JPH02279558A - Al2o3-tic-based ceramic material - Google Patents
Al2o3-tic-based ceramic materialInfo
- Publication number
- JPH02279558A JPH02279558A JP1098498A JP9849889A JPH02279558A JP H02279558 A JPH02279558 A JP H02279558A JP 1098498 A JP1098498 A JP 1098498A JP 9849889 A JP9849889 A JP 9849889A JP H02279558 A JPH02279558 A JP H02279558A
- Authority
- JP
- Japan
- Prior art keywords
- oxide
- terms
- composite oxide
- weight
- expressed
- 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.)
- Granted
Links
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000002542 deteriorative effect Effects 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 230000001771 impaired effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 238000010304 firing Methods 0.000 description 9
- 230000007423 decrease Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- -1 O・AlzO Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- WHOPEPSOPUIRQQ-UHFFFAOYSA-N oxoaluminum Chemical compound O1[Al]O[Al]1 WHOPEPSOPUIRQQ-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はＡ１□０＋−ＴｉＣ系セラミック材料、特に薄
膜磁気ヘッド用基板等に有用なセラミック材料に関する
。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an A1□0+-TiC ceramic material, particularly a ceramic material useful for thin film magnetic head substrates and the like.
近時、フェライトやセンダストを使用したヘッドに代っ
て薄膜磁気ヘッドが高密度記録用ヘッドとして注目され
ており、この薄膜磁気ヘッド用の基板には、
（１） ・・・耐摩耗性に優れている（２）・・・表
面平滑性に優れている
（３）・・・耐チツピング性に優れている（４）・・・
機械加工性に優れている
などの特性が要求されており、このような要求に対して
アルミナ（Ａｌ２Ｏ３）−炭化チタン（Ｔｉｃ）系のセ
ラミンク焼結体が注目されている。Recently, thin-film magnetic heads have been attracting attention as high-density recording heads instead of heads using ferrite or sendust, and the substrates for these thin-film magnetic heads have (1) ... excellent wear resistance. (2)...Excellent surface smoothness (3)...Excellent chipping resistance (4)...
Properties such as excellent machinability are required, and alumina (Al2O3)-titanium carbide (Tic)-based ceramic sintered bodies are attracting attention in response to such requirements.
このセラミック焼結体を用いた場合には上記（１）の耐
摩耗性は容易に得られ易いが、その他の（２） （３）
（４）などの所要特性については得られ難い。When this ceramic sintered body is used, the wear resistance of (1) above can be easily obtained, but other (2) and (3)
It is difficult to obtain required characteristics such as (4).
そのためにＭｇＯ、ＮｉＯ、Ｃｒ２Ｏ３などの焼結助剤
を添加し、そしてホットプレス法、ホットプレス法と）
ＩＩＰ法、又は雰囲気焼成法とＨＩＰ法等との組合わせ
により焼結体回度を理論密度にまで大きくし、その結果
、上記（２）の表面平滑性をある程度向上させることが
できたが、その半面（３）の耐チッピング性や（４）の
機械加工性については未だ満足し得るような所要特性が
得られていない。よって、このような材料を用いて薄膜
磁気ヘッド用基板を製作する場合には、例えば円板状の
焼結体をスライス加工して基板を切り出しているが、そ
の切り出しに当たってチフビングが発生し易くなり、更
には切削抵抗が大きくなり、その結果、歩留りが低下す
るという問題があった。For this purpose, sintering aids such as MgO, NiO, Cr2O3 are added, and hot press method, hot press method)
By using the IIP method or a combination of an atmosphere firing method and a HIP method, etc., the degree of rotation of the sintered body was increased to the theoretical density, and as a result, the surface smoothness mentioned in (2) above could be improved to some extent. On the other hand, the required characteristics (3), chipping resistance, and (4), machinability, have not yet been achieved. Therefore, when manufacturing a substrate for a thin film magnetic head using such a material, for example, a disk-shaped sintered body is sliced to cut out the substrate, but chipping is likely to occur during cutting. Furthermore, there was a problem in that cutting resistance increased, resulting in a decrease in yield.
