JPH06246152A - Metal compound powder producing device - Google Patents
Metal compound powder producing deviceInfo
- Publication number
- JPH06246152A JPH06246152A JP5059310A JP5931093A JPH06246152A JP H06246152 A JPH06246152 A JP H06246152A JP 5059310 A JP5059310 A JP 5059310A JP 5931093 A JP5931093 A JP 5931093A JP H06246152 A JPH06246152 A JP H06246152A
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- JP
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- Prior art keywords
- reaction
- powder
- metal compound
- gas
- metal
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、金属化合物の製造装置
に関し、より詳細にはファインセラミックス原料粉体や
磁性トナー用原料粉体、磁気記録材料用原料粉体に好適
な金属化合物粉体の製造に適した装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for producing a metal compound, and more specifically to a metal compound powder suitable for fine ceramic raw material powder, magnetic toner raw material powder, and magnetic recording material raw material powder. A device suitable for manufacturing.
【０００２】[0002]
【従来の技術】従来より、ファインセラミックスや磁性
トナー、磁気記録材料等の原料として、金属酸化物や金
属塩化物、金属窒化物等の金属化合物の粉体が、広く用
いられている。これらの金属化合物粉体を製造する装置
として、種々の構造を有する製造装置が提案、作成され
ている。2. Description of the Related Art Powders of metal compounds such as metal oxides, metal chlorides and metal nitrides have been widely used as raw materials for fine ceramics, magnetic toners, magnetic recording materials and the like. As an apparatus for manufacturing these metal compound powders, manufacturing apparatuses having various structures have been proposed and created.
【０００３】この種の製造装置の代表的なものは、ロー
タリキルン形の焼成装置である。これは、回転自在で、
一端に反応性ガスの供給口、他端に排気口を備える円筒
状の反応容器と、反応容器を取り囲むように配設された
加熱手段から構成され、金属粉体が装填された反応容器
を加熱手段により高温に保持し、反応容器を回転させな
がら酸化性ガスや窒化性ガス等の反応性ガスを導入する
ことにより、反応容器内部の金属粉体を、金属酸化物や
金属窒化物の粉体に変化させるものである。A typical example of this type of manufacturing apparatus is a rotary kiln type baking apparatus. This is rotatable,
Heating a reaction container loaded with metal powder, which is composed of a cylindrical reaction container having a reactive gas supply port at one end and an exhaust port at the other end, and heating means arranged so as to surround the reaction container. By maintaining the temperature at a high temperature by means and introducing a reactive gas such as an oxidizing gas or a nitriding gas while rotating the reaction container, the metal powder inside the reaction container is converted into a metal oxide or metal nitride powder. To change to.
【０００４】また、上記焼成装置と同様の装置を用い
て、金属粉体の代わりに金属蒸気を、反応性ガスととも
に反応容器内に導入して金属化合物の微粉末を製造する
こともできる。この場合、金属蒸気を取り扱うために、
金属蒸気発生手段及び金属蒸気を反応容器内に導入する
ための供給手段を付加する必要がある。この装置は、主
に還元法により金属窒化物の粉体を製造する場合に用い
られ、反応容器内を還元性のガス雰囲気とし、金属蒸気
や金属塩化物の蒸気とアンモニアとを反応容器に導入し
て反応させて金属窒化物の粉体を生成する場合に好適に
使用される。It is also possible to produce a fine powder of a metal compound by introducing a metal vapor instead of the metal powder into the reaction vessel together with the reactive gas using an apparatus similar to the above-mentioned firing apparatus. In this case, to handle the metal vapor,
It is necessary to add a metal vapor generation means and a supply means for introducing the metal vapor into the reaction vessel. This device is mainly used when producing powder of metal nitride by a reduction method, creates a reducing gas atmosphere in the reaction container, and introduces metal vapor or metal chloride vapor and ammonia into the reaction container. It is preferably used in the case of reacting with each other to produce a metal nitride powder.
