JPH02167857A - High toughness mullite sintered body and its manufacturing method - Google Patents
High toughness mullite sintered body and its manufacturing methodInfo
- Publication number
- JPH02167857A JPH02167857A JP63321937A JP32193788A JPH02167857A JP H02167857 A JPH02167857 A JP H02167857A JP 63321937 A JP63321937 A JP 63321937A JP 32193788 A JP32193788 A JP 32193788A JP H02167857 A JPH02167857 A JP H02167857A
- Authority
- JP
- Japan
- Prior art keywords
- mullite
- sintered body
- weight
- parts
- powder
- 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
Links
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims description 42
- 229910052863 mullite Inorganic materials 0.000 title claims description 42
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000002245 particle Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、高靭性を有するムライト質焼結体及びその製
造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a mullite sintered body having high toughness and a method for producing the same.
（従来の技術及び発明が解決しようとする課題）ムライ
ト質焼結体は、高温における強度の低下が極めて少ない
ことから、高温構造材料としての利用がすすめられてい
る。(Prior Art and Problems to be Solved by the Invention) Mullite sintered bodies are being used as high-temperature structural materials because their strength decreases very little at high temperatures.
しかし、このムライト質焼結体は、窒化珪素焼結体や炭
化珪素焼結体に比して、酸化物であることから耐酸化性
においてすぐれているものの破壊靭性値において及ばず
、この破壊靭性値が小さいことが実用上大きな障害とな
っていた。However, compared to silicon nitride sintered bodies and silicon carbide sintered bodies, this mullite sintered body has excellent oxidation resistance because it is an oxide, but it does not have the same fracture toughness. The small value has been a major obstacle in practical use.
この問題点を解決するために、以下の方法が提案されて
いる。In order to solve this problem, the following method has been proposed.
平均粒子径が１．０μ慴以上のムライト粉末（閏えば電
融ムライト粉末）にＹ２Ｏ１等を添加して緻密化させる
。Mullite powder having an average particle diameter of 1.0 μm or more (or electrofused mullite powder) is densified by adding Y2O1 or the like.
（日本セラミックス協会秋季シンポジウム講演予講集−
Ｐ、 ７３３（１９８８））
この方法では、従来緻密化が困難であった平均粒子径が
１．０ ＡＬｎ以上のムライト粉末を用いて緻密な焼結
体が得られるものの、その焼結体中の粒子のアスペクト
比は小さく、焼結体の破壊靭性値は小さいという欠点を
有している。(Japan Ceramics Association Autumn Symposium Lecture Preliminary Collection-
P, 733 (1988)) With this method, a dense sintered body can be obtained using mullite powder with an average particle size of 1.0 ALn or more, which has been difficult to densify in the past. The disadvantage is that the aspect ratio of the particles is small and the fracture toughness value of the sintered body is small.
（課題を解決するための手段）
本発明は、ムライト質焼結体の微構造を制御し、柱状の
組織を析出させた構造をもつことにより、破壊靭性値の
向上したムライト質焼結体及びその製造方法を提供する
ものである。(Means for Solving the Problems) The present invention provides a mullite sintered body with improved fracture toughness by controlling the microstructure of the mullite sintered body and having a structure in which a columnar structure is precipitated. The present invention provides a method for manufacturing the same.
一般に、ムライト質焼結体は添加物なしで緻密化するこ
とから、ムライト粉末の高純度化と焼結プロセスの検討
が盛んになされている。In general, since mullite sintered bodies can be densified without additives, studies are being actively conducted to improve the purity of mullite powder and the sintering process.
