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EP0009433A1 - Verfahren und Vorrichtung zur Herstellung von Metallpulver aus der Schmelze eines Metalls oder einer Legierung - Google Patents

Verfahren und Vorrichtung zur Herstellung von Metallpulver aus der Schmelze eines Metalls oder einer Legierung Download PDF

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Publication number
EP0009433A1
EP0009433A1 EP79400619A EP79400619A EP0009433A1 EP 0009433 A1 EP0009433 A1 EP 0009433A1 EP 79400619 A EP79400619 A EP 79400619A EP 79400619 A EP79400619 A EP 79400619A EP 0009433 A1 EP0009433 A1 EP 0009433A1
Authority
EP
European Patent Office
Prior art keywords
fluid
enclosure
cryogenic fluid
particles
aforementioned
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
EP79400619A
Other languages
English (en)
French (fr)
Other versions
EP0009433B1 (de
Inventor
Jean Foulard
Gérard Bentz
Jean Galey
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.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
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 Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Priority to AT79400619T priority Critical patent/ATE193T1/de
Publication of EP0009433A1 publication Critical patent/EP0009433A1/de
Application granted granted Critical
Publication of EP0009433B1 publication Critical patent/EP0009433B1/de
Expired legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/12Making metallic powder or suspensions thereof using physical processes starting from gaseous material

