EP0524887A1 - Verfahren und Vorrichtung zur Herstellung von Pulver, insbesondere Metallpulver durch Atomisierung - Google Patents

Verfahren und Vorrichtung zur Herstellung von Pulver, insbesondere Metallpulver durch Atomisierung Download PDF

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Publication number
EP0524887A1
EP0524887A1 EP92402141A EP92402141A EP0524887A1 EP 0524887 A1 EP0524887 A1 EP 0524887A1 EP 92402141 A EP92402141 A EP 92402141A EP 92402141 A EP92402141 A EP 92402141A EP 0524887 A1 EP0524887 A1 EP 0524887A1
Authority
EP
European Patent Office
Prior art keywords
head
atomized
powders
atomization
plasma
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.)
Granted
Application number
EP92402141A
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English (en)
French (fr)
Other versions
EP0524887B1 (de
Inventor
André Accary
Jean L. Coutiere
André Lacour
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.)
Aubert and Duval SA
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Aubert and Duval SA
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 Aubert and Duval SA filed Critical Aubert and Duval SA
Publication of EP0524887A1 publication Critical patent/EP0524887A1/de
Application granted granted Critical
Publication of EP0524887B1 publication Critical patent/EP0524887B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086—Cooling after atomisation
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0896—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid particle transport, separation: process and apparatus
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a method and a device for producing powders and in particular metal powders by atomization.
  • the present invention aims to overcome these technical problems and in particular to be able to disperse a sufficiently hot metallic liquid, without there being any chemical interaction between the dispersing means and the liquid, to create a quenching zone eliminating any possibility of pollution of the atomized metal, and to provide a "cold chain” allowing the powders obtained to be used without polluting them before manufacturing the final solid product, after compaction and sintering.
  • a device for the production of powders and in particular of metallic powders by atomization comprising means for melting the material to be atomized, an atomization enclosure in which is arranged a dispersion head rotating at high speed for diffusing the molten material in atomized form, means for cooling the atomized material and the head and means for collecting the cooled powder material thus obtained, characterized in that said melting means comprise at least one vertical oven inductive plasma producing a gas envelope plasmagens containing the upper face of the dispersion head and said cooling means comprise a first series of members for distributing a cooling fluid disposed in the upper part of the atomization enclosure to create a cold zone at the periphery of the envelope and a second series of bodies for circulating a cooling fluid disposed in the lower part of the enclosure to create a cold zone on the underside of the head.
  • said first series of members for distributing a cooling fluid consists of a ramp of nozzles producing jets of tangential fluid at the surface of said envelope and of nozzles producing a tangential washing at the compound.
  • said envelope of plasma gases consists of a cylindrical tube whose vertical axis is parallel to the vertical axis of the rotary head, and preferably the axis of the cylindrical tube is coincident with the 'axis of the head.
  • said vertical inductive plasma furnace is arranged above the upper face of the rotary head.
  • Another object of the invention is a method for manufacturing powders and in particular metallic powders by atomization, comprising the continuous melting of the material to be atomized flowing vertically and coaxially above a dispersing head rotating at great speed. speed intended to diffuse the molten material in atomized form, in an envelope of plasma-producing gases, then quenching of the atomized material and collection of the cooled powder material thus obtained, characterized in that the material is atomized by fusion by dispersing it by friction on the upper face of the rotary head and quenching by passing said atomized material through a cooling vortex situated at the periphery of the envelope of plasma gas.
  • Yet another object of the invention lies in the ultra pure metallic powders obtained by the above process.
  • the device of the invention can absorb a large heat flow produced by a plasma torch and onto which the liquid material falls.
