EP0009433B1 - Procédé et installation de fabrication de poudre métallique à partir d'un métal ou alliage en fusion - Google Patents

Procédé et installation de fabrication de poudre métallique à partir d'un métal ou alliage en fusion Download PDF

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Publication number
EP0009433B1
EP0009433B1 EP79400619A EP79400619A EP0009433B1 EP 0009433 B1 EP0009433 B1 EP 0009433B1 EP 79400619 A EP79400619 A EP 79400619A EP 79400619 A EP79400619 A EP 79400619A EP 0009433 B1 EP0009433 B1 EP 0009433B1
Authority
EP
European Patent Office
Prior art keywords
liquified gas
particles
chamber
constituted
alloy
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
EP79400619A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0009433A1 (fr
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.)
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 AT79400619T priority Critical patent/ATE193T1/de
Publication of EP0009433A1 publication Critical patent/EP0009433A1/fr
Application granted granted Critical
Publication of EP0009433B1 publication Critical patent/EP0009433B1/fr
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 essentially relates to a process for manufacturing a powder of a metal of one of its alloys or of one of its compounds by condensation, in solid particles, of the vapor of a bath of a metallic material in fusion in a closed treatment enclosure, by means of a cooling fluid brought into contact with said vapor.
  • metal material denotes either a metal proper, or an alloy of at least two metals.
  • the metal powders thus obtained consist of solid particles either of a single metal such as iron, zinc, magnesium, calcium, cadmium, etc., or of a metal alloy, for example a magnesium alloy - zinc, or of a metallic compound, for example zinc oxide or magnesium nitride. These powders find wide applications in various industrial branches, for the manufacture of paints, the treatment of rubbers, in the metallurgical (sintered materials), chemical (catalysts), ceramic, pharmaceutical, etc. industries.
  • US-A-2,934,331 discloses a method for manufacturing metal powder which uses, as cooling fluid, a hydrocarbon sprayed, through nozzles, onto a stream of metallic vapor flowing from an oven containing the metal molten, for example magnesium.
  • the metal particles collected in collectors have an average particle size of 1 or 2 microns and varying from 0.25 microns to approximately 55 microns.
  • DE-A-903,777 discloses a process using a cooling liquid, for example a saline solution, at a temperature below 0 ° C. This process makes it possible to obtain neither a fine particle size nor a chemically pure product.
  • a cooling liquid for example a saline solution
  • 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 of as regular shape as possible and having a minimum particle size dispersion, that is to say located in a range between 0.02 and 0.15 microns and finally having a high chemical purity.
  • 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 liquefied gas 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 liquefied gas results in a constant renewal of the phenomenon of condensation of the vapors above the bath.
  • the liquefied gas is introduced into said enclosure and is continuously evacuated therefrom.
  • Continuous circulation of the liquefied gas allows continuous production of powder at an optimal particle formation regime.
  • the liquefied gas is removed from the enclosure in the liquid phase.
  • the liquefied gas is removed from the enclosure in the gas phase.
  • the liquefied gas consists of a chemically inert body or a mixture of bodies chemically inert with respect to said material.
  • the liquefied gas consists of a chemically active body or a mixture of bodies chemically active with respect to said material.
  • the liquefied gas consists of a mixture of chemically inert bodies and bodies chemically active with respect to said material.
  • the invention also relates to an installation for implementing the aforementioned method, this installation comprising means for continuously discharging a liquefied gas directly onto the surface of the bath, means for transferring, from said enclosure, a current of fluid carrying solid metallic particles in suspension, and a closed separation chamber, connected to said transfer means and receiving the aforementioned stream of fluid, said separation chamber being provided with means for collecting the aforementioned solid particles and means for evacuating said fluid stream freed from 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 spares, 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 spares, 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 dipping slightly in the metal bath M and at inside 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 liquefied gas, for example liquefied nitrogen at -196 ° C, stored in a storage device (not shown), in the reactor 4 by means of a funnel 6 housed in said reactor and opening out in the vicinity of the surface of the metal bath so that said liquefied gas 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 conduit 7.
  • the reactor 4 is supplied with liquefied gas with a sufficient flow rate to permanently maintain, above the metal bath M, a thick layer of liquid phase which exceeds the level of connection of the conduit 7 to the reactor.
  • the solid particles which form in the reactor 4 as a result of the condensation of the metallic vapors thus remain in suspension in the liquid phase which is transferred, by drawing off by means of the conduit 7, into the separation chamber 8.
  • the liquid phase then passes in 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 as a result of the reduction in the volume of the powder following the evaporation of the liquid phase.
  • the rotary support allows these successive filling steps to be carried out.
  • the liquid phase 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 through.
  • the liquid thus filtered is brought, by a first insulated pipe 14, to a recovery tank 15 and therefore it is returned, by a recycling pump 16 and a second insulated pipe 17, to reactor 4.
  • the reactor 4 is supplied with liquefied gas with an insufficient flow rate, to maintain a liquid layer at- above the metal bath.
  • the vapor is condensed at the point of impact of the liquefied gas with the surface of the bath and the metallic particles are entrained out of the enclosure 2 by 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, AI, AI, etc.) or an alloy (brass, bronze, etc.).
  • the choice of the composition of this alloy makes 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 liquefied gas can be constituted by inert liquefied bodies (N 2 , Ar, He, etc ...) or active (O2, H 2 , NH 3 , etc ...) vis-à-vis the metallic material, by liquefied compounds such as hydrocarbons or a mixture formed of inert liquefied bodies and active liquefied bodies or else of inert liquefied bodies and liquefied compounds.
  • inert liquefied bodies N 2 , Ar, He, etc
  • active O2, H 2 , NH 3 , etc
  • the choice of the percentage of the active body 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 body or resulting from the decomposition of said compound.
  • Zinc activity in the alloy 0.16.
  • the powder obtained after separation of the liquefied gas consists of zinc particles with a size between 0.03 and 0.10 microns, and has a specific surface (BET) of 40 m 2 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 Procédé et installation de fabrication de poudre métallique à partir d'un métal ou alliage en fusion Expired EP0009433B1 (fr)

