JPH037626B2 - - Google Patents
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- Publication number
- JPH037626B2 JPH037626B2 JP60166784A JP16678485A JPH037626B2 JP H037626 B2 JPH037626 B2 JP H037626B2 JP 60166784 A JP60166784 A JP 60166784A JP 16678485 A JP16678485 A JP 16678485A JP H037626 B2 JPH037626 B2 JP H037626B2
- Authority
- JP
- Japan
- Prior art keywords
- particles
- metal
- ultrafine
- sintered body
- mixture
- 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.)
- Expired - Lifetime
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- Inorganic Insulating Materials (AREA)
- Powder Metallurgy (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はセラツク粉末等の焼結体の製造法に関
する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing a sintered body such as shellac powder.
（従来の技術）
従来、粒径1μ以上のセラミツク、金属などの
微粒子、粗粒子の集団の焼結体の製造法は、その
粒子の表面を加熱熔融していわゆる粒子相互を焼
結する方法がとられている。(Prior art) Conventionally, the method for producing a sintered body of a group of fine particles or coarse particles of ceramics, metals, etc. with a particle size of 1μ or more involves heating and melting the surfaces of the particles and sintering the particles together. It is taken.
（発明が解決しようとする問題点）
従来の上記焼結法では、例えば、酸化物セラミ
ツクス粉の場合、焼結温度が高くなるほどその粒
子の結晶の成長が進み、焼結体製品の材料として
の性質、特に機械的性質が悪くなる。これに結晶
成長抑制御剤を適量添加して焼結することを行な
うこともあるが、それだけ不純物を含む焼結体と
なり好ましくない。又酸化チタンなどの高誘電性
セラミツクス製品の場合、その融点が1400℃以上
と極めて高く、このままでは熔化が困難なので、
融剤を適量添加して焼結を行なつているが、それ
だけ誘電率の低下した製品となり好ましくない。(Problems to be Solved by the Invention) In the conventional sintering method described above, for example, in the case of oxide ceramic powder, the higher the sintering temperature, the more the crystals of the particles grow, making it difficult to use as a material for sintered products. Properties, especially mechanical properties, deteriorate. Although sintering may be carried out by adding an appropriate amount of a crystal growth inhibitor to the material, this is not preferable as it results in a sintered body containing impurities. In addition, in the case of highly dielectric ceramic products such as titanium oxide, their melting point is extremely high, over 1400℃, and it is difficult to melt them as they are.
Although sintering is carried out by adding an appropriate amount of flux, the resulting product has a correspondingly lower dielectric constant, which is not preferable.
従つて、セラミツク焼結体として、上記の添加
剤を混入しないことが望ましく、而も高融点のセ
ラミツク粒子の焼結体を製造するにはその融点以
上に加熱しないで、比較的低温の加熱でその焼結
体が得られることが好ましい。 Therefore, it is desirable not to mix the above-mentioned additives into the ceramic sintered body, and in order to produce a sintered body of ceramic particles with a high melting point, it is necessary to heat the ceramic particles at a relatively low temperature without heating it above the melting point. It is preferable that the sintered body is obtained.
（問題点を解決するための手段）
本発明は、上記従来の欠点を解消し、0.1μ以上
の粒子、例えばセラミツク粒子自体を熔化せしめ
ることのない低い温度で相互を固着でき、融剤の
使用を省略でき良質の焼結体の製造法を提供する
もので、粒径0.1μ以上の所望量の集団に金属超微
粒子の所望量を均一に混入して粒子間に金属超微
粒子を介在させて成る混合物を作成し、これを真
空下で低温に加熱する１方、真空容器内に導入し
た酸素を該加温状態の混合物に接触させることを
特徴とする。(Means for Solving the Problems) The present invention solves the above-mentioned conventional drawbacks, allows particles of 0.1μ or more, such as ceramic particles, to be fixed to each other at a low temperature without melting them, and uses a flux. This method provides a method for manufacturing a high-quality sintered body that can omit the step 1, and involves uniformly mixing a desired amount of ultrafine metal particles into a group of a desired amount of particles with a particle size of 0.1μ or more, and interposing the ultrafine metal particles between the particles. The method is characterized in that a mixture is prepared and heated to a low temperature under vacuum, while oxygen introduced into a vacuum container is brought into contact with the heated mixture.