Definitions

  • the present invention essentially relates to a process for manufacturing a metallic powder by lowering the temperature of the vapor of a molten metallic material in a closed treatment enclosure, leading to the transformation of said vapor into solid particles.
  • metal material designates either a metal proper, or an alloy of at least two metals.
  • metal powders consist of solid particles either of a single metal such as iron, zinc, magnesium, calcium, cadmium, etc., or of an alloy metallic, for example a magnesium-zinc alloy, or even a metallic compound, for example zinc oxide or magnesium nitride.
  • Such powders find wide applications in various industrial branches, in particular for the manufacture of paints, the treatment of rubbers, in the metallurgical (sintered materials), chemical (catalysts), ceramic, pharmaceutical, etc. industries.
  • a problem currently posed in the powdered metal technique is the obtaining, in industrial quantities, of extremely divided powders having an average particle size of the order of 0.08 microns, consisting of particles having a shape as regular as possible and having a minimum particle size dispersion, that is to say located in a particle size range between 0.02 and 0.13 micron
  • a high vapor pressure causes accelerated evaporation of the metal bath and therefore makes the process applicable on an industrial scale.
  • the use of a cryogenic fluid in the liquid phase causes very rapid cooling, therefore an energetic quenching, of the metallic vapor and allows the direct passage from the gaseous state to the solid state. This change of state and the evacuation of solid particles concomitant with that of the cryogenic fluid results in a constant renewal of the phenomenon of condensation of the vapors above the bath.
  • the solid particles which are thus formed from an incipient suddenly cooled metallic vapor have a regular shape and dimensions not exceeding a few hundred angstroms.
  • the cryogenic fluid is introduced into said enclosure and is continuously removed therefrom.
  • a continuous circulation of cryogenic fluid allows a continuous production of powder at an optimal particle formation regime.
  • the cryogenic fluid is discharged in the liquid phase.
  • the cryogenic fluid is discharged in the gas phase.
  • the cryogenic fluid consists of a chemically inert element or a mixture of chemically inert elements.
  • cryogenic fluid makes it possible to obtain metallic powders formed from chemically pure metals.
  • the cryogenic fluid consists of a chemically active element or a mixture of chemically active elements.
  • cryogenic fluid allows the formation of specific chemical compounds, for example oxides, nitrides or metal hydrides.
  • the cryogenic fluid consists of a mixture of chemically inert elements and chemically active elements.
  • the invention also relates to an installation for implementing the aforementioned method, this installation comprising means for continuously discharging a cryogenic fluid in the liquid phase inside a closed enclosure, means for transferring, out of from said enclosure, a stream of fluid carrying solid metallic particles in suspension, and a closed separation chamber; connected to said transfer means and receiving the above-mentioned fluid stream, said separation chamber being provided with means for collecting the aforementioned solid particles and means for discharging said stream of fluid free of said particles.
  • the installation comprises a melting device 1, for example an induction furnace or a heating crucible, which contains the metallic material M in the liquid state, and is closed by a cover. 2 which thus provides, above the bath, a closed enclosure 3, therefore isolated from the ambient atmosphere in which the metallic vapor is released.
  • a melting device for example an induction furnace or a heating crucible, which contains the metallic material M in the liquid state, and is closed by a cover. 2 which thus provides, above the bath, a closed enclosure 3, therefore isolated from the ambient atmosphere in which the metallic vapor is released.
  • a reactor 4 constituted by a tubular sleeve of section slightly smaller than that of the enclosure, open at its two ends, the lower end plunging slightly into the metal bath M and at the interior of which is concentrated most of the vapor phase of the metallic material.
  • the furnace or the like 1 and the reactor 4 are made of any refractory material, of the type usually used in metallurgy, the furnace being provided with heating means (not shown) which make it possible to maintain the molten metal at the temperature necessary to obtain the desired vapor pressure.
  • a pipe 5 pours out a cryogenic fluid, for example liquefied nitrogen at -196 ° C, stored in a storage device (not shown), in the reactor 4 via a funnel 6 housed in said reactor and opening out in the vicinity of the surface of the metal bath so that said fluid arrives just above the latter.
  • the reactor 4 is connected, by a heat-insulated conduit 7, to a closed separation chamber 8 which communicates with the outside only by a one-way pressure limiting valve 9.
  • In the chamber 8 are housed containers 11 for collecting the particles , these containers being mounted on a rotary support 10 which makes it possible to take them in turn below the duct 7.
  • the reactor 4 is supplied with cryogenic liquid with a sufficient flow rate to permanently maintain, above the metal bath M, a thick layer of cryogenic liquid which exceeds the level of connection of the conduit 7 to the reactor.
  • the solid particles which form in reactor 4 as a result of the condensation of metallic vapors thus remain in suspension in the cryogenic liquid which is transferred, by drawing off by means of the conduit 7, into the separation chamber 8.
  • the cryogenic liquid then passes to the gaseous state, creating and maintaining in the chamber 8 a neutral atmosphere and the solid particles separate by gravity and fall into the containers 11 where they are collected to give a powder.
  • the filling of these containers must be carried out in several stages owing to the reduction in the volume of the powder following the evaporation of the cryogenic liquid.
  • the rotary support allows these successive filling steps to be carried out.
  • the cryogenic liquid charged with particles in suspension and brought into the separation chamber 8 by the conduit 7 is received in separation vessels 12 provided with a filtering wall 13 which retains the particles and lets the liquid pass.
  • the liquid thus filtered is brought, by a first lagged pipe 14, to a recovery tank 15 and from there it is returned, by a recycling pump 16 and a second lagged pipe 17, to reactor 4.
  • the reactor 4 is supplied with cryogenic liquid with an insufficient flow rate to maintain a liquid layer above the metal bath.
  • the vapor is condensed at the point of impact of the cryogenic liquid with the surface of the bath and the metallic particles are entrained out of the enclosure 2 by the fluid in the vapor phase. The recovery of these particles can be done by gravity.
  • the metallic material can consist of a metal (Fe, Cu, Zn, Mg, Al, etc.) or an alloy (brass, bronze, etc.).
  • the choice of the composition of this alloy that is to say the choice of constituents (which have different melting temperatures), and the proportions of these constituents, make it possible to adjust the kinetics of evaporation.
  • an alloy having a high proportion of a metal with a low melting point, such as Mg makes it possible to obtain a metallic vapor formed almost exclusively of said metal with low melting point.
  • the composition of this alloy can be determined so as to obtain, for a chosen temperature of the metal bath, a high vapor pressure of the zinc. The solid particles obtained are then formed exclusively of zinc.
  • the cryogenic fluid can consist of inert liquefied elements (N2, Ar, He, etc ...) or active (02, H2, NH3 etc 7) by liquefied compounds such as hydrocarbons or a mixture formed of inert liquefied elements and active liquefied elements or else inert liquefied elements and liquefied compounds.
  • inert liquefied elements N2, Ar, He, etc
  • active 02, H2, NH3 etc
  • the choice of the percentage of the active element or of the compound makes it possible to adjust the kinetics of the reaction of the combination of the metal with the metalloid which constitutes said element or resulting from the decomposition of said compound.
  • the powder obtained after separation of the cryogenic fluid consists of zinc particles of dimension between 0.03 and 0.10 micron, and has a specific surface (BET) of 40 m2 per gram.
  • the heating of the melting device 1 could be obtained for example by induction, or by means of radiation, for example concentrated solar radiation by means of an optical system or radiation produced by a laser, or also by means of an arc or an electrical resistance so as to obtain a melting and a point or overall overheating of the material to be vaporized.

