EP0120506A2 - Poudre métallique et son procédé de fabrication - Google Patents

Poudre métallique et son procédé de fabrication Download PDF

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Publication number
EP0120506A2
EP0120506A2 EP84103487A EP84103487A EP0120506A2 EP 0120506 A2 EP0120506 A2 EP 0120506A2 EP 84103487 A EP84103487 A EP 84103487A EP 84103487 A EP84103487 A EP 84103487A EP 0120506 A2 EP0120506 A2 EP 0120506A2
Authority
EP
European Patent Office
Prior art keywords
gas
opening
container
pressure
melt
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
EP84103487A
Other languages
German (de)
English (en)
Other versions
EP0120506A3 (en
EP0120506B1 (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 present invention relates in particular to finely divided metal powders and a process for their production.
  • Powder metallurgy has led to the development of materials that are no longer accessible to conventional processing methods such as deformation and machining.
  • Sintered alloys in which finely divided metal powders of different metals are mixed and only alloyed during the sintering process have become particularly important.
  • the shaping in the sinter metallurgy takes place through the sintering process.
  • Sintered metallurgy now requires metal powders that are as finely divided as possible in order to be able to achieve surfaces that are as smooth as possible and to provide the largest possible surface for the formation of sintered alloys. Furthermore, it is desirable to use spherical powder particles which are as dense as possible in order to obtain classifier bodies which are as dense as possible.
  • a process has now been found which allows metal powders to be produced, the powder particles of which are dense and non-porous, and which have a very approximate spherical shape and mean diameters of well below 50 ⁇ .
  • the present patent application therefore relates to pore-free metal powders, which are characterized in that the powder particles have simply curved, smooth surfaces and an average diameter of 5 to 35 ⁇ .
  • Preferred metal powders according to the invention have average powder particle diameters between 5 and 20 ⁇ , preferably between 8 and 15 ⁇ .
  • the powder particles preferred according to the invention also have diameter distributions with a standard deviation of at most 2.5, particularly preferably a standard deviation of at most 2.0. The standard deviation is based on the Number frequency of the powder diameter defined in a production batch without looking at coarse powder particles.
  • Particularly preferred metal powders according to the invention 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. A deviation of 10% from the spherical shape means that the largest diameter of the powder particle is at most 10% larger than the smallest diameter.
  • the powder particles have simply curved surfaces.
  • a simply curved surface should be understood to mean that each tangent on the surface has only one point of contact with the metal particle.
  • All metals or metal alloys can be used as metals. Iron, cobalt, nickel, chromium, aluminum or their alloys are particularly suitable.
  • the metal powder can have a crystalline structure or be amorphous. In particular, it is also possible, e.g. Obtain iron alloys with additives of crystallization inhibitors such as chromium or boron as the metal powder according to the invention.
  • Metal powders of silver, platinum, iridium or alloys according to the invention are suitable for use as catalysts.
  • the present invention also relates to a process for the production of metal powders, which is characterized in that a molten metal stream and gas are allowed to flow into an opening of a container, the ratio of gas pressure near the inflow opening outside the container and gas pressure inside the container is greater than 5 and the opening of the container is selected so that the ratio of the mass flows of gas and molten metal entering the container is greater than 8.
  • 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 ratio of the mass flows of gas and melt should preferably be less than 25, particularly preferably less than 15.
  • the molten metal preferably only occurs at a point in the container opening with the gas flowing into the opening. in contact where the gas pressure has dropped to less than 60% of the pressure before 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.
  • 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, for example, 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 melt filaments tend to disintegrate into droplets.
  • the temperature of the gaseous medium must therefore be chosen to be sufficiently high that the melt filaments 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. It is therefore essential for the production of very fine powders that the formation of sufficiently thin melt fibers takes place before the disintegration into droplets.
  • the melt exits the crucible at that point, i.e. 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 is still of sufficient density to pull out the burst melt flow.
  • the density should preferably still be at least 0.4 bar.
  • the pressure before the opening of 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, wherein the crucible has at least one melt outlet opening, which is arranged symmetrically to the gas passage opening.
  • 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, however, also be designed as circularly symmetrical passage openings, 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 melting crucible can consist, for example, of quartz glass, sintered ceramic or graphite.
  • the melt crucible 1 contains at least one melt outlet nipple 3 on its underside.
  • the melt outlet nipple can, for example, 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, which is embedded, for example, in a ceramic mass 5.
  • the person skilled in the art is able to provide other options for heating the melt, for example high-frequency induction heating, direct electrical heating by means of electrodes which are immersed in the melt, etc.
  • one electrode can be the crucible, for example. It is also possible to provide flame heating inside or outside the crucible.
  • the crucible 1 is arranged within 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 filled with the metal to be fiberized. Then the gaseous medium is let in via the valve 13.
  • the lower gas space 9 is evacuated to a pressure of, for example, 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 remains.
  • 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.
  • FIGS 2 to 4 show alternative embodiments for the formation of the gas passage opening 10.
  • the numerals designate the same elements as in Figure 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 ⁇ and 50 ⁇ .
  • the focus of the diameter distribution is 10 ⁇ . Very few powder particles have diameters above 30 ⁇ . 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.

