JPS5985808A - Production of ultrafine metallic particle - Google Patents
Production of ultrafine metallic particleInfo
- Publication number
- JPS5985808A JPS5985808A JP19452782A JP19452782A JPS5985808A JP S5985808 A JPS5985808 A JP S5985808A JP 19452782 A JP19452782 A JP 19452782A JP 19452782 A JP19452782 A JP 19452782A JP S5985808 A JPS5985808 A JP S5985808A
- Authority
- JP
- Japan
- Prior art keywords
- ultrafine
- metal
- vessel
- metal particles
- arc
- 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
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
Abstract
Description
【発明の詳細な説明】
この発明は、アーク放電を利用してその微粒子径が良く
揃った金属超微粒子を製造できる金属超微粒子の製造装
置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for producing ultrafine metal particles that can produce ultrafine metal particles with well-uniformed particle diameters using arc discharge.
従来、金属超微粒子を製造する装置としてアーク放電を
利用するものには第１図に示すものがある。すなわちガ
ス導入口ＩＡとガス排出口ＩＢとを設けた密閉された容
器１内に支持棒２の先端に固定された陰極用のタングス
テンなどの電極３を挿入し、そして前記容器１の底部を
構成する陽極用の銅ハース４の上面に陰極用の前記電極
３に対向して金属超微粒子を製造すべき陽極用の電極と
同極になり得る金属材料５を載置している。そしてガス
導入口ＩＡから純水素ガスまたは水素ガスと不活性ガス
、例えばアルゴンガス、ヘリウムガス等の混合ガスを容
器１内に導入するとともに前記ガス排出口ＩＡから排出
して容器１内をそのガス圧力６０〜７６０ Ｔｏｒｒ程
度の前記ガス雰囲気とした後に、陰極用の電極３と、陽
極用の電極になり得る強磁性体等の金属材料５との間の
電極間電圧を１０〜１００Ｖとして電°極間にアーク放
電を行ってアーク柱６を形成させると、このアーク柱６
付近から金属材料５の金属超微粒子が多く発生する。こ
のようにして生成される金属超微粒子の一部は陰極用の
支持棒２に付着し、またガス導入口ＩＡから容器１内に
導入されてガス排出口ＩＢから排出される純水素ガス等
のガス流に運ばれて急上昇され前記金属超微粒子の一部
が前記ガス排出口ＩＢ内に設けられた紙やガラス繊維よ
り成るフィルター７に捕集される。しかし、ガスを容器
１内に上記のように流す場合にも流さない場合にも金属
超微粒子の大部分は容器ｌの内壁に付着されるが、これ
等を掻き落して金属超微粒子を回収する。この場合に金
属超微粒子の粒子径が揃っているのは前記支持棒２に付
着されたものである。Conventionally, there is an apparatus shown in FIG. 1 that utilizes arc discharge as an apparatus for producing ultrafine metal particles. That is, an electrode 3 such as tungsten for a cathode fixed to the tip of a support rod 2 is inserted into a sealed container 1 provided with a gas inlet IA and a gas outlet IB, and the bottom of the container 1 is formed. On the upper surface of the copper hearth 4 for the anode, facing the electrode 3 for the cathode, is placed a metal material 5 which can be the same electrode as the electrode for the anode from which ultrafine metal particles are to be produced. Then, pure hydrogen gas or a mixed gas of hydrogen gas and an inert gas, such as argon gas or helium gas, is introduced into the container 1 from the gas inlet IA, and the gas is discharged from the gas outlet IA to fill the container 1 with the gas. After creating the gas atmosphere at a pressure of approximately 60 to 760 Torr, the voltage between the electrodes 3 and the metal material 5 such as a ferromagnetic material that can be used as the anode electrode is set to 10 to 100 V. When arc discharge is performed between the poles to form an arc column 6, this arc column 6
Many ultrafine metal particles of the metal material 5 are generated from the vicinity. Some of the ultrafine metal particles generated in this way adhere to the cathode support rod 2, and some of the ultrafine metal particles are introduced into the container 1 from the gas inlet IA and discharged from the gas outlet IB, such as pure hydrogen gas. A part of the ultrafine metal particles, which are carried by the gas flow and rise rapidly, are collected by a filter 7 made of paper or glass fiber provided in the gas outlet IB. However, most of the ultrafine metal particles are attached to the inner wall of the container l regardless of whether or not the gas is flowed into the container 1 as described above, and these are scraped off to recover the ultrafine metal particles. . In this case, the metal ultrafine particles with uniform particle diameters are those attached to the support rod 2.
