JPH0483753A - Ceramic reinforced with alumina fiber - Google Patents

Ceramic reinforced with alumina fiber

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Publication number
JPH0483753A
JPH0483753A JP2196909A JP19690990A JPH0483753A JP H0483753 A JPH0483753 A JP H0483753A JP 2196909 A JP2196909 A JP 2196909A JP 19690990 A JP19690990 A JP 19690990A JP H0483753 A JPH0483753 A JP H0483753A
Authority
JP
Japan
Prior art keywords
carbon
toughness
whisker
ceramic
whiskers
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.)
Pending
Application number
JP2196909A
Other languages
Japanese (ja)
Inventor
Katsura Hayashi
桂 林
Katsumi Sakagami
勝伺 坂上
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kyocera Corp
Original Assignee
Kyocera Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kyocera Corp filed Critical Kyocera Corp
Priority to JP2196909A priority Critical patent/JPH0483753A/en
Priority to DE69108472T priority patent/DE69108472T2/en
Priority to EP91112447A priority patent/EP0468486B1/en
Priority to US07/735,371 priority patent/US5360772A/en
Publication of JPH0483753A publication Critical patent/JPH0483753A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To obtain the subject ceramic having improved mechanical properties such as fracture toughness and strength by adding a specific amount of carbon to an Al2O3/TiC whisker ceramic. CONSTITUTION:The objective ceramic can be produced by adding 0.05-2wt.% of carbon to an alumina fiber-reinforced ceramic containing 5-60vol.% of titanium carbide whisker. The sinterability and the characteristics of the ceramic composition can be improved by adding 0.1-3wt.% of at least one kind of oxide of element selected from Mg, Y, rare-earth element, Ni, Co and Cr as a sintering assistant.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、ウィスカー等の繊維状物質を含有する繊維強
化セラミックスに関し、詳細には高靭性を有し特に切削
工具や、その他耐摩耗性部品に適したセラミックスに関
する。
Detailed Description of the Invention (Field of Industrial Application) The present invention relates to fiber-reinforced ceramics containing fibrous substances such as whiskers, and more particularly, to fiber-reinforced ceramics that have high toughness and are particularly useful for cutting tools and other wear-resistant parts. Regarding ceramics suitable for.

(従来技術) アルミナ(A1203 )N焼結体は、耐摩耗性に優れ
た材料として各種の産業機械用部品に応用されている反
面、靭性に劣るという欠点を有するために利用分野の拡
大が阻害されている。
(Prior art) Alumina (A1203)N sintered bodies are used in various industrial machinery parts as a material with excellent wear resistance, but the drawback of poor toughness hinders the expansion of the field of use. has been done.

そこで従来から靭性を改善するために各種の改良が提案
されている。
Therefore, various improvements have been proposed to improve toughness.

その1つの例に、炭化珪素(S i C)ウィスカーに
代表される繊維状物質を配合することにより靭性を改善
することが特開昭61−286271号や特開昭62−
41776号等にて提案されている。
One example is JP-A No. 61-286271 and JP-A No. 62-Sho. 61-286271 and JP-A No. 62-1982, which suggest that toughness can be improved by incorporating fibrous substances such as silicon carbide (S i C) whiskers.
It has been proposed in No. 41776, etc.

このようなSiCウィスカーを含有する繊維強化セラミ
ックスはSiC自体の硬度が高く、熱伝導性がよいため
に、切削工具として用いた場合、一部の超耐熱合金の切
削(インコネル718の荒切削)では優れた性能を示し
ている。
Fiber-reinforced ceramics containing such SiC whiskers have high hardness and good thermal conductivity, so when used as a cutting tool, it is difficult to cut some super heat-resistant alloys (rough cutting Inconel 718). It shows excellent performance.