【０００５】この他にも、例えば特開平２−１６４４４
３号公報や、基礎粉体工学講座３０、シリーズII（粉体
を扱う各種操作）第２１章粉体の反応装置(1)、粉体工
学会誌、Ｖｏｌ．１、Ｎｏ．１２（１９９１）、ｐ．７
７１−７８０に記載されているような、反応性ガスの供
給口及び排気口を備えるチャンバ（反応容器）に、高周
波の対向電極や誘導コイル、マイクロウェーブ空洞共振
器等のグロー放電プラズマ発生手段を配設した構造の製
造装置がある。このような製造装置を用いて、反応性ガ
ス雰囲気としたチャンバ内部にグロー放電プラズマを発
生させて、発生したグロー放電プラズマ中に金属粉末を
導入することにより金属化合物粉体を得ることができ
る。また、同様の装置を用いて、アーク放電発生手段に
よりチャンバ内部にアーク放電プラズマを発生させて、
このアーク放電プラズマによりチャンバ内部にチャージ
した金属を蒸発させて金属蒸気とし、これに反応性ガス
を供給することにより金属化合物粉体を得ることもでき
る。このようなプラズマ発生手段を備える装置を用いる
ことにより、粒径０．０１μｍ程度の金属化合物の超微
粒子を製造することができる。In addition to this, for example, Japanese Patent Application Laid-Open No. 2-16444
No. 3, gazette for basic powder engineering 30, series II (various operations for handling powder), Chapter 21, Reactor for powder (1), Journal of Powder Engineering, Vol. 1, No. 12 (1991), p. 7
71-780, a chamber (reaction vessel) having a reactive gas supply port and an exhaust port is provided with a glow discharge plasma generating means such as a high-frequency counter electrode, an induction coil, and a microwave cavity resonator. There is a manufacturing apparatus having a structure provided. By using such a manufacturing apparatus, glow discharge plasma is generated inside the chamber in a reactive gas atmosphere, and the metal powder is introduced into the generated glow discharge plasma, whereby a metal compound powder can be obtained. Further, using the same device, by generating arc discharge plasma in the chamber by the arc discharge generating means,
It is also possible to obtain the metal compound powder by evaporating the metal charged inside the chamber by the arc discharge plasma to form a metal vapor and supplying the reactive gas to the vapor. Ultrafine particles of a metal compound having a particle size of about 0.01 μm can be produced by using an apparatus equipped with such a plasma generating means.
【０００６】[0006]
【発明が解決しようとする課題】これらの装置により生
成される金属化合物の粉体は、最終製品の性能の点で
は、一般的にその粒径が小さい程好ましいとされている
が、逆に粒径が小さくなりすぎるとその加工性に問題が
生じてくる。例えば、磁性トナーでは磁性体粒子を樹脂
などで被覆あるいは樹脂と混練する必要があるが、この
とき粒子が小さすぎると磁性体粒子の充填率が下がり磁
化が小さくなったり、凝集により製品にバラツキが発生
する。It is generally said that the smaller the particle size of the metal compound powder produced by these devices is, the more preferable it is in terms of the performance of the final product. If the diameter becomes too small, there will be a problem in workability. For example, in a magnetic toner, it is necessary to coat or knead the magnetic particles with a resin or the like, but if the particles are too small at this time, the packing rate of the magnetic particles decreases and the magnetization becomes small, or the product is dispersed due to aggregation. Occur.
【０００７】このように、金属化合物粉体は、その用途
に応じた好ましい粒径範囲があり、ファインセラミック
ス原料としては、平均粒径が０．２〜１０μｍ程度、磁
性トナー用磁性粉体としては数μｍ以下、また磁気記録
材料としては０．５〜数μｍ程度であることが望まし
く、概ね平均粒径が１μｍ程度であれば、これらの用途
に共通して、しかも好適な材料として使用することがで
きることが知られている。As described above, the metal compound powder has a preferable particle size range according to its use. As a fine ceramic raw material, the average particle size is about 0.2 to 10 μm, and as a magnetic powder for a magnetic toner. It is desirable that the magnetic recording material has a diameter of several μm or less, and 0.5 to several μm, and if the average particle diameter is approximately 1 μm, it should be used as a suitable material common to these applications. It is known that
【０００８】しかし、前記の製造装置では、粒径１μｍ
程度の金属化合物の微粉末を、効率良く、しかも安価に
得ることは困難であり、例えば、プラズマ発生手段を備
える装置を用いた場合には、粒径が０．０１μｍという
超微粉末を得ることができるものの、逆に１μｍ程度の
粒径のものを多量に得ることが難しく、また、金属や金
属塩化物の蒸気の還元に適した製造装置では、生成金属
化合物が数珠状の凝集体となり、単粒子が得られないと
いう問題を抱えている。However, in the above manufacturing apparatus, the particle size is 1 μm.
It is difficult to efficiently obtain a fine powder of a metal compound at a low cost. For example, when an apparatus equipped with a plasma generating means is used, an ultrafine powder having a particle diameter of 0.01 μm is obtained. However, on the contrary, it is difficult to obtain a large amount of particles having a particle size of about 1 μm, and in a production apparatus suitable for reducing vapor of metal or metal chloride, the produced metal compound becomes a beaded aggregate, There is a problem that single particles cannot be obtained.