（作 用）
本発明の上記方法によれば、導入された酸素
は、加温された混合物に混在の金属超微粒子を酸
化燃焼させ、その酸化燃焼熱で金属超微粒子は熔
融しこの熔融固化を介して0.1μ以上のセラミツク
粉などの酸化物等の粒子相互が結着する結果、１
つの固塊焼結体を得られる。この間金属超微粒子
は、粒子相互を結着した超金属酸化物粒子として
混在したものとなつている。(Function) According to the above-mentioned method of the present invention, the introduced oxygen oxidizes and burns the ultrafine metal particles mixed in the heated mixture, and the ultrafine metal particles are melted by the heat of oxidation and combustion, and the metal ultrafine particles are melted and solidified. As a result of particles of oxides such as ceramic powder having a size of 0.1μ or more bonding together through the
One solid sintered body can be obtained. During this time, the ultrafine metal particles are mixed together as supermetal oxide particles that are bonded to each other.
（実施例） 次に本発明の実施例につき説明する。(Example) Next, examples of the present invention will be described.
真空容器内で、アルミナ、マグネシアなどの粒
径0.1μ以上の微粒又は粗粒から成るセラミツクな
どの金属酸化物粒子の所望量の集団に、徐酸化し
ない又はした任意の金属超微粒子の所望量を混合
する。好ましくは、該金属超微粒子は、金属酸化
物粒子の金属成分と同じ金属のものを混合する。
例えば金属酸化物粒子がアルミナならば金属超微
粒子としては、アルミニウムを、又前者がマグネ
シアならば後者はマグネシウムを混ぜることが好
ましい。 In a vacuum container, a desired amount of any metal ultrafine particles that are not slowly oxidized or that are slowly oxidized are added to a desired amount of metal oxide particles such as ceramics consisting of fine or coarse particles of alumina, magnesia, etc. with a particle size of 0.1 μ or more. Mix. Preferably, the ultrafine metal particles are made of the same metal as the metal component of the metal oxide particles.
For example, if the metal oxide particles are alumina, it is preferable to mix aluminum as the ultrafine metal particles, and if the former is magnesia, it is preferable to mix magnesium with the latter.
金属酸化物粒子集団に対する金属微粒子の添加
量は、30〜60重量％の範囲が一般である。 The amount of metal fine particles added to the metal oxide particle population is generally in the range of 30 to 60% by weight.
尚、金属酸化物としてセラミツクス原料を使用
する場合は、金属超微粒子との配合前に、例え
ば、800〜1100℃に加熱し、酸素雰囲気中で１時
間程度焼成し、或は真空排気を行ない乍ら、10-2
トールの酸素を導入し800℃以下の加熱により、
酸素質不純物の除去を行なう前処理を行なつても
よい。 When using a ceramic raw material as a metal oxide, it should be heated to, for example, 800 to 1100°C and fired in an oxygen atmosphere for about 1 hour, or evacuated before being mixed with ultrafine metal particles. et al., 10 -2
By introducing Thor's oxygen and heating below 800℃,
Pretreatment to remove oxygen impurities may be performed.