(発明が解決しようとする問題点) しかしながら、SiCは鉄、特に酸化鉄と容易に反応し
やすい性質を有するために、A1□03−3iCウイス
カー系工具は多くの場合、他のA1゜03を主体とする
工具に比較して摩耗量が多くなる傾向にある。例えば、
5US304を切削した場合、従来のAh○3系工具で
あれば、十分切削可能な条件であってもSiCウィスカ
ーを含有する工具では急激に摩耗が進展し切削が不可能
となる問題がある。また、鋳鉄の切削においてもAh0
3系工具よりも摩耗量が大きいことが確認されている。
(Problems to be Solved by the Invention) However, since SiC has the property of easily reacting with iron, especially iron oxide, A1□03-3iC whisker-based tools often do not contain other A1゜03. The amount of wear tends to be greater compared to the main tool. for example,
When cutting 5US304, there is a problem that even if a conventional Ah○3 type tool can be used under sufficient cutting conditions, a tool containing SiC whiskers will rapidly wear out and become impossible to cut. Also, when cutting cast iron, Ah0
It has been confirmed that the amount of wear is greater than that of Series 3 tools.

このように、Al4Ch  SiCウィスカー系工具で
は被削材によってその切削性能が大きく変化するという
問題がある。
As described above, the Al4Ch SiC whisker-based tool has a problem in that its cutting performance varies greatly depending on the workpiece material.

ところが、最近に至りこのような被削材との反応性を防
止することを目的として、SiCウィスカーに代わり、
SiCよりも鉄との反応性が低い炭化チタン(Tic)
の繊維状物質(ウィスカー)を添加することが提案され
ているが、セラミックスの抗折強度、靭性、硬度等の特
性の点から未だ十分に検討されておらず、実用的なレヘ
ルに達していないのが現状であった。
However, recently, in order to prevent such reactivity with the work material, SiC whiskers have been replaced with
Titanium carbide (Tic) has lower reactivity with iron than SiC
It has been proposed to add fibrous substances (whiskers), but this has not yet been fully investigated in terms of the properties of ceramics such as flexural strength, toughness, and hardness, and has not reached a practical level. This was the current situation.

(問題点を解決するための手段) 本発明者等は、上記AIZO+l −T ICウィスカ
ー系セラミックスに対して、詳細に検討を重ねた結果、
この材料に対して少量の炭素を添加することにより、破
壊靭性をはじめとする機械的特性を向上できることを知
見し本発明に至った。
(Means for Solving the Problems) As a result of detailed studies on the above AIZO+l-T IC whisker ceramics, the present inventors found that
The present invention was based on the discovery that mechanical properties such as fracture toughness can be improved by adding a small amount of carbon to this material.

即ち、本発明はTiCウィスカーを5〜60体積%の割
合で含有するA1□03質繊維強化セラミックスにおい
て、炭素を0.05〜2重量%の割合で添加したことを
特徴とするもので、さらに上記の系に対してMg、Y、
希土類元素、Ni、Co、Crから選ばれる少なくとも
1種の酸化物を0.1〜3重量%の割合で添加すること
を特徴とするものである。
That is, the present invention is characterized in that carbon is added in a proportion of 0.05 to 2% by weight in an A1□03 fiber-reinforced ceramic containing TiC whiskers in a proportion of 5 to 60% by volume. For the above system, Mg, Y,
It is characterized in that at least one oxide selected from rare earth elements, Ni, Co, and Cr is added in a proportion of 0.1 to 3% by weight.

以下、本発明を詳述する。The present invention will be explained in detail below.

本発明において用いられるTiCウィスカーは、それ自
体、単結晶あるいは多結晶質からなるもので、その平均
径は2μm以下、特に0.2〜0.7μmであることが
好ましい。平均径が2μm以下では、マトリックス成分
であるA1.03との熱膨張差による応力が過度になら
ず、高い抗折強度を維持できるからであり、平均径が大
きく成り過ぎると均一に分散することも難しくなり、強
度、靭性ともバラツキが生じやすく、また切削工具とし
て用いた際に逃げ面の境界摩耗が大きくなるためである
The TiC whiskers used in the present invention are themselves single crystal or polycrystalline, and preferably have an average diameter of 2 μm or less, particularly 0.2 to 0.7 μm. If the average diameter is 2 μm or less, the stress due to the difference in thermal expansion with A1.03, which is a matrix component, will not become excessive and high bending strength can be maintained. If the average diameter is too large, it will not be uniformly dispersed. This is because the strength and toughness tend to vary, and when used as a cutting tool, boundary wear on the flank surface becomes large.

