JPH10226583A - Fiber reinforced ceramic sintered body - Google Patents
Fiber reinforced ceramic sintered bodyInfo
- Publication number
- JPH10226583A JPH10226583A JP9048406A JP4840697A JPH10226583A JP H10226583 A JPH10226583 A JP H10226583A JP 9048406 A JP9048406 A JP 9048406A JP 4840697 A JP4840697 A JP 4840697A JP H10226583 A JPH10226583 A JP H10226583A
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- fibers
- fiber
- sintered body
- oxide layer
- silicon
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はセラミツクス繊維か
らなる不織布を用いた繊維強化セラミツクス焼結体に関
するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fiber-reinforced ceramic sintered body using a nonwoven fabric made of ceramic fibers.
【０００２】[0002]
【従来の技術】従来、長繊維フイラメントを平行に配置
した繊維強化セラミツクス複合材料ａ、長繊維フイラメ
ントを織つて３次元構造に配置した繊維強化セラミツク
ス複合材料ｂ、短繊維を不規則に配向した繊維強化セラ
ミツクス複合材料ｃ、不織布の表面に溶液を用いたデイ
ツプコーテイング、ＣＶＤ、蒸着などの被覆処理を行つ
て繊維の交差部分を固着した繊維プリフオーム材料（米
国特許第4,761,323 号）ｄなどが知られている。しか
し、（ａ）上述の材料ａは繊維を連続的に繰り出しなが
ら成形するものであるので、繊維の配向が一方向にな
り、形状が限定される、（ｂ）材料ｂは３次元織物の形
状が制限され、織物の製造経費が高い、（ｃ）材料ｃは
繊維を均一に分散させることが難しい、（ｄ）材料ｄは
均質な被覆処理が難しく、したがつて平滑な材料表面が
得にくいなどの難点がある。2. Description of the Related Art Conventionally, a fiber-reinforced ceramic composite material a in which long fiber filaments are arranged in parallel, a fiber-reinforced ceramic composite material b in which long fiber filaments are woven and arranged in a three-dimensional structure, and fibers in which short fibers are irregularly oriented. A reinforced ceramics composite material c, a fiber preform material (US Pat. No. 4,761,323) d in which the intersection of the fibers is fixed by performing a coating treatment such as a dip coating using a solution, CVD, or vapor deposition on the surface of the nonwoven fabric, and the like are known. ing. However, since (a) the material a is formed while continuously drawing out the fiber, the orientation of the fiber is in one direction, and the shape is limited. (B) The material b is the shape of a three-dimensional woven fabric. And (c) it is difficult to uniformly disperse the fibers, (d) it is difficult to uniformly coat the material (d), and thus it is difficult to obtain a smooth material surface. There are difficulties such as.
【０００３】[0003]
【発明が解決しようとする課題】本発明の課題は上述の
問題に鑑み、強化繊維の分散が均一で繊維の配向が不規
則であり、機械的強度に優れた繊維強化セラミツクス焼
結体を提供することにある。SUMMARY OF THE INVENTION In view of the above-mentioned problems, an object of the present invention is to provide a fiber-reinforced ceramics sintered body having a uniform dispersion of reinforcing fibers, irregular fiber orientation, and excellent mechanical strength. Is to do.
【０００４】[0004]
【課題を解決するための手段】上記課題を解決するため
に、本発明の構成は繊維強化セラミツクス焼結体の表面
に少くとも１つの酸化物層が形成された強化繊維が均一
に分散し、強化繊維の配向が不規則でありかつ強化繊維
相互の接触部分が前記酸化物層により接合されているこ
とを特徴とする。In order to solve the above-mentioned problems, the present invention provides a fiber-reinforced ceramics sintered body in which at least one oxide layer is formed on the surface thereof, and the reinforcing fibers are uniformly dispersed. The orientation of the reinforcing fibers is irregular, and the contact portions between the reinforcing fibers are joined by the oxide layer.
