JPH02218431A - Powder for plasma pulverizing and its supply method - Google Patents

Powder for plasma pulverizing and its supply method

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Publication number
JPH02218431A
JPH02218431A JP1039429A JP3942989A JPH02218431A JP H02218431 A JPH02218431 A JP H02218431A JP 1039429 A JP1039429 A JP 1039429A JP 3942989 A JP3942989 A JP 3942989A JP H02218431 A JPH02218431 A JP H02218431A
Authority
JP
Japan
Prior art keywords
powder
plasma
nozzle
raw material
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
Application number
JP1039429A
Other languages
Japanese (ja)
Inventor
Jiro Yoshinari
次郎 吉成
Yasumichi Tokuoka
保導 徳岡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TDK Corp
Original Assignee
TDK Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by TDK Corp filed Critical TDK Corp
Priority to JP1039429A priority Critical patent/JPH02218431A/en
Publication of JPH02218431A publication Critical patent/JPH02218431A/en
Pending legal-status Critical Current

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  • Plasma Technology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

PURPOSE:To prevent the clogging of a nozzle by injecting a powder for pulverizing of plasma through the nozzle to a plasma-generated space kept at high temperature. CONSTITUTION:A plasma generating torch 3 is installed in one end and an arc jet 7 is formed by a conventional arc discharge generating means. A raw material powder together with a carrier gas is introduced into the arc jet 7 through a powder transferring apparatus 4 and a nozzle 2 in the radius direction, melted, evaporated, cooled by a cooling means in the downstream side, and recovered as a super fine powder. As the raw material powder to be pulverized super-finely, there are iron, cobalt, nickel, aluminum, zinc, copper, manganese, etc. By this method, production efficiency is improved.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明はプラズマ微粒化用粉体とそれをプラズマ微粒化
工程へ供給する方法に関する。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a powder for plasma atomization and a method for supplying the same to a plasma atomization process.

(従来技術) 磁気記録用磁性粉、触媒用粉末その他多くの分野で金属
、金属酸化物その他の化合物の超微粒子粉末が求められ
ている。このような超微粒子粉末は凝集して2次粒子を
形成し易く、ばらばらの孤立超微粒子の製造は困難であ
る。
(Prior Art) Ultrafine particle powders of metals, metal oxides, and other compounds are required in many fields including magnetic powders for magnetic recording and powders for catalysts. Such ultrafine powder particles tend to aggregate to form secondary particles, and it is difficult to produce isolated ultrafine particles.

超微粒子の製造には従来からガス蒸発法が知られている
。これは金属を真空中で溶融し、気化蒸発させることに
より超微粒子とし、冷却回収する方法である(特公昭6
2−11896号)、シかし、この方法は原料が溶融性
の金属又は合金に限定される問題があり、さらに超高真
空を必要とし、或いは生産性が低いなどの問題を有する
Gas evaporation methods have been known for the production of ultrafine particles. This is a method in which metals are melted in a vacuum and vaporized into ultrafine particles, which are then cooled and collected.
2-11896), however, this method has the problem that the raw material is limited to meltable metals or alloys, and also requires an ultra-high vacuum or has low productivity.

他の方法には、プラズマを利用した超微粒子粉末の製造
方法がある。その典型例も第1図〜第4図に示す、第1
図の装置ではプラズマ容器1の一端に試料とキャリアガ
スをプラズマ中心軸に沿って導入するためのノズル2、
それを取囲むプラズマ形成ガスノズル3.4が配置され
、さらに、容器lの周囲に高周波コイルが配置される。
Other methods include methods for producing ultrafine powder using plasma. Typical examples are shown in Figures 1 to 4.
In the apparatus shown in the figure, a nozzle 2 for introducing the sample and carrier gas along the plasma central axis into one end of the plasma container 1;
A plasma-forming gas nozzle 3.4 is arranged surrounding it, and furthermore a high frequency coil is arranged around the vessel l.