【０００９】これら生成金属化合物の生産性や形状の問
題に加えて、プラズマを発生させたり、原料を一度蒸発
させたりする必要があるため、製造装置自体が高価にな
るとともに、反応条件の制御等の製造プロセスも複雑に
なり、結果的に製造コストが上昇し、製品として高価な
ものになっている。一方、ロータリキルン等の焼成装置
は、装置自体が安価であるとともに、これを使用して金
属化合物粉体を製造する際のプロセスや制御が簡易であ
るために、金属化合物粉体を、安価に、しかも多量に製
造することができるという利点を有するものの、処理で
きる金属粉体の粒径に制限があり、通常粒径が数μｍ〜
数十μｍ程度の粗粒粉末は処理することができるが、粒
径１μｍ程度の粉体を処理しようとすると、粉体は、そ
の表面エネルギーが大きいために、反応中に反応容器の
内壁面に付着したり、粒子同士が焼結を起こして大きな
粒塊となるという欠点も兼ね備えている。この焼結体と
なった粒塊は、硬度が高いために、１μｍ程度の粒径ま
で粉砕するには非常に長い時間を要するという、後処理
工程に大きな問題を残している。In addition to the problems of productivity and shape of these produced metal compounds, it is necessary to generate plasma and vaporize the raw materials once, so that the manufacturing apparatus itself becomes expensive and the reaction conditions are controlled. Manufacturing process is complicated, resulting in an increase in manufacturing cost and an expensive product. On the other hand, the firing device such as a rotary kiln is inexpensive in itself, and since the process and control for producing the metal compound powder using the device are simple, the metal compound powder can be manufactured at low cost. Moreover, although it has an advantage that it can be produced in a large amount, the particle size of the metal powder that can be treated is limited, and the particle size is usually from several μm to
Coarse-grained powder with a size of several tens of μm can be processed, but when a powder with a particle size of about 1 μm is to be processed, the powder has a large surface energy, so that the inner wall surface of the reaction vessel during the reaction is treated. It also has the drawback of sticking to each other and sintering of the particles into a large agglomerate. Since the agglomerates formed into this sintered body have high hardness, it takes a very long time to pulverize to a particle size of about 1 μm, which leaves a big problem in the post-treatment process.
【００１０】このように、従来の製造装置では、ファイ
ンセラミックスや磁性トナー、磁気記録材料等の原料と
して好適な粒径１μｍ程度の金属化合物の微粉末を、安
価に、しかも効率良く得ることは困難であった。従っ
て、本発明の目的は、粒径１μｍ程度の微細な金属化合
物粉体を、多量にかつ、反応後の粉砕等の後処理を必要
せずに効率良く、しかも安価に生成することが可能な製
造装置を提供することにある。As described above, in the conventional manufacturing apparatus, it is difficult to inexpensively and efficiently obtain fine powder of a metal compound having a particle diameter of about 1 μm, which is suitable as a raw material for fine ceramics, magnetic toners, magnetic recording materials and the like. Met. Therefore, the object of the present invention is to produce a fine metal compound powder having a particle size of about 1 μm efficiently and inexpensively without requiring post-treatment such as crushing after reaction. To provide a manufacturing apparatus.
【００１１】[0011]
【課題を解決するための手段】本発明者らは、金属化合
物粉体の製造装置に関する上記課題を解決すべく改良を
重ねた結果、安価な製造装置である焼成装置に改良を加
え、反応性ガスとの反応中に生ずる金属化合物の焼結を
強制的に解くことにより、所望の粒径１μｍ程度の微細
な金属化合物の粉体を多量にかつ効率良く、しかも安価
に得ることができることを見出し、本発明を完成するに
至った。As a result of repeated improvements to solve the above-mentioned problems relating to the apparatus for producing metal compound powder, the present inventors have improved the firing apparatus, which is an inexpensive production apparatus, to improve the reactivity. It was found that by forcibly releasing the sintering of the metal compound generated during the reaction with the gas, a large amount of powder of the fine metal compound having a desired particle size of about 1 μm can be obtained efficiently and at low cost. The present invention has been completed.