しかしながら従来は粒子径が不揃いの金属超微粒子を一
緒に回収するものであるため、粒子径が揃った超微粒子
を効率良く回収することができなかった。このため金属
超微粒子が強磁性体である場合には保磁力が低くなり、
磁気記録媒体用の材料に使用するのには不適当であった
。However, in the past, since ultrafine metal particles with irregular particle sizes were collected together, it was not possible to efficiently recover ultrafine particles with uniform particle sizes. For this reason, if the metal ultrafine particles are ferromagnetic, the coercive force will be low,
It was unsuitable for use as a material for magnetic recording media.
本発明は上述の如き点に鑑みてなされたものでありその
目的とするところは、従来の装置に大幅の変更を加える
ことなく粒径の揃った金属超微粒子を製造でき、また製
品としての信頼性が高い金属超微粒子の製造装置を提供
するのにある。The present invention has been made in view of the above points, and its purpose is to be able to produce ultrafine metal particles of uniform particle size without making major changes to conventional equipment, and to improve reliability as a product. The purpose of the present invention is to provide an apparatus for producing ultrafine metal particles with high properties.
以下本発明の第１実施例を第２図に従って説明する。A first embodiment of the present invention will be described below with reference to FIG.
なお第１図に示す従来の装置と同一部分については同一
符号で示しているので説明は省略する。Note that the same parts as those in the conventional device shown in FIG. 1 are designated by the same reference numerals, and therefore their explanation will be omitted.
８は銅、ステンレス等の材料で形成され底面を上方にし
た中空の逆円錐形の付着手段で、この付着手段８はアー
ク柱６が形成された際に前記金属材料５から発生する金
属超微粒子を捕集するためのものである。Reference numeral 8 denotes a hollow inverted conical adhesion means made of a material such as copper or stainless steel with the bottom facing upward. It is for collecting.
しかもこの付着手段８は陰極用の前記電極３と陽極用の
電極としての銅ハース４に接続すべき金属材料５との上
方で且つアーク柱が立ちのぼる高速のガス流によっ運ば
れる金属超微粒子の流れの領域内に配置される。Moreover, this adhesion means 8 is located above the metal material 5 to be connected to the electrode 3 for the cathode and the copper hearth 4 as the electrode for the anode, and the ultrafine metal particles carried by the high-speed gas flow rising from the arc column. Placed within the region of flow.
９．１０は付着手段８の一例に設けられた導入管と排出
管であり、水などの冷却用の液体がこの導入管９から中
空の前記付着手段８内に導入されて排出管１０から排出
されることにより前記付着手段８は冷却されるようにな
っている。Reference numeral 9.10 denotes an introduction pipe and a discharge pipe provided in an example of the attachment means 8, and a cooling liquid such as water is introduced into the hollow attachment means 8 from this introduction pipe 9 and is discharged from the discharge pipe 10. By doing so, the adhesion means 8 is cooled.
本発明の一実施例は上述のような構成からなり、ガス導
入口ＩＡから純水素、または純水素とアルゴンガス、ヘ
リウムガス等の１種または２種の不活性ガスとの混合ガ
スを容器１内に導入した後にガス排出口ＩＢから排出し
て容器１内のガス圧力を６０〜７０ Ｔｏｒｒ程度のガ
ス雰囲気にする。そして陰極用の電極３と、陽極用の電
極としての銅ハース４に載置されて同極になり得る金属
材料５との間に１０〜１００■の電極間電圧を印加して
アーク放電を行いアーク柱６を形成すると、前記アーク
柱６付近から例えば強磁性体の金属超微粒子が生成され
る。この場合、アーク柱６の近傍で金属超微粒子が生成
されると考えられる。また陰極用の電極３と支持棒２と
は、鉛直線から傾斜させて設けてもよく、しかも陰極用
の電極３と支持棒２とは２本以上の多極にしてもかまわ
ない（第２図山）参照）。このように発生した金属超微
粒子は高速の前記ガス流に運ばさて大部分が上方に運ば
れる。この際、大部分が底面８Ａを上方にした逆円錐形
の付着手段８に付着される。この金属超微粒子はアーク
柱６から上昇するにつれて成長していくが、その過程で
ほど良い位置に付着手段を受けることによって適度な粒
径をもち、かつその粒径が良く揃った金属超微粒子が得
られる。One embodiment of the present invention has the above-described configuration, and pure hydrogen or a mixed gas of pure hydrogen and one or two inert gases such as argon gas or helium gas is supplied to the container 1 from the gas inlet IA. After introducing the gas into the container 1, the gas is discharged from the gas outlet IB to make the gas pressure inside the container 1 a gas atmosphere of about 60 to 70 Torr. Then, an inter-electrode voltage of 10 to 100 μ is applied between the cathode electrode 3 and the metal material 5 placed on the copper hearth 4 as the anode electrode and capable of forming the same polarity to cause arc discharge. When the arc column 6 is formed, ultrafine metal particles of ferromagnetic material, for example, are generated near the arc column 6. In this case, it is thought that ultrafine metal particles are generated near the arc column 6. Further, the cathode electrode 3 and the support rod 2 may be provided at an angle from the vertical line, and the cathode electrode 3 and the support rod 2 may be multipole with two or more (second (See Figure 2). The ultrafine metal particles thus generated are carried by the high-speed gas flow, and most of them are carried upward. At this time, most of it is attached to the inverted conical attachment means 8 with the bottom surface 8A facing upward. These ultrafine metal particles grow as they rise from the arc column 6, and in the process, they receive adhesion means at just the right positions, resulting in ultrafine metal particles that have an appropriate particle size and are well-uniformed. can get.
