EP0125161B1 - Verfahren zur Herstellung von Metallpulver aus einer Metallschmelze - Google Patents

Verfahren zur Herstellung von Metallpulver aus einer Metallschmelze Download PDF

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Publication number
EP0125161B1
EP0125161B1 EP84400733A EP84400733A EP0125161B1 EP 0125161 B1 EP0125161 B1 EP 0125161B1 EP 84400733 A EP84400733 A EP 84400733A EP 84400733 A EP84400733 A EP 84400733A EP 0125161 B1 EP0125161 B1 EP 0125161B1
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EP
European Patent Office
Prior art keywords
process according
liquid
metallic material
fluid
cryogenic fluid
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
Application number
EP84400733A
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English (en)
French (fr)
Other versions
EP0125161A1 (de
Inventor
Albert-Gilbert Goursat
Gilles Vernet
Jean-Francis Rimbert
Jean Foulard
Thierry Darle
Jean Bigot
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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 LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority to AT84400733T priority Critical patent/ATE27780T1/de
Publication of EP0125161A1 publication Critical patent/EP0125161A1/de
Application granted granted Critical
Publication of EP0125161B1 publication Critical patent/EP0125161B1/de
Expired 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
    • B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material

Definitions

  • the present invention relates to a process for the manufacture of metallic powders, in particular ultra-fine powders, from a molten metallic material.
  • metal powders powders constituted by solid particles either of a single metal such as iron, zinc, magnesium, etc., or of a metallic alloy for example a magnesium-zinc alloy , or even a metallic compound, for example zinc oxide, magnesium nitride, etc.
  • metal material is meant either a pure or substantially pure metal, or an alloy of two or more metals.
  • a cryogenic fluid in the liquid phase it consists in pouring onto the metal bath, brought to a temperature such that its vapor pressure is at least 1 mm of mercury, a cryogenic fluid in the liquid phase, to evacuate outside the enclosure the cryogenic fluid which contains, in suspension, the solid particles formed, to separate the latter from said fluid and to collect them to obtain the abovementioned powder.
  • a cryogenic fluid in the liquid phase allows very rapid cooling of the metallic vapors coming from the bath and their direct passage from the gaseous state to the solid state.
  • the process described in EP-A-0 009 433, has the advantage of making it possible to obtain, either from a pure metal, or from alloys, solid particles having a regular shape and a small particle size. (from 100 A to 2000 A).
  • this method has the drawback of being usable only for obtaining metal powders whose vapor pressure corresponds to medium temperatures.
  • volatile metals such as lead, zinc, magnesium
  • less volatile metals such as iron, nickel, cobalt
  • materials generally constituting the metal crucibles n ' do not have sufficient mechanical strength to withstand temperatures above 2000 ° C.
  • the subject of the invention is precisely a process which overcomes the drawbacks mentioned above and makes it possible to obtain powders of elements whose vapor pressure corresponds to very high temperatures.
  • the method for manufacturing metallic powder according to the invention consists in bringing into contact with a cryogenic fluid in the liquid phase, in a closed treatment enclosure, a metallic material, heated to a temperature such that its vapor pressure is at least minus 1 mm of mercury, to evacuate from the enclosure the cryogenic fluid which contains, in suspension, the solid particles formed, to separate the latter from said fluid, and to collect them to obtain the aforementioned metallic powder. It is characterized in that, by induction of high frequency current, said metallic material is heated and levitated in the cryogenic liquid.
  • the principle of levitation fusion is to place a metal part in an inductor of suitable shape traversed by high frequency currents.