【００１２】即ち、前記課題は、ガスの供給口及び排出
口を備え、回転手段により回転される反応容器と、該反
応容器を取り囲むように配設される加熱手段とから構成
される金属化合物製造装置において、反応容器内部には
原料粉体とともに粉砕媒体が導入されることを特徴とす
る金属化合物製造装置により解決することができる。ま
た、同様の課題は、上記反応容器を、ガスの供給口及び
排出口を備え、回転手段により回転される反応外管と、
ガスの供給部及び排出部を備え、原料粉体及び粉砕媒体
が導入される反応室とから構成するともに、この反応室
を、反応外管内部に内挿して、反応外管の回転に伴い回
転させることを特徴とする金属化合物製造装置によって
も解決することができる。[0012] That is, the above-mentioned object is to produce a metal compound, which comprises a reaction vessel having a gas supply port and a gas exhaust port and rotated by a rotating means, and a heating means arranged so as to surround the reaction vessel. In the apparatus, the pulverization medium is introduced into the reaction container together with the raw material powder, which can be solved by the apparatus for producing a metal compound. Further, a similar problem is that the reaction container is provided with a gas supply port and a gas discharge port, and a reaction outer tube rotated by a rotating means,
It is equipped with a gas supply part and a discharge part, and a reaction chamber into which the raw material powder and the grinding medium are introduced, and this reaction chamber is inserted inside the reaction outer tube and rotated with the rotation of the reaction outer tube. The problem can also be solved by a metal compound manufacturing apparatus characterized by the above.
【００１３】これにより、粒径１μｍ程度の微細な金属
化合物粉体を、多量にかつ、反応後の粉砕等の後処理を
必要せずに効率良く、しかも安価に生成することが可能
な製造装置を提供することができる。As a result, a production apparatus capable of producing a large amount of fine metal compound powder having a particle size of about 1 μm efficiently and inexpensively without the need for post-treatment such as crushing after the reaction. Can be provided.
【００１４】[0014]
【実施例】本発明に係る金属化合物粉体の製造装置に関
して、添付図面を参照して詳細に説明する。ただし、本
発明は以下に記載される実施例に限定されずに、種々の
変更が可能である。金属化合物粉体の製造装置１は、図
１に示されるように、鉄、チタン等の金属あるいはステ
ンレススチール、インコネル等の合金からなり、水平に
配置される円筒状の反応容器２と、反応容器２を取り囲
むように配設される加熱炉３及び、反応容器２を図中矢
印Ｒ方向に回転させるモータ等の回転駆動装置４とから
構成される。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A metal compound powder manufacturing apparatus according to the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the examples described below, and various modifications are possible. As shown in FIG. 1, a metal compound powder manufacturing apparatus 1 is made of a metal such as iron and titanium or an alloy such as stainless steel and Inconel, and is a cylindrical reaction container 2 that is horizontally arranged and a reaction container. It is composed of a heating furnace 3 arranged so as to surround 2 and a rotation driving device 4 such as a motor for rotating the reaction vessel 2 in the direction of arrow R in the figure.
【００１５】反応容器２は、その一端にガス供給口５、
他端にガス排気口６を備え、ガス供給口５には、ガスボ
ンベ７に充填された反応性ガスやキャリアガス等を反応
容器２内に供給するための供給管８が連結され、ガス排
気口６には、反応容器２の内部に流入したガスを外部に
排出するための排気管９が連結されている。ガス供給口
５と供給管８との隙間及び、ガス排気口６と排気管９と
の隙間は、適当な密封手段によりシールされている。排
気管９から排出されたガスは、空冷トラップ１０、油ト
ラップ１１及び水トラップ１２を通り、浄化されて系外
に排出される。The reaction vessel 2 has a gas supply port 5 at one end,
The gas exhaust port 6 is provided at the other end, and the gas supply port 5 is connected to a supply pipe 8 for supplying the reactive gas or the carrier gas filled in the gas cylinder 7 into the reaction container 2, An exhaust pipe 9 is connected to 6 for exhausting the gas flowing into the reaction container 2 to the outside. The gap between the gas supply port 5 and the supply pipe 8 and the gap between the gas exhaust port 6 and the exhaust pipe 9 are sealed by an appropriate sealing means. The gas discharged from the exhaust pipe 9 passes through the air-cooling trap 10, the oil trap 11 and the water trap 12 and is purified and discharged to the outside of the system.