【０００５】[0005]
【発明の実施の形態】本発明では強化繊維として、セラ
ミツクス短繊維から不織布を加工し、該不織布に酸化処
理、コーテイングなどを施して、不織布の表面に酸化物
層を形成し、該酸化物層により不織布の繊維相互の接触
部分を接合する。得られた不織布を強化材に用い、不織
布の隙間にセラミツクスのスラリーを重点した後に焼成
して繊維強化セラミツクス焼結体を形成する。BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, a nonwoven fabric is processed from a ceramic short fiber as a reinforcing fiber, and the nonwoven fabric is subjected to an oxidation treatment and a coating to form an oxide layer on the surface of the nonwoven fabric. By this, the contact portions between the fibers of the nonwoven fabric are joined. The obtained nonwoven fabric is used as a reinforcing material, and a ceramic slurry is formed by emphasizing a ceramic slurry in gaps between the nonwoven fabrics and firing.
【０００６】[0006]
［実施例１］図１に示すように、太さ５〜２０μｍのSi
-C-Ti-O 繊維を長さ３０〜５０ｍｍに切断して短繊維２
をつくり、短繊維２の配向を不規則にして積層し、カー
デイングを施して不織布２０を作製する。次いで、不織
布２０を温度１０００℃の大気中で１０時間加熱した。
その結果、図２に示すように、不織布２０の短繊維２の
表面に２酸化ケイ素（SiO2）からなる厚さ最大５μｍの
酸化物層６が形成され、かつ短繊維相互の接触部分４が
酸化物層６により接合された不織布２０が得られた。酸
化前の不織布２０と酸化後の不織布２０とについて圧縮
試験を行つた結果、酸化後の不織布２０の方が大きな弾
性率を示し、剛性が向上したことが分かつた。[Example 1] As shown in FIG.
-C-Ti-O fiber cut into 30-50mm length and short fiber 2
The nonwoven fabric 20 is manufactured by laminating the short fibers 2 in an irregular orientation and performing carding. Next, the nonwoven fabric 20 was heated in the air at a temperature of 1000 ° C. for 10 hours.
As a result, as shown in FIG. 2, an oxide layer 6 having a maximum thickness of 5 μm made of silicon dioxide (SiO 2 ) is formed on the surface of the short fiber 2 of the nonwoven fabric 20 and the contact portion 4 between the short fibers is formed. The nonwoven fabric 20 joined by the oxide layer 6 was obtained. A compression test was performed on the non-woven fabric 20 before oxidation and the non-woven fabric 20 after oxidation, and it was found that the non-woven fabric 20 after oxidation showed a higher elastic modulus and improved rigidity.
【０００７】スリツプキヤスト法により、不織布２０の
短繊維相互の隙間に、ケイ素（Si）と、焼結助剤である
アルミナ（Al2O3 ）とイツトリア（Y2O3）を原料とする
セラミツクスのスラリーを充填して成形体を作製した。
強化材として酸化前の不織布２０を用いた場合は、不織
布２０にスラリーを充填する時に、スラリーが不織布２
０の隙間から潰れてしまい、良好な成形体が得られなか
つた。しかし、強化材として酸化後の不織布２０を用い
た場合は、スラリーが不織布２０の隙間から潰れことは
なく、不織布２０の隙間にセラミツクスのスラリーが充
填され、良好な成形体が得られた。[0007] A ceramic made from silicon (Si), alumina (Al 2 O 3 ) as a sintering aid, and yttria (Y 2 O 3 ) as raw materials in gaps between short fibers of the nonwoven fabric 20 by a slip casting method. Was formed into a compact.
When the non-woven fabric 20 before oxidation is used as the reinforcing material, when the non-woven fabric 20 is filled with the slurry,
Thus, the molded product was crushed from the gap 0, and a good molded product could not be obtained. However, when the oxidized nonwoven fabric 20 was used as the reinforcing material, the slurry did not collapse from the gap between the nonwoven fabrics 20, and the gap between the nonwoven fabrics 20 was filled with the slurry of ceramics, and a good molded product was obtained.
