JPH04132657A - Heat-resistant alumina ceramics - Google Patents
Heat-resistant alumina ceramicsInfo
- Publication number
- JPH04132657A JPH04132657A JP2253627A JP25362790A JPH04132657A JP H04132657 A JPH04132657 A JP H04132657A JP 2253627 A JP2253627 A JP 2253627A JP 25362790 A JP25362790 A JP 25362790A JP H04132657 A JPH04132657 A JP H04132657A
- Authority
- JP
- Japan
- Prior art keywords
- spinel
- heat
- alumina ceramics
- resistant alumina
- dispersed
- 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 title claims abstract description 16
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 23
- 239000011029 spinel Substances 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 abstract description 5
- 229910052594 sapphire Inorganic materials 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 2
- 229910026161 MgAl2O4 Inorganic materials 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N Al2O Inorganic materials [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 230000002747 voluntary effect Effects 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、１耐熱アルミナセラミツクスに関するもので
あり、史に詳しくは、高温で使用可能な構造材料、ある
いは切削工具材料として好適なアルミナセラミックスに
関するものでらる。Detailed Description of the Invention "Field of Industrial Application" The present invention relates to heat-resistant alumina ceramics, and more specifically to alumina ceramics suitable as structural materials that can be used at high temperatures or cutting tool materials. You can get something.
「従来の技術」
従来より、種々のアルミナセラミックスが製造されてお
り、純度、微構造Ｖこよりその特性が変化することが知
られている。例えば、創意書店発行ｒファインセフミッ
クスハンドブック」Ｐ、４６１には、アルミナ含有量９
０〜９９％のアルミナセラミックスの強度の温ＩＷ依存
性について、アルミナ含有量の増大とともに強度が向」
二することが記載されている。"Prior Art" Various alumina ceramics have been produced in the past, and it is known that their properties vary depending on their purity and microstructure. For example, in "Fine Safety Mix Handbook" published by Sosei Shoten, P. 461, the alumina content is 9.
Regarding the temperature IW dependence of the strength of 0-99% alumina ceramics, the strength increases as the alumina content increases.
It describes two things to do.
ま之、近年アルミナ粒子内に微細なＳｉＣ粒子全分散さ
せ、強度、靭性を向上させようとする試みも成さルてい
る。（特開昭６４−８７５５２号公報）
「発明が解決しようとする課題」
従来のアルミナセラミックスｉ、１０００“０位までの
低温域の特性に優れるものはあったが１２００°Ｃ以上
の？ｔｉ温で機械的特性が劣化するという問題点があっ
た。本開明はこの問題点を解決する耐熱アルミナセラミ
ックスを提供する。However, in recent years, attempts have been made to completely disperse fine SiC particles within alumina particles to improve strength and toughness. (Japanese Unexamined Patent Publication No. 64-87552) ``Problem to be solved by the invention'' Conventional alumina ceramics have excellent properties in the low temperature range of 1000°C or higher, but the There has been a problem that the mechanical properties are deteriorated in the process.The present invention provides a heat-resistant alumina ceramic that solves this problem.
「課題を解決するための手段及び作用」その手段は、α
−Ａ １２０３及びその粒界に分散しているスピネｌ
Ｍ ｇ Ａ １２０４よりなる焼結体において、上記ス
ピネルの粒子径’ｋ ０．１μｍ以下とし、その含有１
ｔをＭｇＯ換算で１．５〜３．０重量係とするところに
ある。“Means and actions to solve the problem” The means are α
-A 1203 and spinel dispersed in its grain boundaries
In the sintered body made of M g A 1204, the particle diameter 'k of the spinel is 0.1 μm or less, and the content 1
t is set at 1.5 to 3.0 weight factor in terms of MgO.