また逆円錐形の付着手段は、導入管９から水等の冷却用
の液体が導入され、排出管１ｏから排出されることによ
って冷却されるので金属超微粒子は効率良く付着手段８
に付着しかつ熱的に安定な状態に保持される。その後、
付着手段８に付着された一定粒径の金属超微粒子を掻き
落して容器１外に回収する。この量は、金属材料５から
発生される金属超微粒子全体の８割以上になる。第３図
は、得られる金属超微粒子の粒径分布の一例である。金
属材料５が強磁性体金属として例えばＦｅ１０ｗｔ％Ｎ
ｉ合金の場合には保磁力１２００００以上、単位重量当
りの飽和磁気モーメント１５０ｅｍｕ／ｇ、磁場配向を
させないで測定した場合の角形比０．４５以上の金属合
金超微粒子が得られる。Further, since the inverted conical attachment means is cooled by introducing a cooling liquid such as water from the inlet pipe 9 and discharging it from the discharge pipe 1o, the metal ultrafine particles are efficiently transferred to the attachment means 8.
and is maintained in a thermally stable state. after that,
Ultrafine metal particles of a certain particle size adhered to the adhesion means 8 are scraped off and collected outside the container 1. This amount accounts for 80% or more of the total ultrafine metal particles generated from the metal material 5. FIG. 3 shows an example of the particle size distribution of the obtained ultrafine metal particles. The metal material 5 is a ferromagnetic metal such as Fe10wt%N.
In the case of i-alloy, ultrafine metal alloy particles having a coercive force of 120,000 or more, a saturation magnetic moment per unit weight of 150 emu/g, and a squareness ratio of 0.45 or more when measured without magnetic field orientation can be obtained.
このようにして得られた強磁性体よりなる金属超微粒子
は、高保磁力、高飽和磁密度の磁気テープ等の磁気記録
媒体用材料に使用することができる。The ultrafine metal particles made of ferromagnetic material thus obtained can be used as materials for magnetic recording media such as magnetic tapes with high coercive force and high saturation magnetic density.
第４図（イ）（ロ）は本発明の第２実施例を示し、この
実施例においては逆円錐形の付着手段８の外周表面を波
状又は放射状に形成して前記第１実施例のものよりその
表面積を広くしたことにより金属材料５からの金属超微
粒子の付着効率を高くした点が前記第１実施例と異なる
。4(a) and 4(b) show a second embodiment of the present invention, in which the outer circumferential surface of the inverted conical adhesion means 8 is formed in a wavy or radial shape, and is similar to the first embodiment. This embodiment differs from the first embodiment in that the adhesion efficiency of ultrafine metal particles from the metal material 5 is increased by increasing the surface area.
また第５図（イ） （ロ）は本発明の第３実施例であり
、この実施例においては付着手段８を数枚の翼板部８Ｃ
を放射状に配置して形成したことにより同様に第４図（
イ） （ロ）に示したように単なる円錐形の付着手段８
のものより金属超微粒子の付着効率を高くした点が前記
第１実施例と異なる。Further, FIGS. 5(a) and 5(b) show a third embodiment of the present invention, and in this embodiment, the adhesion means 8 is attached to several blade parts 8C.