【０００８】得られた成形体を温度１３００℃の窒素雰
囲気で反応焼成して、繊維強化セラミツクス焼結体Ａを
得た。上述のようにして得られた本発明による繊維強化
セラミツクス焼結体Ａは、図３に示すように不規則に積
層された強化繊維の隙間に炭化ケイ素が分散し、４点曲
げ強度が４００MPa 、破壊靭性値が１５MPa・m1/2という
優れた特性を示した。本発明による繊維強化セラミツク
ス焼結体Ａはどの方向から切り出しても、同様の強度と
靭性が得られた。これは不織布２０の短繊維２が不規則
に積層し、かつ短繊維２が均一な厚さに分散している結
果である。The obtained compact was fired in a nitrogen atmosphere at a temperature of 1300 ° C. to obtain a fiber-reinforced ceramic sintered body A. As shown in FIG. 3, the fiber-reinforced ceramic sintered body A according to the present invention obtained as described above has silicon carbide dispersed in the gaps between the reinforcing fibers randomly stacked, and has a four-point bending strength of 400 MPa, Excellent properties such as a fracture toughness value of 15 MPa · m 1/2 were exhibited. The same strength and toughness were obtained when the fiber-reinforced ceramics sintered body A according to the present invention was cut out from any direction. This is a result of the fact that the short fibers 2 of the nonwoven fabric 20 are irregularly stacked and the short fibers 2 are dispersed in a uniform thickness.
【０００９】図４に示すように、本発明による繊維強化
セラミツクス焼結体Ａでは、自己酸化により短繊維２の
表面に形成された２酸化ケイ素（SiO2）からなる第１の
酸化物層６は、短繊維２の表面から第１の酸化物層６の
外表面へ向うにつれて、酸素の含有量が増加し、かつケ
イ素と炭素の含有量が減少する、いわゆる傾斜組織にな
つている。溶液を用いたデイツプコーテイング、ＣＶ
Ｄ、蒸着などによる被覆処理では、上述のような傾斜組
織を作るのは非常に困難である。さらに、自己酸化によ
り短繊維２の表面に形成された２酸化ケイ素（SiO2）か
らなる第１の酸化物層６は、表面が平滑である。これに
対し、ＣＶＤ、蒸着などにより形成した被覆では、表面
が粗くなり、強度低下の原因になる。As shown in FIG. 4, in the fiber-reinforced ceramic sintered body A according to the present invention, the first oxide layer 6 made of silicon dioxide (SiO 2 ) formed on the surface of the short fiber 2 by self-oxidation. Has a so-called inclined structure in which the content of oxygen increases and the content of silicon and carbon decreases as going from the surface of the short fiber 2 to the outer surface of the first oxide layer 6. Dip coating using solution, CV
It is very difficult to form the above-mentioned gradient structure in the coating treatment by D, vapor deposition, or the like. Furthermore, the surface of the first oxide layer 6 made of silicon dioxide (SiO 2 ) formed on the surface of the short fiber 2 by self-oxidation is smooth. On the other hand, a coating formed by CVD, vapor deposition, or the like has a rough surface, which causes a reduction in strength.
【００１０】［実施例２］実施例１により作製した酸化
後の不織布２０を、アルミニウム，ジルコニウム，チタ
ンなどの金属のアルコキシドの溶液に浸漬し、温度８０
０℃の大気中で熱処理し、図５に示すように、不織布２
０の表面の２酸化ケイ素（SiO2）からなる第１の酸化物
層６の外表面に、アルミナ（Al2O3 ）からなる第２の酸
化物層８と、ジルコニア（ZrO2）からなる第３の酸化物
層１０とを形成した。次いで、不織布２０の短繊維相互
の隙間へ、ケイ素（Si），アルミナ（Al2O3 ），イツト
リア（Y2O3）を原料とするセラミツクスのスラリーを充
填して成形体を作製した。この成形体を温度１３００℃
の窒素雰囲気で反応焼成し、次いで温度１５００℃で焼
成して繊維強化セラミツクス焼結体Ｂを得た。本発明に
よる繊維強化セラミツクス焼結体Ｂは、曲げ強度が６０
０MPa 、破壊靭性値が２０MPa・m1/2という優れた特性の
ものである。これは、不織布２０の短繊維２の表面に形
成された酸化物の複合層６，８，１０が、短繊維２の耐
熱性を高めるとともに、窒化ケイ素粒子（Si3N4 ）１４
および粒界相１２からなる基材１６との間に適度な反応
層として働くことによるものと考えられる。Example 2 The oxidized nonwoven fabric 20 prepared in Example 1 was immersed in a solution of an alkoxide of a metal such as aluminum, zirconium, or titanium.