一方、ウィスカーの長径/短径で表されるアスペクト比
が小さすぎると繊維強化の効果が小さく高い靭性が得ら
れにくく、逆に大きすぎると原料としての取扱が難しく
、均一に分散することができないために高い靭性を得る
ことが難しくなる。
On the other hand, if the aspect ratio expressed by the long axis/breadth axis of the whisker is too small, the effect of fiber reinforcement will be small and it will be difficult to obtain high toughness.On the other hand, if it is too large, it will be difficult to handle as a raw material and it will not be possible to disperse it uniformly. This makes it difficult to obtain high toughness.

よって、アスペクト比の平均は3〜100、特に10〜
30のものが好適に使用される。
Therefore, the average aspect ratio is 3 to 100, especially 10 to 100.
30 is preferably used.

このようなTiCウィスカーは、例えば酸化チタンウィ
スカーを炭化処理したり、CVD法により合成すること
ができる。
Such TiC whiskers can be synthesized, for example, by carbonizing titanium oxide whiskers or by CVD.

このTiCウィスカーは、アルミナを主成分とするマト
リックス成分中に全量中5〜70体積%、特に25〜5
0体積%になるように分散含有させる。ウィスカーの量
を上記の範囲に設定したのは、ウィスカー量が5体積%
未満では、ウィスカー添加による靭性向上効果が小さく
、70体積%を越えると系全体の焼結性が低下する。な
お、機械的特性および焼結の容易性を考慮すれば、Ti
Cウィスカーの添加量は25〜45体積%であり、最適
には30〜40体積%がよい。
These TiC whiskers are contained in a matrix component mainly composed of alumina, with a concentration of 5 to 70% by volume, especially 25 to 5% by volume of the total amount.
It is dispersed and contained so that it becomes 0% by volume. The whisker amount was set to the above range because the whisker amount was 5% by volume.
If it is less than 70% by volume, the effect of improving the toughness by whisker addition is small, and if it exceeds 70% by volume, the sinterability of the entire system will decrease. Note that considering mechanical properties and ease of sintering, Ti
The amount of C whiskers added is 25 to 45% by volume, and optimally 30 to 40% by volume.

本発明によれば、上記Al2O3−T iCウィスカー
系において炭素を0.05〜2重量%、特に0.5〜1
重量%の割合で添加することが重要である。
According to the invention, carbon is present in the Al2O3-T iC whisker system in an amount of 0.05 to 2% by weight, in particular 0.5 to 1% by weight.
It is important to add in proportions by weight.

この炭素粉末は平均粒径1μm以下、特に0.5μm以
下の炭素粉末や焼成により炭素を発生しうるフェノール
樹脂等の有機化合物を添加するか、あるいは予めTiC
ウィスカーの表面に塗布された炭素であってもよい。な
お、炭素の量を上記の範囲に設定したのは、炭素の添加
量が0.05重量%より少ないと靭性向上効果が小さく
、2重量%を越えると焼結性および焼結体の硬度や強度
が低下する。
This carbon powder is prepared by adding carbon powder with an average particle size of 1 μm or less, especially 0.5 μm or less, or adding an organic compound such as a phenol resin that can generate carbon when fired, or by adding TiC powder in advance.
It may also be carbon applied to the surface of the whisker. The reason for setting the amount of carbon in the above range is that if the added amount of carbon is less than 0.05% by weight, the effect of improving toughness will be small, and if it exceeds 2% by weight, the sinterability and hardness of the sintered body will deteriorate. Strength decreases.