4 (
b) A mere conical attachment means 8 as shown in (b)
This embodiment differs from the first embodiment in that the adhesion efficiency of ultrafine metal particles is made higher than that of the first embodiment.
第６図（イ）（ロ）は本発明の第４実施例であり、この
実施例においては付着手段８が内芯材８Ｄ１と、この内
芯材８Ｄ＋を覆うようにその外周に嵌合、配置される外
装材８Ｄ２とから形成される。そして前記内芯材８Ｄ＋
はその外周に数枚の翼板部８Ｇ＋を放射状に配置して
形成され、また外装材８Ｄ２は前記内芯材８Ｄ＋の外周
に配置された放射状の前記翼板部８０１間に挿入される
放射状の数枚の翼板部８Ｃ２を内側に設けて形成された
ことにより前記第３実施例より表面積を太きくして金属
超微粒子の付着効率を高められる。FIGS. 6(a) and 6(b) show a fourth embodiment of the present invention, and in this embodiment, the attachment means 8 is fitted onto the outer periphery of the inner core material 8D1 and the inner core material 8D+ so as to cover the inner core material 8D1, It is formed from the exterior material 8D2 that is placed. And the inner core material 8D+
is formed by radially arranging several vane plate portions 8G+ on its outer periphery, and the exterior material 8D2 is formed by radial blade portions 8G+ inserted between the radial vane portions 801 disposed on the outer periphery of the inner core material 8D+. By forming several vanes 8C2 on the inside, the surface area can be increased compared to the third embodiment, and the adhesion efficiency of ultrafine metal particles can be increased.
また第７図（イ） （ロ）に示すものは本発明の第５実
施例であり、この実施例においては付着手段８が平板８
Ｅを縦横に格子状に組み合わされて形成され７たことに
より、付着手段８の表面積を大きくして金属超微粒子の
付着効率を高くしている。Moreover, what is shown in FIGS. 7(a) and 7(b) is a fifth embodiment of the present invention, and in this embodiment, the adhesion means 8 is attached to a flat plate 8.
By combining E in a lattice pattern 7 vertically and horizontally, the surface area of the adhesion means 8 is increased and the adhesion efficiency of ultrafine metal particles is increased.
さらに第８図（イ）（ロ）に示すものは本発明の第６実
施例であり、この実施例においては付着手段８として円
形、多角形等の板材８Ｆを陰極用の電極３に対して水平
に配置したことにより、表面積の割りに金属超微粒子の
付着効率を高くしている。Furthermore, what is shown in FIGS. 8(a) and 8(b) is a sixth embodiment of the present invention, and in this embodiment, a circular, polygonal, etc. plate 8F is attached to the cathode electrode 3 as the attachment means 8. By arranging it horizontally, the adhesion efficiency of ultrafine metal particles is increased relative to the surface area.
上述のように本発明はアーク放電を用いて金属超微粒子
の製造を行う従来の装置に比べて装置自体に大幅の変更
を加えることなく適度な粒径をもちかつ粒径のよく揃っ
た金属超微粒子を効率良く製造できる。従って金属材料
に強磁性体を用いて之から製造される強磁性体の金属超
微粒子を用いて磁気テープ等の磁気記録媒体を製作した
場合には高保磁力、高飽和磁束密度のものが得られ、製
品としての信頼性が向上する。As mentioned above, the present invention can produce metal ultrafine particles with appropriate particle size and uniform particle size without making any major changes to the apparatus itself compared to conventional equipment that uses arc discharge to produce metal ultrafine particles. Fine particles can be produced efficiently. Therefore, when a magnetic recording medium such as a magnetic tape is manufactured using ultrafine ferromagnetic metal particles produced by using a ferromagnetic material as a metal material, a medium with high coercive force and high saturation magnetic flux density can be obtained. , the reliability of the product is improved.