第2図の装置ではプラズマ形成ガスがプラズマ容器lの
一端のガスノズル3.4から導入され、一方試料とキャ
リアガスは容器lの側壁を貫通するノズル2からプラズ
マ中心軸に対し半径方向に導入される。第3図の装置で
は、中心ガスノズル6により直流アークジェットが形成
され、試料とキャリアガスはノズル6の周りのノズル2
から半径方向に導入され、アークジェットにより気化分
散され、さらに高周波コイル5により高周波プラズマが
形成される。第4図は、DCプラズマを用いた装置で、
プラズマトーチ13によって直流アークジェット17が
形成され、試料とキャリアガスは、ノズル12によって
、半径方向に導入され、アークジェットにより気化分散
される。容器lは、保温されることが好ましく、内部に
断熱材15及び耐熱材16が配置される。断熱材15の
材質としては、繊維状カーボン、アルミナ、ジルコニア
などが好ましい、耐熱材16の材質としては、グラファ
イト、窒化ホウ素、タングステン、その他の耐熱性合金
材料を用いることが好ましい。
In the apparatus of FIG. 2, the plasma-forming gas is introduced through a gas nozzle 3.4 at one end of the plasma vessel l, while the sample and carrier gas are introduced radially with respect to the plasma central axis through a nozzle 2 penetrating the side wall of the vessel l. Ru. In the apparatus shown in FIG. 3, a DC arc jet is formed by a central gas nozzle 6, and the sample and carrier gas are passed through nozzles 2 around the nozzle 6.
The plasma is introduced in the radial direction from the plasma, vaporized and dispersed by an arc jet, and then a high frequency plasma is formed by the high frequency coil 5. Figure 4 shows a device using DC plasma.
A DC arc jet 17 is formed by the plasma torch 13, and the sample and carrier gas are introduced radially through the nozzle 12 and vaporized and dispersed by the arc jet. The container l is preferably kept warm, and a heat insulating material 15 and a heat resistant material 16 are arranged inside. The material of the heat insulating material 15 is preferably fibrous carbon, alumina, zirconia, etc., and the material of the heat resistant material 16 is preferably graphite, boron nitride, tungsten, or other heat resistant alloy material.

(従来技術の問題点) これらの方法はいずれも各種超微粒子粉末を比較的良好
に形成し得るが、試料導入ノズル2の出口が高熱にさら
され、溶融試料によるノズルの狭小化により能率の低下
が起きる。
(Problems with the prior art) All of these methods can form various ultrafine powders relatively well, but the exit of the sample introduction nozzle 2 is exposed to high heat, and the nozzle becomes narrow due to the molten sample, resulting in a decrease in efficiency. happens.

(発明の目的) 本発明の目的は、プラズマ微粉化方法に関してノズルの
狭小化ないし閉塞の生じるおそれのない粉体原料及びそ
の供給方法を提供することにある。
(Objective of the Invention) An object of the present invention is to provide a powder raw material and a method for supplying the same, which are free from the possibility of narrowing or clogging of a nozzle in a plasma pulverization method.

(発明の概要) 本発明の上記目的は、カーボン等の昇華性物質を混合或
いは表面被覆した金属、金属酸化物、その他の無機物粉
体を用い、これをノズルを介してプラズマ微粒化装置へ
導入することにより達成される。
(Summary of the Invention) The above object of the present invention is to use metal, metal oxide, or other inorganic powder mixed with or surface coated with a sublimable substance such as carbon, and to introduce this into a plasma atomization device through a nozzle. This is achieved by

本発明によると、カーボン等の昇華性物質は、粉体がノ
ズル出口の高温にさらされたときに溶融を開始しても、
粉体がノズル出口に付着するのを防止し、常時ノズル出
口を清浄な状態に維持することができる。従って、超微
粒子粉末の生成能率の低下を防止し、生産性を常に高く
維持することができる効果が得られる。
According to the present invention, even if the sublimable substance such as carbon starts to melt when the powder is exposed to the high temperature at the nozzle outlet,
It is possible to prevent powder from adhering to the nozzle outlet and to maintain the nozzle outlet in a clean state at all times. Therefore, it is possible to prevent a decrease in the production efficiency of ultrafine particle powder and maintain high productivity at all times.

(発明の詳細な説明) 以下の説明は特に第4図に示したプラズマ微粒化装置に
関連して行うが、一般にノズル出口が高温度にさらされ
ることにより原料粉体がノズル出口で溶融するような微
粒化装置を用いる場合に適用できることに留意されたい
(Detailed Description of the Invention) The following explanation will be made with particular reference to the plasma atomization device shown in FIG. Note that this is applicable when using a fine atomization device.

