EP2421997A2 - Production de particules métalliques arrondies - Google Patents

Production de particules métalliques arrondies

Info

Publication number
EP2421997A2
EP2421997A2 EP10745842A EP10745842A EP2421997A2 EP 2421997 A2 EP2421997 A2 EP 2421997A2 EP 10745842 A EP10745842 A EP 10745842A EP 10745842 A EP10745842 A EP 10745842A EP 2421997 A2 EP2421997 A2 EP 2421997A2
Authority
EP
European Patent Office
Prior art keywords
melt
particles
metal
turntable
granulation
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
EP10745842A
Other languages
German (de)
English (en)
Other versions
EP2421997B1 (fr
Inventor
Harald Eibisch
Michael Grimm
Mathias Gruber
Mark Hartmann
Andreas Lohmüller
Michael Loos
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.)
Non Ferrum GmbH
Original Assignee
Non Ferrum GmbH
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 Non Ferrum GmbH filed Critical Non Ferrum GmbH
Publication of EP2421997A2 publication Critical patent/EP2421997A2/fr
Application granted granted Critical
Publication of EP2421997B1 publication Critical patent/EP2421997B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • 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
    • 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
    • B22F2009/0896—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 particle transport, separation: process and apparatus

Definitions

  • the invention relates to a device for producing roundish metal particles of high size and shape uniformity; Process for producing roundish metal particles of high size and shape uniformity and the use of the method.
  • the invention further includes the granules made by the method, apparatus and systems of the invention.
  • the granulate particles produced in this way are particularly suitable, for example, for applications in which a particular flowability of the granulate is desired as far as possible without the formation of abrasion or particles of smaller particle size, as in thixomolding.
  • a mechanical granulating apparatus or cutting apparatus can produce particles of fine structure, but it lacks the roundness, which causes a low internal friction of the granules in the dumping, conveying and pressing. Such particles often have poor uniformity of grain size and grain shape, and of course are not spheroidal. Furthermore, it is cost- effective, if not impossible, to produce granules with as large a grain as possible by mechanical granulation. Finally, the process itself is expensive, since the mechanical machining of billets and the like. Is expensive and much remains unzerspantes residual material that must be returned to the casting process. Also, metal granules produced by the cutting process generally suffer from uneven composition in general since irregularities such as inclusions are transferred from the billet to the powder.
  • Powders from the melt apply either atomization, with molten Metal - often in mixture with gas - is explosively atomised from a nozzle at high speed, which leads to rather chunky parts, or produce roundish grains by the so-called rotating-disc process, wherein molten metal from a melt container or furnace on a rotating disk drips and is thrown there with cooling - preferably against an ascending gas flow, which slows down the falling velocity of the droplets and thus flattening their elongated drop shape in the case.
  • the beads made by melting form a much finer grain structure than the particles made from powdered castables, which has proved to be particularly advantageous in metal injection molding (Czerwinski F. Materials Science and Engineering A 367, 2004, p - 271).
  • Conventional turntable devices for making metal spheres include means for melting the metal and casting the metal on a rotating base which tosses the molten metal to form spheroidal particles. See, for example, JP 51-64456, JP 07-179912, JP 63-33508 and JP 07-173510. Such typical rotary disc devices produce spheroidal powders of relatively poor sphericity, limited micro dimensions, and improved uniformity of composition and shape.
  • molten metal is conveyed from a melting furnace in a granulating tube (5) to melt outlet openings (16) in a granulation chamber (20). Furthermore, the device has a granulating turntable (1) below the granulating tube (5), which has at least one outlet for a molten metal jet on the turntable (1), wherein the rotating turntable (1) from the at least one outlet of the granulating tube (5 dripping molten metal in the form of roundish droplets. The melt drops solidify on the cold surface of the turntable to granules particles (12).
  • An inert gas supply means (15) supplies specially selected gas to the molten metal discharged from the melt outlets (16) into a granulation chamber (20) in a manner preventing contact of the molten metal jet with air and oxidation of the metal.