従って、本発明は上記問題点を解決することを主たる目
的とし具体的にはＡ１□０．の硬度を劣化させることな
く、耐チンピング性に優れた材料を提供するにある。Therefore, the main purpose of the present invention is to solve the above problems, and specifically, A1□0. The object of the present invention is to provide a material with excellent chimping resistance without deteriorating the hardness of the material.
本発明者等は上記問題点に対し、研究を重ねた結果、Ａ
１．０．−Ｔｉｃの主成分に対し、ｙ 、 ｙｂの少な
（とも１種、？Ｉｇ、 Ｃａの少な（とも１種、Ｚｒを
含む組成から成るセラミック材料において、Ｙおよび／
またはｙｂとＡｌとの複合酸化物とＭｇ及び／またはＣ
ａとＡｌとの複合酸化物を生成させることによって、Ａ
１□０３の粒成長を十分に抑制しながら、焼結性を高め
ることができ、耐チンビッグ性を大きく向上し得ること
を知見した。As a result of repeated research on the above problems, the present inventors found that A.
1.0. - In a ceramic material consisting of a composition containing a small amount of y, yb (both 1 type, ?Ig, Ca (both 1 type, Zr) with respect to the main component of Tic, Y and /
Or a composite oxide of yb and Al and Mg and/or C
By producing a composite oxide of a and Al, A
It has been found that the sinterability can be improved while the grain growth of 1□03 can be sufficiently suppressed, and the chin-big resistance can be greatly improved.
即ち、本発明のＡｌＢ１２−ＴｉＣ系セラミック材料は
組成上、Ａｌを酸化物換算で６０乃至８０重量％と、炭
化物換算で２０乃至４０重量％とから成る主成分に対し
、Ｙ、Ｙｂの少なくとも１種を酸化物換算で０゜５〜４
０重量％、Ｚｒを酸化物換算で２．０〜６゜０重量％お
よびＭｇｓ Ｃａの少なくとも１種を酸化物換算で１．
０〜５．０重量％の割合で含有してなるものであって、
これらの組成のうちセラミック材料中にＹ、、Ｙｂの少
なくとも１種とＡ１との複合酸化物を全量中０．２〜４
．６重量％、Ｍｇ５Ｃａの少なくとも１種とＡ１との複
合化合物を全量中０．７〜１６．０重量％の割合で含有
することを特徴とするものである。That is, the AlB12-TiC ceramic material of the present invention has a composition in which the main component is 60 to 80% by weight of Al in terms of oxide and 20 to 40% by weight in terms of carbide, and at least 1% of Y and Yb. Seeds as oxides 0°5-4
0% by weight, 2.0 to 6.0% by weight of Zr in terms of oxide, and 1.0% by weight of at least one of MgsCa in terms of oxide.
Containing in a proportion of 0 to 5.0% by weight,
Among these compositions, the ceramic material contains a composite oxide of at least one of Y, Yb and A1 in a total amount of 0.2 to 4.
．． 6% by weight, and contains a composite compound of at least one type of Mg5Ca and A1 in a proportion of 0.7 to 16.0% by weight based on the total amount.
本発明のセラミック材料の主成分においてＹ、ｙｂは主
としてＡｌと複合酸化物を形成することによって焼結性
を大きく向上させる効果を有する半面、同時に粒成長を
促進する効果もをする。Among the main components of the ceramic material of the present invention, Y and yb have the effect of greatly improving sinterability by forming a composite oxide with Al, but at the same time they also have the effect of promoting grain growth.