  • the interaction between the magnetic field and the currents induced in the metal part allows this one to float, to levitate, without any contact with a material support.
  • the metallic material is heated by levitation fusion makes it possible to be able to bring it without problem to temperatures greater than 2000 ° C. and to obtain, thanks to the bringing into contact with the liquid cryogenic, solid particles from metals that are only volatile at very high temperatures.
  • the metallic material in fusion when, according to the invention, the metallic material in fusion is maintained in the cryogenic liquid, the latter, separated from said material by a gaseous layer due to the phenomenon of calefaction, heats up in the vicinity of the metallic material in fusion; the cold vapors thus formed condense the metallic vapors coming from the material and immediately transform them into solid particles which are entrained upwards by the remaining vapors of the cryogenic liquid. This results in a shift in the liquid metal - metal vapor balance which causes the suction of other metal vapors which are immediately condensed in the form of solid particles and carried upwards.
  • the treatment enclosure is maintained either at atmospheric pressure or at a pressure higher than atmospheric pressure.
  • the fact of working at a pressure higher than atmospheric pressure makes it possible to increase the speed of production of metallic powders.
  • the gaseous layer, surrounding and separating the molten metallic material from the cryogenic liquid is less thick: thus, the cold vapors of the cryogenic liquid cool the metallic vapors more quickly and, as a result, the phenomenon of aspira tion described above is faster.
  • the metal is heated in levitation, it is subjected to stirring caused by the circulation currents due to the interaction between magnetic field and currents induced within said metal; this increases and renews the heat exchanges with the cryogenic liquid.
  • the cryogenic fluid used is a chemically active fluid chosen as a function of the desired metallic compound.
  • the installation shown in the attached figure includes a quartz treatment enclosure 1, closed, therefore isolated from the ambient atmosphere, provided with a pipe 2 for supplying cryogenic liquid and provided at its upper part with a pipe d 'evacuation 3 which opens into a recovery container 4.
  • a levitation melting device of which only the turns 5 of the inductor are shown, is placed in the vicinity of the lower part of the enclosure 3; the inductor used is an inductor of known type, consisting of a conical winding of a few turns (copper tubes cooled by a stream of water) surmounted by one or two turns developing in opposite directions.
  • Liquid argon is introduced via line 2 at a rate sufficient for the liquid argon bath 6 to permanently fill approximately half of the enclosure 1 so that the metallic material 7, heated in levitation, is constantly immersed in said bath 6.
  • the level of the liquid argon bath 6 is controlled by a level detector 8.
  • the container 4 contains an organic liquid 9, chemically inert with respect to the metal constituting the particles, such as a hydrocarbon, for example hexane, and the pipe 3 plunges into said liquid 9. There is bubbling of the argon gas containing the particles in hexane; the argon gas is evacuated through a pipe 10 opening into the upper part of the container 4 and the metallic particles remain in suspension in hexane which then plays the role of conditioning liquid.
  • an organic liquid 9 chemically inert with respect to the metal constituting the particles, such as a hydrocarbon, for example hexane
  • a strip 11 comprising heating resistors supplied by an electric generator 12, is wound on a part of the pipe 3.
  • an alumina crucible 13 is placed in the bottom of the latter.
  • the invention advantageously applies to the manufacture of ultra-fine metal powders from low volatile metals, these powders can be made up either of a single metal, or of a metal alloy, or of a metal compound; it can also be applied to the selective elimination of one or more metals in powder form from a mixture of molten metals.

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

Claims (12)