Heat treatment in the air at 0 ° C., as shown in FIG.
On the outer surface of the first oxide layer 6 made of silicon dioxide (SiO 2 ) on the surface 0, a second oxide layer 8 made of alumina (Al 2 O 3 ) and zirconia (ZrO 2 ) are formed. A third oxide layer 10 was formed. Next, a gap between the short fibers of the nonwoven fabric 20 was filled with a slurry of ceramics made of silicon (Si), alumina (Al 2 O 3 ), and yttria (Y 2 O 3 ) as a raw material to produce a molded body. This molded body is heated to 1300 ° C.
Then, the mixture was fired at a temperature of 1500 ° C. to obtain a fiber-reinforced ceramic sintered body B. The fiber-reinforced ceramic sintered body B according to the present invention has a bending strength of 60.
It has excellent properties of 0 MPa and a fracture toughness value of 20 MPa · m 1/2 . This is because the oxide composite layers 6, 8, and 10 formed on the surfaces of the short fibers 2 of the nonwoven fabric 20 increase the heat resistance of the short fibers 2 and increase the silicon nitride particles (Si 3 N 4 ) 14.
This is considered to be due to the fact that it acts as an appropriate reaction layer between the base material 16 and the grain boundary phase 12.
【００１１】図５に示すように、本発明による繊維強化
セラミツクス焼結体Ｂでは、２酸化ケイ素（SiO2）から
なる第１の酸化物層６の外表面に、アルミナ（Al2O3 ）
からなる第２の酸化物層８と、ジルコニア（ZrO2）から
なる第３の酸化物層１０とが形成されるので、密着強度
が高くなる。As shown in FIG. 5, in the fiber-reinforced ceramic sintered body B according to the present invention, alumina (Al 2 O 3 ) is formed on the outer surface of the first oxide layer 6 made of silicon dioxide (SiO 2 ).
Since the second oxide layer 8 made of and the third oxide layer 10 made of zirconia (ZrO 2 ) are formed, the adhesion strength is increased.
【００１２】図６に示すように、本発明による繊維強化
セラミツクス焼結体Ｂでも、自己酸化により短繊維２の
表面に形成された２酸化ケイ素（SiO2）からなる第１の
酸化物層６は、短繊維２の表面から第１の酸化物層６の
外表面へ向うにつれて、酸素の含有量が増加し、かつケ
イ素と炭素の含有量が減少する、いわゆる傾斜組織にな
つている。As shown in FIG. 6, the fiber-reinforced ceramic sintered body B according to the present invention also has a first oxide layer 6 made of silicon dioxide (SiO 2 ) formed on the surface of the short fiber 2 by self-oxidation. Has a so-called inclined structure in which the content of oxygen increases and the content of silicon and carbon decreases as going from the surface of the short fiber 2 to the outer surface of the first oxide layer 6.
【００１３】上述の各実施例では、不織布２０の繊維に
Si-C-Ti-O 繊維を用いているが、本発明はこれに限定さ
れるものではなく、不織布２０の繊維にSi-Ti-C-O 繊
維、Si-Zr-C-O 繊維、Si-N-O系繊維を用いても同様の効
果が得られる。また、基材１６は窒化物、炭化物、酸化
物などでも同様の効果が得られる。さらに、第２の酸化
物層８と第３の酸化物層１０には、基材１６の種類や焼
結助剤の種類により、他の物質を適用できる。In each of the above embodiments, the fibers of the nonwoven fabric 20
Although Si-C-Ti-O fibers are used, the present invention is not limited to this, and the fibers of the nonwoven fabric 20 may be Si-Ti-CO fibers, Si-Zr-CO fibers, or Si-NO fibers. The same effect can be obtained by using. The same effect can be obtained even when the base material 16 is a nitride, a carbide, an oxide, or the like. Further, other substances can be applied to the second oxide layer 8 and the third oxide layer 10 depending on the type of the base material 16 and the type of the sintering aid.
