WO1999033598A1 - Procede de production de poudre metallique - Google Patents

Procede de production de poudre metallique Download PDF

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Publication number
WO1999033598A1
WO1999033598A1 PCT/JP1998/005867 JP9805867W WO9933598A1 WO 1999033598 A1 WO1999033598 A1 WO 1999033598A1 JP 9805867 W JP9805867 W JP 9805867W WO 9933598 A1 WO9933598 A1 WO 9933598A1
Authority
WO
WIPO (PCT)
Prior art keywords
metal powder
molten metal
cooling liquid
nozzle
present
Prior art date
Application number
PCT/JP1998/005867
Other languages
English (en)
Japanese (ja)
Inventor
Masato Kikukawa
Shigemasa Matsunaga
Tsuneta Inaba
Osamu Iwatsu
Tohru Takeda
Original Assignee
Fukuda Metal Foil & Powder Co., Ltd.
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 Fukuda Metal Foil & Powder Co., Ltd. filed Critical Fukuda Metal Foil & Powder Co., Ltd.
Priority to KR1020007003025A priority Critical patent/KR100548213B1/ko
Priority to JP2000590804A priority patent/JP3999938B2/ja
Priority to PCT/JP1999/003338 priority patent/WO2000038865A1/fr
Priority to EP99926764A priority patent/EP1063038B1/fr
Priority to DE69936711T priority patent/DE69936711T2/de
Priority to US09/509,592 priority patent/US6336953B1/en
Priority to CNB998014036A priority patent/CN100364700C/zh
Publication of WO1999033598A1 publication Critical patent/WO1999033598A1/fr