【００１６】また、反応容器２の内部には、金属粉体１
３とともに粉砕媒体１４が導入される。粉砕媒体１４
は、金属粉体を初め金属酸化物など目的とする金属化合
物粉体の原料となる原料粉体１３に汚染の影響を与え
ず、かつ熱的、機械的強度に優れた小球体や棒状体から
なり、それらを単独にあるいはそれらを組み合わせたも
のである。ここで、原料粉体１３及び粉砕媒体１４は、
加熱手段３の温度分布を考慮すると、反応性ガスとの反
応中に加熱手段３の長手方向略中央に位置することが好
ましいが、反応容器２の回転に伴って、導入された原料
粉体１３及び粉砕媒体１４が、反応容器全長にわたって
分散することを防ぐために、反応容器２の略中央部に適
当な間隔を置いて、隔壁１５を反応容器２の内壁全周に
わたって立設してもよい。この場合、ガス供給管８及び
排気管９は、反応性ガスを効率良く供給及び排気するた
めに、隔壁１５にできるだけ接近するように設ける。Inside the reaction vessel 2, the metal powder 1
A grinding medium 14 is introduced together with 3. Grinding medium 14
Is a small spherical body or a rod-shaped body which does not affect the raw material powder 13 which is a raw material of a target metal compound powder such as metal powder including metal oxide and which has excellent thermal and mechanical strength. , Either alone or in combination. Here, the raw material powder 13 and the grinding medium 14 are
Considering the temperature distribution of the heating means 3, it is preferable that the heating means 3 is located at the approximate center in the longitudinal direction during the reaction with the reactive gas, but the raw material powder 13 introduced along with the rotation of the reaction vessel 2 is rotated. In order to prevent the crushing medium 14 from being dispersed over the entire length of the reaction container 2, the partition wall 15 may be provided upright over the entire inner wall of the reaction container 2 with an appropriate interval in the approximate center of the reaction container 2. In this case, the gas supply pipe 8 and the exhaust pipe 9 are provided as close as possible to the partition wall 15 in order to efficiently supply and exhaust the reactive gas.
【００１７】原料粉体１３及び粉砕媒体１４の反応容器
２内部への導入方法としては、ガス供給口５あるいは排
気口６を通じて隔壁１５間に導入してもよいし、あるい
は、反応容器２のガス供給口５を備える面あるいは排気
口６を備える全体を取り外し可能な構造として、これら
の面を取り外して形成される開口部から隔壁１５間に導
入してもよい。The raw material powder 13 and the grinding medium 14 may be introduced into the reaction vessel 2 through the gas supply port 5 or the exhaust port 6 between the partition walls 15, or the gas in the reaction vessel 2 may be introduced. The surface provided with the supply port 5 or the entire surface provided with the exhaust port 6 may be provided as a detachable structure and introduced between the partition walls 15 through an opening formed by removing these surfaces.
【００１８】また、原料粉体１３及び粉砕媒体１４の導
入方法に関連して、図２に示されるように、反応容器２
のガス供給口５側に、原料粉体１３が装填された原料粉
体導入部材１６を、また排気口６側には、反応により生
成する金属化合物１７を回収するための金属化合物受け
部材１８を各々付設して、原料粉体１３を金属粉体導入
部材１６から反応容器２に導入して、図中矢印方向へ移
動させながら反応性ガスと反応させて金属化合物粉体１
７に転化し、生成物を金属化合物受け部材１８に回収す
るという連続製造装置とすることも可能である。Further, in relation to the method of introducing the raw material powder 13 and the grinding medium 14, as shown in FIG.
A raw material powder introducing member 16 loaded with the raw material powder 13 is provided on the gas supply port 5 side, and a metal compound receiving member 18 for recovering a metal compound 17 produced by the reaction is provided on the exhaust port 6 side. Attached to each of them, the raw material powder 13 is introduced from the metal powder introducing member 16 into the reaction container 2, and is reacted with the reactive gas while moving in the direction of the arrow in the figure to react with the metal compound powder 1
It is also possible to use a continuous production apparatus in which the metal compound is converted into the product 7 and the product is collected in the metal compound receiving member 18.
【００１９】この時、粉砕媒体１４は、予め反応容器２
に内蔵させておいて、金属粉体１３だけを反応容器２の
外部から導入してもよいし、あるいは、金属粉体導入部
材１６と同様の粉砕媒体導入部材（図示せず）を付設し
て、反応容器２内部に導入してもよい。更に、原料粉体
１３及び粉砕媒体１４の図中矢印方向への移動を制御す
るために、反応容器２の内壁に制御板１９を螺旋状に立
設してもよい。また、反応容器２を水平から適切な角度
に傾斜させることは、この連続化の作用効果を増大させ
るのに好適である。At this time, the crushing medium 14 is previously used in the reaction container 2
The metal powder 13 alone may be introduced from the outside of the reaction vessel 2, or a grinding medium introducing member (not shown) similar to the metal powder introducing member 16 may be attached. It may be introduced into the reaction vessel 2. Further, in order to control the movement of the raw material powder 13 and the grinding medium 14 in the direction of the arrow in the figure, a control plate 19 may be provided upright on the inner wall of the reaction vessel 2 in a spiral shape. Moreover, inclining the reaction container 2 from the horizontal to an appropriate angle is suitable for increasing the effect of this continuation.
