JPS60215572A - Manufacture of magnesia partially stabilized zirconia - Google Patents
Manufacture of magnesia partially stabilized zirconiaInfo
- Publication number
- JPS60215572A JPS60215572A JP59072181A JP7218184A JPS60215572A JP S60215572 A JPS60215572 A JP S60215572A JP 59072181 A JP59072181 A JP 59072181A JP 7218184 A JP7218184 A JP 7218184A JP S60215572 A JPS60215572 A JP S60215572A
- Authority
- JP
- Japan
- Prior art keywords
- magnesia
- zirconia
- powder
- raw material
- partially stabilized
- 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
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】
本発明はマグネシア部分安定化ジルコニアの製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing magnesia partially stabilized zirconia.
従来、マグネシア部分安定化ジルコニアは高純度（Ｓ
ｉ ０２０．０３ｗｔ％以下）で、微細な（一般的には
平均粒径０．７ｇｍ以下の）原料粉を用い、これを焙焼
した後粉砕し、更に成形し、高温で焼成することにより
製造されている。Conventionally, magnesia partially stabilized zirconia has a high purity (S
i020.03wt% or less) and fine (generally average particle size of 0.7gm or less) raw material powder, which is roasted, then crushed, further shaped, and then baked at a high temperature. has been done.
しかし、高純度で微細な原料粉を用いるため、高価にな
り、原料粉、焙焼粉の粉砕に時間がかかる等工業的な制
約が多く、成形時の取扱いも困難である。また、十分な
強度を得るためには、焼結後急冷し、時効を必要とする
ため焼成操作が複雑になっている。However, since high-purity and fine raw material powder is used, it is expensive, has many industrial restrictions such as the time it takes to grind the raw material powder and roasted powder, and is difficult to handle during molding. Furthermore, in order to obtain sufficient strength, the sintering process is complicated because it requires rapid cooling and aging after sintering.
本発明は上記事情に鑑みてなされたものであり、高純度
で微細な原料粉を用いたり、時効処理を施したりしなく
ても、十分な強度を有するマグネシア部分安定化ジルコ
ニアを製造し得る方法を提供しようとするものである。The present invention has been made in view of the above circumstances, and provides a method for producing magnesia partially stabilized zirconia having sufficient strength without using high-purity, fine raw material powder or without aging treatment. This is what we are trying to provide.
すなわち、本発明のマグネシア部分安定化ジルコニアの
製造方法は、平均粒径０．８〜１０ｐｍのジルコニア原
料粉とマグネシア原料粉とをマグネシア含有率が８〜１
３ｍｏ１％となるように乾式又は湿式混合し焙焼した後
、平均粒径が０．８〜１゜＃Ｌｍとなるように粉砕し、
更に成形し、１４５０〜１７５０℃で焼成した後、炉冷
することを特徴とするものである。That is, in the method for producing magnesia partially stabilized zirconia of the present invention, a zirconia raw material powder with an average particle size of 0.8 to 10 pm and a magnesia raw material powder are mixed with a magnesia content of 8 to 1.
After dry or wet mixing and roasting to a concentration of 3 mo1%, pulverization to an average particle size of 0.8 to 1° #Lm,
It is characterized in that it is further molded, fired at 1450 to 1750°C, and then cooled in a furnace.
このような方法によれば、粗粒を用い、焼成後の時効処
理が不要となるにもかかわらず、従来と同程度の強度を
有するマグネシア部分安定化ジルコニアを製造すること
ができ、工業的な制約の減少、取扱いの容易さ、焼成操
作の簡便化などの効果を得ることができる。According to this method, it is possible to produce magnesia partially stabilized zirconia having the same strength as conventional methods, even though coarse particles are used and aging treatment after firing is not required. Effects such as reduced restrictions, ease of handling, and simplified firing operation can be obtained.
本発明において、原料粉の平均粒径を０．８〜ＬＯ１１
，ｍの範囲に限定したのは、上記範囲を逸脱すると、焼
結体の強度が低下するためである。In the present invention, the average particle size of the raw material powder is 0.8 to LO11.
, m because the strength of the sintered body decreases if it deviates from the above range.
また、本発明において、ジルコニア原料粉とマグネシア
原料粉とをマグネシア含有率が８〜１３ＩＩｌｏＩ％と
なるように混合するのは、上記範囲を逸脱すると、単斜
晶相の多い結晶組成となり、やはり焼結体の強度が減少
するためである。In addition, in the present invention, the zirconia raw material powder and the magnesia raw material powder are mixed so that the magnesia content is 8 to 13IIloI%. If the above range is exceeded, the crystal composition will be rich in monoclinic phase, which will also result in sintering. This is because the strength of the solid body decreases.