上記の混合物の所定の型内に充填した後直ちに
或は上面から軽くプレスしたり、超音波などで振
動を与え比較的緻密に詰めた状態とした後、この
成形型を加熱し、その混合物の温度を200〜500℃
程度に加熱保持する。１方、真空容器内酸素を導
入する（圧力で200トール位）。然るときは、その
加熱により混合物中の空気を追い出して酸素の混
合物中への侵入が良好となる。又該混合物をその
低温加熱に保持した状態では、金属超微粒子に接
触しその酸化が行なわれ極めて短時間に高温状態
となると共にその自己発熱により超微粒子は溶融
しこの溶融を介し金属酸化物粒子相互に結着され
る。この場合、上記の加温保持により、混合物の
中心部における金属超微粒子も表層部の金属超微
粒子と同様の良好な酸化燃焼をもたらし全体とし
て均一焼結をもたらす。かくしてその酸化燃焼後
の冷却により金属超微粒子は金属酸化物超微粒子
となり、焼結粒子がこれと同じ金属酸化物であれ
ば、全体として例えばアルミナの焼結体が得られ
る。このように、本発明によれば、0.1μ以上のセ
ラミツク粒子が、高融点金属酸化物であつても、
従来のようにその融点以上に即ち約200以上の加
温に加熱する必要がない。従つて又結晶成長も実
質上生ぜしめることなく、機械的特性の良好な焼
結体が得られ、従つて又結晶成長抑制剤や融剤な
どの不純物を添加してその融点を1300〜1400℃程
度に下げる必要がなく、経済的に且つ容易に純粋
な金属酸化物焼結体が得られる。このように、本
発明によれば、金属超微粒子が真空容器内の酸素
により容易に燃焼しその自己の燃焼熱により熔融
して、金属酸化物粒子相互のバインダーとして作
用せしめることにより、比較的低温の最高でも
1000℃付近に昇温する程度で、焼結体を得るよう
にした点に特徴がある。 Immediately after filling the above mixture into a predetermined mold, or by lightly pressing it from the top or applying vibrations using ultrasonic waves to make it relatively densely packed, the mold is heated, and the mixture is Temperature 200~500℃
Heat and maintain at a moderate temperature. On the other hand, introduce oxygen into the vacuum container (at a pressure of about 200 torr). In such a case, the heating will drive out the air in the mixture, allowing oxygen to enter the mixture better. In addition, when the mixture is kept heated at a low temperature, it comes into contact with ultrafine metal particles, oxidizes them, reaches a high temperature in a very short time, and the ultrafine particles melt due to self-heating, and through this melting, metal oxide particles are formed. mutually bound. In this case, by maintaining the temperature as described above, the ultrafine metal particles in the center of the mixture undergo good oxidation combustion similar to the ultrafine metal particles in the surface layer, resulting in uniform sintering as a whole. Thus, by cooling after the oxidative combustion, the metal ultrafine particles become metal oxide ultrafine particles, and if the sintered particles are the same metal oxide, a sintered body of, for example, alumina can be obtained as a whole. Thus, according to the present invention, even if the ceramic particles of 0.1μ or more are high melting point metal oxides,
There is no need to heat it above its melting point, that is, above about 200° C., as in the past. Therefore, a sintered body with good mechanical properties can be obtained without substantially causing crystal growth, and by adding impurities such as crystal growth inhibitors and fluxes, the melting point can be lowered to 1300 to 1400°C. A pure metal oxide sintered body can be obtained economically and easily without the need to lower the quality. As described above, according to the present invention, the ultrafine metal particles are easily combusted by the oxygen in the vacuum container and melted by their own heat of combustion, allowing the metal oxide particles to act as a binder for each other, thereby allowing the metal oxide particles to be heated at a relatively low temperature. Even the best of
The unique feature is that a sintered body can be obtained by raising the temperature to around 1000℃.
金属超微粒子の種類は、アルミナなど通常セラ
ミツク原料であるものの金属成分であるものは全
て好ましく使用できる。又、粒径0.1μ以上の粒子
は、金属酸化物の他、焼結体の使用目的によつて
は、無機質粒子、金属炭化物、金属窒化物などの
粒子の集団固塊の製造にも適用できる。又、粒径
0.1μ以上の粒子では、最大粒径約20μまでが適当
である。 As for the type of ultrafine metal particles, any metal component such as alumina, which is usually a raw material for ceramics, can be preferably used. In addition, particles with a particle size of 0.1μ or more can be used to produce agglomerates of particles such as metal oxides, inorganic particles, metal carbides, and metal nitrides, depending on the purpose of the sintered body. . Also, particle size
For particles larger than 0.1μ, a maximum particle size of up to about 20μ is suitable.
尚、焼結終了後は、必要に応じその焼結体を加
圧して更に緻密な組織の焼結体とすることもでき
る。 Note that after the sintering is completed, the sintered body can be pressurized as necessary to form a sintered body with a more dense structure.
金属超微粒子は、金属超微粒子生成装置の真空
容器で金属を蒸発させて得たものを外部に取り出
すことなくこれに連接した本発明の真空処理装置
の前記真空容器内に導入したものをそのまま利用
するようにしてもよいが、徐酸化後外部にとり出
して予め作成しておいたものを使用することもで
きる。 The metal ultrafine particles are obtained by evaporating metal in the vacuum container of the metal ultrafine particle generation device, and are directly used as they are introduced into the vacuum container of the vacuum processing device of the present invention, which is connected to this without taking it out to the outside. However, it is also possible to take out the material after gradual oxidation and use one prepared in advance.