【００２０】本発明に係る金属化合物の製造装置の他の
例として、図３に示される構造のものがある。製造装置
１は、図１に示された装置とは反応容器２の構造が異な
る以外は同様である。反応容器２は、インコネル等の金
属または合金からなり、その一端にガス供給口５、他端
にガス排気口６を備える円筒状の反応外管２０と、反応
外管２０とは別体に形成される反応室２１とから構成さ
れる。Another example of the apparatus for producing a metal compound according to the present invention has the structure shown in FIG. The manufacturing apparatus 1 is the same as the apparatus shown in FIG. 1 except that the structure of the reaction vessel 2 is different. The reaction vessel 2 is made of a metal or alloy such as Inconel and has a cylindrical reaction outer tube 20 having a gas supply port 5 at one end and a gas exhaust port 6 at the other end, and the reaction outer tube 20 is formed separately. And the reaction chamber 21.
【００２１】反応室２１は、反応外管２０よりも小径の
円筒体で、その一端にガス供給部２２、他端にガス排出
部２３を備える。また、反応室２１は、その内部に原料
粉体１３とともに粉砕媒体１４が装填され、既述した理
由により反応外管２０の長手方向略中央に内挿される。
反応室２１の反応容器２内部への導入方法は、反応外管
２０のガス供給口５を備える面あるいは排気口６を備え
る面全体を取り外し可能な構造として、これらの面を取
り外して形成される開口部から反応外管２０の内部に挿
入する。反応終了後の反応室２１の取り出しも同様にし
て行われる。The reaction chamber 21 is a cylindrical body having a diameter smaller than that of the reaction outer tube 20, and has a gas supply section 22 at one end and a gas discharge section 23 at the other end. Further, the reaction chamber 21 is loaded with the raw material powder 13 and the pulverizing medium 14 inside thereof, and is inserted substantially in the longitudinal center of the reaction outer tube 20 for the reason described above.
The method for introducing the reaction chamber 21 into the reaction vessel 2 is formed by removing the surfaces of the reaction outer tube 20 having the gas supply port 5 or the entire surface having the exhaust port 6 and removing these surfaces. It is inserted into the reaction outer tube 20 through the opening. After the reaction is completed, the reaction chamber 21 is taken out in the same manner.
【００２２】また、反応室２１を独立部材としたことに
より、複数の種類の原料粉体を別々の反応室に装填し
て、これらを同時に反応外管２０内に並べて配置するこ
とにより、一度の処理により複数の種類の金属化合物を
得ることも可能である。反応容器２の回転は、反応外管
２０を回転させることにより行われる。この反応外管２
０の回転に伴い、内挿された反応室２１も回転する。こ
の時、反応室２１の直径が反応外管２０のそれよりも小
さいために、反応室２１の方がより高速で回転し、これ
により原料粉体１３と粉砕媒体１４との接触がより促進
される。Further, by using the reaction chamber 21 as an independent member, a plurality of kinds of raw material powders are loaded into different reaction chambers, and at the same time, they are arranged side by side in the reaction outer tube 20, so that one reaction It is also possible to obtain multiple types of metal compounds by treatment. The reaction container 2 is rotated by rotating the reaction outer tube 20. This reaction tube 2
With the rotation of 0, the inserted reaction chamber 21 also rotates. At this time, since the diameter of the reaction chamber 21 is smaller than that of the reaction outer tube 20, the reaction chamber 21 rotates at a higher speed, which promotes the contact between the raw material powder 13 and the grinding medium 14. It
【００２３】反応外管２０に設けられたガス供給口５に
は、ガスボンベ７からの反応性ガスやキャリアガス等を
反応外管２０及びその内部に挿入された反応室２１に供
給するための供給管８が連結され、ガス排気口６には、
流入ガスを外部に排出するための排気管９が連結されて
いる。ガス供給口５と供給管８との隙間及び、ガス排気
口６と排気管９との隙間は、適当な密封手段によりシー
ルされている。また、排気管９から排出されたガスは、
空冷トラップ１０、油トラップ１１及び水トラップ１２
を通り、浄化されて系外に排出される。The gas supply port 5 provided in the outer reaction tube 20 is provided for supplying the reaction gas from the gas cylinder 7 and the carrier gas to the outer reaction tube 20 and the reaction chamber 21 inserted therein. The pipe 8 is connected to the gas exhaust port 6,
An exhaust pipe 9 for discharging the inflow gas to the outside is connected. The gap between the gas supply port 5 and the supply pipe 8 and the gap between the gas exhaust port 6 and the exhaust pipe 9 are sealed by an appropriate sealing means. Also, the gas discharged from the exhaust pipe 9 is
Air-cooled trap 10, oil trap 11 and water trap 12
After being purified, it is discharged to the outside of the system.