本発明の耐熱アルミナセラミックスにおいては、微細な
スピネル粒子がα−ＡＩ２０３粒子間の粒界に分散して
いることが直要である。粒界（２つの粒子間）に分散し
た微細スピネル粒子は、高温において、すべり、粒界割
れを妨害することにより、耐熱性を改善するものと考え
られる。粒径が０．１μｍを超えると、スピネル粒子は
粒界（２つの粒子間）に存在することは離しくなり、粒
界全頁いて存在、あるいは８直点（３つの粒子間）に析
出するため、かえって高温特性を劣化させる。In the heat-resistant alumina ceramic of the present invention, it is directly important that fine spinel particles are dispersed in the grain boundaries between α-AI203 particles. The fine spinel particles dispersed at grain boundaries (between two grains) are thought to improve heat resistance by preventing slippage and intergranular cracking at high temperatures. When the grain size exceeds 0.1 μm, spinel grains are less likely to exist at the grain boundary (between two grains), and either exist at the entire grain boundary or precipitate at eight straight points (between three grains). Therefore, the high temperature characteristics are deteriorated instead.
スピネルの含有型はＭｇＯ換算で１．５〜ａｗｔチでお
る坐が必要である１、５ｗｔ％より少ないと微細スピネ
ル粒子の粒界における分散量が充分でないために、耐熱
性が改善されず、また、３ｗｔ％より多くなるとスピネ
ル粒子は微細に分散し難くなり、粒界を貫いて析出、あ
るいは３重点に析出し易くなる。The spinel content needs to be 1.5 to awt in terms of MgO. If it is less than 1.5 wt%, the heat resistance will not be improved because the amount of fine spinel particles dispersed at the grain boundaries will not be sufficient. Moreover, when the amount exceeds 3 wt%, it becomes difficult for spinel particles to be finely dispersed, and they tend to precipitate through grain boundaries or to precipitate at triple points.
本発の耐熱アルミナセラミックスにおける微細スピネル
粒子の粒径は、透過型電子顕微鏡観察により測定するこ
とができる。第１図にその結果の一例をボす。The particle size of the fine spinel particles in the heat-resistant alumina ceramic of the present invention can be measured by observation with a transmission electron microscope. Figure 1 shows an example of the results.
本発明の耐熱アルミナセラミックスの耐熱性とは、毘温
における強度、耐クリープ性、疲労抵抗性などｔｉｔ味
するが、こｎらの耐熱性は、内部摩擦の制御により向上
嘔せることができる。The heat resistance of the heat-resistant alumina ceramics of the present invention refers to strength at ambient temperatures, creep resistance, fatigue resistance, etc., and these heat resistances can be improved by controlling internal friction.
すなわち、内部摩擦の増加は耐熱性の低下と密接に関連
しており、内部摩擦の温度依存性を測定することにより
、材料の耐熱温度を推定することができる。That is, an increase in internal friction is closely related to a decrease in heat resistance, and by measuring the temperature dependence of internal friction, the heat resistance temperature of a material can be estimated.
本発明の耐熱アルミナセラミックスの製造には、粒径１
μｍ以下の微粒かつ純度９９．９％以上の高純度の原料
を用いることが望ましい。原料の粒径が粗大でおると、
焼結性が劣り、また原料中の不純物はその量が過剰であ
ると高温特性を著しく低下させる。原料のＡ １２０３
粉末は、焼成後（１−Ａｌ２Ｏ３になるものであれば、
ｒ −Ａｌ２Ｏ３等でもよい。Ｍｇ成分はＭｇＯあるい
はＡ １２０３と反応してスピネ／Ｌ’ （ＭｇＡｌ２
Ｏ４）を生成するものであれはＭｇ ＣＯａ等の塩類で
もよい。The production of the heat-resistant alumina ceramics of the present invention requires a particle size of 1
It is desirable to use a raw material with fine particles of .mu.m or less and high purity of 99.9% or more. If the particle size of the raw material is coarse,
The sinterability is poor, and if the amount of impurities in the raw material is excessive, the high temperature properties will be significantly reduced. Raw material A 1203
If the powder becomes 1-Al2O3 after firing,
r-Al2O3 etc. may also be used. The Mg component reacts with MgO or A 1203 to form spine/L' (MgAl2
Salts such as Mg COa may be used as long as they generate O4).