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 EP0009433A1 (fr) 1980-04-02
EP0009433B1 true EP0009433B1 (fr) 1981-09-09

Family

ID=9212724

Family Applications (1)

Application Number Title Priority Date Filing Date
EP79400619A Expired EP0009433B1 (fr) 1978-09-18 1979-09-06 Procédé et installation de fabrication de poudre métallique à partir d'un métal ou alliage en fusion

Country Status (8)

Country Link
US (1) US4309214A (enrdf_load_stackoverflow)
EP (1) EP0009433B1 (enrdf_load_stackoverflow)
JP (1) JPS5541999A (enrdf_load_stackoverflow)
AT (1) ATE193T1 (enrdf_load_stackoverflow)
CA (1) CA1139970A (enrdf_load_stackoverflow)
DE (1) DE2960783D1 (enrdf_load_stackoverflow)
ES (1) ES483267A0 (enrdf_load_stackoverflow)
FR (1) FR2435988A1 (enrdf_load_stackoverflow)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103990807A (zh) * 2014-04-21 2014-08-20 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

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2545394B1 (fr) * 1983-05-04 1985-09-06 Air Liquide Procede de fabrication de poudres metalliques a partir d'un materiau metallique en fusion
FR2545393B1 (fr) * 1983-05-04 1985-09-06 Air Liquide Procede de production de particules solides metalliques a partir d'un bain metallique
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
FR2660584A1 (fr) * 1990-04-10 1991-10-11 Rdm Ste Civile Procede et dispositif de compactage de poudres.
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

Family Cites Families (12)

* 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
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 (enrdf_load_stackoverflow) * 1971-05-31 1973-01-12
US3856513A (en) * 1972-12-26 1974-12-24 Allied Chem Novel amorphous metals and amorphous metal articles
FR2299932A1 (fr) * 1975-02-07 1976-09-03 Anvar Lithium tres finement divise et son procede de fabrication
PL194807A1 (pl) * 1976-12-28 1978-07-03 Zaklady Bieli Cynkowej Olawa Sposob kondensacji par cynkowych na drobnoziarnisty pyl cynkowy oraz urzadzenie do stosowania tego sposobu
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103990807A (zh) * 2014-04-21 2014-08-20 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
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

Also Published As

Publication number Publication date
JPS5541999A (en) 1980-03-25
ATE193T1 (de) 1981-09-15
ES8100937A1 (es) 1980-12-01
CA1139970A (fr) 1983-01-25
FR2435988A1 (fr) 1980-04-11
FR2435988B1 (enrdf_load_stackoverflow) 1981-03-20
ES483267A0 (es) 1980-12-01
EP0009433A1 (fr) 1980-04-02
JPS5620327B2 (enrdf_load_stackoverflow) 1981-05-13
DE2960783D1 (en) 1981-11-26
US4309214A (en) 1982-01-05

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