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Powder Metallurgy (AREA)
EP79400619A 1978-09-18 1979-09-06 Verfahren und Vorrichtung zur Herstellung von Metallpulver aus der Schmelze eines Metalls oder einer Legierung Expired EP0009433B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT79400619T ATE193T1 (de) 1978-09-18 1979-09-06 Verfahren und vorrichtung zur herstellung von metallpulver aus der schmelze eines metalls oder einer legierung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7826648 1978-09-18
FR7826648A FR2435988A1 (fr) 1978-09-18 1978-09-18 Procede et installation de fabrication de poudre metallique a partir d'un metal ou alliage en fusion

Publications (2)

Publication Number Publication Date
EP0009433A1 true EP0009433A1 (de) 1980-04-02
EP0009433B1 EP0009433B1 (de) 1981-09-09

Family

ID=9212724

Family Applications (1)

Application Number Title Priority Date Filing Date
EP79400619A Expired EP0009433B1 (de) 1978-09-18 1979-09-06 Verfahren und Vorrichtung zur Herstellung von Metallpulver aus der Schmelze eines Metalls oder einer Legierung

Country Status (8)

Country Link
US (1) US4309214A (de)
EP (1) EP0009433B1 (de)
JP (1) JPS5541999A (de)
AT (1) ATE193T1 (de)
CA (1) CA1139970A (de)
DE (1) DE2960783D1 (de)
ES (1) ES8100937A1 (de)
FR (1) FR2435988A1 (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2545394A1 (fr) * 1983-05-04 1984-11-09 Air Liquide Procede de fabrication de poudres metalliques a partir d'un materiau metallique en fusion
FR2545393A1 (fr) * 1983-05-04 1984-11-09 Air Liquide Procede de production de particules solides metalliques a partir d'un bain metallique
FR2660584A1 (fr) * 1990-04-10 1991-10-11 Rdm Ste Civile Procede et dispositif de compactage de poudres.

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2626797B1 (fr) * 1988-02-04 1991-04-19 Commissariat Energie Atomique Procede et installation pour l'amelioration de la qualite d'une poudre metallique ou ceramique
US5922403A (en) * 1996-03-12 1999-07-13 Tecle; Berhan Method for isolating ultrafine and fine particles
US6228187B1 (en) 1998-08-19 2001-05-08 Air Liquide America Corp. Apparatus and methods for generating an artificial atmosphere for the heat treating of materials
US6468497B1 (en) * 2000-11-09 2002-10-22 Cyprus Amax Minerals Company Method for producing nano-particles of molybdenum oxide
US7572430B2 (en) * 2000-11-09 2009-08-11 Cyprus Amax Minerals Company Method for producing nano-particles
US6491863B2 (en) 2000-12-12 2002-12-10 L'air Liquide-Societe' Anonyme A' Directoire Et Conseil De Surveillance Pour L'etude Et L'exploitation Des Procedes George Claude Method and apparatus for efficient utilization of a cryogen for inert cover in metals melting furnaces
US7384448B2 (en) * 2004-02-16 2008-06-10 Climax Engineered Materials, Llc Method and apparatus for producing nano-particles of silver
CN103990807B (zh) * 2014-04-21 2017-04-12 江苏科创金属新材料有限公司 一种用于锌粉制备装置的节能设备