またウィスカーを分散するためのマトリックスはA l
 z 01を主体とするが、焼結助剤としてMg、Y、
希土類元素、Ni、Co、Crから選ばれる少なくとも
1種以上の酸化物を添加することによりマトリックス成
分としての焼結性を高め、特性の向上を図ることができ
る。しかしこの助剤量が多すぎると焼結体の靭性が低下
する。よってこれらの焼結助剤は、全量中0.1〜3重
量%、特に0゜5〜2重量%の割合で添加するのがよい
。なお、ここで用いられる希土類元素としてはYb、N
d、Er、Ce、Sm、Gd、Dy等が挙げられる。
Also, the matrix for dispersing whiskers is A l
The main component is Mg, Y, and sintering aids.
By adding at least one or more oxides selected from rare earth elements, Ni, Co, and Cr, the sinterability as a matrix component can be enhanced and the properties can be improved. However, if the amount of this auxiliary agent is too large, the toughness of the sintered body decreases. Therefore, these sintering aids are preferably added in an amount of 0.1 to 3% by weight, particularly 0.5 to 2% by weight, based on the total amount. Note that the rare earth elements used here include Yb, N
d, Er, Ce, Sm, Gd, Dy, etc.

本発明の繊維強化セラミックスを製造するには、まず前
記TiCウィスカー、アルミナ粉末、炭素粉末、必要に
応じて焼結助剤を前述した割合で混合、粉砕後に所望の
成形手段、金型プレス、押し出し成形、射出成形、冷間
静水圧成形等によって成形後、焼成する。
To produce the fiber-reinforced ceramics of the present invention, first, the TiC whiskers, alumina powder, carbon powder, and if necessary, a sintering aid are mixed in the above-mentioned proportions, pulverized, and then molded using a desired molding method, die press, or extrusion. After molding by molding, injection molding, cold isostatic pressing, etc., it is fired.

焼成は、普通焼成、ホットプレス法、熱間静水圧焼成法
等が適用され、1650°C−1850°Cの温度でA
rやHe等の不活性ガスもしくはカーボン等の存在する
還元性雰囲気およびそれらの加圧もしくは減圧雰囲気中
で0.5〜6時間行う。特に高密度の焼結体を得るため
には、普通焼成あるいはホットプレス法によって対理論
密度比96%以上の焼結体を作成し、この焼結体をさら
に熱間静水圧焼成すればよい。
For firing, ordinary firing, hot press method, hot isostatic pressing method, etc. are applied, and A
The reaction is carried out for 0.5 to 6 hours in a reducing atmosphere in which an inert gas such as r or He or carbon exists, and in a pressurized or reduced pressure atmosphere thereof. In order to obtain a particularly high-density sintered body, a sintered body having a theoretical density ratio of 96% or more may be prepared by normal firing or hot pressing, and this sintered body may be further subjected to hot isostatic pressure firing.

7・(作用) TiCウィスカーの表面には通常Ti0z等の酸化物が
その表面に存在する。このようなウィスカーをA 1 
z O]マトリックス中に分散すると表面のTiO□と
A 1 t O3が反応し癒着する。繊維強化セラミッ
クスにおいてマトリックス成分とウィスカー成分が反応
するとウィスカー添加により靭性向上を担うウィスカー
の引き抜き効果が低下するために靭性の向上が低下する
7. (Function) Oxides such as TiOz usually exist on the surface of TiC whiskers. A whisker like this
z O] When dispersed in the matrix, TiO□ and A 1 t O3 on the surface react and adhere to each other. When the matrix component and the whisker component react in fiber-reinforced ceramics, the addition of whiskers reduces the effect of pulling out the whiskers, which are responsible for improving toughness, and thus the improvement in toughness decreases.

そこで、炭素粉末を添加することによりTiCウィスカ
ー表面の酸素が還元除去され、マトリックス成分とウィ
スカー成分との反応を抑制しウィスカーの引き抜き効果
を顕著に発揮させるこにより焼結体の靭性を向上するこ
とできる。
Therefore, by adding carbon powder, the oxygen on the surface of the TiC whisker is reduced and removed, suppressing the reaction between the matrix component and the whisker component, and significantly exerting the whisker pulling effect, thereby improving the toughness of the sintered body. can.

また、焼結助剤の添加によりマトリックス成分の焼結性
を高めることにより高密度が図られ、焼結体全体の強度
靭性を高めることができる。
Further, by increasing the sinterability of the matrix component by adding a sintering aid, high density can be achieved, and the strength and toughness of the entire sintered body can be increased.