また、本発明において、成形体を１４５０〜１７５０
’Ｃの焼成温度で焼成するのは、焼成温度が上記範囲を
逸脱すると、やはり焼結体の強度が低下するためである
。In addition, in the present invention, the molded body has a temperature of 1450 to 1750
The reason for firing at a firing temperature of 'C' is that if the firing temperature deviates from the above range, the strength of the sintered body will decrease.
なお、本発明においてジルコこア原料粉としては高純度
ジルコニア粉又は低純度バデライト粉のいずれを用いて
もよい。In the present invention, the zirconia raw material powder may be either high-purity zirconia powder or low-purity baddellite powder.
また、マグネシア原料粉としては高純度マグネシア−ジ
ルコニア共沈粉又は低純度の塩基性炭酸マグネシウムも
しくは′＠酸マグネシウムのいずれを用いてもよい。Further, as the magnesia raw material powder, either high-purity magnesia-zirconia co-precipitated powder or low-purity basic magnesium carbonate or magnesium chloride may be used.
これらの原料粉のほかに第３成分として例えばアルミナ
を添加してもよい。In addition to these raw material powders, for example, alumina may be added as a third component.
これら原料粉の焙焼条件は７００〜１３００’０で０．
５〜５時間であることが望ましい。また、成形体の焼成
時間は１〜１０時間であることが望ましい。The roasting conditions for these raw material powders are 700 to 1300'0.
It is desirable that the time be 5 to 5 hours. Moreover, the baking time of the molded body is preferably 1 to 10 hours.
このような方法により製造されるマグネシア部分安定化
ジルコニアは、マグネシア含有率８〜１３％、平均結晶
粒径１０ｇｍ以上で結晶粒径の均一性がよい粗粒の組織
を有し、かつ結晶組成が単斜晶相２０〜４０重量％、正
方晶相１０〜３０重量％、立方晶相３０〜７０重量％と
なる。Magnesia partially stabilized zirconia produced by such a method has a magnesia content of 8 to 13%, an average crystal grain size of 10 gm or more, a coarse grain structure with good crystal grain size uniformity, and a crystal composition of The monoclinic phase is 20 to 40% by weight, the tetragonal phase is 10 to 30% by weight, and the cubic phase is 30 to 70% by weight.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず、原料粉として平均粒径０．５〜１２ＪＬｍのバデ
ライト粉とマグネシア−ジルコニア共沈粉をを用い、こ
れらを混合し焙焼した後、粉砕し、更に成形して１５０
０℃で２時間又は１７００℃で２時間焼成した後、炉冷
して試験片を得た。上記バデライト粉の平均粒径と試験
片の曲げ強さとの関係を第１図に示す。First, baddellite powder and magnesia-zirconia co-precipitated powder with an average particle size of 0.5 to 12 JLm were used as raw material powders, and after mixing and roasting them, they were crushed, further molded, and
After firing at 0°C for 2 hours or at 1700°C for 2 hours, the sample was cooled in a furnace to obtain a test piece. FIG. 1 shows the relationship between the average particle diameter of the baddellite powder and the bending strength of the test piece.
第１図から明らかなように、平均粒径が０．８ｐｍ未満
又は１０ｐＬｍを超えると、曲げ強さが著しく低下して
いる。平均粒径が０．８ｇｍ未満になると曲げ強さが低
下するのは、試験片中の結晶粒が混粒になるためである
と考えられる。As is clear from FIG. 1, when the average particle size is less than 0.8 pm or more than 10 pLm, the bending strength is significantly reduced. The reason why the bending strength decreases when the average grain size is less than 0.8 gm is considered to be because the crystal grains in the test piece become mixed grains.
次に、原料粉として平均粒径がそれぞれ１．０７１ｍ、
１．８ｇｍ及び８．２ｐＬｍのバデライト粉とマグネシ
ア−ジルコニア共沈粉とを用い、これらを混合した後、
粉砕し、更に成形してそれぞれ１４００ ’０１１５０
０°Ｃ及び１７００’Ｃで２時間焼成した後、炉冷して
試験片を得た。上記焼成温度と試験片の曲げ強さとの関
係を第２図に示す。Next, as raw material powder, the average particle size was 1.071 m,
After mixing 1.8 gm and 8.2 pLm baddellite powder and magnesia-zirconia co-precipitated powder,
Crushed and further molded to 1400 '01150 each
After firing at 0°C and 1700'C for 2 hours, the sample was cooled in a furnace to obtain a test piece. FIG. 2 shows the relationship between the above firing temperature and the bending strength of the test piece.