焼結は大気中１４００°Ｃ〜１７００”Ｃで行うことが
できるが、ホットプレスやＨＩＰによっても緻密化でき
る。Sintering can be carried out in the air at 1400°C to 1700''C, but densification can also be achieved by hot pressing or HIP.
「実施例」
平均粒径０．４μｍ１純度９９．９９％のａ−Ａｌ２Ｏ
３粉末に、平均粒径０．６μｍ１純度９９．９５％のＭ
ｇＯ粉末を第１表に示す割合で配合した。乾燥し友配合
粉末を、静水圧プレスにより ２ ｔｏｎ／ｉの圧力で
ｌ１０Ｘ１０Ｘ６０ｎに成形し、大気中１５００℃〜１
５５０℃で焼結を行い、アルミナセラミックスを得ｆｃ
。"Example" Average particle size 0.4 μm 1 purity 99.99% a-Al2O
3 powder, average particle size 0.6 μm 1 purity 99.95% M
gO powder was blended in the proportions shown in Table 1. The dried Tomo blended powder was molded into a size of 110 x 10 x 60 nm using a hydrostatic press at a pressure of 2 tons/i, and heated at 1,500°C to 1,000 ℃ in the atmosphere.
Sintering is performed at 550℃ to obtain alumina ceramics fc
.
このセラミックスの特性を以下の方法により測定し、結
果を第１表に示した。The characteristics of this ceramic were measured by the following method, and the results are shown in Table 1.
（１）内部摩擦：室温から１８５０°Ｃにおいてねじり
振動法により測定（→第３図参照）第１表中の値は１３
００°Ｃの内部摩擦（Ｑ ）
（２）抗折強度：室温及び１３００℃にてＪＩＳＲ−１
６０１及びＪＩＳ Ｒ−１６０４に従う８点曲げ強度
（８）結晶相の同定＝Ｘ線回折
第１表に示すように、本発明により得られたアルミナセ
ラミックス（Ｎｃｌ〜３）は、１３０ｏ ”ｃにおける
内部Ｗ１襟（Ｑ−’ ）が８×１０ 以下と小さい。さ
らに、室温から１３００°Ｃにかけての強度低下が極め
て小さく、１８００°Ｃにおいても４００ ＭＰａ以上
の高強度を示した。(1) Internal friction: Measured by the torsional vibration method at room temperature to 1850°C (see Figure 3) The value in Table 1 is 13
Internal friction (Q) at 00°C (2) Flexural strength: JISR-1 at room temperature and 1300°C
601 and JIS R-1604 (8) Identification of crystal phase = X-ray diffraction As shown in Table 1, the alumina ceramics (Ncl ~ 3) obtained by the present invention has an internal The W1 collar (Q-') is as small as 8x10 or less.Furthermore, the decrease in strength from room temperature to 1300°C is extremely small, and even at 1800°C, it showed a high strength of 400 MPa or more.
一方比較例として示したセラミックス隘４゜５は、スピ
ネル粒子が存在しないか、又はα−Ａｌ２Ｏ３の粒界に
おけるスピネルの分散量が少ないため、また、磁６〜８
はスピネル粒子が微細に分散していないため、それぞれ
１３００ ”Ｃの内部摩擦が大きくなり、１３００−Ｃ
での強度が著しく低下した。On the other hand, the ceramic size 4°5 shown as a comparative example has no spinel particles or the amount of spinel dispersed at the grain boundaries of α-Al2O3 is small.
Since the spinel particles are not finely dispersed, the internal friction of 1300"C becomes large, and 1300"C
The strength at
このように比軟例は本発明のアルミナセラミソクヌに対
ｌ−で耐熱性が著しく劣る。As described above, the heat resistance of the comparatively soft material is significantly inferior to that of the alumina ceramic material of the present invention.