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
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
DE19833311343 DE3311343A1 (de) 1983-03-29 1983-03-29 Metallpulver und verfahren zu dessen herstellung
DE3311343 1983-03-29

Publications (3)

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

Family

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)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0220418A1 (fr) * 1985-09-24 1987-05-06 Gerking, Lüder, Dr.-Ing. Procédé et installation pour la fabrication de poudre très fine sous forme sphérique
FR2605538A1 (fr) * 1986-10-27 1988-04-29 Serole Bernard Tuyere d'atomisation par gaz a ecoulement liquide stabilise aerodynamiquement
EP0372918A2 (fr) * 1988-12-08 1990-06-13 Elkem A/S Poudre de silicium et procédé de sa préparation
WO2001072431A1 (fr) * 2000-03-28 2001-10-04 Nisco Engineering Ag Procede et dispositif pour produire des gouttes de meme dimension

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DE3533954A1 (de) * 1985-09-24 1987-03-26 Agfa Gevaert Ag Automatisch be- und entladbare roentgenfilmkassette und hierfuer geeignetes roentgenfilmkassettenbe- und -entladegeraet
JPH0628570B2 (ja) * 1986-02-13 1994-04-20 雪印乳業株式会社 カプセル体の製造方法及び装置
JPS63262405A (ja) * 1987-04-20 1988-10-28 Fukuda Metal Foil & Powder Co Ltd 金属粉末製造方法
DE3730147A1 (de) * 1987-09-09 1989-03-23 Leybold Ag Verfahren zur herstellung von pulvern aus geschmolzenen stoffen
DE3735787A1 (de) * 1987-09-22 1989-03-30 Stiftung Inst Fuer Werkstoffte Verfahren und vorrichtung zum zerstaeuben mindestens eines strahls eines fluessigen stoffs, vorzugsweise geschmolzenen metalls
DE3737130C2 (de) * 1987-11-02 1996-01-18 Gerking Lueder Dr Ing Verfahren und Vorrichtung zum Herstellen von Feinstpulver
US4880162A (en) * 1988-06-15 1989-11-14 Air Products And Chemicals, Inc. Gas atomization nozzle for metal powder production
ES2052851T3 (es) * 1988-09-07 1994-07-16 Daido Steel Co Ltd Aparato para la produccion de polvo de metal.
DE3843859A1 (de) * 1988-12-24 1990-06-28 Messer Griesheim Gmbh Herstellung von titanpulvern durch verduesung der schmelze
DE3913649A1 (de) * 1989-04-26 1991-01-17 Krupp Pulvermetall Gmbh Verfahren und anlage zum herstellen metallischer pulver aus einer metallschmelze durch gasverduesen
US5238482A (en) * 1991-05-22 1993-08-24 Crucible Materials Corporation Prealloyed high-vanadium, cold work tool steel particles and methods for producing the same
JPH05117724A (ja) * 1992-04-16 1993-05-14 Fukuda Metal Foil & Powder Co Ltd 金属粉末製造方法
DE19607114A1 (de) * 1995-01-28 1996-12-05 Lueder Dr Ing Gerking Fäden aus Schmelzen mittels kalter Gasstrahlen
US5905000A (en) 1996-09-03 1999-05-18 Nanomaterials Research Corporation Nanostructured ion conducting solid electrolytes
US6933331B2 (en) * 1998-05-22 2005-08-23 Nanoproducts Corporation Nanotechnology for drug delivery, contrast agents and biomedical implants
US5788738A (en) * 1996-09-03 1998-08-04 Nanomaterials Research Corporation Method of producing nanoscale powders by quenching of vapors
DE19758111C2 (de) * 1997-12-17 2001-01-25 Gunther Schulz Verfahren und Vorrichtung zur Herstellung feiner Pulver durch Zerstäubung von Schmelzen mit Gasen