  • the atomized material then enters a quenching zone at the periphery of the head formed by a cylindrical tube of plasma gas moving parallel to the vertical axis of the head and enveloped in cold fluid.
  • the powders obtained are recovered in a collection zone comprising at least one chamber containing a neutral gas in the gaseous, liquid or solid state, before their use in formed or shaped products.
  • the powders obtained by the process of the invention with very rapid cooling are ultra pure and have a very fine particle size.
  • Figure 1 is a schematic representation of the atomizing device of the present invention.
  • FIG. 2 is an enlarged view of the central part of the device in FIG. 1.
  • FIG. 3 represents the quenching zone with the members for distributing the cooling fluid.
  • FIGS. 4a and 4b schematically represent embodiments of the means for melting and supplying molten metal to the atomization enclosure.
  • the material to be melted and to be atomized is introduced by supply means A into the apparatus, for example in the initial form of a cylindrical bar 1 whose diameter is related to the power of the melting means, notably consisting of a plasma oven B.
  • the material to be atomized is initially in the form of pieces of various sizes, powders, shots or else may be directly brought to the molten state in the device.
  • the bar 1 is placed vertically in the axis of the oven B, the valve V1 then being closed, maintaining the oven B and the enclosure C under a neutral atmosphere. After vacuuming and purging the bar supply chamber several times, valve V1 is open. The bar 1 is then lowered with a hydropneumatic or electromechanical cylinder regulated at the speed which corresponds to the desired flow rate. It is preheated in the preheating furnace 3 by the induced currents with one or more inducing turns 5 at a frequency between 10 and 30 kHz, depending on its diameter.
  • the bar then enters the inductive plasma oven 4.
  • the plasma is ignited by creating an electric arc between the bar brought to high voltage and a retractable mobile electrode 8 located at ground.
  • a retractable mobile electrode 8 located at ground.
  • the vein or the liquid drops of molten materials pass more or less long over the hottest part of the plasma to, on the one hand, reach overheating and , on the other hand, pass through the most reactive area of the oven.
  • a cold cage 7 is used to protect the oven enclosure, and polished to increase the thermal efficiency of the plasma.
  • the bar 1 is thus heated at its periphery by direct induction of the HF fields - skin effect -, and by thermal conduction and convection of the plasma gases. It melts in a cone, point directed downwards, with an angle whose opening depends on the nature of the plasma gases. There is thus a casting which is, depending on the power of the furnace and the penetration of the bar into the plasma, continuous or not and perfectly axial. As for the diameter of the liquid stream or of the drops, it depends on the flow of liquid and the opening of the cone.
  • the material to be atomized is first received in fusion in a cold crucible (as in French patent 2 697 050) from which it flows by gravity passing through an electromagnetic and / or composite nozzle before enter the atomization enclosure as shown in Figures 4a and 4b.
  • the electromagnetic and / or composite nozzle constitutes a means of feeding and regulating the flow of molten metal and optionally makes it possible to maintain the metal in the desired thermal state.
  • the device shown in FIGS. 4a and 4b comprises means B for melting the solid material (metal) M consisting for example of a plasma torch.
  • the molten material then flows into a cold crucible 100 to form a bath of molten metal.
  • the heat losses on the surface of the bath are possibly compensated by additional heating means B ′.
  • the material in the molten state then flows vertically through the bottom of the crucible through an electromagnetic nozzle 101 (FIG. 4a) or composite 102 (FIG. 4b).
  • French Patent No. 87 00 866 already describes a composite nozzle 102 used for controlling a flow of liquid metal operating for example with a coil 102b at 450 kHz.
  • the electromagnetic nozzle 101 comprises a peripheral coil 101b inducing a high frequency field so as to create a constriction of the liquid stream thus causing a variation in the flow of molten material.
  • the molten material then enters the atomization enclosure to come into contact with the dispersion head 9.
  • the molten material flows into the atomization enclosure C at the center of the upper face of a dispersion or atomization head driven in rotation by the spindle 10 at a speed of up to '' at 125,000 rpm.