粒成長は最終焼結体のアルミナ粒子の脱粒を起こさせた
り、耐チッピング性を低下させるため、この粒成長は十
分に抑制する必要がある。そこで、Ｍｇ５Ｃａｓ Ｚｒ
を添加することによってこのｙ 、 ｙｂの焼結性向上
効果を阻害することなく粒成長を抑制することが可能と
なった。特に、Ｍｇ、ＣａはＡｔと複合酸化物を形成す
ることによってさらにその効果を助長する。これらの理
由からｙ 、 ｙｂの添加量が酸化物換算で０．５重量
％を下回ると、焼結性が低下し、高密度の焼結体が得ら
れず３．０重量％を超えると強度が低下し好ましくない
。またＭｇ、 Ｃａの少なくとも１種が酸化物換算で１
．０重量２を下回るかまたはＺｒが酸化物換算で２．０
重量％を下回ってもＹ 、 Ｙｂの粒成長を抑制するこ
とができず、耐チッピング性が低下する。これらの好ま
しい範囲はｙ 、 ｙｂが酸化物換算で１．５〜２．５
重量％、Ｍｇ、Ｃａの少なくとも１種が酸化物換算で２
．０〜４，０重Ｉχ、Ｚｒが酸化物換算で３．０〜５．
０重量２である。Grain growth causes shedding of alumina particles in the final sintered body and reduces chipping resistance, so it is necessary to sufficiently suppress this grain growth. Therefore, Mg5Cas Zr
By adding , it became possible to suppress grain growth without inhibiting the sinterability improvement effect of y and yb. In particular, Mg and Ca further enhance the effect by forming a composite oxide with At. For these reasons, if the amount of y and yb added is less than 0.5% by weight in terms of oxides, the sinterability will decrease and a high-density sintered body cannot be obtained, and if it exceeds 3.0% by weight, the strength will decrease. decreases, which is not desirable. In addition, at least one of Mg and Ca has an oxide value of 1
．． 0 weight less than 2 or Zr is 2.0 in terms of oxide
Even if it is less than % by weight, the grain growth of Y and Yb cannot be suppressed, resulting in a decrease in chipping resistance. These preferred ranges are y and yb of 1.5 to 2.5 in terms of oxide.
Weight%, at least one of Mg and Ca is 2% in terms of oxide
．． 0 to 4.0 weight Iχ, Zr is 3.0 to 5.0 in terms of oxide.
0 weight 2.
なお、ＺｒはＺｒ０ｇ＃体では組織中に正方晶または立
方晶として室温で存在させる事は困難であるがＣａ、
Ｍｇ、 Ｙ 、 Ｙｂの酸化物の共存によって正方晶あ
るいは立方晶ＺｒＯ□として共存させることができ、Ｚ
ｒＯ，粒子の分散によって強靭性を高めることができる
。この時の正方晶あるいは立方晶Ｚｒ０１の量は全Ｚｒ
０ｚｊｌ中３０％以上であることが耐チッピング性の点
から望ましい。In addition, it is difficult for Zr to exist in the structure as a tetragonal or cubic crystal at room temperature in the Zr0g# form, but Ca,
By coexisting Mg, Y, and Yb oxides, they can coexist as tetragonal or cubic ZrO□, and Z
Toughness can be increased by dispersing rO and particles. At this time, the amount of tetragonal or cubic Zr01 is the total Zr
It is desirable that the content be 30% or more in terms of chipping resistance.
また、主成分であるＡｌ２ｏ、およびＴｉＣに関しては
Ａｌが酸化物換算で６０重量％未満又はＴｉが炭化物換
算で４０重量％を超えた場合には耐チッピング性が著し
く低下し、そして、Ｔｉが２０重量％未満又はＡｌが８
０重量％を超えた場合には材料の硬変が小さくなり、耐
摩耗性が劣化し、機械加工性が著しく低下する。Regarding Al2o and TiC, which are the main components, if Al is less than 60% by weight in terms of oxide or Ti is more than 40% by weight in terms of carbide, the chipping resistance will be significantly reduced, and if Ti is less than 20% by weight in terms of carbide, Less than 8% by weight or Al
If it exceeds 0% by weight, hardening of the material becomes small, wear resistance deteriorates, and machinability significantly decreases.
