EP0120506B1 - Poudre métallique et son procédé de fabrication - Google Patents

Poudre métallique et son procédé de fabrication Download PDF

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Publication number
EP0120506B1
EP0120506B1 EP84103487A EP84103487A EP0120506B1 EP 0120506 B1 EP0120506 B1 EP 0120506B1 EP 84103487 A EP84103487 A EP 84103487A EP 84103487 A EP84103487 A EP 84103487A EP 0120506 B1 EP0120506 B1 EP 0120506B1
Authority
EP
European Patent Office
Prior art keywords
gas
container
opening
pressure
molten metal
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
EP84103487A
Other languages
German (de)
English (en)
Other versions
EP0120506A3 (en
EP0120506A2 (fr
Inventor
Alfred Prof. Dr.-Ing. Walz
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.)
Dr-Ing Lueder Gerking Te Berlijn Bondsrepubliek
Original Assignee
Walz Alfred Prof Dr-Ing
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 Walz Alfred Prof Dr-Ing filed Critical Walz Alfred Prof Dr-Ing
Priority to AT84103487T priority Critical patent/ATE34109T1/de
Publication of EP0120506A2 publication Critical patent/EP0120506A2/fr
Publication of EP0120506A3 publication Critical patent/EP0120506A3/de
Application granted granted Critical
Publication of EP0120506B1 publication Critical patent/EP0120506B1/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
    • B22F9/06—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
    • 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
    • B22F2009/088—Fluid nozzles, e.g. angle, distance