【００２４】上記構造の製造装置１を用いて、原料粉体
１３及び粉砕媒体１４を反応容器２あるいは反応室２１
に導入して、反応温度の下、所定時間反応容器２あるい
は反応室２１を回転させながら反応性ガスを流して、原
料粉体を所望の金属化合物に転化させることにより、金
属化合物粉体が得られる。反応中、原料粉体１３並びに
生成する金属化合物粉体は、粉砕媒体１４により、絶え
ず解砕あるいは粉砕作用を受けるために、焼結が強制的
に抑制され、所望の１μｍ程度の金属化合物の粉体が得
られる。Using the manufacturing apparatus 1 having the above structure, the raw material powder 13 and the grinding medium 14 are fed to the reaction vessel 2 or the reaction chamber 21.
And a reaction gas is flowed while rotating the reaction vessel 2 or the reaction chamber 21 at a reaction temperature for a predetermined time to convert the raw material powder into a desired metal compound to obtain a metal compound powder. To be During the reaction, the raw material powder 13 and the produced metal compound powder are constantly crushed or crushed by the crushing medium 14, so that the sintering is forcibly suppressed and the powder of the desired metal compound of about 1 μm is obtained. The body is obtained.
【００２５】[0025]
【発明の効果】以上説明したとおり、本発明によると、
金属化合物の製造装置を、原料粉体と反応性ガスとの反
応と同時に、生成する金属化合物の粉砕を行う構造とし
たことにより、従来の装置では得られなかった粒径１μ
ｍ程度の金属化合物の粉体を多量にかつ安価に製造する
ことができる。As described above, according to the present invention,
The metal compound production device has a structure in which the metal compound produced is pulverized at the same time as the reaction between the raw material powder and the reactive gas.
It is possible to produce a large amount of metal compound powder of about m at low cost.
【００２６】また、反応容器を反応外管と反応室との２
部材から構成することにより、原料粉体及び粉砕媒体の
取扱いがより簡単になり、作業性や生産性を向上させる
ことができる。さらに、反応室２２を独立部材としたこ
とにより、複数の種類の金属粉体を別々の反応室に装填
して、これらを同時に反応外管内に並べて配置すること
により、一度の処理により複数の種類の金属化合物粉体
を得ることも可能である。Further, the reaction vessel is composed of a reaction outer tube and a reaction chamber.
By using a member, the raw material powder and the grinding medium can be handled more easily, and workability and productivity can be improved. Further, by using the reaction chamber 22 as an independent member, a plurality of types of metal powders are loaded into different reaction chambers, and these are arranged side by side in the reaction outer tube at the same time. It is also possible to obtain the metal compound powder of
【００２７】加えて、反応容器を連続製造方式とした場
合には、金属粉体の連続処理が可能になり、生産性を向
上させることができる。In addition, when the reaction vessel is of continuous production system, the metal powder can be continuously treated, and the productivity can be improved.
【図１】 本発明に係る金属化合物製造装置の一実施例
を示す図である。FIG. 1 is a diagram showing an example of an apparatus for producing a metal compound according to the present invention.
【図２】 図１に示される金属化合物製造装置を連続製
造装置とした図である。FIG. 2 is a diagram in which the metal compound manufacturing apparatus shown in FIG. 1 is used as a continuous manufacturing apparatus.
【図３】 本発明に係る金属化合物製造装置の他の実施
例を示す図である。FIG. 3 is a diagram showing another embodiment of the metal compound manufacturing apparatus according to the present invention.
