EP0587993A1 - Réservoir de métal liquide ultra-pur, son procédé de fabrication ainsi que l'installation de production de poudre métallique très pure - Google Patents

Réservoir de métal liquide ultra-pur, son procédé de fabrication ainsi que l'installation de production de poudre métallique très pure Download PDF

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Publication number
EP0587993A1
EP0587993A1 EP93108457A EP93108457A EP0587993A1 EP 0587993 A1 EP0587993 A1 EP 0587993A1 EP 93108457 A EP93108457 A EP 93108457A EP 93108457 A EP93108457 A EP 93108457A EP 0587993 A1 EP0587993 A1 EP 0587993A1
Authority
EP
European Patent Office
Prior art keywords
purity metal
vessel
lid
vessel body
molten
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
EP93108457A
Other languages
German (de)
English (en)
Other versions
EP0587993B1 (fr
Inventor
Hiroaki C/O Chuo-Kenkyusho Kohmoto
Noriaki C/O Chuo-Kenkyusho Murahashi
Rokuro C/O Chuo-Kenkyusho Sato
Tohru C/O Chuo-Kenkyusho Kohno
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.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials Corp
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
Priority claimed from JP13285692A external-priority patent/JPH0730366B2/ja
Priority claimed from JP4132857A external-priority patent/JPH0791572B2/ja
Application filed by Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Publication of EP0587993A1 publication Critical patent/EP0587993A1/fr
Application granted granted Critical
Publication of EP0587993B1 publication Critical patent/EP0587993B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
    • B22D41/14—Closures
    • B22D41/44—Consumable closure means, i.e. closure means being used only once
    • B22D41/48—Meltable closures
    • 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
    • B22F2009/0892—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 casting nozzle; controlling metal stream in or after the casting nozzle
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a vessel for melting a high-purity metal (referred to simply as “melting vessel”) without causing contamination of the metal and to a method of producing such a melting vessel.
  • the invention also is concerned with an apparatus for melting high-purity metal employing the vessel and with an apparatus for producing powder of high-purity metal with a high degree of uniformity of particle size.
  • powdered high-purity metal referred to simply as "powder producing apparatus”, hereafter
  • a melting vessel for melting a high-purity metal therein
  • a gas jetting means which directs a gas to the molten high-purity metal falling from the vessel.
  • Improvements also have been achieved in this field of technique, such as the use of a refractory metal, e.g., tantalum, molybdenum or rhenium, as the vessel material. Such improvements, however, are still unsatisfactory for the reason stated above.
  • the known melting vessels do not have any means for adjusting the size of the molten metal outlet port formed in the vessel bottom. Thus, the vessels could not be stably used in the gas atomizing method.
  • a vessel for melting a high-purity metal comprising a vessel body provided with a cooling jacket and with an opening of a predetermined size formed in the bottom thereof, and a lid made of the same material as the high-purity metal to be molten and closing the bottom opening of the vessel body.
  • a high-purity metal including: a melting vessel having a vessel body provided with an opening of a predetermined size formed in the bottom thereof, and a lid made of the same material as the high-purity metal to be molten and closing the bottom opening of the vessel body; a cooling system for cooling the inner surface region of the vessel body; a beam generating device; a measuring device for measuring the size of an output port formed in the lid and an analyzer; and a control device which controls one or both of the beam output power of the beam generating device and the rate of cooling effected by the cooling system in accordance with the output from the measuring device.
  • the melting vessel of the present invention has a vessel body having an opening of a predetermined size formed in the bottom thereof, means for cooling the inner surface region of the vessel wall and a lid made of the same material as the metal to be molten in the vessel and closing the bottom opening of the vessel.
  • the lid may be attached to the vessel body by, for example, preparing the lid of the same metal as the metal to be molten and fitting the lid into the opening.
  • the lid may be formed by a process including the steps of preparing a closure member having a substantially flattened upper surface, closing the bottom opening by the closure member by bringing the latter into abutment with the lower bottom surface of the vessel body, melting a small amount of the metal to be molten in the vessel so as to allow the molten metal to fill the concavity defined by the closure member and the vessel bottom wall surrounding the opening, and allowing the metal to solidify so as to fill the opening.
  • the melting vessel has a vessel body denoted by 2 which is a substantially cylindrical cup-like bottom-equipped structure having an internal cavity or recess 8.
  • the vessel body 2 is made of copper.
  • a tapered opening 10 converging downward is formed in the center of the bottom of the vessel body 2.
  • the vessel body 2 is double-walled to provide a jacket space 12 which communicates with the interior of the pipes 14 and 16 connected to the side wall of the vessel body 2. The arrangement is such that cooling water is supplied into the jacket space 12 through the pipe 14 so as to cool the inner surface region of the vessel body 2 and is then discharged through the pipe 16.
  • a lid 6 having a tapered outer peripheral surface 6a fits in the opening 10 of the vessel body 2, so as to close the opening 10.
  • This lid 6 is made of the same metal material as the melting object, i.e., the high-purity metal to be molten in the vessel.
  • the melting vessel of this embodiment includes the vessel body 2 and the lid 6.
  • the lid 6 may be separately formed in another vessel and then fitted in the opening 10 to close the latter.
  • the lid 6 may be formed by a method which will be described hereinunder with reference to Fig. 2.
  • a closure member 50 having a flattened upper surface.