本発明によれば、上述したようにｙ 、 ｙｂとＡｌ、
あるｕｓｅ；！Ｍｇ、 ＣａとＡｌとの複合酸化物を形
成させることが重要であって、ｙ 、 ｙｂの少なくと
も１種とＡｌとの第１の複合酸化物、例えば、ＹＪｌｓ
Ｏ＋ｚ、ＹｂｚＡ１ｓＯ＋ｚ（７）存在によッテ、Ａｌ
２Ｏ２とＴｉｃ □）ぬれ性を改善するとともに焼結性
を向上させることができる。一方、Ｃａｓ Ｍｇの少な
くとも１種とＡｌとの第２の複合酸化物、例えば、Ｍｇ
Ｏ・ＡｌｚＯ，、ＣａＯ・Ａｌｚ（ｈ等のスピネルの存
在によって、Ａｌ２Ｏ２の粒成長を抑制し、微細なＡ１
□０３結晶粒子からなる組織を得ることができる。According to the present invention, as described above, y, yb and Al,
Some use;! It is important to form a composite oxide of Mg, Ca and Al, and a first composite oxide of Al and at least one of y and yb, for example, YJls
O+z, YbzA1sO+z(7) existence, Al
2O2 and Tic □) Can improve wettability and sinterability. On the other hand, a second composite oxide of at least one type of Cas Mg and Al, for example, Mg
The presence of spinels such as O・AlzO, and CaO・Alz(h) suppresses the grain growth of Al2O2, resulting in fine Al
A structure consisting of □03 crystal grains can be obtained.
本発明によればこのような複合酸化物が特定の割合で存
在することが重要で、前記第１の複合酸化物が全量中０
．２〜４．６重量％の割合で、また前記第２の複合酸化
物が全量中０．７〜１６．０重量％の割合で存在するこ
とが望ましい。According to the present invention, it is important that such a complex oxide exists in a specific proportion, and the first complex oxide is present in a total amount of 0.
．． It is desirable that the second composite oxide is present in a proportion of 2 to 4.6% by weight, and in a proportion of 0.7 to 16.0% by weight based on the total amount.
これら複合酸化物の量の上記の割合に限定した理由は、
第１の複合酸化物が０．２重量％未満では焼結性改善効
果が得られず、４．６重量％を超えると、材料の強度が
低下する。The reason why the amount of these composite oxides is limited to the above ratio is as follows.
If the first composite oxide is less than 0.2% by weight, the effect of improving sinterability cannot be obtained, and if it exceeds 4.6% by weight, the strength of the material decreases.
一方、第２の複合酸化物が０．７重量％を下回ると粒成
長抑制効果が小さく 、Ａｌ２Ｏ３の粒成長が著しく起
こり、耐チツピング性が悪くなる。また１６重量％を超
えるとＡｈＯｚと複合酸化物との熱膨張差に起因すると
思われるクランクが結晶内に発生する。On the other hand, if the content of the second composite oxide is less than 0.7% by weight, the effect of suppressing grain growth will be small, and grain growth of Al2O3 will occur significantly, resulting in poor chipping resistance. Moreover, if it exceeds 16% by weight, cranks will occur in the crystal, which is thought to be caused by the difference in thermal expansion between AhOz and the composite oxide.
本発明のセラミック材料を製造するにあたっては、主成
分の１つであるＴｉＣ原料にＴｉＯ２を添加したＴｉｃ
−Ｔｉｅ、原料を用いることが望ましく、これによって
ＴｔＣ原料に付着されている遊離炭素がＴｉ１ｔと反応
し、これにより、ＴｉＣの結晶化度が向上して焼結性が
高まり、その結果、均質且つ緻密化された結晶状態が得
られ、表面平滑性が向上する。In manufacturing the ceramic material of the present invention, TiO2 is added to the TiC raw material, which is one of the main components.
-Tie, raw material is preferably used, whereby the free carbon attached to the TtC raw material reacts with Ti1t, thereby improving the crystallinity of TiC and increasing the sinterability, resulting in a homogeneous and A densified crystalline state is obtained and surface smoothness is improved.
しかも、Ｔｉ０ｚはＴｉＣ粒子及びＡ１□０３粒子のそ
れぞれの表面で固溶化され、そのためにＴｉＣ結晶粒子
とＴｆＣ結晶粒子の間、又はＴｉＣ結晶粒子とＡ１．０
、結晶粒子の間のそれぞれの粒子間結合が一層大きくな
り、その結果、焼結体表面を研摩しても粒脱落がなくな
り、優れた表面平滑性が得られる。Moreover, Ti0z is formed into a solid solution on the surfaces of TiC particles and A1
, the interparticle bonds between the crystal grains become even larger, and as a result, even if the surface of the sintered body is polished, grains do not fall off, and excellent surface smoothness is obtained.