1. Verfahren zur Herstellung eines metallischen Pulvers oder einer metallischen Verbindung durch Verringern der Temperatur des Dampfes eines metallischen Materiales in Schmelze mit Umwandlung dieses Dampfes in feste Teilchen, wobei man mit einem Tiefsttemperaturfluid in flüssiger Phase in einem geschlossenen Behandlungsbehälter ein metallisches Material in Berührung bringt, welches auf eine Temperatur derart erwärmt ist, daß seine Dampfspannung mindestens 1 mm Quecksilber beträgt, man aus dem Behälter das Tiefsttemperaturfluid, welches die gebildeten festen Teilchen in Suspension enthält, abzieht, letztere aus dem Fluid separiert und sie sammelt, um das genannte metallische Pulver zu erhalten, dadurch gekennzeichnet, daß man durch Induktionsstrom hoher Frequenz das metallische Material erwärmt und es in der Tiefsttemperaturflüssigkeit in Schwebe hält.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet. daß man das Tiefsttemperaturfluid einführt und es in kontinuierlicher Weise aus dem Behälter entleert.
3. Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß man das Tiefsttemperaturfluid aus dem Behälter in gasförmiger Phase entleert.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß man die festen Teilchen von dem Tiefsttemperaturfluid separiert und sie durch Durchblasen in einer Flüssigkeit sammelt.
5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die Durchblasflüssigkeit eine gegenüber dem Metall, welches die Teilchen bildet, chemisch inerte Flüssigkeit ist.
6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß die Durchblasflüssigkeit eine organische Flüssigkeit ist, wie z. B. Hexan.
7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das metallische Material ein reines oder im wesentlichen reines Metall ist.
8. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das metallische Material eine Legierung aus zwei oder mehreren Metallen ist.
9. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das Tiefsttemperaturfluid ein gegenüber dem metallischen Material chemisch inertes Fluid ist, wie z. B. Stickstoff, Argon, Helium.
10. Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß das Tiefsttemperaturfluid ein chemisch aktives Fluid ist, welches in Funktion von der gewünschten metallischen Verbindung ausgewählt ist.
11. Verfahren nach einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, daß man den Behandlungsbehälter auf einem Druck hält, der gleich dem Atmosphärendruck ist.
12. Verfahren nach einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, daß man den Behandlungsbehälter auf einem Druck über dem Atmosphärendruck hält.
EP84400733A 1983-05-04 1984-04-12 Verfahren zur Herstellung von Metallpulver aus einer Metallschmelze Expired EP0125161B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84400733T ATE27780T1 (de) 1983-05-04 1984-04-12 Verfahren zur herstellung von metallpulver aus einer metallschmelze.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8307414A FR2545394B1 (fr) 1983-05-04 1983-05-04 Procede de fabrication de poudres metalliques a partir d'un materiau metallique en fusion
FR8307414 1984-05-04

Publications (2)

Publication Number Publication Date
EP0125161A1 EP0125161A1 (de) 1984-11-14
EP0125161B1 true EP0125161B1 (de) 1987-06-16

Family

ID=9288573

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84400733A Expired EP0125161B1 (de) 1983-05-04 1984-04-12 Verfahren zur Herstellung von Metallpulver aus einer Metallschmelze

Country Status (6)

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US (1) US4521244A (de)
EP (1) EP0125161B1 (de)
JP (1) JPS59208003A (de)
AT (1) ATE27780T1 (de)
DE (1) DE3464214D1 (de)
FR (1) FR2545394B1 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5922403A (en) 1996-03-12 1999-07-13 Tecle; Berhan Method for isolating ultrafine and fine particles
CN103508489B (zh) * 2012-06-21 2016-08-10 深圳富泰宏精密工业有限公司 纳米二氧化钛制备装置及应用该装置制备纳米二氧化钛的方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE903777C (de) * 1944-07-01 1954-02-11 Eisenwerke Muelheim Meiderich Verfahren zum Herstellen von Metallpulver, wie insbesondere von Stahl- oder Eisenpulver, mittels eines Granulationsverfahrens
FR2299932A1 (fr) * 1975-02-07 1976-09-03 Anvar Lithium tres finement divise et son procede de fabrication
US4124377A (en) * 1977-07-20 1978-11-07 Rutger Larson Konsult Ab Method and apparatus for producing atomized metal powder
FR2435988A1 (fr) * 1978-09-18 1980-04-11 Air Liquide Procede et installation de fabrication de poudre metallique a partir d'un metal ou alliage en fusion

Also Published As

Publication number Publication date
FR2545394B1 (fr) 1985-09-06
ATE27780T1 (de) 1987-07-15
JPS59208003A (ja) 1984-11-26
EP0125161A1 (de) 1984-11-14
DE3464214D1 (en) 1987-07-23
FR2545394A1 (fr) 1984-11-09
US4521244A (en) 1985-06-04

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