Links

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 to a method for producing a metal powder, and more particularly, to a method for producing a metal powder that is fine, pseudo spherical, and has a narrow particle size distribution.
  • metal powders for manufacturing products such as injection molding materials, magnetic materials, and conductive materials have a significant effect on the characteristics of products manufactured using them, resulting in higher quality.
  • metal powder that is fine, pseudo-spherical and has a narrow particle size distribution.
  • the atomizing method of producing a metal powder by spraying a cooling medium (spraying medium) onto a molten metal stream is known as the ⁇ method of efficiently producing metal powders.
  • the atomization method using a gas as a cooling medium is called a gas atomization method
  • the atomization method using a liquid as a cooling medium is called a liquid atomization method.
  • the gas atomization method for example, a method using a nozzle described in U.S. Pat. No. L659.291 and U.S. Pat. No. 3,235.783 is known.
  • the dispersed molten metal droplet before solidification concentrates near the collision part of the liquid jet and the liquid jet. Cooling suddenly due to intense contact with Therefore, the dispersed molten metal droplet force, the metal powder obtained to contact and stick in a tuft
  • the end contains coarse particles, is irregularly shaped, and has a wide particle size distribution 0
  • Japanese Patent No. 552253 Japanese Patent Publication No. 43-6389
  • Japanese Patent Publication No. 3-55522 Japanese Patent Publication No. 2-56403
  • improvements of a conical jet type liquid atomizing method for example, Japanese Patent No. 552253 (Japanese Patent Publication No. 43-6389), Japanese Patent Publication No. 3-55522 and Japanese Patent Publication No. 2-56403 describe improvements of a conical jet type liquid atomizing method.
  • the invention described in Japanese Patent Publication No. 2-56403 is a technology for generating a liquid jet by injecting a cooling liquid from a tangential direction and a normal direction of a nozzle. Under such conditions, only coarse powder and metal powder can be obtained.
  • the present invention develops a new liquid jet having a form different from that of a conventional liquid jet, and applies the special liquid jet to a liquid atomization method to thereby obtain a conventional liquid jet. It is an object of the present invention to provide a technology capable of efficiently producing a finer, pseudospherical, and narrower particle size distribution metal powder than the atomization method.
  • the inventor of the present application has conducted various studies to solve the above-described problems, and as a result, in a metal powder manufacturing method of manufacturing a metal powder by spraying a cooling liquid onto a flowing molten metal stream, the cooling liquid includes the molten metal stream.
  • the cooling liquid includes the molten metal stream.
  • FIG. 1 is a transverse sectional view (a) and a longitudinal sectional view (b) of an operating state of an annular nozzle attached to a metal powder production apparatus of the present invention.
  • FIG. 2 is a perspective view conceptually showing a one-lobe hyperboloid liquid jet discharged from the annular nozzle shown in FIG.
  • FIG. 3 is an electron micrograph of a metal powder produced according to the present invention and the prior art.
  • FIG. 4 is a view showing a conventional liquid atomizing method.
  • FIG. 1 shows an embodiment of an annular nozzle 1 for carrying out the method for producing metal powder of the present invention.
  • FIG. 1 (a) is a cross-sectional view of the annular nozzle, and FIG. It is a longitudinal cross-sectional view.
  • the annular nozzle 1 shown in FIG. 1 is attached to a metal powder production apparatus such that the flowing molten metal stream 6 passes through the hole 2 of the annular nozzle.
  • the annular nozzle 1 has an inlet 3, a swirl chamber 4, and an annular slit 5.
  • the coolant injected from the inlet 3 swirls inside the swirl chamber 4 and then passes through the hole 2.
  • the molten metal is discharged from the ring-shaped slit 5 toward the molten metal flow.
  • this annular nozzle 1 Will be described in more detail.
  • the inlet 3 is provided along the diagonal of the swirl chamber 4 of the present nozzle, the coolant can be injected into the swirl chamber 4 at a high pressure.
  • the annular nozzle of the present invention it is sufficient for the annular nozzle of the present invention to have at least one inlet, but in the present embodiment, two inlets are provided so that the coolant can be introduced at a high E.
  • the inlet is not necessarily formed along the tangential direction of the swirl chamber, but may be formed in the normal direction of the swirl chamber.
  • the swirling chamber 4 is formed so as to surround the periphery of the hole 2 of the annular nozzle 1. Therefore, the cooling liquid injected into the swirling chamber 4 is discharged after swirling the periphery of the molten metal flow 6 passing through the litter section 2 in advance.
  • the outer peripheral portion in the swirling chamber 4 has a cavity region 7 free from obstacles so that the coolant injected from the inlet spreads throughout the swirling chamber. Therefore, the coolant can be injected into the annular nozzle at a high pressure.
  • a plurality of guide wings 8 are provided inside the above-mentioned hollow area ⁇ in the swirl chamber 4.
  • the guide vanes 8 serve to stabilize the flow of the coolant and to guide the coolant further inward while swirling. Then, the coolant is discharged from each part of the annular slit 5 formed along the inner surface of the hole 2 at a substantially uniform pressure.
  • a passage or a groove for turning the coolant into the swirl chamber is provided. It may be rotated in the evening or the like.
  • the coolant is guided toward the annular slit 5 while swirling in the swirl chamber 4, and the inside of the swirl chamber 4 gradually becomes narrower as approaching the annular slit 5.