  • the gas supply can be done in countercurrent, perpendicular to the melt jet and obliquely to parallel to the melt jet. Possibly. a pulsating upward and downward movement of the granulating tube (5) for separating the melt jet into drops can be provided.
  • the granulating turntable (1) is cooled.
  • the granulation tube (5) has a blind flange in one embodiment.
  • a high pressure can easily be built up and the melt is applied as quickly as possible.
  • the granulating tube (5) is returned to the melting furnace (3), whereby a regular mixing of the melt and high reproducibility of the particle composition is ensured.
  • a feed pump in / on the melting furnace (3) for conveying the molten metal to / in the granulation (5) is provided.
  • a method according to the invention for producing roundish metal particles of high size and sphericity uniformity has the following steps: - Melting of the metallic starting material;
  • Typical metals which are processed by the granulation process according to the invention for high reactivity in the melt are selected from the group consisting of Al, Mg, Ca, Zn and their alloys - but the process can also be used for other metals.
  • the cooling of the dispersed droplets by gas is advantageously accomplished by means of a predetermined cooling gas of one or more inert gases in an open or closed granulation chamber 20 which provides the controlled atmosphere.
  • spherical particles of fine grain structure of high shape and size uniformity from the melt is possible.
  • Such particles having a fine grain structure are particularly suitable for applications such as thixomolding, sintering, metal injection molding and similar powder metallurgy processes.
  • the inventive method is particularly suitable for the production of granules of magnesium or magnesium alloys.
  • metal also refers to their respective alloys as well as the metal with minor impurities.
  • Spheroid is understood to mean any round shape, such as, for example, spheres, bulge shapes, elliptical shapes, etc., which has no sharp or angular edges.
  • the access of reacting with the melt gases such as water vapor, oxygen, nitrogen is avoided as possible.
  • the melting takes place under a protective cover or protective atmosphere and the transport of the melt through a closed pipe system to the outlet openings or nozzles.
  • the melt can be circulated, whereby a constant return does not take place on the turntable ejected melt in the furnace and thus a permanent mixing of the melt volume is achieved while maintaining a high homogeneity of the product and a homogeneous temperature distribution.
  • the high flow velocity in the pipe is advantageous, so that impurities (eg oxides) are permanently transported, are not deposited in the pipe and clog it from the inside.
  • the pipe itself can be heated over the whole area or only over part of the area, for example only in the lower area, in order to increase the convection there and to avoid settling of reaction products of the melt.
  • the shape and size of the particles are influenced inter alia by density, viscosity, surface tension and diameter of the jet emerging from the discharge opening (nozzle diameter, nozzle material). With increasing speed occur: dripping, Rayleigh decay, wave decay, sputtering (these terms are in Schubert, Manual of Mechanical Process Engineering, Volume 1, published by Wiley VCH, 2001, which is incorporated by reference in its entirety to avoid repetition).
  • the dependence of the droplet size has already been calculated by Schmidt (Schmidt, P .: "Atomization of liquids" - review lecture apparatus engineering, University of Essen 1984, to which reference is also made in full).
  • the maximum static pressure that a drop can withstand before decay was calculated by Schmidt 1984 and Vauck 2000 (Vauck, WRA: Basic Operations of Chemical Process Engineering, DVG Verlag, 11th Edition, 2000, incorporated herein by reference). As soon as the dynamic pressure exceeds the static pressure, Rayleigh decays. Thus, the droplet size can be calculated for certain alloys and plant parameters and, in part, the particle size can be controlled.
  • Adjusting the relationship between devices and methods according to the invention enables the production of relatively round, spheroidal, elliptical or lin ⁇ senförmiger particles of different size and diverse applicability, such as during sintering, Thixomolding (metal injection molding), pressing, etc.
  • the invention provides methods, devices and systems for producing granular particles of uniform spheroidal shape and high sphericity consisting of metal and its alloys by use of an improved rotating disc apparatus.
