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WO2009153865A1 - Appareil et procédé de production de micropoudre - Google Patents

Appareil et procédé de production de micropoudre Download PDF

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Publication number
WO2009153865A1
WO2009153865A1 PCT/JP2008/061128 JP2008061128W WO2009153865A1 WO 2009153865 A1 WO2009153865 A1 WO 2009153865A1 JP 2008061128 W JP2008061128 W JP 2008061128W WO 2009153865 A1 WO2009153865 A1 WO 2009153865A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
rod
raw material
powder
heating
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.)
Ceased
Application number
PCT/JP2008/061128
Other languages
English (en)
Japanese (ja)
Inventor
浩章 岡
斉彰 岡
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.)
Sanki Dengyo Co Ltd
Original Assignee
Sanki Dengyo 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 Sanki Dengyo Co Ltd filed Critical Sanki Dengyo Co Ltd
Priority to PCT/JP2008/061128 priority Critical patent/WO2009153865A1/fr
Publication of WO2009153865A1 publication Critical patent/WO2009153865A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B22F9/10—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 using centrifugal force
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the 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
    • 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
    • B22F2009/0888—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 construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control

Definitions

  • the centrifugal spraying method and atomizing method (Japanese Patent Laid-Open No. 2006-2176, Japanese Patent Laid-Open No. 10-85583) adopted as a conventional fine powder production method have a very wide particle size distribution of the produced powder, and the fine powder
  • Japanese Patent Laid-Open No. 10-85583 adopted as a conventional fine powder production method have a very wide particle size distribution of the produced powder, and the fine powder
  • a centrifugal spraying method using a rotating crucible for the purpose of manufacturing for example, “a fine powder forming method using a rotating crucible and its apparatus (Japanese Patent Laid-Open No. 2007-332406)” has been proposed.
  • the atomization technology by melting and holding molten metal using levitation without using a ceramic crucible for the purpose of melting at a certain level or lower is well known ( Leviatomize process).
  • the Leviatomize process is a method of melting so that the molten metal does not contact the crucible by the interaction between the induction coil and the current induced in the molten metal by high-frequency induction, and the molten metal held in space vigorously fluctuates. Therefore, although there is no hindrance to the spraying method that does not require stable quasi-static pouring, it cannot be adopted in the spraying method that requires a quiet pouring flow with respect to the rotating crucible as in the present invention.
  • the present invention is a technique devised to solve these problems, and the molten material can be manufactured almost completely in a non-contact manner with the refractory, and the poured molten metal is placed in a rotating crucible. Because it is sprayed in an extremely short time of contact, contamination from the crucible is very slight even for active metals.
  • the present invention provides a spherical fine particle production apparatus that can be applied to a wide range of inorganic and organic substances used in the chemical industry, etc., and a production method using the centrifugal spray method.
  • the powder production method is such that the rod raw material is gripped by the support device (5) provided in the housing (1), charged into the crucible (6) disposed below, heated and melted, and the rod raw material is obtained.
  • the crucible is melted in the crucible, the inside of the crucible is heated from the inside, the crucible is rotated around its central axis, the rod raw material melted and dropped in the crucible is raised along the crucible wall, and the crucible is opened from the opening at the upper end of the crucible.
  • the powder manufacturing method is characterized in that the rod raw material melted by centrifugal force due to rotation is scattered in a spray form, the sprayed powder is cooled and collected in a product container (11) in the housing. .
  • MIM metal injection molding material
  • Titatan alloys are generally used as aircraft materials, chemical equipment materials, etc., but titanium is difficult to process, and powder metallurgy has attracted attention.
  • the conventional press-molding powder metallurgy method is used, but a metal powder injection molding method (Metal Injection Molding: hereinafter referred to as MIM) has been developed, in which the raw material powder is wrapped in a binder.
  • MIM Metal Injection Molding
  • the compact has a high density, a small surface roughness, and a spherical and dense fine powder with a high packing density is desirable in order to improve the density of the compact after sintering.
  • the spherical fine powder is more fluid. It's easy to do.
  • the production of the powder according to the present invention can provide a powder suitable for such use.
  • Heat can be efficiently heated on the inner surface of a rotating crucible that is reinforced with strength.
  • the shape of the crucible is relatively cylindrical, has a certain depth (H), and the opening diameter (D) has a D / H of about 10 to 0.5 (FIG. 2). This is because spraying becomes difficult when D exceeds 10, and uniform spraying cannot be performed when D is less than 0.5.
  • the molten metal poured in the vicinity of the crucible rotation center flows through the crucible inner surface with a liquid film of 1 mm or less, for example, by the centrifugal force of the crucible rotation, along the side surface from the bottom of the crucible. It is desirable to insert (Fig. 2).
  • the rotating crucible is heated from the inner surface by inserting a high-frequency induction coil into the crucible together with a susceptor such as carbon (Fig. 4)
  • a susceptor such as carbon
  • laser irradiation or a halogen lamp method using a condensing mirror (FIG. 5) can also be applied.
  • the shape of the crucible may be any shape that allows uniform spraying from a uniform opening,
  • the side wall is cylindrical, and the side wall may be within ⁇ 15 degrees about the vertical. If this range is exceeded, smooth and uniform spraying becomes difficult.
  • the induction coil for melting the raw material rod and the induction coil for rotating crucible heating independently using two high-frequency power sources. Both may be heated (dissolved) with a double coil.
  • two high-frequency power supplies are used, it may be impossible to control them when the generated frequencies are close to each other.