  • the cooling liquid is discharged from the annular slit 5 as a high-speed liquid jet. If the liquid jet is released toward the molten gold flow passing through the hole 2, the position of the annular slit is not limited to the inner surface of the hole, but may be on the lower surface of the annular nozzle 1. It may be formed. Further, the present invention is not limited to a circular annular slit as shown in the drawings, but may have other shapes (for example, an elliptical shape or a rectangular shape). Etc.) may be used.
  • the liquid jet 13 discharged from the annular nozzle 1 has a single-leaf hyperboloid 9 as shown in FIG.
  • a virtual line 10 indicating the discharge direction of the liquid jet discharged from each part of the annular slit 5 is described in the one-lobe hyperboloid liquid jet shown in FIGS. 1 and 2.
  • the liquid jets 13 (imaginary lines 10) discharged from the respective portions of the annular slit 5 approach each other once, but flow so as to be crowded without colliding with each other.
  • the method for producing metal powder of the present invention is not limited to a method using an annular nozzle having a swirling chamber 4 and an annular slit 5 as shown in FIG.
  • the outlets of a plurality of pencil jet type nozzle parts 14 are arranged in an annular shape along the annular slit 5 in FIG. 1, and the liquid from each pencil jet type nozzle part along the imaginary line 10 is shown.
  • the jet may be emitted in a one-lobe hyperboloid.
  • a plurality of pencil jet type nozzle parts arranged in a ring form the ring nozzle of the present invention.
  • the use of the metal powder manufacturing apparatus having the annular nozzle 1 as described above makes it possible to efficiently produce a finer, pseudo-spherical, and narrower particle size distribution metal powder than the conventional liquid atomization method. .
  • the metal powder is produced as follows.
  • the liquid jet is discharged in a one-lobe hyperboloidal shape as described above.
  • this liquid jet is composed of an incompressible fluid, the energy density is high, and the liquid jet is in the middle. It can flow stably all the time without colliding with each other
  • the pressure inside the one-hyperboloid formed by the high-speed liquid jet decreases rapidly as it approaches the constriction. Therefore, the molten metal flow
  • the molten metal flow 6 is regularly and continuously dispersed with uniform energy until passing through the constricted portion 11, and the fine molten metal flows. Drops.
  • the dispersed molten gold droplets solidify into gold m powder, or in the present invention, these molten metal droplets can be solidified gently without contacting each other. In other words, even if the molten metal droplets become fine as described above, if the molten metal droplets come into contact with each other before solidification, the resulting gold powder becomes an irregular shape.
  • the molten metal droplet can pass through the constricted portion and move to the lower part of the one-lobe hyperboloid without contacting each other.
  • the molten metal droplet before solidification according to the present invention is essentially one-lobe hyperbolic; it is relatively slowly cooled without traversing, so that it becomes a sphere due to surface tension.
  • the molten gold droplets which are finely dispersed regularly and continuously at a uniform energy by the liquid jet are solidly and gently solidified without contacting each other. Therefore, it is considered that the present invention can efficiently produce a finer, pseudospherical, and narrower particle size distribution metal powder than the conventional method.
  • the flow rate of the liquid jet 13 is not particularly limited, but is not less than 10 Om / sec, more preferably not less than 130 m / sec, most preferably not less than I5 Om / sec, and more preferably Is preferably 20 m / sec or more.
  • the pressure inside the constricted part 11 of the liquid jet is 50 to 750 mmHg with respect to the atmospheric pressure.
  • the pressure is reduced to 100 to 750 mmHg, and optimally to 150 to 700 tnmHg (that is, 1 to 5 (h ⁇ -750 mmHg, more preferably to 100 to ⁇ 750 mmHg, optimally to 0 to Because the vapor pressure of the liquid exists, for example, when using water at normal temperature (2 O'C) as the cooling liquid, the pressure inside the constricted section should be large.
  • the discharge direction of the liquid jet is not particularly limited as long as the liquid jet is discharged in a one-lobe hyperboloidal shape. However, preferably, the liquid jet is discharged at a descent angle 0 and a swirl angle ⁇ described below.
  • the descending angle 0 and the turning angle ⁇ are defined as follows.
  • the velocity V of the liquid jet is defined as the velocity component V x in the tangential direction of the annular slit (X-axis direction in Fig. 4), the velocity component V in the normal direction of the circular slit (Y-axis direction in Fig. 4), , And the velocity component V, in the vertical direction (the z-axis direction in Fig. 3).
  • the turning angle ⁇ is defined as an angle formed by the resultant force of V x and V, with respect to the y-axis.
  • the descending angle 0 is defined as the angle formed by the resultant force of V y and V, with respect to the z-axis.
  • the turning angle ⁇ is 1 ° 30 °, and 3 ° ⁇ 20. Optimally, it is preferable that 5 ° ⁇ ⁇ ⁇ 20 °.
  • the descent angle 0 is 5 ° 60
  • the amount of coolant (ie, liquid jet) released per unit time with respect to the amount of molten metal flowing down per unit time is not particularly limited, and can be set arbitrarily.
  • (Flow rate of molten gold): (coolant discharge rate) is preferably 1: 2 to 100, more preferably 1: 3 to 50, and most preferably 1: 5 to 30. ing.
  • the present invention can be applied to any metal including a metal element, a metal compound, an alloy and an intermetallic compound. Further, according to the present invention, it is possible to produce a metal powder having desired characteristics by setting atomizing conditions according to the characteristics of a metal.