  • the shape of the dispersion head 9 is determined according to the optimal thermal mapping and advantageously, it is produced in the form of a cylinder whose dimensions are determined by the nature of the constituent material and the temperature sought on the upper side coming into contact with the molten material according to the particle size sought for the powders.
  • the upper face of the head is preferably located in a substantially horizontal plane and is crossed vertically by a heat flow generated by the plasma gases heated by induction by the inductor 6.
  • the plasma zone consists of an envelope of plasma gas in cylindrical tube shape whose vertical axis is parallel, being close to or coincident with the vertical axis of said head 9.
  • the underside of the cylindrical head 9 and the spindle 10 are cooled by axial circulation 11 of a fluid cooling which can be either water for the most important thermal fluxes, or a gas or a liquid gas such as argon or helium for example, in the case where a surface temperature of the head is desired more high.
  • the atomizing cylindrical head 9 is either made of copper, or of tungsten, or of a refractory alloy or not depending on the surface temperature which must be reached.
  • the underside of the cylinder constituting said head 9 is advantageously provided with a hemispherical cavity licked by the cooling fluid 11 circulating axially.
  • the cooling of the underside of the head 9 creates a temperature gradient in the mass thereof which is included for copper between 60 and 180 ° C / cm and between 200 and 500 ° C / cm for tungsten.
  • the supply of heat by the plasma to the liquid metal up to the very surface of the head and the thermal resistance between the liquid material and the said head mean that the dispersed material remains liquid (despite the heat extracted through the head)
  • atomization means "erosion” consisting in diffusing and dispersing the liquid by friction and thus avoiding its "wetting" with the upper side of the head.
  • the liquid particles pass directly from the plasma zone 12 which envelops the head, to a quench zone 13 consisting of a cooling medium, two-phase or not, forming a vortex around the plasma.
  • FIG. 3 there is a ramp of eighteen nozzles 15 distributing a total flow of liquid argon sufficient to obtain complete cooling of the powders.
  • the nozzle ejection axis X 15 is inclined relative to the plane of the upper face of the head 9 with a jet width determined so as to obtain rapid cooling and a rotation effect of opposite direction (counter-rotating) to that of the head 9 in order to brake the movement of powders.
  • the nozzle ejection orifice 15 is located above the powder ejection triangle.
  • the refrigerant vortex 13 thus formed entrains the liquid and then solid particles in spiral trajectories, thus avoiding, on the one hand, direct impacts with the walls of the enclosure C, on the other hand, gas turbulence towards the top of the device, turbulence which may disturb the plasma and atomization.
  • the nozzles 16 oriented towards the walls of the enclosure project onto them a mist of argon which flows along the walls, thus driving the powders down and thus ensuring a tangential washing to the enclosure.
  • the mixture of liquid and powder is deposited at the bottom of enclosure C.
  • the powder obtained is therefore deposited at the bottom of the enclosure C and is recovered in the container 17.
  • the cooling and the collection of the powder are thus carried out using a neutral gas in the gaseous, liquid or solidified state after immersion of the collected powder in the liquid phase.
  • the invention also provides the possibility of combining in the same unit several atomization devices arranged around the energy sources: medium frequency preheating generator (MF) and plasma torch generator (HF).
  • MF medium frequency preheating generator
  • HF plasma torch generator
  • the operation is semi-continuous, in sequence of 2 bars.
  • D denotes a flow, P a pressure, T a temperature, V a valve, B a flange.
  • the method and the device of the invention make it possible to manufacture powders from various families of materials and in particular superalloys based on nickel, titanium and titanium alloys, aluminum, Niobium alloys, etc.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
EP92402141A 1991-07-25 1992-07-24 Verfahren und Vorrichtung zur Herstellung von Pulver, insbesondere Metallpulver durch Atomisierung Expired - Lifetime EP0524887B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9109462A FR2679473B1 (fr) 1991-07-25 1991-07-25 Procede et dispositif de production de poudres et notamment de poudres metalliques par atomisation.
FR9109462 1991-07-25