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1495961A (en) * 1923-02-15 1924-05-27 Int Precipitation Co Process for the production of metal powder or dust
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
US2934331A (en) * 1955-12-22 1960-04-26 Thomas J Walsh Apparatus for making a metal slurry product
FR2299932A1 (fr) * 1975-02-07 1976-09-03 Anvar Lithium tres finement divise et son procede de fabrication
FR2375940A1 (fr) * 1976-12-28 1978-07-28 Zaklady Bieli Cynkowej Olawa Procede de condensation de vapeurs de zinc en une poudre de zinc a grains fins et dispositif pour la mise en oeuvre de ce procede

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3042511A (en) * 1959-02-09 1962-07-03 Dow Chemical Co Apparatus for condensation of a metal vapor
US3165396A (en) * 1961-01-09 1965-01-12 Nat Res Corp Deflection of metal vapor away from the vertical in a thermal evaporation process
US3151971A (en) * 1961-03-03 1964-10-06 Nat Res Corp Vacuum vapor condensation process for producing fine metal powders
JPS482666U (de) * 1971-05-31 1973-01-12
US3856513A (en) * 1972-12-26 1974-12-24 Allied Chem Novel amorphous metals and amorphous metal articles
US4124377A (en) * 1977-07-20 1978-11-07 Rutger Larson Konsult Ab Method and apparatus for producing atomized metal powder
US4169730A (en) * 1978-01-24 1979-10-02 United States Bronze Powders, Inc. Composition for atomized alloy bronze powders

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1495961A (en) * 1923-02-15 1924-05-27 Int Precipitation Co Process for the production of metal powder or dust
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
US2934331A (en) * 1955-12-22 1960-04-26 Thomas J Walsh Apparatus for making a metal slurry product
FR2299932A1 (fr) * 1975-02-07 1976-09-03 Anvar Lithium tres finement divise et son procede de fabrication
FR2375940A1 (fr) * 1976-12-28 1978-07-28 Zaklady Bieli Cynkowej Olawa Procede de condensation de vapeurs de zinc en une poudre de zinc a grains fins et dispositif pour la mise en oeuvre de ce procede

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2545394A1 (fr) * 1983-05-04 1984-11-09 Air Liquide Procede de fabrication de poudres metalliques a partir d'un materiau metallique en fusion
FR2545393A1 (fr) * 1983-05-04 1984-11-09 Air Liquide Procede de production de particules solides metalliques a partir d'un bain metallique
EP0125161A1 (de) * 1983-05-04 1984-11-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Verfahren zur Herstellung von Metallpulver aus einer Metallschmelze
EP0125173A1 (de) * 1983-05-04 1984-11-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Verfahren zur Herstellung erstarrter Metallkörper aus der Schmelze eines Metalls
FR2660584A1 (fr) * 1990-04-10 1991-10-11 Rdm Ste Civile Procede et dispositif de compactage de poudres.

Also Published As

Publication number Publication date
ES483267A0 (es) 1980-12-01
JPS5620327B2 (de) 1981-05-13
US4309214A (en) 1982-01-05
JPS5541999A (en) 1980-03-25
ATE193T1 (de) 1981-09-15
FR2435988A1 (fr) 1980-04-11
EP0009433B1 (de) 1981-09-09
DE2960783D1 (en) 1981-11-26
ES8100937A1 (es) 1980-12-01
CA1139970A (fr) 1983-01-25
FR2435988B1 (de) 1981-03-20

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