Definitions

  • the invention relates to a method and an apparatus for producing fine metal powders.
  • a method for producing metal powders in which a molten metal stream and gas are allowed to flow into an opening of a container.
  • the melting cone is broken up turbulently by a propellant gas jet at the angle relative to the melting cone axis.
  • the resulting relatively coarse powder parts can then only be comminuted by exploding the melt, which has been overheated by 250 ° C., by the vapor pressure of the strongly overheated powder parts. This results in relatively non-uniform particles of various sizes.
  • the invention is based on the object of specifying a method and an associated device which make it possible to produce metal powder with powder particles of smaller diameter and a relatively narrow particle size distribution.
  • This object is achieved by the features of claim 1, as far as the method is concerned, and the features of claim 5, as far as the device is concerned.
  • Advantageous further developments result from the associated subclaims.
  • the metal powders produced by the invention have average powder particle diameters between 5 and 35 ⁇ m, preferably between 5 and 201 ⁇ m and preferably between 8 and 15 ⁇ m.
  • the powder particles also have diameter distributions with a standard deviation of at most 2.5.
  • the metal powders consist predominantly of approximately strictly spherical individual powder particles, 90% of the powder particles forming the metal powder should have a deviation of less than 10% from the spherical shape: the powder particles also have simply curved surfaces, which is of essential importance for the sintered metallurgy.
  • molten metal stream and gas are allowed to flow into an opening of a container, the ratio of gas pressure in the vicinity of the inflow opening outside the container and gas pressure inside the container being predetermined to be greater than 5 and the opening of the container is also selected such that the The ratio of the mass flows of gas and molten metal entering the container is greater than 8.
  • the melt stream is first drawn out into fibers under the action of the gas flowing at supersonic speed. These fibers then disintegrate into droplets that form the powder particles after solidification.
  • the temperature of the gas flowing through the opening in the container should be in the range between 0.7 and 1.5 times the solidification temperature of the melt in ° K before the inflow.
  • the molten metal preferably only comes into contact with the gas flowing into the opening at a point in the container opening at which the gas pressure has dropped to less than 60% of the pressure before the opening, i.e. at a point where the gas already has almost the speed of sound.
  • the pressure at the point at which the melt and gas come into contact should be at least a fifth, preferably still at least a third, of the gas pressure before the container opening.
  • the gas should preferably have supersonic speed at the first point of contact with the molten metal.
  • All gases that do not react with the molten metal can be used as gases. Oxygen should therefore generally be avoided. Highly pure inert gases such as helium or argon are preferably used. Hydrogen can also be used for metals that do not form hydrides. Nitrogen can be used for metals that do not form nitrides. Combustion gases such as carbon monoxide can also be advantageous under certain conditions. It is also possible to achieve special effects by controlling the gas composition. For example, by using a gas with a low oxygen partial pressure, metal powders with a superficial oxide layer can be obtained, which e.g. can advantageously be used as catalysts.
  • the finest metal powder is formed by the process according to the invention via the intermediate stage of the formation of melt threads, the melt threads representing a thermodynamically extremely unstable intermediate state due to the high ratio of surface tension to viscosity. Because of their instability, the filaments tend to disintegrate into droplets.
  • the temperature of the gaseous medium must therefore be chosen to be sufficiently high that the melt threads do not solidify into droplets before decay.
  • the intermediate fiber stage is formed in a very short time. The melt bursts when entering the strong pressure drop and is pulled out into fibers by the high gas velocity. For the production of very fine powders it is therefore essential that sufficiently thin melt fibers are formed into droplets before they break down.
  • the melt therefore preferably emerges from the crucible at the point, ie it comes into contact with the gas at which the highest pressure gradient of the gas flow is present and at the same time the gas flow already has a sufficiently high speed but still a sufficient density for drawing out the burst melt flow .
  • the density should preferably still be at least 0.4 bar.
  • the pressure before opening the container can be 1 to 30 bar, preferably 1 to 10 bar.
  • a pressure of 1 bar is generally sufficient.
  • the nozzle should be as short as possible in the direction of flow, so that the pressure gradient below the point of the narrowest nozzle cross section is as large as possible.
  • the melt For the formation of powders, the melt must not solidify in the intermediate fiber state.
  • the solidification of fibers can generally be prevented by controlling the gas temperature. Metals with a higher solidification temperature give off their heat mainly through radiation.
  • such metals are preferably heated in the crucible to temperatures of a few 100 ° K above the solidification temperature.
  • the present invention also relates to a device for producing metal powders, which consists of two gas spaces, the gas spaces being connected by at least one gas passage opening, which furthermore has means for generating a pressure difference between the two gas spaces, which also has a crucible in the gas space with the contains higher pressure, the crucible having at least one melt outlet opening which is arranged symmetrically coaxially or concentrically to the gas passage opening.
  • the gas passage opening is designed in such a way that during operation of the device the gas at a certain speed first extracts the melt flow into fibers and then the fibers disintegrate into droplets.
  • the gas passage opening can be designed as a slot-shaped opening, the melting crucible having a plurality of melt outlet openings arranged in the central plane of the slot-shaped gas passage opening.
  • the gas passage openings can also be designed as circularly symmetrical passage openings, with a melt outlet opening being provided in the axis of each gas passage opening.
  • the melt outlet openings are preferably designed in the form of melt outlet nipples.
  • the melt outlet nipples preferably open in the plane of the narrowest cross section of the gas passage opening.
  • the length of the gas passage opening in the axial direction should not exceed the diameter of the gas passage opening at the narrowest point.
  • the gas passage opening should preferably widen from the point of the narrowest cross section in the flow direction with an opening angle of more than 90 °, particularly preferably more than 120 °.
  • the melt outlet nipples of the crucible should extend into the gas passage opening to such an extent that the melt outlet openings open in the plane in which the gas passage opening begins to widen.
  • FIG. 1 shows a metal melting crucible 1 which contains the metal melt 2.
  • the crucible can e.g. consist of quartz glass, sintered ceramic or graphite.
  • the crucible 1 contains at least one melt outlet nipple 3 on its underside.
  • the melt outlet nipple can e.g. have an opening of 0.3 to 1 mm in diameter.
  • the melting pot is also heated.
  • the crucible can be heated by means of a resistance heater 4, e.g. is embedded in a ceramic mass 5, take place.
  • the person skilled in the art is able to provide other options for heating the melt, e.g. high-frequency induction heating, direct electrical heating by means of electrodes which are immersed in the melt, etc.
  • a graphite crucible e.g.
  • the crucible 1 is arranged inside a container 6, which is divided into an upper gas space 8 and a lower gas space 9 by a partition 7.
  • the gas spaces 8 and 9 are connected by a passage opening 10.
  • the passage opening 10 is formed by a molded part 11 fitted into the partition 7.
  • the upper gas space 8 has a gas supply line 12 with a valve 13 for adjusting the gas pressure in the upper gas space 8.
  • the lower gas space 9 contains a gas discharge line 14 with a feed pump 15 for adjusting and maintaining the gas pressure in the lower gas space 9.
  • the bottom of the lower gas space 9 is conical and has a lock 16 for discharging the metal powder formed.
  • a conical intermediate floor 17 can be provided, which serves to collect and separate the metal powder from the gas.
  • Thermal insulation 18 can be provided in particular for the upper gas space.
  • the crucible 1 is added to the shredded metal filled. Then the gaseous medium is let in via the valve 13.
  • the lower gas space 9 is evacuated to a pressure of, for example, 1.3x10 3 to 1.3x10 4 Pa (10 to 100 torr) by means of the pump 15 and at the same time, so much gas is supplied via the valve 13, that a pressure of, for example, 1 bar is maintained in the upper gas space.
  • the gas supplied can have the temperature of the melt 2, for example.
  • Metal can be fed into the crucible 1, for example by pushing a metal ingot 21 through the upper crucible opening 22, the ingot melting in contact with the melt 2.
  • the molded part 11, which forms the gas passage opening 10, is preferably formed from heat-resistant material, for example ceramic or quartz glass.
  • FIG. 2 to 4 show alternative embodiments for the formation of the gas passage opening 10.
  • the numerals designate the same elements as in FIG. 1.
  • a molten metal is produced from solder with a melting point of 300 ° C. Air is used as the gaseous medium. A pressure of 1 bar prevails in the upper gas space 8. A pressure of 0.01 bar is maintained in the lower gas space 9.
  • the nipple 3 of the quartz crucible 1 arranged in the concentric gas passage opening 10 of 3 mm diameter has an open cross section of 0.5 mm diameter and a wall thickness of the nipple of 0.2 mm.
  • the helium gas supplied via line 12 has the temperature of the molten metal of 300 ° C. 19 g of metal powder per second are obtained from a melt outflow opening 3.
  • the powder consists of spheres with diameters between 5 ⁇ m and 50 ⁇ m.
  • the focus of the diameter distribution is 10 ⁇ m. Very few powder particles have diameters above 30 1 1m. Sporadic deviations from the spherical shape are obtained. These powder particles have an elliptical shape. The individual powder particles have a smooth surface on which individual crystallites can be recognized as differently reflecting areas without the spherical shape being disturbed.