さて、第4図に示されたプラズマ微粒化装置は一端にプ
ラズマ発生トーチ3を有し、慣用のアーク放電発生手段
によってアークジェット7を形成する。原料粉体はキャ
リアガスと共に粉体搬送装置4から半径方向ノズル2を
経てアークジェット7へ導入され、溶融、蒸発し、下流
側の冷却手段(図示せず)で冷却、超微粒子化されて回
収される。
Now, the plasma atomization apparatus shown in FIG. 4 has a plasma generating torch 3 at one end, and forms an arc jet 7 by a conventional arc discharge generating means. The raw material powder is introduced into the arc jet 7 from the powder conveying device 4 through the radial nozzle 2 along with the carrier gas, where it is melted and evaporated, cooled by a cooling means (not shown) on the downstream side, turned into ultrafine particles, and recovered. be done.

このプラズマ微粒化法により超微粒化される粉体には、
鉄、コバルト、ニッケル、アルミ、亜鉛、銅、マンガン
等の金属、酸化鉄、酸化コバルト、リン酸鉄、酸化アル
ミ、酸化銅、酸化亜鉛等の金属化合物等がある。これら
の粉体はアーク及びプラズマにより溶融され且つ超微粒
化される。
The powder that is made into ultra-fine particles by this plasma atomization method includes:
Examples include metals such as iron, cobalt, nickel, aluminum, zinc, copper, and manganese, and metal compounds such as iron oxide, cobalt oxide, iron phosphate, aluminum oxide, copper oxide, and zinc oxide. These powders are melted and ultra-fine by arc and plasma.

化合物や金属粉体は溶融合体して合金、固溶体、或いは
混合物を形成するなど、必ずしも元の粉体の状態を保持
しない。
Compounds and metal powders do not necessarily maintain their original powder state, such as by melting and amalgamating them to form alloys, solid solutions, or mixtures.

キャリアガス、アーク及びプラズマ用のガスはA r 
%N s % H* 、COlOs 、A t r等で
ある。原料粉末に混合される或いはこれを被覆するため
の昇華性物質粉体はカーボン、窒化ホウ素、窒化アルミ
、酸化ナトリウム等が使用でき、特にカーボンの使用が
好ましい、昇華性物質の必要な条件は、ノズル出口で溶
融原料粉体のノズル壁へのバリヤとなること、アークジ
ェット及びプラズマにより昇華することである。上記の
列挙物質はいずれもこの条件を満足する。
Carrier gas, arc and plasma gas are Ar
%Ns%H*, COIOs, Atr, etc. Carbon, boron nitride, aluminum nitride, sodium oxide, etc. can be used as the sublimable substance powder to be mixed with the raw material powder or to coat it, and the use of carbon is particularly preferable.The necessary conditions for the sublimable substance are as follows: It serves as a barrier to the nozzle wall of the molten raw material powder at the nozzle exit, and it sublimes due to the arc jet and plasma. All of the substances listed above satisfy this condition.

被覆又は混合昇華物質を有する原料粉体はなるべく顆粒
に予備成形すると、本発明の目的を一層良く達成するこ
とができる。顆粒化の方法は任意の慣用技術による。
The object of the present invention can be better achieved if the raw material powder with the coated or mixed sublimation material is preferably preformed into granules. The method of granulation is by any conventional technique.

以下に本発明の実施例及び比較例を述べる。なお、以下
の例ではノズルブロックとして第4図に示したものを用
い、試料導入ノズル径を10mmとした。
Examples and comparative examples of the present invention will be described below. In the following example, the nozzle block shown in FIG. 4 was used, and the sample introduction nozzle diameter was 10 mm.

実施例1 酸化鉄粉体に、カーボンブラックを30wt%添加混合
し加湿らにスプレードライにより顆粒状態とした。これ
を出口19KWのAr−N、プラズマジェット中に毎分
1gの割合で、連続的に投入したところ、導入口に於け
る粉体或いはメルトの付着は認められなかった。
Example 1 30 wt % of carbon black was added and mixed to iron oxide powder, and the mixture was made into granules by humidification and spray drying. When this was continuously introduced into an Ar-N plasma jet with an outlet of 19 KW at a rate of 1 g per minute, no powder or melt adhesion was observed at the inlet.

実施例2 酸化鉄粉体に、カーボンブラックを5wt%添加混合加
湿、これを出口20KWのA r−Nxプラズマジェッ
ト中に毎分1gの割合で、連続的に投入したところ、導
入口に於ける粉体或いはメルトの付着は認められなかっ
た。
Example 2 5 wt% of carbon black was added to iron oxide powder, mixed and humidified, and this was continuously introduced into a 20 KW Ar-Nx plasma jet at a rate of 1 g per minute. No powder or melt adhesion was observed.