  • the closure member 50 is brought into abutment with the lower bottom surface of the vessel body 2 to cover the opening 10.
  • a small amount of the metal M which is the same metal as the high-purity metal to be industrially molten in the vessel 2 is placed in the vessel.
  • This small amount of metal M is then molten by, for example, application of a voltage between the vessel body 2 and the metal M, while the vessel body 2 and the closure member 50 are being cooled. Consequently, the molten metal M flows into the recess 60 defined by the closure member 50 and the bottom wall of the vessel body 2 around the opening 10.
  • the molten metal M is then allowed to solidify within the recess 60.
  • the closure member 50 is removed from the vessel body 2, whereby the lid 6 "fitting" in the opening 10 is obtained in the same form as that shown in Fig. 1.
  • the-melting vessel In operation of the melting vessel of this embodiment, the-melting vessel is charged with an appropriate amount of high-purity metal and is molten by, for example, application of a voltage between the vessel body 2 and the high-purity metal to be molten, while the vessel body is cooled by a cooling medium such as water circulated through the jacket space 12.
  • a cooling medium such as water circulated through the jacket space 12.
  • the portion of the molten high-purity metal contacting the cooled inner wall surface of the vessel body 2 is cooled to solidify so as to form a thin solidified layer or shell covering the entire area of the inner wall surface of the vessel body 2.
  • This solidified metal layer is stably held as long as the cooling of the vessel body 2 is continued. Since the thin solidified metal layer is of the same metal as the high-purity metal molten in the vessel body 2, there is no risk that the metal, i.e., copper constituting the vessel body 2 is molten to contaminate the molten high-purity metal in the vessel body 2.
  • the lid 6 is not substantially molten because it is cooled as the vessel body 2 is cooled. That is to say, the cooling of the vessel body 2 is so controlled as to satisfy also the demand to maintain the lid 6 in solid state. Upper part of the lid 6 contacting the molten high-purity metal may be molten but this does not cause any contamination of the molten high-purity metal because the lid 6 is of the same high-purity metal as that molten in the vessel body 2.
  • the high-purity metal molten in the vessel body 2 is then made to fall downward from the vessel body 2 for the purpose of, for example, production of the metal powder.
  • a beam such as a laser beam, electron beam or a plasma beam is applied to the center of the lid 6 by a beam generator 32 which is disposed right above the lid 6, so that the central portion of the lid 6 is molten by the beam energy so as to form an outlet 6b.
  • the molten high-purity metal is discharged through this outlet 6b.
  • the size of the outlet is easily adjustable by controlling the rate of cooling of the vessel body 2 and the beam power.
  • the described embodiment of the melting vessel and vessel forming method of the present invention contamination of the molten high-purity metal, which inevitably occurred in the known art, is avoided whole through the period of operation including the melting period and discharging period in which the molten high-purity metal is discharged downward.
  • the size of the outlet port for discharging the molten high-purity metal downward can easily be adjusted.
  • the described embodiments enables steady supply of a molten high-purity metal to a process such as a gas-atomizing powder production process, without any risk of contamination of the molten high-purity metal.
  • the present invention also provides an apparatus for producing powder of a high-purity metal by using the above-described melting vessel for high-purity metal.
  • the powder producing apparatus in order to attain uniform particle size of the powder, is embodied in various forms as stated below, with specific consideration of the size of the bottom outlet port formed in the lid, as well as the particle size distribution of the powder which is formed by gas-atomization effected on the molten high-purity metal discharged through the bottom outlet port.
  • Fig. 4 shows an embodiment of the powder production apparatus of the present invention, in which a control is done by adjusting the size or diameter of the outlet port formed in the bottom of the melting vessel.
  • a melting vessel is composed of a vessel body 2 and a lid 6.
  • the vessel body 2 is a substantially cylindrical cup-shaped bottom equipped vessel having an internal recess 8.
  • a tapered opening 10 is formed in the center of the bottom of the vessel body 2 so as to converge downward.
  • the vessel body 2 is double-walled so that an internal jacket space 12 is formed in communication with pipes 14 and 16 connected to the side wall of the vessel body 2.
  • the pipe 14 and the pipe 16 are respectively connected to a water supply pipe 22 and a water return pipe 24 of a cooling system 20 which constitutes cooling means.
  • the arrangement is such that cooling water is supplied through the pipe 14 into the jacket space 12 so as to cool the inner surface region of the vessel body 2 and then discharged and collected through the pipe 16.
  • the cooling system 20 supplies cooling water of a constant temperature and has a function to measure the calorific value removed by cooling per unit time (cooling rate) on the basis of the difference between the constant temperature of water supplied into the melting vessel and the temperature of the water collected therefrom, as well as functions to control the initial temperature of the cooling water to be supplied and the volume of the cooling water delivered per unit time.
  • the lid 6 is made of the same high-purity metal as the high-purity metal which is to be industrially molten in the melting vessel body 2.
  • the lid 6 has a tapered outer peripheral surface 6a which closely fits the tapered wall defining the opening 10 in the vessel body 2 thereby closing the opening 10.
  • Gas jetting devices 18, 18 disposed under the melting vessel body 2 have nozzles 18a, 18a which jet an inert gas such as Ar gas of a constant pressure to the stream of the molten high-purity metal discharged from the melting vessel body 2, thereby atomizing the molten metal to form particles of the high-purity metal.
  • an inert gas such as Ar gas of a constant pressure