このようにＴｉＣ原料の一部をＴｉＯ□で置換すると、
上記２点の理由により表面平滑性が向上するが、そのた
めのＴｉＯ２原料配合率はＡ１□０３、ＴｉＣの合計量
１００重量部に対し、２乃至８重量部の範囲内に設定す
ればよい。When a part of the TiC raw material is replaced with TiO□ in this way,
The surface smoothness is improved due to the above two reasons, and the TiO2 raw material blending ratio for this purpose may be set within the range of 2 to 8 parts by weight based on 100 parts by weight of the total amount of A1□03 and TiC.
このようなＡ１ｚＯｉ粉末と、ＴｉＣ粉末あるいはＴｉ
ＣとＴｉＯ□とからなる粉末を主成分とし、これに副成
分としてＹあるいはＹｂ、、ＣａあるいはＭｇの化合物
を前述した割合になるように添加し混合する。これらは
いずれも酸化物として添加させ、成形、焼成することに
よって前述した第１の複合酸化物および第２の複合酸化
物が形成されるが場合によっては第１および第２の複合
酸化物を予め調製しておき、主成分に対し添加すること
も当然可能である。Such A1zOi powder and TiC powder or Ti
A powder consisting of C and TiO□ is used as a main component, and a compound of Y, Yb, Ca, or Mg is added as a subcomponent to the powder in the proportions described above and mixed. The first and second composite oxides described above are formed by adding these as oxides, molding and firing, but in some cases the first and second composite oxides may be added in advance. Of course, it is also possible to prepare it in advance and add it to the main component.
一方、ＺｒはＺｒＯ□として主成分に添加されるが、Ｚ
ｒ０ｚは焼結体ではｙ、ｏ、、Ｙｂ２Ｏ３、ＭｇＯ、Ｃ
ａＯ等のＺｒＯ□に対する安定化剤が存在することから
焼成によって安定化剤がＺｒＯ□中に固溶し正方晶Ｚｒ
Ｏ□あるいは立方晶ＺｒＯ２に相変態するが、この相変
態を補償することを目的として、混合時に予め安定化剤
を固溶させたＺｒ０ｚ粉末を用いることもできる。On the other hand, Zr is added to the main component as ZrO□, but Zr
r0z is y, o, , Yb2O3, MgO, C in the sintered body
Since there is a stabilizer such as aO for ZrO
The phase transforms into O□ or cubic ZrO2, but for the purpose of compensating for this phase transformation, it is also possible to use Zr0z powder in which a stabilizer is dissolved in advance during mixing.
焼成は、具体的にはホットプレス法、あるいは熱間静水
圧焼成法（ＨＩＰ法）が挙げられるが、特にＨＩＰ法が
高密度体を得る上で望ましい。この旧Ｐ法ではまず、ホ
ットプレス法あるいは真空焼成法によって１６００〜１
７５０℃で予備焼成して理論密度９５％以上の焼結体を
得、さらに１４００〜１５５０℃で圧力１０００〜２０
００ａｔｍの雰囲気下で旧Ｐ焼成する。Specific examples of the firing include a hot press method or a hot isostatic pressure firing method (HIP method), and the HIP method is particularly desirable for obtaining a high-density body. In this old P method, first, a hot press method or a vacuum firing method is used to obtain a
A sintered body with a theoretical density of 95% or more is obtained by pre-firing at 750°C, and then at a pressure of 1000-20°C at 1400-1550°C.
Old P is fired in an atmosphere of 00 atm.
本発明では、複合酸化物の生成によって焼成温度を低く
設定できることからＡ１□０３の粒成長が十分に抑制さ
れ微細な組織のセラミック材料を得ることができる。In the present invention, since the firing temperature can be set low due to the formation of the composite oxide, grain growth of A1□03 can be sufficiently suppressed and a ceramic material with a fine structure can be obtained.