Publications (2)

Publication Number Publication Date
EP0524887A1 true EP0524887A1 (de) 1993-01-27
EP0524887B1 EP0524887B1 (de) 1997-04-09

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EP92402141A Expired - Lifetime EP0524887B1 (de) 1991-07-25 1992-07-24 Verfahren und Vorrichtung zur Herstellung von Pulver, insbesondere Metallpulver durch Atomisierung

Country Status (5)

Country Link
US (2) US5340377A (de)
EP (1) EP0524887B1 (de)
CA (1) CA2074684A1 (de)
DE (1) DE69218846T2 (de)
FR (1) FR2679473B1 (de)

Cited By (1)

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CN106216704A (zh) * 2016-10-10 2016-12-14 江西悦安超细金属有限公司 一种进料装置以及等离子组合离心雾化制粉装置

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GB2354256B (en) * 1999-09-15 2001-11-07 Korea Atomic Energy Res Uranium high-density dispersion fuel
JP2001254103A (ja) * 2000-03-13 2001-09-18 Sanei Kasei Kk ナノコンポジット構造を有する金属粒子及び自己組織化によるその製造方法
US20030156964A1 (en) * 2000-06-26 2003-08-21 Masami Kikuchi Method and apparatus for producing magnetic rare earth alloy powder, method for producing bonded magnet, method for producing rare earth sintering magnet, and method and apparatus for improving purity of inert gas
US7913884B2 (en) * 2005-09-01 2011-03-29 Ati Properties, Inc. Methods and apparatus for processing molten materials
CN100413617C (zh) * 2006-08-18 2008-08-27 陕西科技大学 一种制备金属超微粉体的装置及其方法
US8268035B2 (en) * 2008-12-23 2012-09-18 United Technologies Corporation Process for producing refractory metal alloy powders
WO2011054113A1 (en) * 2009-11-05 2011-05-12 Ap&C Advanced Powders & Coatings Inc. Methods and apparatuses for preparing spheroidal powders
CN101906516B (zh) * 2010-09-02 2012-01-11 唐山市长智农工具设计制造有限公司 金属制件淬火介质循环利用装置
PL3730208T3 (pl) 2014-03-11 2024-06-24 Tekna Plasma Systems Inc. Proces do wytwarzania cząstek proszku przez atomizację materiału wsadowego w postaci elementu podłużnego
WO2016191854A1 (en) * 2015-06-05 2016-12-08 Pyrogenesis Canada Inc. Plasma apparatus for the production of high quality spherical powders at high capacity
US11198179B2 (en) * 2015-07-17 2021-12-14 Ap&C Advanced Powders & Coating Inc. Plasma atomization metal powder manufacturing processes and system therefor
CA3020720C (en) 2016-04-11 2020-12-01 Ap&C Advanced Powders & Coatings Inc. Reactive metal powders in-flight heat treatment processes
US11110540B2 (en) * 2016-05-02 2021-09-07 Electronics And Telecommunications Research Institute Extruder for metal material and 3D printer using the same
EP3504020B1 (de) 2016-08-24 2023-04-19 5n Plus Inc. Pulverzerstäubungsherstellungsverfahren mit metallen oder legierungen mit niedrigem schmelzpunkt
TWI618589B (zh) * 2016-12-23 2018-03-21 悅城科技股份有限公司 製造材料粉末的方法及裝置
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JP7012350B2 (ja) * 2017-12-18 2022-01-28 株式会社大阪真空機器製作所 遠心アトマイザ用回転ディスク装置、遠心アトマイザ、および、金属粉末の製造方法
CN108097977B (zh) * 2018-02-01 2021-02-12 广东美瑞克微金属磁电科技有限公司 一种铁硅铝软磁合金粉末的等离子雾化制取方法
EP3752304B1 (de) 2018-02-15 2023-10-18 5n Plus Inc. Herstellungsverfahren durch verdüsung von metall- oder legierungspulvern mit niedrigem schmelzpunkt
CN109128206B (zh) * 2018-09-25 2020-11-24 中国人民解放军陆军装甲兵学院 一种逐液滴离心雾化法高效制备超细球形金属粉末的装置及方法
CN111014700A (zh) * 2019-12-11 2020-04-17 湖南天际智慧材料科技有限公司 一种真空无坩埚熔炼等离子体制备高纯纳米材料的装置
CN110883338A (zh) * 2019-12-11 2020-03-17 湖南天际智慧材料科技有限公司 一种射频等离子体制备微纳米粉末材料的装置
CN111331147A (zh) * 2020-03-18 2020-06-26 甘肃省机械科学研究院有限责任公司 一种制备AlSi9Mg超细粉的方法
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FR2629573A1 (fr) * 1988-04-05 1989-10-06 Aubert & Duval Acieries Tete de fusion continue pour metaux ou alliages

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FR2276121A1 (fr) * 1974-06-28 1976-01-23 United Kingdom Government Appareil et procede de production d'un objet metallique par atomisation centrifuge d'un metal fondu
WO1987005548A1 (en) * 1986-03-13 1987-09-24 Cheney Richard F Powder atomizing methods and apparatus
FR2595595A1 (fr) * 1986-03-17 1987-09-18 Aubert & Duval Acieries Procede de refroidissement et de collecte de poudres metalliques produites par atomisation de metal liquide
FR2629573A1 (fr) * 1988-04-05 1989-10-06 Aubert & Duval Acieries Tete de fusion continue pour metaux ou alliages

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106216704A (zh) * 2016-10-10 2016-12-14 江西悦安超细金属有限公司 一种进料装置以及等离子组合离心雾化制粉装置
CN106216704B (zh) * 2016-10-10 2018-05-04 江西悦安超细金属有限公司 一种进料装置以及等离子组合离心雾化制粉装置

Also Published As

Publication number Publication date
EP0524887B1 (de) 1997-04-09
CA2074684A1 (en) 1993-01-26
FR2679473B1 (fr) 1994-01-21
FR2679473A1 (fr) 1993-01-29
US5529292A (en) 1996-06-25
DE69218846D1 (de) 1997-05-15
US5340377A (en) 1994-08-23
DE69218846T2 (de) 1997-10-23

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