以下、本発明を次の例で説明する。The invention will now be explained with the following examples.

(実施例) 平均粒径1μm以下、純度99.9%以上のAh03粉
末と、所望により第1表の酸化物および炭素粉末を秤量
後、回転ミルにて12時間混合粉砕した。この混合粉末
に平均粒径1μm、アスペクト比が10〜30のTiC
ウィスカーを所定量添加し、回転ミルで12時間混合し
た。混合後のスラリーを乾燥してホットプレス用原料と
した。
(Example) After weighing Ah03 powder with an average particle size of 1 μm or less and a purity of 99.9% or more, and optionally the oxides and carbon powders shown in Table 1, they were mixed and ground in a rotary mill for 12 hours. TiC with an average particle size of 1 μm and an aspect ratio of 10 to 30 is added to this mixed powder.
A predetermined amount of whiskers was added and mixed on a rotary mill for 12 hours. The slurry after mixing was dried and used as a raw material for hot pressing.

この原料をカーボン型に充填し、所定の温度で1時間、
300kg/cm2の圧力でホットプレス焼成してJI
S規格に基づく抗折試験片を作成した。
This raw material is filled into a carbon mold and kept at a predetermined temperature for 1 hour.
JI by hot press firing at a pressure of 300 kg/cm2
A bending test piece based on the S standard was prepared.

また、第1表中試料Nα20〜26に関しては炭素粉末
を添加する変わりに、TiCウィスカーとしてその表面
に1重量%相当分の炭素を塗布したものを使用した。
In addition, for samples Nα20 to Nα26 in Table 1, instead of adding carbon powder, TiC whiskers whose surfaces were coated with carbon equivalent to 1% by weight were used.

得られた各試料を研磨して3点曲げ抗折強度を、ピンカ
ース硬度、また鏡面にポリッシング加工し1M法で靭性
(KIC)を測定した。
Each of the obtained samples was polished to measure three-point bending strength, Pinkers hardness, and mirror-polished toughness (KIC) using the 1M method.

また、顕微鏡写真から組織観察し焼結性について評価し
た。
In addition, the structure was observed from microscopic photographs and the sinterability was evaluated.

結果は、第1表に示す。The results are shown in Table 1.

C以下余白) 第1表のよれば、炭素粉末を全く添加しない試料間1で
は、その靭性値が4.5MP a −m””程度と低い
。これに対して、炭素を添加することによって抗折強度
および靭性等を向上することができるが、炭素量が2重
量%を越える試料Nα6では焼結性が大きく低下し焼結
体にボイドが発生し抗折強度が低下し靭性は測定するこ
とができなかった。
According to Table 1, the toughness value of Sample 1, in which no carbon powder was added, was as low as about 4.5 MPa-m"". On the other hand, adding carbon can improve the bending strength and toughness, but in sample Nα6 with a carbon content exceeding 2% by weight, the sinterability is greatly reduced and voids occur in the sintered body. However, the bending strength decreased and the toughness could not be measured.

また、焼結助剤を添加しない試料Nα7では焼結温度を
高めることによって優れた特性を得ることができるが、
焼結助剤を適量添加することによって焼成温度を低くす
るとともに特性の安定性を図ることができる。しかし、
焼結助剤量が3重量%を越える試料N11112では、
抗折強度、靭性ともに低下した。
In addition, excellent properties can be obtained by increasing the sintering temperature in sample Nα7, which does not contain a sintering aid, but
By adding an appropriate amount of a sintering aid, the firing temperature can be lowered and the stability of properties can be improved. but,
For sample N11112 in which the amount of sintering aid exceeds 3% by weight,
Both bending strength and toughness decreased.

さらに、TiCウィスカーの添加量に関しては全く添加
しない試料Nα20では、抗折強度、靭性ともに低い値
であった。また、60体積%を越える試料陥、26では
、焼結性が低下し特性は大きく低下した。
Furthermore, regarding the amount of TiC whiskers added, sample Nα20, in which no TiC whiskers were added, had low values for both bending strength and toughness. In addition, in sample No. 26 where the sample depth exceeded 60% by volume, the sinterability decreased and the properties significantly decreased.