  • the target material The frequency of several tens of kilohertz to several megahertz is generally required, but the crucible heating uses a susceptor having conductivity such as carbon and the frequency of several kilohertz. And mutual interference between the two high-frequency power sources can be avoided.
  • various heating means can be considered as the means of sequential melting from the end of the rod-shaped raw material to be supplied, and the high frequency induction heating generally adopted in the FZ (floating zone) method of silicon single crystal is the most.
  • FZ floating zone
  • the carbon heater used was a cylindrical heater with slits in the vertical direction as shown in FIG.
  • the cylindrical heater is a cylindrical heater with a bottom, avoiding the pouring part near the center of the bottom so that the bottom of the crucible can also be heated (Fig. 3 (B)).
  • the rotating crucible was maintained at about 1150 ° C while applying 35,000 revolutions per minute.
  • Comparative Example 1 After melting 50 kg of pure titanium with a crucible containing CaO as the main component, the inner surface that comes into contact with the molten metal is poured out into a tundish made of ceramics containing CaO as the main component, and installed at the bottom. The nozzle was poured into a rotating crucible containing CaO as a main component at a predetermined speed. The material and rotation speed of the rotating crucible, the hot water supply speed to the rotating crucible, etc. were carried out under conditions as close to Example 1 as possible, and compared with the powder produced in Example 1.
  • Example 1 In addition, before the amount of remaining molten metal in the first melt completely disappeared, the melting was started for the second time while shutting off from the atmosphere using the raw material charging mechanism, and about 100 kg of powder was continuously processed.
  • the produced powder had a large degree of contamination as a whole compared with Example 1, and oxidation oxidation was particularly remarkable at the end of the pulverization treatment. This is presumed to be the result of about 1 hour having elapsed from dissolution to powdering treatment.
  • the particle size distribution of the produced powder was similar to Example 1.
  • Comparative Example 2 Using TD In the same manner as in Comparative Example 1, 50 kg of pure copper was dissolved twice and poured into a rotating crucible sequentially through a tundish. Since molten pure copper is less active than molten titanium, general materials mainly composed of MgO were selected for melting crucibles, tundish, and rotating crucibles. The particle size distribution of the produced powder was almost the same as that of Example 2, but the oxygen content was considerably larger than that of the powder obtained in Example 2. Table 1 summarizes the main test conditions and the characteristics of the produced powder for the three examples of the present invention and Comparative Examples 1 and 2. The particle size is smaller than that of the conventional method, the shape is spherical, and the particle size distribution width is small.
  • FIG. 6 shows an example of a photograph of the fine powder shape produced, which is very close to a perfect circle and shows that the diameter distribution is uniform. The invention's effect
  • Copper powder for conductive paste The powder to be used for the conductive pace is required to have a spherical shape and a fine size from the viewpoint of uniform coatability and fluidity, and the powder size is several microns in diameter.
  • the powder by can be desirably utilized.
  • Thermal spray material In addition to being able to obtain multi-layer coatings without heat effects, and directly coating materials and materials that are impossible with conventional technology, it is highly productive as a component manufacturing device, and the device cost is low. , Surface coating technology using “high-speed particle impact technology” has attracted attention, and Ti, Co, chromium-Nickel alloy, cemented carbide powder, etc. are used for aircraft engine parts for the purpose of improving heat resistance and oxidation resistance, It is used as a surface coating technology for generator turbine blades and boiler tubes.
  • fine powders of about 20 ⁇ m or less are preferable, and it is essential that the particles used are nearly spherical in order to prevent the scattering speed from being reduced during carrier transport by the carrier gas, and for the fluidity and deformation mechanism during particle collision. Furthermore, the demand for uniform particle size from the viewpoint of efficiency is strong, and it has been found that the powder produced by the present invention is desirable.
  • MIM metal injection molding material
  • Titatan alloys are generally used as aircraft materials and chemical equipment materials because they have the advantages of light weight and high strength, and have excellent corrosion resistance.
  • titanium is difficult to process, and aircraft.
  • the raw material powder is wrapped with a binder as a powder metallurgy method.
  • MIM Metal Injection Molding
  • spherical and dense fine powder with higher packing density is desirable, and spherical fine powder is more likely to flow. From the viewpoint of reducing product defects, spherical fine powder is indispensable.
  • the fine powder produced according to the present invention can be used as a material for such a method.
  • the present invention can be widely used as a fine powder production apparatus for plastics, medicines, foodstuffs and the like.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention porte sur un appareil de production de poudre comprenant un boîtier (ou chambre) (1), une unité de stockage de matière première en forme de bâtonnet (3) disposée dans le boîtier, une unité de support (5) pour saisir la matière première en forme de bâtonnet, l'introduire dans un creuset (6) disposé en dessous et maintenir l'ensemble pendant le chauffage et la fonte, des moyens de chauffage (7) pour faire fondre la matière première en forme de bâtonnet dans le creuset, des moyens (8) pour chauffer l'intérieur du creuset depuis l'intérieur, un dispositif rotatif (9) pour faire tourner le creuset autour de son axe central de façon à amener la matière première en forme de bâtonnet qui a fondu et s'est déversée dans le creuset à s'élever le long de la paroi du creuset et à se disperser sous forme pulvérisée à partir d'une ouverture de creuset en raison de la force centrifuge, et un conteneur pour produit (11) pour collecter un produit résultant de la dispersion sous forme pulvérisée et du refroidissement dans le boîtier.
PCT/JP2008/061128 2008-06-18 2008-06-18 Appareil et procédé de production de micropoudre Ceased WO2009153865A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/JP2008/061128 WO2009153865A1 (fr) 2008-06-18 2008-06-18 Appareil et procédé de production de micropoudre