第２図から明らかなように、１４５０℃未満、すなわち
ｔ ４００ ’Ｃ！では曲げ強さが著しく低下している
。また、平均粒径８．２ｐ、ｒｎのものを除き、１７０
０ ’（！における焼成で最も曲げ強さが高くなってい
る。As is clear from Figure 2, it is less than 1450°C, that is, t 400'C! The bending strength is significantly reduced. In addition, except for those with an average particle size of 8.2p and rn, 170
The bending strength is highest when fired at 0'(!).
以上の試験のほかに第３成分の影響を調べるために以下
のような試験を行なった。In addition to the above tests, the following tests were conducted to investigate the influence of the third component.
すなわち、原料粉として高純度ジルコニア粉とマグネシ
ア−ジルコニア共沈粉とを用い、これらにアルミナを添
加して混合し焙焼した後、粉砕し、更に成形して１５０
０°Ｃで２時間焼成した。That is, high-purity zirconia powder and magnesia-zirconia co-precipitated powder are used as raw material powders, and alumina is added to these powders, mixed, roasted, crushed, and further molded to form a powder with a diameter of 150 mm.
It was baked at 0°C for 2 hours.
得られた焼結体は炉冷又はｔｏｏｏ℃もしくは８００℃
から空冷して試験片を得た。The obtained sintered body is cooled in a furnace or at too high or 800°C.
A test piece was obtained by air cooling.
上記アルミナ添加量と曲げ強さとの関係を第３図に示す
。FIG. 3 shows the relationship between the amount of alumina added and the bending strength.
第３図から明らかなように、アルミナ添加量が３ｍｏ１
％を超える場合には、原料粉の平均粒径が所定の範囲内
であっても焼結体の結晶粒が混粒となり易いため試験片
の強度が低下している。As is clear from Figure 3, the amount of alumina added is 3mol1.
%, even if the average particle size of the raw material powder is within a predetermined range, the crystal grains of the sintered body tend to become mixed grains, resulting in a decrease in the strength of the test piece.
なお、焼結体中の単斜晶相の量は１０００ ’Ｏあるい
は８００ ’Ｃがら空冷した場合でも炉冷した場合でも
大差がなかった。これは、おそらく原料粉が粗粒である
ため正方晶から単斜晶への熱変態を急冷によって回避す
ることが困難なためであると考えられる。逆に、あまり
急激に冷却すると、かえって熱歪による割れを生じるお
それがある。There was no significant difference in the amount of monoclinic phase in the sintered body whether the sintered body was air cooled at 1000'O or 800'C or cooled in a furnace. This is probably because the raw material powder is coarse grained, making it difficult to avoid thermal transformation from tetragonal to monoclinic by rapid cooling. On the other hand, if the material is cooled too quickly, cracks may occur due to thermal strain.
このようなことから、更に強度を向上させる手段として
は、第３成分の微細析出を利用し得る可能性がある。For this reason, there is a possibility that fine precipitation of the third component can be used as a means to further improve the strength.
ただし、アルミナはＭｇとＡｌを含む化合物となり、マ
トリックス中のＭｇ濃度を下げることから正方晶の安定
性を低下させ、単斜晶相の量を所定の範囲以上に増加さ
せるので、変態歪による割れを発生し易くする原因とな
る。したがって、焼結体の強度を向上させるための第３
成分としてアルミナを用いることは不適当であると考え
られる。なお、現在のところ適当な第３成分は見つかっ
ていない。However, alumina becomes a compound containing Mg and Al, which lowers the Mg concentration in the matrix, lowers the stability of the tetragonal crystal, and increases the amount of monoclinic phase beyond a specified range, causing cracks due to transformation strain. This can make it more likely to occur. Therefore, the third method for improving the strength of the sintered body is
It is considered inappropriate to use alumina as a component. Note that no suitable third component has been found at present.
以上詳述した如く本発明のマグネシア部分安定化ジルコ
ニアの製造方法によれば、高純度で微細な原料粉を用い
たり、時効処理を施したりしなくても、十分な強度を有
するマグネシア部分安定化ジルコニアを製造することが
でき、工業的な制約が少ないうえに成形時の取扱いが容
易であり、焼成操作も簡便になる等顕著な効果を奏する
ものである。As detailed above, according to the method for producing magnesia partially stabilized zirconia of the present invention, magnesia partially stabilized zirconia having sufficient strength can be produced without using high-purity, fine raw material powder or without aging treatment. It is possible to produce zirconia, has few industrial restrictions, is easy to handle during molding, and has remarkable effects such as simplifying the firing operation.