  • FIG. 1 shows an embodiment of the system according to the invention with the granulation device
  • FIGS. 2A and 2B show a structure of a mechanical granulate and a granulate produced by melt metallurgy (AZ 91).
  • FIGS. 3A and 3B schematically show different embodiments of the transport tube
  • Fig. 4 produced according to the invention granules of magnesium alloy AZ 91.
  • Fig. 1 the system according to the invention is shown schematically. From a melting furnace 3, melt 6 is fed into the granulating tube 5 with nozzles 16 by means of a feed pump 2. The melt exits the nozzles 16 into the inert gas-filled granulation chamber 20 and forms drops 8. The drops fall on the turntable 1, solidify to particles 12 and are passed through a scraper 13 in a container 2. Inert gas 14 is passed through lines 15 to the emerging from the nozzle 16 melt, which prevents the formation of oxides, nitrides and the like to the nozzle 16 of the granulation tube 5 and the granules, and promotes the disintegration of the melt jet to 8 drops.
  • FIG. 3 schematically shows various embodiments of the course of the granulation tube 5.
  • a granulating system with return 7 is shown schematically.
  • a pump P is arranged, which ensures regular promotion of the melt.
  • the return of non-discharged melt through the return pipe 7 in the furnace is apparent.
  • Fig. 3b an embodiment without return, in which the granulation tube 5 terminates in a blind flange is shown.
  • Fig. 4 shows various granules of a plant according to the invention. Clearly here is a roundish lens shape of the present invention produced from the melt Mg granules visible.
  • FIG. 2 a shows a light micrograph of the microstructure of a step through a magnesium alloy AZ91 particle produced according to the invention from the melt
  • FIG. 2 b shows the microstructure of a particle made from cast ingots of the same alloy.
  • the invention provides methods, devices and systems for producing metal granules wherein the particles have uniform spheroidal shape - as shown in FIG. 4.
  • At least one jet of molten metal which has been broken down into droplets, is directed onto a rotating dish.
  • the molten steel is supplied with inert gas, here predominantly helium.
  • a bell made of baffles below the Granulierrohres prevented as a granulation chamber outflow of the protective gas and maintains an atmosphere that prevents oxidation of the exiting the nozzle melt, upright.
  • the droplets hit the cold, preferably cooled turntable.
  • the turntable removes heat from the melt droplet so quickly that a rapid solidification of the melt results in a granular particle with a fine-grained microstructure.
  • the rotational movement of the plate prevents the melting droplets from meeting / coalescing, thus ensuring solidification of the droplets into discrete particles.
  • the particles are pushed here by the trained here as a strip scraper over the edge of the plate in a container. Also conceivable are other means for removing the solidified particles such as brushes, blowers, etc.
  • the pressure in the granulation tube 5 is generated in this embodiment by a centrifugal pump ⁇ .
  • a centrifugal pump ⁇ In general, all known pumping methods and systems for building up the melt pressure or the melt flow in the pouring tube suitable, such as piston pumps, induction pumps, pneumatic pumping systems, but also for pressurizing the furnace chamber and pump-free delivery systems, which work, for example, on the principle of communicating tubes can be used.
  • the shape and size of the granulate particles can be influenced by various system parameters. These include, inter alia, the distance of the Giefirohres to the turntable so the drop height of emerging from the nozzle melt; the nozzle diameter, the melt pressure, the melt temperature and the design of the granulation tube (with or without return). In addition, determine temperature, flow velocity, composition and angle of attack of the protective gas and the temperature of the turntable, the shape and size of the granular particles. Depending on the combination of parameters, the particle shape is different spheroid z. B. platelet, lens, spherical or cylindrical. For example, increasing the rotational speed of the plate causes a more elongate shape of the formed particle.
  • the metallic starting materials Prior to granulation, the metallic starting materials, for example magnesium die-cast scrap, are selected under a protective gas atmosphere from the group consisting of noble gases such as argon, neon and helium or nitrogen, carbon dioxide or dry air with additions of sulfur dioxide, sulfur hexafluoride or r-134a or Mixtures thereof melted in the melting furnace 3.