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

Claims (7)

1. Procédé de fabrication de fines poudres métalliques, dans lequel on laisse affluer un courant de métal en fusion et du gaz dans une ouverture d'un réservoir, le rapport entre la pression du gaz au voisinage de l'ouverture d'admission située en amont du réservoir et la pression du gaz à l'intérieur du réservoir, est fixé à l'avance à une valeur supérieure à 5, l'ouverture est choisie de telle façon que le rapport entre le débit massique du gaz et celui du métal en fusion entrant dans le réservoir soit supérieur à 8 et le courant de métal en fusion est d'abord étiré en filaments sous l'action du gaz s'écoulant à une vitesse supersonique, les filaments se désintégrant en gouttelettes qui forment après solidification les particules de la poudre.
2. Procédé selon la revendication 1, caractérisé en ce que le gaz affluant dans le réservoir présente avant son admission une température se situant dans l'intervalle entre 0,7 fois et 1,5 fois la température de solidification en °K de la matière en fusion.
3. Procédé selon la revendication 1, caractérisé en ce que le métal en fusion est mis en contact avec le gaz en un endroit de l'ouverture du récipient où la pression du gaz est tombée à moins de 60% de la pression régnant en amont de l'ouverture.
4. Procédé selon la revendication 3, caractérisé en ce que le métal en fusion est mis en contact avec le gaz en un endroit de l'ouverture du récipient où la pression du gaz est encore au moins égale à un cinquième, et de préférence au moins égale à un tiers, de la presssion régnant en amont de l'ouverture du récipient.
5. Dispositif pour fabriquer de fines poudres métalliques, comprenant deux enceintes à gaz reliées entre elles par au moins une ouverture de passage du gaz, des moyens pour etablir une difference de pression entre les deux enceintes à gaz, un creuset disposé dans l'enceinte à gaz où la pression est la plus elevée et comportant au moins une ouverture de sortie de la matière en fusion qui est disposée de façon symetrique coaxialement ou concentriquement par rapport a l'ouverture de passage du gaz, et dans lequel l'ouverture de passage du gaz est agencée de telle façon que, au cours du fonctionnement du dispositif, le gaz étire d'abord en filaments le courant de la matière en fusion grâce à une vitesse déterminée et les filaments se désintègrent ensuite en gouttelettes.
6. Dispositif selon la revendication 5, caractérisé en ce que, à partir de sa zone de moindre section, l'ouverture de passage du gaz s'élargit dans le sens du courant, selon un angle d'au moins 90° et de préférence de 120°.
7. Dispositif selon la revendication 5 ou 6, caractérisé en ce que l'ouverture de sortie de la matière en fusion débouche à peu près dans le plan de la partie la plus étroite de l'ouverture de passage du gaz.
EP84103487A 1983-03-29 1984-03-29 Poudre métallique et son procédé de fabrication Expired EP0120506B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84103487T ATE34109T1 (de) 1983-03-29 1984-03-29 Metallpulver und verfahren zu dessen herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3311343 1983-03-29
DE19833311343 DE3311343A1 (de) 1983-03-29 1983-03-29 Metallpulver und verfahren zu dessen herstellung

Publications (3)

Publication Number Publication Date
EP0120506A2 EP0120506A2 (fr) 1984-10-03
EP0120506A3 EP0120506A3 (en) 1984-11-21
EP0120506B1 true EP0120506B1 (fr) 1988-05-11

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ID=6194947

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84103487A Expired EP0120506B1 (fr) 1983-03-29 1984-03-29 Poudre métallique et son procédé de fabrication

Country Status (6)

Country Link
US (1) US4534917A (fr)
EP (1) EP0120506B1 (fr)
JP (1) JPS59229402A (fr)
AT (1) ATE34109T1 (fr)
CA (1) CA1224947A (fr)
DE (1) DE3311343A1 (fr)

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Also Published As

Publication number Publication date
DE3311343A1 (de) 1984-10-04
ATE34109T1 (de) 1988-05-15
EP0120506A3 (en) 1984-11-21
CA1224947A (fr) 1987-08-04
JPS59229402A (ja) 1984-12-22
JPH0253482B2 (fr) 1990-11-16
DE3311343C2 (fr) 1987-04-23
US4534917A (en) 1985-08-13
EP0120506A2 (fr) 1984-10-03

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