【００１４】[0014]
【発明の効果】本発明は上述のように、繊維強化セラミ
ツクス焼結体の表面に少くとも１つの酸化物層が形成さ
れた強化繊維が均一に分散し、強化繊維の配向が不規則
でありかつ強化繊維相互の接触部分が前記酸化物層によ
り接合されているものであり、セラミツクス繊維からな
る不織布を酸化させて第１の酸化物層を形成したもの、
または第１の酸化物層の外表面に第２の酸化物層を形成
したものを、繊維強化セラミツクス焼結体の強化材に使
用するので、強化材の形状を自由に設定できる。強化材
としての不織布に形状を付与した後に酸化させて第１の
酸化物層を形成するか、さらに第１の酸化物層の外表面
に第２の酸化物層を形成すれば、不織布の剛性が向上
し、成型時の繊維の配合が容易になり、繊維の分散を均
一に、かつ繊維の配向を不規則にできる。As described above, according to the present invention, the reinforcing fibers having at least one oxide layer formed on the surface of the fiber-reinforced ceramics sintered body are uniformly dispersed, and the orientation of the reinforcing fibers is irregular. And a contact portion between the reinforcing fibers is bonded by the oxide layer, and a first oxide layer is formed by oxidizing a nonwoven fabric made of ceramics fibers;
Alternatively, since the second oxide layer formed on the outer surface of the first oxide layer is used as the reinforcing material of the fiber-reinforced ceramic sintered body, the shape of the reinforcing material can be freely set. If a non-woven fabric as a reinforcing material is given a shape and then oxidized to form a first oxide layer, or if a second oxide layer is further formed on the outer surface of the first oxide layer, the rigidity of the non-woven fabric is increased. Is improved, the blending of the fibers at the time of molding is facilitated, the dispersion of the fibers can be made uniform, and the orientation of the fibers can be made irregular.
【００１５】不織布の酸化後に繊維の表面に形成した２
酸化ケイ素の傾斜組織からなる第１の酸化物層が緩衝層
として働き、第２の酸化物層との密着強度が向上され
る。2 formed on the surface of the fiber after oxidation of the nonwoven fabric
The first oxide layer having a graded structure of silicon oxide functions as a buffer layer, and the adhesion strength with the second oxide layer is improved.
【００１６】不織布の短繊維の第１の酸化物層の外表面
に形成した第２の酸化物層が、基材との反応を適切に制
御するので、繊維強化セラミツクス焼結体の機械的強度
が向上される。Since the second oxide layer formed on the outer surface of the first oxide layer of the short fibers of the nonwoven fabric appropriately controls the reaction with the substrate, the mechanical strength of the fiber-reinforced ceramic sintered body is improved. Is improved.
【図１】本発明に係る繊維強化セラミツクス焼結体に用
いる不織布の平面図である。FIG. 1 is a plan view of a nonwoven fabric used for a fiber-reinforced ceramic sintered body according to the present invention.
【図２】同不織布を拡大して示す平面断面図である。FIG. 2 is an enlarged plan sectional view showing the nonwoven fabric.
【図３】本発明に係る繊維強化セラミツクス焼結体の組
織図である。FIG. 3 is a structural diagram of a fiber-reinforced ceramic sintered body according to the present invention.
【図４】同繊維強化セラミツクス焼結体の酸化物層の組
成を表す線図である。FIG. 4 is a diagram showing a composition of an oxide layer of the fiber-reinforced ceramic sintered body.
【図５】本発明の変更実施例に係る繊維強化セラミツク
ス焼結体の組織図である。FIG. 5 is a structural diagram of a fiber-reinforced ceramic sintered body according to a modified example of the present invention.
【図６】同繊維強化セラミツクス焼結体の酸化物層の組
成を表す線図である。FIG. 6 is a diagram showing a composition of an oxide layer of the fiber-reinforced ceramic sintered body.