  • a protective gas atmosphere from the group consisting of noble gases such as argon, neon and helium or nitrogen, carbon dioxide or dry air with additions of sulfur dioxide, sulfur hexafluoride or r-134a or Mixtures thereof melted in the melting furnace 3.
  • noble gases such as argon, neon and helium or nitrogen
  • carbon dioxide or dry air with additions of sulfur dioxide, sulfur hexafluoride or r-134a or Mixtures thereof melted in the melting furnace 3.
  • salts which leads to the formation of a protective layer of liquid salt on the melt surface and thus prevents a reaction of the melt with the air.
  • a method of the invention for producing small spheroidal particles of fine crystalline composition and highly uniform size and shape comprises the following steps: ⁇ melting the metallic starting material; ⁇ passing the molten metal in a heated granulating tube through a turntable.
  • Embodiments may include, for example:
  • Metal powders made by the machining process also generally suffer from uneven composition in general.
  • the external gas pressure on the circumference of the dispersed droplets is preferably atmospheric pressure.
  • Magnesium die casting scrap of alloy AZ91 is melted in an electrically heated melting furnace under nitrogen with 0.20% r-134 a at 680 0 C.
  • the melting furnace is a centrifugal pump, which at 5500 revolutions per minute, the magnesium melt in a from the melt furnace promotes leading, blind ending, closed, heated granulation tube with 16 dispensing nozzles. Under the dispensing nozzles runs a water-cooled turntable.
  • a melt jet forms, which decays to droplets at a drop height of 120 mm.
  • Helium is conducted as a protective gas against the melt jet.
  • Guiding plates around the granulation tube form a bell, which prevent the escape of helium upwards and forms a granulation chamber 20 and a helium atmosphere for protecting the melt from oxidation between the granulation tube and turntable.
  • the rotation of the plate is carried out according to the requirements of the particle shape at a speed of 4-10 revolutions per minute.
  • the result is lenticular particles high form uniformity.
  • the particles are guided with a scraper from the turntable into a container. By subsequent sieving large, sometimes not dimensionally stable particles can be separated.
  • FIG. 4 shows 3 sieve fractions of so-produced granules of the magnesium alloy AZ91.
  • FIG. 2a A light microscopic picture of a cross section of the particles thus produced is shown in FIG. 2a in comparison with a cross section through particles from the conventional machining method. It is noticeable that the section through the particles produced by machining shows considerably larger bodies and transition zones than the fine-crystalline structure of the casting particles produced by the granulation method from the melt.
  • the Mg particles produced according to the invention are superior to the particles produced by machining processes both in terms of their microstructure and their external shape.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne un dispositif pour la production de particules métalliques arrondies de grande régularité de taille et de forme à partir d'une matière fondue. L'invention concerne également un procédé pour la production de particules métalliques arrondies de grande régularité de taille et de forme à partir d'un métal fondu hautement réactif. Le procédé selon l'invention comprend les étapes suivantes : fusion du matériau métallique de départ à l'abri de l'air; transport du métal fondu dans un tube de granulation fermé du four de fusion vers au moins un orifice de sortie de matière fondue; sortie de la matière fondue par l'orifice de sortie de matière fondue au-dessus d'un plateau tournant sous forme de jet de matière fondue qui se décompose en gouttes discrètes avant de tomber sur le plateau tournant; amenée d'un flux de gaz protecteur dans la zone de la matière fondue sortant de l'orifice de sortie de matière fondue; réception de la matière fondue sur le plateau tournant sous forme de gouttes discrètes de matière fondue; solidification des gouttes de matière fondue en particules granulées par contact avec la surface plus froide du plateau tournant; évacuation des particules granulées du plateau tournant pour conditionnement ou poursuite du traitement.
EP10745842.4A 2009-02-25 2010-02-25 Production de particules métalliques arrondies Not-in-force EP2421997B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102009010600A DE102009010600A1 (de) 2009-02-25 2009-02-25 Herstellung von rundlichen Metallpartikeln
PCT/DE2010/000324 WO2010097079A2 (fr) 2009-02-25 2010-02-25 Production de particules métalliques arrondies