第１図は原料粉の一つであるバデライト粉の平均粒径と
試験片の曲げ強さとの関係を示す特性図、第２図は焼成
温度と試験片の曲げ強さとの関係を示す特性図、第３図
はアルミナの添加量と試験片の曲げ強さとの関係を示す
特性図である。
第２図
達べ１度じＣ）
第３図
アし５す碧鋤ｎ量（ｍｏ？、％）Figure 1 is a characteristic diagram showing the relationship between the average particle size of baddellite powder, which is one of the raw material powders, and the bending strength of the test piece. Figure 2 is a characteristic diagram showing the relationship between the firing temperature and the bending strength of the test piece. , FIG. 3 is a characteristic diagram showing the relationship between the amount of alumina added and the bending strength of the test piece. Fig. 2: 1 degree C) Fig. 3: A 5 S Hekisho n amount (mo?, %)
Claims (4)
粉とマグネシア原料粉とをマグネシア含有率が８〜１３
ｍｏ１％となるように乾式又は湿式混合し焙焼した後、
平均粒径が０．８〜１０ＩＬｍとなるように粉砕し、更
に成形し、１４５０〜１７５０°Ｃで焼成した後、炉冷
することを特徴とするマグネシア部分安定化ジルコニア
の製造方法。(1) Zirconia raw material powder with an average particle size of 0.8 to 1107 t and magnesia raw material powder with a magnesia content of 8 to 13
After dry or wet mixing and roasting to a mo of 1%,
A method for producing magnesia partially stabilized zirconia, which comprises pulverizing the powder to have an average particle size of 0.8 to 10 ILm, further molding, firing at 1450 to 1750°C, and then cooling in a furnace.
は低純度バデライト粉を用いる特許請求の範囲第１項記
載のマグネシア部分安定化ジルコニアの製造方法。(2) The method for producing partially stabilized magnesia zirconia according to claim 1, in which high-purity zirconia powder or low-purity baddellite powder is used as the zirconia raw material powder.
ルコニア共沈粉又は低純度の塩基性炭酸マグネシウムも
しくは硫酸マグネシウムを用いる特許請求の範囲第１項
記載のマグネシア部分安定化ジルコニアの製造方法。(3) The method for producing magnesia partially stabilized zirconia according to claim 1, in which high purity magnesia-zirconia co-precipitated powder or low purity basic magnesium carbonate or magnesium sulfate is used as the magnesia raw material powder.
する特許請求の範囲第１項記載のマグネシア部分安定化
ジルコニアの製造方法。(4) The method for producing magnesia partially stabilized zirconia according to claim 1, wherein 3 mo1% or less of alumina is added as a third component.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59072181A JPS60215572A (en) | 1984-04-11 | 1984-04-11 | Manufacture of magnesia partially stabilized zirconia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59072181A JPS60215572A (en) | 1984-04-11 | 1984-04-11 | Manufacture of magnesia partially stabilized zirconia |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS60215572A true JPS60215572A (en) | 1985-10-28 |
Family
ID=13481792
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59072181A Pending JPS60215572A (en) | 1984-04-11 | 1984-04-11 | Manufacture of magnesia partially stabilized zirconia |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60215572A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01201065A (en) * | 1987-09-29 | 1989-08-14 | Ube Ind Ltd | High-strength magnesia sintered material and production thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4918906A (en) * | 1972-04-11 | 1974-02-19 | ||
| JPS5827230A (en) * | 1981-08-11 | 1983-02-17 | Nippon Telegr & Teleph Corp <Ntt> | Partial erasing method for picture |
-
1984
- 1984-04-11 JP JP59072181A patent/JPS60215572A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4918906A (en) * | 1972-04-11 | 1974-02-19 | ||
| JPS5827230A (en) * | 1981-08-11 | 1983-02-17 | Nippon Telegr & Teleph Corp <Ntt> | Partial erasing method for picture |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01201065A (en) * | 1987-09-29 | 1989-08-14 | Ube Ind Ltd | High-strength magnesia sintered material and production thereof |
| JPH0672042B2 (en) * | 1987-09-29 | 1994-09-14 | 宇部興産株式会社 | High strength magnesia sintered body and its manufacturing method |
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