  • the relative apparent density of the metal powder obtained by the present invention is preferably 28% or more, more preferably 30 or more, and optimally 32% or more.
  • the relative tab density of the metal powder obtained by the present invention is preferably 45% or more, more preferably 50% or more, and most preferably 55% or more.
  • the median diameter of the metal powder is preferably 50 ⁇ or less, more preferably 35 m or less, optimally 25 // m or less, and most optimally 15 / m or less.
  • the metal powder has a median diameter of 25 m or less, the following fine powder having a specific particle size is contained in a predetermined ratio.
  • It contains at least 20% by weight, preferably 40% by weight or more, and most preferably 45% by weight or more of fine powder having a particle size of less than ⁇ 0 fim.
  • Fine powder having a diameter of IQ um or less is preferably at least 35% by weight or more. More than 45% by weight, optimally more than 50% by weight.
  • Fine powder having a particle size of 1 ⁇ m or less is contained at least 0.01% by weight or more, preferably 0.05% by weight or more, and most preferably 0.1% by weight or more.
  • the geometric standard deviation of the metal powder obtained by the present invention is preferably 3.0 or less, more preferably 2.5 or less, and most preferably 2.3 or less.
  • the width of the particle size distribution can be evaluated by the geometric standard deviation.
  • the specific surface area of the metal powder obtained by the present invention is preferably 4000 cm 2 / g or less, more preferably 3000 cmVg or less, and most preferably 2500 cm 2 / g or less.
  • metal powder was manufactured according to the conventional method using a conventional nozzle for generating a conical jet (Comparative Examples 1 to 8). Table 1 shows these atomizing conditions.
  • the pressure in the constriction was measured using a pipe with a cross-sectional area of 20 mm or less of the cross-sectional area in the constriction.
  • a pressure gauge is connected to one opening of the pipe. Then, the pipe was inserted from above along the central axis 12 of the one-lobe hyperboloid such that the other opening of the pipe was positioned inside the constricted portion 11. Also The velocity of the liquid jet was calculated from the cooling injection pressure measured at the inlet 3 by using Bernoulli's theorem.
  • the relative tap density was calculated based on (tap density) x 10 (true density) x 100.
  • the median diameter was measured using a laser diffraction scattering method (volume) using a micro track manufactured by Nikkiso Co., Ltd.
  • the content of fine powder having a diameter of 10 m, 5 m and 1 / m or less in the metal powder was measured by using a laser diffraction scattering method (volume%).
  • the specific surface area was measured according to the BET method of the gas phase adsorption method.
  • the oxygen content was measured according to the non-dispersive infrared absorption method.
  • Yield is the percentage of the metal powder having a particle size of 45 / m or less in the metal powder having a particle size of 1 mm or less selected according to J ISZ8801.
  • the metal powder according to the present invention is significantly different from the metal powder of the comparative example in that the metal powder contains a through powder of 1 m or less within a range that can be confirmed by a laser diffraction scattering method.
  • the geometric standard deviation of the metal powder according to the invention is smaller than in the comparative example. This indicates that the width of the abundance distribution of the metal powder obtained by the present invention is narrower than that of the metal powder of the comparative example.
  • the oxygen content of the metal powder according to the present invention is smaller than that of the comparative example. This is considered to be because the metal powder of the present invention has a pseudospherical shape, so that the surface contact is small and oxidation is difficult.
  • the yield according to the invention is higher than in the comparative example.
  • the molten metal stream is regularly and continuously dispersed by the liquid jet, and the dispersed molten metal is cooled slowly without contacting each other. From the t electron micrograph, it is clear that the edges of the metal powder of the present invention have been removed, and that the metal powder of the present invention is more pseudospherical than the metal powder of the comparative example.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un procédé permettant de produire de la poudre métallique par pulvérisation d'un liquide de refroidissement sur un écoulement de métal en fusion. Ce procédé se caractérise par le fait que ce liquide de refroidissement est éjecté en continu vers l'écoulement de métal en fusion, lequel traverse une buse en forme d'anneau disposée de manière à entourer ledit écoulement de métal en fusion sous la forme d'un hyperboloïde à une nappe. Cette invention permet de produire efficacement une poudre métallique à la fois fine et pseudosphérique, qui présente en outre de répartition particulaire sur une faible largeur.
PCT/JP1998/005867 1997-12-25 1998-12-24 Procede de production de poudre metallique WO1999033598A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
KR1020007003025A KR100548213B1 (ko) 1998-12-24 1999-06-23 금속 분말 제조 방법 및 장치
JP2000590804A JP3999938B2 (ja) 1998-12-24 1999-06-23 金属粉末製造方法
PCT/JP1999/003338 WO2000038865A1 (fr) 1998-12-24 1999-06-23 Procede de fabrication de poudre metallique
EP99926764A EP1063038B1 (fr) 1998-12-24 1999-06-23 Procede et appareil de fabrication de poudre metallique
DE69936711T DE69936711T2 (de) 1998-12-24 1999-06-23 Verfahren und vorrichtung zum herstellen von metallpulver
US09/509,592 US6336953B1 (en) 1998-12-24 1999-06-23 Method for preparing metal powder
CNB998014036A CN100364700C (zh) 1998-12-24 1999-06-23 制备金属粉末的方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP35647397 1997-12-25
JP9/356473 1997-12-25