Publications (2)

Publication Number Publication Date
EP2421997A2 true EP2421997A2 (fr) 2012-02-29
EP2421997B1 EP2421997B1 (fr) 2015-04-08

Family

ID=42665979

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10745842.4A Not-in-force EP2421997B1 (fr) 2009-02-25 2010-02-25 Production de particules métalliques arrondies

Country Status (7)

Country Link
US (1) US20120195786A1 (fr)
EP (1) EP2421997B1 (fr)
BR (1) BRPI1008736A2 (fr)
CA (1) CA2753577A1 (fr)
DE (2) DE102009010600A1 (fr)
MX (1) MX2011008947A (fr)
WO (1) WO2010097079A2 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013000249A1 (de) 2013-01-08 2014-07-10 Volkswagen Aktiengesellschaft Vorrichtung zur Herstellung von Metallgranulat aus der Semi-Solid-Phase
DE102013000248B4 (de) 2013-01-08 2019-10-17 Volkswagen Aktiengesellschaft Vorrichtung zur Herstellung von Metallgranulat aus der Flüssigphase
KR102240416B1 (ko) 2016-08-24 2021-04-15 5엔 플러스 아이엔씨. 저융점 금속 또는 합금 분말 미립화 제조 공정
JP6926844B2 (ja) * 2017-08-31 2021-08-25 セイコーエプソン株式会社 チクソモールディング用原料、チクソモールディング用原料の製造方法および成形体
JP2021514028A (ja) 2018-02-15 2021-06-03 ５エヌ プラス インコーポレイテッド 高融点金属または合金粉末アトマイズ製造プロセス
CN112497563B (zh) * 2020-11-12 2022-05-20 建德市春盛塑业有限公司 一种塑料颗粒及其制备工艺
EP4382228A1 (fr) * 2022-12-07 2024-06-12 Fehrmann GmbH Appareil d'atomisation pour produire de la poudre métallique, son utilisation et procédé de fonctionnement d'un appareil d'atomisation
CN117921013B (zh) * 2024-02-01 2024-09-13 安徽中体新材料科技有限公司 一种钛合金粉末制备装置

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Publication number Priority date Publication date Assignee Title
DE739743C (de) * 1936-02-08 1943-10-16 Hermann Plauson Verfahren zur Herstellung feinsten Metallpulvers aus fluessigem Metall
GB746301A (en) * 1953-03-18 1956-03-14 Dow Chemical Co Atomizing magnesium
DE1081741B (de) * 1953-03-18 1960-05-12 Dow Chemical Co Verfahren zum Herstellen von Magnesiumlegierungen in Kugelform
GB754180A (en) * 1953-09-18 1956-08-01 Dow Chemical Co Atomizing aluminium or aluminium alloys
JPS5164456A (ja) 1974-12-02 1976-06-03 Nisshin Steel Co Ltd Kyujokinzokufunmatsuno seizoho oyobi sochi
DE2936691C2 (de) * 1979-09-11 1984-08-02 Itoh Metal Abrasive Co., Ltd., Nagoya, Aichi Vorrichtung zur Erzeugung sphärischer Teilchen oder Fasern
US4687510A (en) * 1983-01-24 1987-08-18 Gte Products Corporation Method for making ultrafine metal powder
JPS6333508A (ja) 1986-07-25 1988-02-13 Natl Res Inst For Metals 金属粉末または合金粉末の製造方法
JPH07173510A (ja) 1992-05-15 1995-07-11 Shin Etsu Chem Co Ltd 球状金属微粒子の製造方法
JPH0754019A (ja) * 1993-08-17 1995-02-28 Nippon Sozai Kk 多段階分裂及び急冷による粉末の作製法
JPH07179912A (ja) 1993-12-22 1995-07-18 Minerva Kiki Kk 球状金属粒子の生産方法
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Also Published As

Publication number Publication date
WO2010097079A3 (fr) 2011-12-29
WO2010097079A4 (fr) 2012-03-01
EP2421997B1 (fr) 2015-04-08
CA2753577A1 (fr) 2010-09-02
BRPI1008736A2 (pt) 2016-03-08
DE102009010600A1 (de) 2010-11-11
WO2010097079A2 (fr) 2010-09-02
DE202010018019U1 (de) 2013-08-09
US20120195786A1 (en) 2012-08-02
MX2011008947A (es) 2012-02-08

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