１ 金属化合物製造装置 ２ 反応容器 ３ 加熱炉 ４ 回転駆動手段 ５ ガス供給口 ６ ガス排気口 ７ ガスボンべ ８ ガス供給管 ９ ガス排気管 １０ 空冷トラップ １１ 油トラップ １２ 水トラップ １３ 原料粉体 １４ 粉砕媒体 １５ 隔壁 １６ 原料粉体導入部材 １７ 金属化合物粉体 １８ 金属化合物受け部材 １９ 制御板 ２０ 反応外管 ２１ 反応室 ２２ ガス供給部 ２３ ガス排出部 DESCRIPTION OF SYMBOLS 1 Metal compound manufacturing apparatus 2 Reaction container 3 Heating furnace 4 Rotation drive means 5 Gas supply port 6 Gas exhaust port 7 Gas cylinder 8 Gas supply pipe 9 Gas exhaust pipe 10 Air cooling trap 11 Oil trap 12 Water trap 13 Raw powder 14 Grinding medium 15 partition wall 16 raw material powder introduction member 17 metal compound powder 18 metal compound receiving member 19 control plate 20 reaction outer tube 21 reaction chamber 22 gas supply unit 23 gas discharge unit
フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｆ２７Ｂ 7/14 7516−4Ｋ Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI technical display area F27B 7/14 7516-4K
Claims (2)
段により回転される反応容器と、該反応容器を取り囲む
ように配設される加熱手段とから構成される金属化合物
製造装置において、前記反応容器内部には原料粉体とと
もに粉砕媒体が導入されることを特徴とする金属化合物
製造装置。1. An apparatus for producing a metal compound, comprising: a reaction container having a gas supply port and a gas exhaust port and rotated by a rotating means; and a heating means arranged so as to surround the reaction container, An apparatus for producing a metal compound, characterized in that a grinding medium is introduced into the reaction container together with the raw material powder.
口を備え、回転手段により回転される反応外管と、ガス
の供給部及び排出部を備え、原料粉体及び粉砕媒体が導
入される反応室とから構成されるとともに、前記反応室
は、前記反応外管内部に出し入れ可能に内挿されて該反
応外管の回転に伴い回転することを特徴とする請求項１
に記載の金属化合物製造装置。2. The reaction container comprises a gas supply port and a gas discharge port, a reaction outer tube rotated by a rotating means, a gas supply unit and a gas discharge unit, and a raw material powder and a grinding medium are introduced therein. And a reaction chamber that is inserted into and removed from the reaction outer tube and rotates with the rotation of the reaction outer tube.
The metal compound manufacturing apparatus as described in 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05931093A JP3250684B2 (en) | 1993-02-25 | 1993-02-25 | Metal compound powder production equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05931093A JP3250684B2 (en) | 1993-02-25 | 1993-02-25 | Metal compound powder production equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06246152A true JPH06246152A (en) | 1994-09-06 |
| JP3250684B2 JP3250684B2 (en) | 2002-01-28 |
Family
ID=13109674
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05931093A Expired - Fee Related JP3250684B2 (en) | 1993-02-25 | 1993-02-25 | Metal compound powder production equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3250684B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002333283A (en) * | 2001-05-09 | 2002-11-22 | Murata Mfg Co Ltd | Heat treatment furnace and gas supply method therefor |
| WO2013031197A1 (en) * | 2011-09-02 | 2013-03-07 | 東洋炭素株式会社 | Powder stirring device |
| JP2013091012A (en) * | 2011-10-24 | 2013-05-16 | Toyo Tanso Kk | Powder stirring device |
| CN104971677A (en) * | 2014-04-02 | 2015-10-14 | 杜茂松 | Dynamic high-temperature atmosphere reaction method and device under effect of electric field |
-
1993
- 1993-02-25 JP JP05931093A patent/JP3250684B2/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002333283A (en) * | 2001-05-09 | 2002-11-22 | Murata Mfg Co Ltd | Heat treatment furnace and gas supply method therefor |
| JP4524951B2 (en) * | 2001-05-09 | 2010-08-18 | 株式会社村田製作所 | Heat treatment furnace and gas supply method for heat treatment furnace |
| WO2013031197A1 (en) * | 2011-09-02 | 2013-03-07 | 東洋炭素株式会社 | Powder stirring device |
| CN103764267A (en) * | 2011-09-02 | 2014-04-30 | 东洋炭素株式会社 | Powder stirring device |
| EP2752235A1 (en) * | 2011-09-02 | 2014-07-09 | Toyo Tanso Co., Ltd. | Powder stirring device |
| EP2752235A4 (en) * | 2011-09-02 | 2015-04-15 | Toyo Tanso Co | Powder stirring device |
| JP2013091012A (en) * | 2011-10-24 | 2013-05-16 | Toyo Tanso Kk | Powder stirring device |
| CN104971677A (en) * | 2014-04-02 | 2015-10-14 | 杜茂松 | Dynamic high-temperature atmosphere reaction method and device under effect of electric field |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3250684B2 (en) | 2002-01-28 |
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