２：短繊維 ４：接触部分 ６：第１の酸化物層（Si
O2） ８：第２の酸化物層（Al2O3 ） １０：第３の酸
化物層（ZrO2） １２：粒界層 １４：窒化ケイ素粒子
（Si3N4 ） ２０：不織布2: short fiber 4: contact portion 6: first oxide layer (Si
O 2 ) 8: Second oxide layer (Al 2 O 3 ) 10: Third oxide layer (ZrO 2 ) 12: Grain boundary layer 14: Silicon nitride particles (Si 3 N 4 ) 20: Non-woven fabric
Claims (5)
とも１つの酸化物層が形成された強化繊維が均一に分散
し、強化繊維の配向が不規則でありかつ強化繊維相互の
接触部分が前記酸化物層により接合されていることを特
徴とする繊維強化セラミツクス焼結体。1. A reinforcing fiber having at least one oxide layer formed on the surface of a fiber-reinforced ceramics sintered body is uniformly dispersed, the orientation of the reinforcing fibers is irregular, and the contacting portions between the reinforcing fibers are formed. A fiber-reinforced ceramics sintered body joined by the oxide layer.
前記強化繊維に接する内側がケイ素と酸素を主成分とし
て構成され、前記酸化物層の内側から外側へ向つて酸素
含有量が増加しかつケイ素含有量が減少する、請求項１
に記載の繊維強化セラミツクス焼結体。2. The oxide layer of the reinforcing fiber, wherein the inside of the oxide layer in contact with the reinforcing fiber is composed mainly of silicon and oxygen, and the oxygen content is from the inside to the outside of the oxide layer. And the silicon content decreases.
2. A fiber-reinforced ceramic sintered body according to item 1.
素、アルミニウム、ジルコニウムの内の少くとも１つの
元素を主成分とする第２の酸化物層が形成されている、
請求項１に記載の繊維強化セラミツクス焼結体。3. A second oxide layer containing at least one of oxygen, aluminum and zirconium as a main component is formed on an outer surface of the oxide layer of the reinforcing fiber.
The fiber-reinforced ceramic sintered body according to claim 1.
る炭化ケイ素系繊維、ケイ素とチタンと炭素と酸素から
なる炭化ケイ素系繊維、ケイ素とジルコニウムと炭素と
酸素からなる炭化ケイ素系繊維、ケイ素と窒素と炭素か
らなる窒化ケイ素系繊維の内の少くとも１つである、請
求項１に記載の繊維強化セラミツクス焼結体。4. A silicon carbide fiber comprising silicon, carbon and oxygen, a silicon carbide fiber comprising silicon, titanium, carbon and oxygen, a silicon carbide fiber comprising silicon, zirconium, carbon and oxygen, and silicon. The fiber-reinforced ceramic sintered body according to claim 1, wherein the fiber-reinforced ceramics sintered body is at least one of silicon nitride-based fibers comprising nitrogen, nitrogen and carbon.
ニウム、炭素、窒素の内の少くとも１つの元素を含んで
いる、請求項１に記載の繊維強化セラミツクス焼結体。5. The fiber-reinforced ceramic sintered body according to claim 1, wherein the oxide layer of the reinforcing fiber contains at least one element of titanium, zirconium, carbon, and nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9048406A JPH10226583A (en) | 1997-02-17 | 1997-02-17 | Fiber reinforced ceramic sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9048406A JPH10226583A (en) | 1997-02-17 | 1997-02-17 | Fiber reinforced ceramic sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH10226583A true JPH10226583A (en) | 1998-08-25 |
Family
ID=12802434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9048406A Pending JPH10226583A (en) | 1997-02-17 | 1997-02-17 | Fiber reinforced ceramic sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH10226583A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6538255B1 (en) | 1999-02-22 | 2003-03-25 | Nikon Corporation | Electron gun and electron-beam optical systems and methods including detecting and adjusting transverse beam-intensity profile, and device manufacturing methods including same |
-
1997
- 1997-02-17 JP JP9048406A patent/JPH10226583A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6538255B1 (en) | 1999-02-22 | 2003-03-25 | Nikon Corporation | Electron gun and electron-beam optical systems and methods including detecting and adjusting transverse beam-intensity profile, and device manufacturing methods including same |
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