第1表において、本発明に基づき作成した試料は、いず
れも抗折強度60kg/mm2以上、靭性5.OMP 
a −m””以上、ビッカース硬度1800kg/mm
2以上が達成された。
In Table 1, all the samples prepared based on the present invention have a bending strength of 60 kg/mm2 or more and a toughness of 5. OMP
a-m"" or more, Vickers hardness 1800 kg/mm
2 or more was achieved.

(発明の効果) 以上詳述した通り、本発明のA1□O:l  T iC
ウィスカー系セラミックスは、これまでのA l z 
O3SiCウイスカー系に比較して酸化鉄との反応性が
低減されるという効果を維持しつつ、その靭性、耐摩耗
性ならびに強度をさらに向上することができるために、
あらゆる被削材に対応しうる工具用材料として、あるい
はその他の機械部品として繊維強化セラミックスの用途
を拡大することができる。
(Effect of the invention) As detailed above, A1□O:l T iC of the present invention
Whisker ceramics are
While maintaining the effect of reducing reactivity with iron oxide compared to the O3SiC whisker system, it is possible to further improve its toughness, wear resistance, and strength.
The use of fiber-reinforced ceramics can be expanded as a material for tools that can be used with all kinds of work materials, or as other machine parts.

特許出願人(663)京セラ株式会社Patent applicant (663) Kyocera Corporation

Claims (2)

【特許請求の範囲】[Claims] (1)炭化チタンウイスカーを5〜60体積%の割合で
含有するアルミナ質繊維強化セラミックスにおいて、炭
素を0.05〜2重量%の割合で添加したことを特徴と
するアルミナ質繊維強化セラミックス。
(1) An alumina fiber-reinforced ceramic containing titanium carbide whiskers in a proportion of 5 to 60% by volume, characterized in that carbon is added in a proportion of 0.05 to 2% by weight.
(2)炭化チタンウイスカーを5〜60体積%の割合で
含有するアルミナ質繊維強化セラミックスにおいて、炭
素を0.05〜2重量%、Mg、Y、希土類元素、Ni
、Co、Crから選ばれる少なくとも1種の酸化物を0
.1〜3重量%の割合で添加したことを特徴とするアル
ミナ質繊維強化セラミックス。
(2) In alumina fiber-reinforced ceramics containing titanium carbide whiskers at a ratio of 5 to 60% by volume, 0.05 to 2% by weight of carbon, Mg, Y, rare earth elements, and Ni
, Co, and Cr.
.. An alumina fiber-reinforced ceramic characterized in that it is added at a rate of 1 to 3% by weight.
JP2196909A 1990-07-25 1990-07-25 Ceramic reinforced with alumina fiber Pending JPH0483753A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2196909A JPH0483753A (en) 1990-07-25 1990-07-25 Ceramic reinforced with alumina fiber
DE69108472T DE69108472T2 (en) 1990-07-25 1991-07-24 Ceramic material reinforced with aluminum oxide fibers and process for its manufacture.
EP91112447A EP0468486B1 (en) 1990-07-25 1991-07-24 A ceramic material, reinforced by the incorporation of alumina fibers and process for production thereof
US07/735,371 US5360772A (en) 1990-07-25 1991-07-24 Ceramic material reinforced by the incorporation of TiC, TiCN and TiN whiskers and processes for production thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2196909A JPH0483753A (en) 1990-07-25 1990-07-25 Ceramic reinforced with alumina fiber

Publications (1)

Publication Number Publication Date
JPH0483753A true JPH0483753A (en) 1992-03-17

Family

ID=16365674

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2196909A Pending JPH0483753A (en) 1990-07-25 1990-07-25 Ceramic reinforced with alumina fiber

Country Status (1)

Country Link
JP (1) JPH0483753A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100383858C (en) * 2005-01-06 2008-04-23 Tdk株式会社 Magnetic head slider material, magnetic head slider, and method for manufacturing magnetic head slider material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100383858C (en) * 2005-01-06 2008-04-23 Tdk株式会社 Magnetic head slider material, magnetic head slider, and method for manufacturing magnetic head slider material

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