「発明の効果」
本発明によれば、粒イ釜０．１μｍ以下のスピネル粒子
をα−Ａ １２０３粒子間の粒界に分散させることによ
り、１３００°Ｃ以上の耐熱性に優れたアルミナセラミ
ックス全提供することができる。``Effects of the Invention'' According to the present invention, by dispersing spinel particles of 0.1 μm or less in the grain boundaries between α-A 1203 particles, alumina ceramics with excellent heat resistance of 1300°C or higher can be produced. can be provided.
／/
第１図はスピネルの含有量がＭｇＯ換算で２ｗｔ係の耐
熱アルミナセヲミックスの結晶構造ヲ示す透過型電子′
ｙＡ倣鏡（ＴＥＭ）写真である。
第２図は第１図写真を説明する模式図である。
第３図はスピネルの含有量がＭｇＯ換算で１〜１０ｗｔ
％のＩ＋＋ｉｔ ｐ＝アルミナセフミックスの内部摩擦
と温度との関係を示すグラフである。
特許出願人 日本特殊陶業株式会社
回 岡 本 平同
松 下 健 −
代
理
人
矢
野
正
行
第１図
トーーーーＨ
０，１１Ｌ九
（自発）
５、補正の対象
明細書中、発明の詳細な説明の欄。Figure 1 shows the crystal structure of a heat-resistant alumina sewomix with a spinel content of 2wt in terms of MgO.
This is a yA copy mirror (TEM) photograph. FIG. 2 is a schematic diagram illustrating the photograph in FIG. 1. Figure 3 shows the content of spinel in terms of MgO of 1 to 10wt.
% I++it p=Graph showing the relationship between internal friction and temperature of alumina cefmix. Patent Applicant: Nihon Spark Plug Co., Ltd., Okamoto, Hiramatsu, Ken Shimo - Agent, Masayuki Yano Figure 1 - H 0,11L9 (voluntary) 5. Detailed explanation of the invention in the specification to be amended.
Claims (2)
スピネルＭｇＡｌ＿２Ｏ＿４よりなる焼結体において、
上記スピネルの粒子径が０．１μｍ以下であってその含
有量がＭｇＯ換算で１．５〜３．０重量％であることを
特徴とする耐熱アルミナセラミックス。(1) In a sintered body consisting of α-Al_2O_3 and spinel MgAl_2O_4 dispersed in its grain boundaries,
A heat-resistant alumina ceramic, characterized in that the particle size of the spinel is 0.1 μm or less and the content thereof is 1.5 to 3.0% by weight in terms of MgO.
×１０＾−＾３以下である請求項１に記載の耐熱アルミ
ナセラミックス。(2) Internal friction (Q^-^1) at 1300℃ is 8
The heat-resistant alumina ceramics according to claim 1, wherein the heat-resistant alumina ceramic is not more than ×10^-^3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2253627A JP2879169B2 (en) | 1990-09-21 | 1990-09-21 | Heat resistant alumina ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2253627A JP2879169B2 (en) | 1990-09-21 | 1990-09-21 | Heat resistant alumina ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04132657A true JPH04132657A (en) | 1992-05-06 |
| JP2879169B2 JP2879169B2 (en) | 1999-04-05 |
Family
ID=17253978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2253627A Expired - Lifetime JP2879169B2 (en) | 1990-09-21 | 1990-09-21 | Heat resistant alumina ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2879169B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016106068A (en) * | 2010-07-12 | 2016-06-16 | コーニング インコーポレイテッド | High static fatigue alumina isopipe |
| DE112020006480T5 (en) | 2020-01-10 | 2022-11-17 | Kyocera Corporation | HEAT RESISTANT ELEMENT |
-
1990
- 1990-09-21 JP JP2253627A patent/JP2879169B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016106068A (en) * | 2010-07-12 | 2016-06-16 | コーニング インコーポレイテッド | High static fatigue alumina isopipe |
| DE112020006480T5 (en) | 2020-01-10 | 2022-11-17 | Kyocera Corporation | HEAT RESISTANT ELEMENT |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2879169B2 (en) | 1999-04-05 |
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