本発明により作成した焼結体は、電子材料、機
械的構造材、がい子など、従来の各種のセラミツ
ク製品の応用分野に使用されることが一般である
が、焼結体の超微粒子や粒子の種類などによりそ
の他の化学工業、建築材料などにも利用できる。 The sintered body produced according to the present invention is generally used in the application fields of various conventional ceramic products such as electronic materials, mechanical structural materials, and insulators. Depending on the type, it can also be used in other chemical industries, building materials, etc.
次に更に具体的な実施例につき説明する。 Next, more specific examples will be described.
実施例
粒径1μの酸化ニツケルの粒子５ｇに、予め表
面を徐酸化したニツケル超微粒子５ｇを真空装置
内に入れ良く混合したものを型に入れ、10-4トー
ルの真空下で300℃に加熱し混合物中の空気を排
除する。Example: 5 g of nickel oxide particles with a particle size of 1μ and 5 g of nickel ultrafine particles whose surface has been slowly oxidized in advance are placed in a vacuum device, mixed well, and the mixture is placed in a mold and heated to 300°C under a vacuum of 10 -4 Torr. and eliminate air from the mixture.
その後真空容器内に酸素を導入し、40〜50トー
ルの酸素を混合物と接触させた。 Oxygen was then introduced into the vacuum vessel and 40-50 Torr of oxygen was brought into contact with the mixture.
混合物の平均温度が1250℃にまで上昇するの
が、光学的測定により観測された、引きつづき上
記より低い酸素導入圧10トールで混合物を反応さ
せ、酸化燃焼終了後、常温まで冷却し外部に取り
出した。かくして所定形状の酸化ニツケル粒子集
団が酸化ニツケル超微粒子を介して結着した酸化
ニツケル焼結成形品が得られた。 It was observed by optical measurement that the average temperature of the mixture rose to 1250℃.The mixture was then reacted at a lower oxygen introduction pressure of 10 Torr than the above, and after the oxidation combustion was completed, it was cooled to room temperature and taken out outside. Ta. In this way, a sintered nickel oxide molded article in which a group of nickel oxide particles having a predetermined shape was bound together via ultrafine nickel oxide particles was obtained.
（発明の効果）
このように本発明によるときは、金属超微粒子
の所望量を粒径0.1μ以上の粒子の集団に混合する
と共に真空下で低温加熱後、これに導入酸素で酸
化燃焼するようにしたので、高融点の粒子でもこ
れを加熱熔融することなく、又融剤の添加を必要
とせず良質の焼結体を製造し得る効果を有する。(Effects of the Invention) According to the present invention, a desired amount of ultrafine metal particles is mixed into a group of particles with a particle size of 0.1μ or more, heated at a low temperature under vacuum, and then oxidized and burned with oxygen introduced therein. Therefore, it is possible to produce a high-quality sintered body without heating and melting even particles with a high melting point, and without adding a flux.
Claims (1)
の所望量を均一に混入して粒子間に金属超微粒子
を介在させて成る混合物を作成し、これを真空下
で低温に加熱する１方、真空容器内に導入した酸
素を該加温状態の混合物に接触させることを特徴
とする焼結体の製造法。1. A desired amount of ultrafine metal particles is uniformly mixed into a desired amount of a population with a particle size of 0.1μ or more to create a mixture with ultrafine metal particles interposed between the particles, and this is heated to a low temperature under vacuum.1 On the other hand, a method for producing a sintered body, which comprises bringing oxygen introduced into a vacuum container into contact with the heated mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60166784A JPS6230669A (en) | 1985-07-30 | 1985-07-30 | Manufacture of sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60166784A JPS6230669A (en) | 1985-07-30 | 1985-07-30 | Manufacture of sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6230669A JPS6230669A (en) | 1987-02-09 |
| JPH037626B2 true JPH037626B2 (en) | 1991-02-04 |
Family
ID=15837610
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60166784A Granted JPS6230669A (en) | 1985-07-30 | 1985-07-30 | Manufacture of sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6230669A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7465297B2 (en) * | 2022-03-17 | 2024-04-10 | 日東電工株式会社 | Sputtering Equipment |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6054272B2 (en) * | 1979-02-15 | 1985-11-29 | 黒崎窯業株式会社 | Refractory manufacturing method |
-
1985
- 1985-07-30 JP JP60166784A patent/JPS6230669A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6230669A (en) | 1987-02-09 |
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