しかし、こうして得られるムライト質焼結体は比較的均
一な組織を有しており、そのため亀裂進展に対する抵抗
力が小さいという欠点を有していた。そこでかかる欠点
を克服すべく鋭意研究を進めて来た結果、ムライト前駆
体（本明、４Ｉ＠において、焼成によりムライトとなる
ものをいう〉またはムライト粉末の平均粒子径が１．０
μｍ未満である出発原料にＹ２Ｏ，を添加して焼結する
ことにより焼結体にアスペクト比３以上の柱状Ｍｌ織を
自在に析出させることを得、その結果、ムライト質焼結
体の破壊靭性値を大幅に向上させることを見出だすに至
った。However, the mullite sintered body obtained in this way has a relatively uniform structure, and therefore has the disadvantage of low resistance to crack propagation. As a result of intensive research to overcome these drawbacks, we have found that the average particle diameter of mullite precursor (in the present invention, 4I@ refers to a substance that becomes mullite by firing) or mullite powder is 1.0.
By adding Y2O to the starting material having a particle diameter of less than μm and sintering it, it is possible to freely precipitate a columnar Ml weave with an aspect ratio of 3 or more in the sintered body, and as a result, the fracture toughness of the mullite sintered body is improved. We have found that the value can be significantly improved.
すなわち、本発明は
（１）組成が
ＡＩ、 ０ 、 ７２〜７６重量部、残部 Ｓ！ＯＪか
らなるムライト １００重量部
Ｙ２Ｏ，１〜１０重量部
であり、平均アスペクト比３以上の柱状晶からなり、か
つ密度が３．０ ｇ／ａｌｌ’ 以上であることを特
徴とするムライト質焼結体。That is, the present invention has (1) a composition of AI, 0, 72 to 76 parts by weight, and the balance S! Mullite consisting of 100 parts by weight of OJ, 1 to 10 parts by weight of Y2O, consisting of columnar crystals with an average aspect ratio of 3 or more, and having a density of 3.0 g/all' or more. body.
（２）組成が
Ａ１□ＯＢ ７２〜７６重量部、残部 ＳｉＯ２からな
るムライト前駆体マたはムライト粉末の平均粒子径が１
．０μ鴎未溝である出発原料に、上記ムライト前駆体（
ムライト質焼結体）またはムライト粉末１００重量部あ
たり、Ｙ２Ｏ，を１〜１０重量部添加して、１６００〜
１８００’Ｃで焼結することを特徴とするムライト質焼
結体の製造方法を提供するものである。(2) The average particle diameter of the mullite precursor matrix or mullite powder consisting of A1□OB 72 to 76 parts by weight and the balance SiO2 is 1
．． The above mullite precursor (
per 100 parts by weight of mullite sintered body) or mullite powder, add 1 to 10 parts by weight of Y2O,
The present invention provides a method for producing a mullite sintered body characterized by sintering at 1800'C.
本発明において、Ｙ２Ｏ，の添加量が上記範囲を下回る
と柱状粒子の生成は極めてわずかなものとなり、破壊靭
性値向上に寄与しなくなり、上記範囲を上回ると柱状粒
子は巨大化しすぎ焼結体内に多くの空孔を生みｔｌｉ械
的な性質を低下させてしまう。In the present invention, if the amount of Y2O added is less than the above range, the formation of columnar particles will be extremely small and will not contribute to improving the fracture toughness value, and if it exceeds the above range, the columnar particles will become too large and will not be contained within the sintered body. This creates many pores and deteriorates the mechanical properties.
またムライト前駆体またはムライト粉末の平均粒子径が
１．０μｍ未満でなくてはならず、これを越える勉径を
有するものに対しては、Ｙ２Ｏ，を添加しても単にわず
かに液相を生成させ緻密化に寄与するのみにとどまり、
破壊靭性を向上させるようなアスペクト比の大きい柱状
粒子を生成させることができない。In addition, the average particle size of the mullite precursor or mullite powder must be less than 1.0 μm, and if the particle size exceeds this, even if Y2O is added, only a slight liquid phase will be formed. It only contributes to densification,
It is not possible to generate columnar particles with a large aspect ratio that would improve fracture toughness.
本発明における焼結温度は１６００〜１８００℃でなく
てはならず、この範囲を下回ると緻密化は進行せず、こ
の範囲を上回ると異常粒成長が発生し、焼結体の機械的
性質が著しく低下してしまう。The sintering temperature in the present invention must be between 1600 and 1800°C; below this range, densification will not proceed, and above this range, abnormal grain growth will occur and the mechanical properties of the sintered body will deteriorate. It will drop significantly.