DE29924924U1 (de) 1999-01-19 2006-12-21 BEGO Bremer Goldschlägerei Wilh. Herbst GmbH & Co. KG Formkörper zur Verwendung als Zahnersatz und dentales Hilfsteil
DE19929709C2 (de) * 1999-06-24 2001-07-12 Lueder Gerking Verfahren zur Herstellung von im Wesentlichen endlosen feinen Fäden und Verwendung der Vorrichtung zur Durchführung des Verfahrens
AU2147701A (en) * 1999-10-15 2001-04-23 Applikations-und Technikzentrum fur Enegieverfaahrens-, Umwelt- Und Stromungstechnik (ATZ-EVUS) Method for producing a powder
DE10001968B4 (de) * 1999-10-15 2004-02-12 Applikations- Und Technikzentrum Für Energieverfahrens-, Umwelt- Und Strömungstechnik (Atz-Evus) Verfahren zur Herstellung eines Pulvers
AT409136B (de) * 2000-05-19 2002-05-27 Tribovent Verfahrensentwicklg Einrichtung zum zerstäuben und zerkleinern von flüssigen schmelzen
US6444009B1 (en) * 2001-04-12 2002-09-03 Nanotek Instruments, Inc. Method for producing environmentally stable reactive alloy powders
US6855426B2 (en) 2001-08-08 2005-02-15 Nanoproducts Corporation Methods for producing composite nanoparticles
DE10150931A1 (de) * 2001-10-11 2003-04-30 Lueder Gerking Verbesserte Gemischbildung in Verbrennungskraftmaschinen
US7708974B2 (en) 2002-12-10 2010-05-04 Ppg Industries Ohio, Inc. Tungsten comprising nanomaterials and related nanotechnology
AT412093B (de) * 2003-03-11 2004-09-27 Tribovent Verfahrensentwicklg Vorrichtung zum zerstäuben von schmelzen
DE10340606B4 (de) * 2003-08-29 2005-10-06 Gerking, Lüder, Dr.-Ing. Vorrichtung zum Verdüsen eines Schmelzestrahls und Verfahren zum Verdüsen von hochschmelzenden Metallen und Keramikschmelzen
AT7094U3 (de) * 2004-06-17 2005-03-25 Imr Metalle Und Technologie Gm Verfahren und vorrichtung zum zerstäuben von flüssigkeitsfilmen
JP4504775B2 (ja) * 2004-10-04 2010-07-14 日本アトマイズ加工株式会社 導電ペースト
BRPI0622077A2 (pt) * 2006-10-24 2014-05-20 Beneq Oy Dispositivo para produção de nanopartículas
CN103043665B (zh) * 2013-01-24 2014-11-26 厦门大学 一种硅粉的制备方法
DE102013022096B4 (de) 2013-12-20 2020-10-29 Nanoval Gmbh & Co. Kg Vorrichtung und Verfahren zum tiegelfreien Schmelzen eines Materials und zum Zerstäuben des geschmolzenen Materials zum Herstellen von Pulver
DE102015010209A1 (de) 2015-08-05 2016-03-17 Daimler Ag Vorrichtung zum Versehen eines Substrats mit einem Werkstoff
JP6544836B2 (ja) * 2017-07-03 2019-07-17 株式会社 東北テクノアーチ 金属粉末の製造装置及びその製造方法
AU2018367932A1 (en) * 2017-11-14 2020-06-11 Pyrogenesis Canada Inc. Method and apparatus for producing fine spherical powders from coarse and angular powder feed material
EP3747574A1 (fr) 2019-06-05 2020-12-09 Hightech Metal ProzessentwicklungsgesellschaftmbH Procédé et dispositif de fabrication de poudre de matière
DE102021208605A1 (de) 2021-08-06 2023-02-09 Sms Group Gmbh Wechselsystem für eine Tundish-Einheit, Tundish-Einheit für ein Wechselsystem, Verdüsungsanlage sowie Verfahren zum Verdüsen von Metallschmelze
DE102021212367A1 (de) 2021-11-03 2023-05-04 Sms Group Gmbh Verdüsungs-Einheit zum Verdüsen von metallenen Schmelzen, insbesondere für pulvermetallurgische Zwecke
DE102022211865A1 (de) 2022-11-09 2024-05-16 Gfe Metalle Und Materialien Gmbh Vorrichtung zur Verdüsung eines Schmelzstromes mittels eines Verdüsungsgases