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）
Ａｌ２０３粉末（純度９９．９χ）、ＴｉＣ原料（純度
９９．５２）、ＺｒＯ□原料ＵｇＯが１０モルχ固溶し
ており、主として立方晶結晶である） 、ＣａＣ０ｚ
、Ｍｇ（ＯＨ）ｚ 、 Ｙ２Ｏ３、ｙｂｏ、の各原料を
第１表に示す配合比率で混合して出発原料と成し、振動
ミルにより粉砕ならびに混合を行い、平均粒子径０．８
μｍの混合粉末を作製した。(Example) Al203 powder (purity 99.9χ), TiC raw material (purity 99.52), ZrO□ raw material UgO are dissolved in 10 mol χ solid solution, mainly cubic crystals), CaC0z
, Mg(OH)z, Y2O3, and ybo are mixed at the compounding ratio shown in Table 1 to form a starting material, which is pulverized and mixed using a vibration mill to obtain an average particle size of 0.8.
A mixed powder of μm size was prepared.
これヲ０．５ｔ／ｃＩＩＩｚの圧力で成形し、アルゴン
ガス雰囲気中、１６００℃で予備焼成した。次に、これ
を１４５０℃の温度で２０００Ｋｇ／ｃｍ”の圧力の不
活性ガス中で熱間静水圧焼成し、５００℃／ｈｒの速度
で室温まで冷却した。This was molded at a pressure of 0.5t/cIIIz and preliminarily fired at 1600°C in an argon gas atmosphere. Next, this was subjected to hot isostatic firing in an inert gas at a temperature of 1450° C. and a pressure of 2000 Kg/cm”, and cooled to room temperature at a rate of 500° C./hr.
得られた焼結体に対し、Ｘ線回折により、Ａ１□Ｏ８に
対する複合酸化物のＸ線強度比を求め、予め作成したＡ
ｌ２Ｏ２と複合酸化物との量比を変えてＸ線強度比を求
めた検量線から、焼結体中の複合酸化物の含有量を求め
た。The obtained sintered body was subjected to X-ray diffraction to determine the X-ray intensity ratio of the composite oxide to A1□O8, and the
The content of the composite oxide in the sintered body was determined from a calibration curve in which the X-ray intensity ratio was determined by changing the ratio of l2O2 to the composite oxide.
また、各試料に対して、鏡面加工性、ピンカース硬度、
耐チッピング性を評価した。In addition, for each sample, mirror workability, Pinkers hardness,
Chipping resistance was evaluated.
鏡面加工性はスズのラップ盤を用い、ダイヤモンド砥粒
（０，５〜３．０μｍ）により鏡面加工し、その鏡面を
４００倍の金属顕微鏡で調べ、気孔、脱粒の確認された
ものを×、確認されないものを○とした。For mirror finish processing, use a tin lapping machine to mirror finish with diamond abrasive grains (0.5 to 3.0 μm), examine the mirror surface with a metallurgical microscope at 400x magnification, and select those with confirmed pores and shedding. Items that were not confirmed were marked as ○.
また、耐チッピング性は５００のメタルボルトのホイー
ルを用いて、角折を切断し、加工部に発生したチフビン
グの大きさを大きい方から１０点選びその平均サイズを
測定し、平均サイズが２０μｍ以下のものを０１２０μ
ｍを超えるものを×とした。In addition, chipping resistance was measured by cutting the corner using a 500 metal bolt wheel, selecting 10 points from the largest size of chipping that occurred on the processed part, and measuring the average size. 0120μ
Those exceeding m were marked as ×.
この時の切削条件はホイール回転数３５００ｒｐｍ、送
り６０ｍｍ／ｗｉｎであった。The cutting conditions at this time were a wheel rotation speed of 3500 rpm and a feed rate of 60 mm/win.
結果は第１表に示す。The results are shown in Table 1.
第１表の結果からも明らかな通り、本発明の範囲内の試
料では、いずれもピンカース硬度１８５０以上が達成さ
れるとともに、鏡面加工性においても、気孔や脱粒が確
認され、また耐チッピング性においてもチフピングサイ
ズ２０μｍ以下の良好な特性を示した。なお、本発明の
範囲外の試料である隘１６〜２６の試料はいずれも満足
し得るものでなかった。As is clear from the results in Table 1, all of the samples within the scope of the present invention achieved a Pinkers hardness of 1850 or higher, and pores and grain shedding were confirmed in mirror workability, as well as chipping resistance. It also showed good characteristics with a chipping size of 20 μm or less. Incidentally, none of the samples in Nos. 16 to 26, which are samples outside the scope of the present invention, were satisfactory.