焼結方法は、公知の各種方法が採用され１例えば、ホッ
トプレス法、熱間静水圧法などがあげられる。As the sintering method, various known methods are employed, such as a hot press method and a hot isostatic pressure method.
焼結時間は焼結温度との関係で適宜選択することができ
るが２時間以上が好ましい。The sintering time can be appropriately selected depending on the sintering temperature, but is preferably 2 hours or more.
これらの条件を満たずことにより、本発明により緻密化
した焼結体はその組成によらず平均強度において２０〜
２５ｋｇ／ｉｎ ２を有したうえで、高靭性化の効果が
達成される構造となる。By satisfying these conditions, the sintered body densified according to the present invention has an average strength of 20 to 20, regardless of its composition.
25 kg/in 2 and the structure achieves the effect of increasing toughness.
（作用）
上記の条件のもと、上記の割合でＹ２Ｏ，を添加し、焼
結することにより、何故本発明の効果が発生するかにつ
いては、未だ十分には解明されていないが以下のような
理由によるものと思われる９上記の条件のもと、上記の
割合でＹ２Ｏ，を添加し、焼結すると緻粉木ムライト前
駆体または倣粉末ムライトとＶ、Ｏ，が速やかに反Ｌ６
シムライト粒子を柱状に成長させるに必要な液田を生威
し、これをらとにムライト粒子が焼結体において３次元
的に成長することにより、亀裂進展をくいとめる＃ｆｉ
Ｂが焼結体内部に生まれるためであると考えられる。(Function) It is not yet fully understood why the effect of the present invention is produced by adding Y2O in the above ratio and sintering under the above conditions, but as follows. 9 Under the above conditions, when Y2O is added in the above ratio and sintered, the fine wood mullite precursor or imitation powder mullite and V, O, quickly form anti-L6
#fi creates a liquid field necessary to grow simlite particles into a columnar shape, and from this, mullite particles grow three-dimensionally in the sintered body to prevent crack propagation.
This is thought to be because B is generated inside the sintered body.
以上の理由から上記の条件のちと、上記の割合てＹ２０
．ｆ！−添ゐ口５、焼結することにより緻密化した焼結
１水は亀裂進展をさまたける構造となり高い破壊靭性値
を有するようになる。For the above reasons, after the above conditions, the above ratio is Y20
．． f! - Sintering port 5: The sintered water densified by sintering has a structure that prevents crack propagation and has a high fracture toughness value.
（発明の効果）
以上説明したように、本発明のムライト質焼結体は高い
破壊靭性値を有するセラミックスであり、ｂ℃来のムラ
イｌ−質焼結体の１史用範囲を拡張することが可ＩＩＥ
となる。(Effects of the Invention) As explained above, the mullite sintered body of the present invention is a ceramic having a high fracture toughness value, and it is possible to expand the historical range of mullite sintered body since b℃. Possible IIE
becomes.
また、本発明の方法により、上記のムライト質−Ｆｔ粘
結体製逍することができる。Further, the method of the present invention can produce the above-mentioned mullite-Ft caking body.
（実總例）
実施例１〜１１ 比較例１〜１１
下記のムライト粉末のいずれかと
下表のＡ：粒径０．５μｍ、ムライト質粉末Ｂ二平均粒
７．ｉ’Ｂ１．０μｍ以上の広い粒度分布を持つ電融ム
ライト粉末。(Actual Examples) Examples 1 to 11 Comparative Examples 1 to 11 Any of the following mullite powders and A: particle size 0.5 μm, mullite powder B bi-average particles 7. i'B Electrofused mullite powder with a wide particle size distribution of 1.0 μm or more.