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DE2111613A1 (de) * 1971-03-11 1972-09-21 Deutsche Edelstahlwerke Ag Vorrichtung zum Gasverduesen von schmelzfluessigem Metall zu Pulver

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GB952457A (en) * 1959-03-23 1964-03-18 Kenkichi Tachiki Atomization
GB1123825A (en) * 1965-10-15 1968-08-14 Toho Zinc Co Ltd Production of metal powders
DE1758844A1 (de) * 1968-08-19 1971-03-04 Gerliwanow Wadim G Verfahren zum Gewinnen von feindispersen Metall- und Legierungspulvern
DE2111613A1 (de) * 1971-03-11 1972-09-21 Deutsche Edelstahlwerke Ag Vorrichtung zum Gasverduesen von schmelzfluessigem Metall zu Pulver

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0220418A1 (fr) * 1985-09-24 1987-05-06 Gerking, Lüder, Dr.-Ing. Procédé et installation pour la fabrication de poudre très fine sous forme sphérique
FR2605538A1 (fr) * 1986-10-27 1988-04-29 Serole Bernard Tuyere d'atomisation par gaz a ecoulement liquide stabilise aerodynamiquement
EP0372918A2 (fr) * 1988-12-08 1990-06-13 Elkem A/S Poudre de silicium et procédé de sa préparation
EP0372918A3 (fr) * 1988-12-08 1991-07-24 Elkem A/S Poudre de silicium et procédé de sa préparation
WO2001072431A1 (fr) * 2000-03-28 2001-10-04 Nisco Engineering Ag Procede et dispositif pour produire des gouttes de meme dimension

Also Published As

Publication number Publication date
JPS59229402A (ja) 1984-12-22
EP0120506A3 (en) 1984-11-21
JPH0253482B2 (fr) 1990-11-16
EP0120506B1 (fr) 1988-05-11
DE3311343A1 (de) 1984-10-04
US4534917A (en) 1985-08-13
CA1224947A (fr) 1987-08-04
DE3311343C2 (fr) 1987-04-23
ATE34109T1 (de) 1988-05-15

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