（発明の効果）
以上、詳述した遺り、本発明のセラミック材料は複合酸
化物の生成によって、焼結性を改善し、低温焼成が可能
となり、Ａｌ□０３の粒成長を十分に抑制し、微細な組
織の材料が得られる。これにより、鏡面加工性、耐チッ
ピング性、表面硬度に優れることから、スライシング加
工等に際し、製造歩留りを著しく高めることができる。(Effects of the Invention) As described above in detail, the ceramic material of the present invention improves sinterability by forming a composite oxide, enables low-temperature firing, and sufficiently suppresses grain growth of Al□03. , a material with a fine structure is obtained. As a result, it has excellent mirror workability, chipping resistance, and surface hardness, so it is possible to significantly increase the manufacturing yield during slicing processing and the like.
本発明のセラミック材料は、上記の利点から薄膜磁気ヘ
ッド用基板、磁気ディスク用基板、精密加工用治具の構
成材料等として利用できる。Due to the above-mentioned advantages, the ceramic material of the present invention can be used as a constituent material of thin-film magnetic head substrates, magnetic disk substrates, precision machining jigs, and the like.
Claims (1)
算で２０乃至４０重量％のＴｉから成る主成分１００重
量部に対し、Ｙ、Ｙｂの少なくとも１種を酸化物換算で
０．５乃至４．０重量部、Ｚｒを酸化物換算で２．０〜
６．０重量部およびＭｇ、Ｃａの少なくとも１種を酸化
物換算で１．０乃至５．０重量部の割合で含有して成る
セラミック材料において、Ｙ、Ｙｂの少なくとも１種と
Ａｌとの複合酸化物を全量中０．２乃至４．６重量％、
またＭｇ、Ｃａの少なくとも１種とＡｌとの複合酸化物
を０．７乃至１６重量％の割合で含有することを特徴と
するＡｌ＿２Ｏ＿３−ＴｉＣ系セラミック材料。For 100 parts by weight of the main component consisting of 60 to 80% Al in terms of oxide and 20 to 40% by weight of Ti in terms of carbide, at least one of Y and Yb is added in an amount of 0.5 to 4% in terms of oxide. 0 parts by weight, Zr 2.0 to 2.0 in terms of oxide
6.0 parts by weight and at least one of Mg and Ca in a proportion of 1.0 to 5.0 parts by weight in terms of oxide, a composite of at least one of Y and Yb and Al. 0.2 to 4.6% by weight of oxide in the total amount,
Further, an Al_2O_3-TiC ceramic material containing a composite oxide of Al and at least one of Mg and Ca in a proportion of 0.7 to 16% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1098498A JP2699104B2 (en) | 1989-04-18 | 1989-04-18 | A1 Lower 2 O Lower 3-TiC ceramic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1098498A JP2699104B2 (en) | 1989-04-18 | 1989-04-18 | A1 Lower 2 O Lower 3-TiC ceramic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02279558A true JPH02279558A (en) | 1990-11-15 |
| JP2699104B2 JP2699104B2 (en) | 1998-01-19 |
Family
ID=14221307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1098498A Expired - Lifetime JP2699104B2 (en) | 1989-04-18 | 1989-04-18 | A1 Lower 2 O Lower 3-TiC ceramic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2699104B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5425909A (en) * | 1992-07-20 | 1995-06-20 | Industrial Technology Research Institute | Heat treatment for particle reinforced alumina ceramic composite |
| JP2005272291A (en) * | 2004-02-26 | 2005-10-06 | Kyocera Corp | Aluminum oxide titanium nitride-based sintered compact, substrate for magnetic head using the same, ultrasonic motor, dynamic pressure bearing, and method for manufacturing the same |
-
1989
- 1989-04-18 JP JP1098498A patent/JP2699104B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5425909A (en) * | 1992-07-20 | 1995-06-20 | Industrial Technology Research Institute | Heat treatment for particle reinforced alumina ceramic composite |
| JP2005272291A (en) * | 2004-02-26 | 2005-10-06 | Kyocera Corp | Aluminum oxide titanium nitride-based sintered compact, substrate for magnetic head using the same, ultrasonic motor, dynamic pressure bearing, and method for manufacturing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2699104B2 (en) | 1998-01-19 |
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