酸化イツトリウム粉末（三菱化成工業（株）製；粒径１
μｌ）の粉末をエタノール中ボールミルを用いて２４時
時間式混合し、得られた混合粉末を２０００ｋｇ／ ｃ
ｘＡの圧力のもと成形し、得られた成形体を常圧におい
て焼結した。Yttrium oxide powder (manufactured by Mitsubishi Chemical Industries, Ltd.; particle size 1)
μl) of powder was mixed in ethanol for 24 hours using a ball mill, and the resulting mixed powder was mixed at 2000 kg/c.
It was molded under a pressure of xA, and the obtained molded body was sintered at normal pressure.
機械的強度は、ＪＩＳ Ｒ１６０１（１９８１）の規定
によって測定し、破壊靭性値はマイクロインデンテーシ
ョン法により測定した。Mechanical strength was measured according to the provisions of JIS R1601 (1981), and fracture toughness was measured by the microindentation method.
上記の条件以外の条件及び上記の測定結果を下表に示す
。Conditions other than the above conditions and the above measurement results are shown in the table below.
第１図は実施例５のムライト質焼結体の破膜面を示す走
査型電子顕微鏡写真であり、第２図は比較例１０のムラ
イト質焼結体の破膜面を示す走査型電子類ｍ鏡写真であ
る。FIG. 1 is a scanning electron microscope photograph showing the membrane rupture surface of the mullite sintered body of Example 5, and FIG. 2 is a scanning electron microscope photograph showing the membrane rupture surface of the mullite sintered body of Comparative Example 10. This is a mirror photo.
Claims (2)
なるムライト１００重量部 Ｙ＿２Ｏ＿３１〜１０重量部 であり、平均アスペクト比３以上の柱状晶からなり、か
つ密度が３．０ｇ／ｃｍ＾３以上であることを特徴とす
るムライト質焼結体。(1) The composition is 100 parts by weight of mullite consisting of 372 to 76 parts by weight of Al_2O_ and the balance is 31 to 10 parts by weight of Y_2O_2, the composition is composed of columnar crystals with an average aspect ratio of 3 or more, and the density is 3.0 g/cm^3 or more. A mullite sintered body characterized by:
なるムライト前駆体またはムライト粉末の平均粒子径が
１．０μｍ未満である出発原料に、上記ムライト前駆体
（ムライト換算）またはムライト粉末１００重量部あた
りＹ＿２Ｏ＿３を１〜１０重量部添加して、１６００〜
１８００℃で焼結することを特徴とするムライト質焼結
体の製造方法。(2) 100 parts by weight of the above mullite precursor (mullite equivalent) or mullite powder is added to the starting material having a composition of 372 to 76 parts by weight of Al_2O_ and the balance being SiO_2 and the average particle size of the mullite powder is less than 1.0 μm. Add 1 to 10 parts by weight of Y_2O_3 per 1600 to
A method for producing a mullite sintered body, characterized by sintering at 1800°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63321937A JPH02167857A (en) | 1988-12-22 | 1988-12-22 | High toughness mullite sintered body and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63321937A JPH02167857A (en) | 1988-12-22 | 1988-12-22 | High toughness mullite sintered body and its manufacturing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02167857A true JPH02167857A (en) | 1990-06-28 |
Family
ID=18138083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63321937A Pending JPH02167857A (en) | 1988-12-22 | 1988-12-22 | High toughness mullite sintered body and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02167857A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0850900A1 (en) * | 1996-12-23 | 1998-07-01 | SMH Management Services AG | Zirconia based article, its use as wear resistant part of a wristwatch and method for its production |
| CN1089325C (en) * | 1996-12-23 | 2002-08-21 | Smh管理服务有限公司 | Zirconia based ceramic article, use of such article as wear resistant exterior part for wristwatch and method for obtaining such article |
-
1988
- 1988-12-22 JP JP63321937A patent/JPH02167857A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0850900A1 (en) * | 1996-12-23 | 1998-07-01 | SMH Management Services AG | Zirconia based article, its use as wear resistant part of a wristwatch and method for its production |
| CN1089325C (en) * | 1996-12-23 | 2002-08-21 | Smh管理服务有限公司 | Zirconia based ceramic article, use of such article as wear resistant exterior part for wristwatch and method for obtaining such article |
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