Publications (1)

Publication Number Publication Date
WO1999033598A1 true WO1999033598A1 (fr) 1999-07-08

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1998/005867 WO1999033598A1 (fr) 1997-12-25 1998-12-24 Procede de production de poudre metallique

Country Status (1)

Country Link
WO (1) WO1999033598A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017031462A (ja) * 2015-07-31 2017-02-09 Ｊｆｅスチール株式会社 水アトマイズ金属粉末の製造方法
JP6533352B1 (ja) * 2018-07-27 2019-06-19 株式会社東北マグネットインスティテュート 高速流体噴射装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01123012A (ja) * 1987-11-09 1989-05-16 Kawasaki Steel Corp 微粉製造用ノズル
JPH04131451U (ja) * 1991-05-24 1992-12-03 三井三池化工機株式会社 ノズル構造
JPH0622338U (ja) * 1992-05-29 1994-03-22 日新技研株式会社 粉末作製装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01123012A (ja) * 1987-11-09 1989-05-16 Kawasaki Steel Corp 微粉製造用ノズル
JPH04131451U (ja) * 1991-05-24 1992-12-03 三井三池化工機株式会社 ノズル構造
JPH0622338U (ja) * 1992-05-29 1994-03-22 日新技研株式会社 粉末作製装置

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017031462A (ja) * 2015-07-31 2017-02-09 Ｊｆｅスチール株式会社 水アトマイズ金属粉末の製造方法
JP6533352B1 (ja) * 2018-07-27 2019-06-19 株式会社東北マグネットインスティテュート 高速流体噴射装置
WO2020021701A1 (fr) * 2018-07-27 2020-01-30 株式会社東北マグネットインスティテュート Dispositif d'éjection de fluide haute vitesse

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