  • a size measurement device 26 such as a camera, disposed near the bottom side of the melting vessel body 2, measures the size, e.g., diameter, of the outlet port formed in the center of the lid 6.
  • the size measuring device 26 is connected to a control device 30 serving as control means, through an analyzer 28 which performs image processing and other operations.
  • the measuring device 26 and the analyzer 28 in cooperation form a port diameter detecting means.
  • the control device 30 includes a central processing unit (CPU), a program ROM and various I/O interfaces.
  • a beam generating device 32 which is disposed right above the lid 6 emits and directs a beam towards the central portion of the lid 6.
  • the beam generating device 32 is connected to the control device 30 mentioned before.
  • the beam generating device 32 may be of the type which generates a laser beam, an electron beam, a plasma beam or an arc beam.
  • the control device 30 also is connected to the cooling system 20 to control the cooling rate.
  • the melting vessel body 2 is charged with an appropriate amount of high-purity metal and is molten by, for example, application of a voltage between the vessel body 2 and the high-purity metal to be molten, while the inner surface region of the vessel body 2 is cooled by a cooling medium such as water circulated through the jacket space 12.
  • a cooling medium such as water circulated through the jacket space 12.
  • the portion of the molten high-purity metal contacting the cooled inner wall surface 2a of the vessel body 2 is cooled to solidify so as to form a thin solidified layer or shell covering the entire area of the inner wall surface 2a of the vessel body 2.
  • This solidified metal layer is stably held as long as the cooling of the vessel body 2 is continued. Since the thin solidified metal layer is of the same metal as the high-purity metal molten in the vessel body 2, there is no risk that the metal, i.e., copper constituting the vessel body 2 is molten to contaminate the molten high-purity metal in the vessel body 2.
  • the lid 6 is not substantially molten because it is cooled as the vessel body 2 is cooled. That is to say, the cooling of the vessel body 2 is so controlled as to satisfy also the demand to maintain the lid 6 in solid state. Upper part of the lid 6 contacting the molten high-purity metal may be molten but this does not cause any contamination of the molten high-purity metal because the lid 6 is of the same high-purity metal as that molten in the vessel body 2.
  • a beam is applied by the beam generating device 32 to the central portion of the lid 6 so as to perforate the central region 6b of the lid 6 thereby forming an outlet port. Consequently, the molten high-purity metal inside the vessel body 2 progressively flows out downward through the outlet port, and the downward fall of the molten high-purity metal is cooled and solidified and, in addition, micronized upon collision with the inert gas jetted from the gas jetting devices 18, whereby a powder of the high-purity metal is produced continuously.
  • control device 30 operates to control either one or both of the beam power of the beam generating device 32 and the cooling device 20, based on information concerning the size of the outlet port derived from the measuring device 26 and the analyzer 28, so as to maintain the size of the outlet port constant.
  • control device 30 operates such that, for example, when the size of the outlet port is greater than an appropriate size, the cooling rate is increased to enhance the effect of cooling of the lid 6 thereby reducing the size of the outlet port, whereas, when the size of the outlet port is smaller than the appropriate value, the beam power is increased relative to the cooling rate so as to apply greater heat to the central region 6b of the lid 6 to enlarge the outlet port.
  • the size of the outlet port formed in the lid 6 is maintained constant, so that the molten high-purity metal is discharged steadily at a constant rate, thereby ensuring that the produced metal powder has high degree of uniformity of particle size.
  • the powder production apparatus shown in Fig. 5 lacks the size measuring device 26 and the analyzer 28 employed in the embodiment shown in Fig. 4 but, instead, incorporates a particle size measuring device 40 which constitutes particle size detecting means.
  • This particle size measuring device 40 measures particle size of the product powder by making use of laser diffraction. Part of the high-purity metal powder produced through the gas jetting devices 18, 18 is made to pass through the particle size measuring device 40 for measurement of the powder particle size.
  • the output data from the particle size measuring device 40 is delivered to the control device 30.
  • the process for producing high-purity metal powder in this embodiment is substantially the same as that in the embodiment shown in Fig. 4.
  • the control of the beam output and/or the cooling rate is conducted based upon the powder particle size obtained from the particle size measuring device 40, in contrast to the preceding embodiment of Fig. 4 in which the control is performed in accordance with the data concerning the size of the outlet port derived from the measuring device 26.
  • the embodiment shown in Fig. 5 ensures that the product powder has a high degree of uniformity of the particle size.
  • control device 30 operates such that, for example, when the measured powder particle size is greater than an appropriate size, the cooling rate is increased to enhance the effect of cooling of the lid 6 thereby reducing the size of the outlet port, whereas, when the size of the outlet port is smaller than the appropriate value, the beam power is increased relative to the cooling rate so as to apply greater heat to the central region 6b of the lid 6 to enlarge the outlet port.
  • high-purity metal used in this specification should be understood to cover not only pure metals but also alloys and intermetallic compounds.
EP93108457A 1992-05-25 1993-05-25 Réservoir de métal liquide ultra-pur, son procédé de fabrication ainsi que l'installation de production de poudre métallique très pure Expired - Lifetime EP0587993B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP13285692A JPH0730366B2 (ja) 1992-05-25 1992-05-25 高純度金属粉末の製造装置
JP132856/92 1992-05-25
JP132857/92 1992-05-25
JP4132857A JPH0791572B2 (ja) 1992-05-25 1992-05-25 高純度金属溶解用容器及びその製造方法