実施例3 酸化鉄、酸化コバルト及びリン酸鉄の混合粉体に、カー
ボンブラックを25wt%添加混合し加湿プレードライ
により顆粒状態とした。これを出口17.5KWのA 
r −N sプラズマジェット中に毎分1gの割合で、
連続的に投入したところ、導入口に於ける粉体及びメル
トの付着は認められなかった。
Example 3 25 wt% of carbon black was added to a mixed powder of iron oxide, cobalt oxide, and iron phosphate, and the mixture was made into granules by humidified play drying. This is the exit A of 17.5KW.
r - N s at a rate of 1 g per minute in the plasma jet,
When it was continuously introduced, no powder or melt adhesion was observed at the inlet.

比較例 酸化鉄、酸化コバルト及びリン酸鉄の混合粉体を、スプ
レードライにより顆粒状態とした。これを出口17.5
KWのAr−Nxプラズマジェット中に毎分1gの割合
で、連続的に投入したところ、導入口に於いて、メルト
が付着し、50分後に、導入口はメルトによって塞がれ
た。
Comparative Example A mixed powder of iron oxide, cobalt oxide and iron phosphate was made into granules by spray drying. Exit 17.5
When it was continuously introduced into KW's Ar-Nx plasma jet at a rate of 1 g per minute, melt adhered to the inlet, and after 50 minutes, the inlet was blocked by the melt.

4、    の   tl 日 第1図、第2図及び第3図はプラズマ微粉化装置の異っ
た三つの方式を示す説明図、及び第4図は本発明の方法
を実施する装置の1例を示す断面図である。
Figures 1, 2 and 3 are explanatory diagrams showing three different types of plasma atomization equipment, and Figure 4 shows an example of an equipment for carrying out the method of the present invention. FIG.

15τ14臂15τ14 arm

Claims (4)

【特許請求の範囲】[Claims] (1)昇華性物質を混合或いは表面被覆したプラズマ微
粉化用粉末。
(1) Powder for plasma pulverization mixed with or surface coated with a sublimable substance.
(2)昇華性物質がカーボンである前記第1項記載のプ
ラズマ微粉化用粉末。
(2) The powder for plasma pulverization according to item 1 above, wherein the sublimable substance is carbon.
(3)前記第1項または第2項記載のプラズマ微粉化用
粉末をノズルを通して高温に保持されたプラズマ空間に
投入することを特徴とする粉体供給方法。
(3) A powder supply method, characterized in that the powder for plasma pulverization according to the above item 1 or 2 is introduced into a plasma space maintained at a high temperature through a nozzle.
(4)プラズマ微粉化用粉末は顆粒状に予成形されたも
のである前記第3項記載の粉体供給方法。
(4) The method for supplying powder according to item 3, wherein the powder for plasma pulverization is preformed into granules.
JP1039429A 1989-02-21 1989-02-21 Powder for plasma pulverizing and its supply method Pending JPH02218431A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1039429A JPH02218431A (en) 1989-02-21 1989-02-21 Powder for plasma pulverizing and its supply method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1039429A JPH02218431A (en) 1989-02-21 1989-02-21 Powder for plasma pulverizing and its supply method

Publications (1)

Publication Number Publication Date
JPH02218431A true JPH02218431A (en) 1990-08-31

Family

ID=12552752

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1039429A Pending JPH02218431A (en) 1989-02-21 1989-02-21 Powder for plasma pulverizing and its supply method

Country Status (1)

Country Link
JP (1) JPH02218431A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112658271A (en) * 2020-12-16 2021-04-16 杭州电子科技大学 Efficient composite gas atomization powder preparation device and method
CN112658272A (en) * 2020-12-16 2021-04-16 杭州电子科技大学 High-cooling-gradient plasma arc-gas atomization composite powder making device and method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112658271A (en) * 2020-12-16 2021-04-16 杭州电子科技大学 Efficient composite gas atomization powder preparation device and method
CN112658272A (en) * 2020-12-16 2021-04-16 杭州电子科技大学 High-cooling-gradient plasma arc-gas atomization composite powder making device and method
CN112658271B (en) * 2020-12-16 2023-04-25 杭州电子科技大学 Efficient combined type gas atomization powder preparation device and method
CN112658272B (en) * 2020-12-16 2023-04-28 杭州电子科技大学 High-cooling gradient plasma arc-gas atomization composite powder preparation device and method

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