ceramic reinforced with the same, and process for preparing said reinforced ceramic |
| US07/200,265 US4929472A (en) | 1987-06-26 | 1988-05-31 | Surface-coated SiC whiskers, processes for preparing the same, ceramic reinforced with the same, and process for preparing said reinforced ceramic |
| FR8807395A FR2617201A1 (en) | 1987-06-26 | 1988-06-03 | SIC FIBERS WITH SURFACE COATING, PROCESSES FOR THEIR PREPARATION, REINFORCED CERAMIC THEREOF AND PROCESS FOR PREPARING THE SAME |
| DE3844729A DE3844729C2 (en) | 1987-06-26 | 1988-06-09 | Coated silicon carbide whiskers for ceramic matrix composites |
| DE3819560A DE3819560A1 (en) | 1987-06-26 | 1988-06-09 | SIC-WHISKER, CERAMIC MATERIALS REINFORCED WITH THEM AND METHOD FOR THE PRODUCTION THEREOF |
| US07/479,025 US4975302A (en) | 1987-06-26 | 1990-02-12 | Surface-coated SiC whiskers, processes for preparing the same, ceramic reinforced with the same, and process for preparing said reinforced ceramic |
| GB9104670A GB2241943B (en) | 1987-06-26 | 1991-03-06 | Surface coated sic whiskers,processes for preparing the same,ceramic reinforced with the same,and process for preparing said reinforced ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62157520A JPS643081A (en) | 1987-06-26 | 1987-06-26 | Production of sic whisker reinforced ceramic |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JPH013081A JPH013081A (en) | 1989-01-06 |
| JPS643081A JPS643081A (en) | 1989-01-06 |
| JPH0481547B2 true JPH0481547B2 (en) | 1992-12-24 |
Family
ID=15651468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62157520A Granted JPS643081A (en) | 1987-06-26 | 1987-06-26 | Production of sic whisker reinforced ceramic |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS643081A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04130058A (en) * | 1990-09-20 | 1992-05-01 | Japan Metals & Chem Co Ltd | Composite silicon carbide sintered body containing silicon carbide whisker |
| JP2704475B2 (en) * | 1991-11-29 | 1998-01-26 | 宇部興産株式会社 | Inorganic fiber reinforced ceramic composite |
-
1987
- 1987-06-26 JP JP62157520A patent/JPS643081A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS643081A (en) | 1989-01-06 |
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