Publications (2)

Publication Number Publication Date
EP0587993A1 true EP0587993A1 (fr) 1994-03-23
EP0587993B1 EP0587993B1 (fr) 1998-08-12

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EP93108457A Expired - Lifetime EP0587993B1 (fr) 1992-05-25 1993-05-25 Réservoir de métal liquide ultra-pur, son procédé de fabrication ainsi que l'installation de production de poudre métallique très pure

Country Status (2)

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EP (1) EP0587993B1 (fr)
DE (1) DE69320278T2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT407846B (de) * 1998-11-18 2001-06-25 Boehler Edelstahl Metallurgisches gefäss
WO2013129996A1 (fr) * 2012-02-29 2013-09-06 Erasteel Kloster Ab Système de pulvérisation de métal et procédé pour atomiser une poudre métallique

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3665083A (en) * 1968-10-14 1972-05-23 Trw Inc Apparatus for melting titanium
EP0199199A2 (fr) * 1985-04-19 1986-10-29 General Electric Company Dispositif et procédé pur la fusion à l'arc plasma
EP0420393A1 (fr) * 1989-09-27 1991-04-03 Crucible Materials Corporation Système et méthode pour atomiser un matériau à base de titanium
EP0427379A2 (fr) * 1989-11-09 1991-05-15 Crucible Materials Corporation Procédé de préparation de poudre de titane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3665083A (en) * 1968-10-14 1972-05-23 Trw Inc Apparatus for melting titanium
EP0199199A2 (fr) * 1985-04-19 1986-10-29 General Electric Company Dispositif et procédé pur la fusion à l'arc plasma
EP0420393A1 (fr) * 1989-09-27 1991-04-03 Crucible Materials Corporation Système et méthode pour atomiser un matériau à base de titanium
EP0427379A2 (fr) * 1989-11-09 1991-05-15 Crucible Materials Corporation Procédé de préparation de poudre de titane

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT407846B (de) * 1998-11-18 2001-06-25 Boehler Edelstahl Metallurgisches gefäss
WO2013129996A1 (fr) * 2012-02-29 2013-09-06 Erasteel Kloster Ab Système de pulvérisation de métal et procédé pour atomiser une poudre métallique
US9707621B2 (en) 2012-02-29 2017-07-18 Erasteel Klister AB System for metal atomisation and method for atomising metal powder

Also Published As

Publication number Publication date
EP0587993B1 (fr) 1998-08-12
DE69320278D1 (de) 1998-09-17
DE69320278T2 (de) 1999-03-25

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