第１図はアーク放電を用いて金属超微粒子を製造する従
来の装置の一例を示した断面図、第２図ｔａｌは同じく
本発明の第１実施例を示した断面図、第２図（ｂ）は同
じく他の変形例を示した断面図、第３図は同じく本発明
の第１実施例の装置を用いて製造した場合のＦ ｅ −
Ｎ ｉ合金金属超微粒子の粒径分布曲線を示した特性図
、第４図（イ）は本発明の第２実施例を示した上面図、
（ロ）は同じく側面図、第５図（イ）は本発明の第３実
施例を示した上面図、（ロ）は同じ（側面図、第６図（
イ）は第４実施例を示した上面図、（ロ）は同じく側面
図、第７図（イ）は第５実施例を示した上面図、（ロ）
は同じく側面図、第８図（イ）は第６実施例を示した上
面図、（ロ）は同じく側面図である。
１・・・・・・容器、２・・・・・・支持棒、３・・・
・・・陰極用の電極、４・・・・・・陽極用の電極とし
ての桐ハース、５・・・・・・金属材料、６・・・・・
・アーク柱、７・・・・・・フィルター、８・・・・・
・付着手段、８Ａ・・・・・・底面、８Ｃｔ８Ｃ＋ｓ８
Ｃ２・・・・・・翼板部、８Ｄｔ・・・・・・内芯材、
８Ｄ２・・・・・・外装材、８Ｅ・・・・・・平板、８
Ｆ・・・・・・板材。
特許出願人 パイオニア株式会社
０FIG. 1 is a sectional view showing an example of a conventional apparatus for manufacturing ultrafine metal particles using arc discharge, FIG. ) is a sectional view similarly showing another modification, and FIG.
A characteristic diagram showing the particle size distribution curve of Ni alloy metal ultrafine particles, FIG. 4 (A) is a top view showing the second embodiment of the present invention,
(B) is the same side view, FIG. 5 (A) is a top view showing the third embodiment of the present invention, (B) is the same (side view,
A) is a top view showing the fourth embodiment, (B) is a side view, and FIG. 7(A) is a top view showing the fifth embodiment.
8(A) is a top view showing the sixth embodiment, and FIG. 8(B) is a side view. 1...Container, 2...Support rod, 3...
... Electrode for cathode, 4 ... Paulownia hearth as electrode for anode, 5 ... Metal material, 6 ...
・Arc column, 7...Filter, 8...
・Adhesion means, 8A...Bottom surface, 8Ct8C+s8
C2... Wing plate part, 8Dt... Inner core material,
8D2... Exterior material, 8E... Flat plate, 8
F...Plate material. Patent applicant Pioneer Corporation 0
Claims (1)
を得る金属超微粒子の製造方法であって、アーク柱の略
直上に発生した金属超微粒子を付着させる付着手段を設
けたことを特徴とする金属超微粒子の製造装置。A method for producing ultrafine metal particles by subjecting a metal material to plasma arc discharge to obtain ultrafine metal particles, the method comprising an attachment means for adhering the ultrafine metal particles generated substantially directly above an arc column. Ultrafine particle manufacturing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19452782A JPS5985808A (en) | 1982-11-08 | 1982-11-08 | Production of ultrafine metallic particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19452782A JPS5985808A (en) | 1982-11-08 | 1982-11-08 | Production of ultrafine metallic particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5985808A true JPS5985808A (en) | 1984-05-17 |
Family
ID=16326012
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19452782A Pending JPS5985808A (en) | 1982-11-08 | 1982-11-08 | Production of ultrafine metallic particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5985808A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5460701A (en) * | 1993-07-27 | 1995-10-24 | Nanophase Technologies Corporation | Method of making nanostructured materials |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS505149A (en) * | 1973-05-15 | 1975-01-20 | ||
| JPS5544123A (en) * | 1978-09-20 | 1980-03-28 | Kamiichi Denshi Kk | Device for automatically shutting off main valve |
| JPS56136634A (en) * | 1980-03-29 | 1981-10-26 | Res Dev Corp Of Japan | Production of ultra-fine powder and particle using laser beam |
| JPS58104103A (en) * | 1981-12-17 | 1983-06-21 | Natl Res Inst For Metals | Method and device for producing fine metallic particle |
-
1982
- 1982-11-08 JP JP19452782A patent/JPS5985808A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS505149A (en) * | 1973-05-15 | 1975-01-20 | ||
| JPS5544123A (en) * | 1978-09-20 | 1980-03-28 | Kamiichi Denshi Kk | Device for automatically shutting off main valve |
| JPS56136634A (en) * | 1980-03-29 | 1981-10-26 | Res Dev Corp Of Japan | Production of ultra-fine powder and particle using laser beam |
| JPS58104103A (en) * | 1981-12-17 | 1983-06-21 | Natl Res Inst For Metals | Method and device for producing fine metallic particle |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5460701A (en) * | 1993-07-27 | 1995-10-24 | Nanophase Technologies Corporation | Method of making nanostructured materials |
| US5874684A (en) * | 1993-07-27 | 1999-02-23 | Nanophase Technologies Corporation | Nanocrystalline materials |
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