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2008/061128 WO2009153865A1 (fr) 2008-06-18 2008-06-18 Appareil et procédé de production de micropoudre

Publications (1)

Publication Number Publication Date
WO2009153865A1 true WO2009153865A1 (fr) 2009-12-23

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PCT/JP2008/061128 Ceased WO2009153865A1 (fr) 2008-06-18 2008-06-18 Appareil et procédé de production de micropoudre

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2386371A1 (fr) * 2010-05-12 2011-11-16 Otto Hauser Procédé et dispositif destinés à la fabrication de poudre de métal
US10711339B2 (en) * 2008-12-18 2020-07-14 Arcelormittal France Industrial vapor generator for depositing an alloy coating on a metal strip
CN111906323A (zh) * 2020-08-13 2020-11-10 中天上材增材制造有限公司 一种用于高效在线连续生产的气雾化装置及其方法
CN113579240A (zh) * 2021-07-30 2021-11-02 深圳市中金岭南科技有限公司 一种金属合金的离心雾化制备装置及锌合金的制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60162703A (ja) * 1984-02-04 1985-08-24 Agency Of Ind Science & Technol 金属粉末の製造方法
JPH04123844A (ja) * 1990-09-10 1992-04-23 Daido Steel Co Ltd 金属の連続溶解鋳造方法および連続溶解鋳造装置
JPH0593213A (ja) * 1991-06-04 1993-04-16 Sumitomo Shichitsukusu Kk チタンおよびチタン合金粉末の製造方法
JPH06133988A (ja) * 1992-10-23 1994-05-17 Olympus Optical Co Ltd 歯科技工用鋳造機
JP2007332406A (ja) * 2006-06-13 2007-12-27 Sanki Dengyo Kk 回転ルツボを使用した微粉末成形方法とその装置

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60162703A (ja) * 1984-02-04 1985-08-24 Agency Of Ind Science & Technol 金属粉末の製造方法
JPH04123844A (ja) * 1990-09-10 1992-04-23 Daido Steel Co Ltd 金属の連続溶解鋳造方法および連続溶解鋳造装置
JPH0593213A (ja) * 1991-06-04 1993-04-16 Sumitomo Shichitsukusu Kk チタンおよびチタン合金粉末の製造方法
JPH06133988A (ja) * 1992-10-23 1994-05-17 Olympus Optical Co Ltd 歯科技工用鋳造機
JP2007332406A (ja) * 2006-06-13 2007-12-27 Sanki Dengyo Kk 回転ルツボを使用した微粉末成形方法とその装置

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10711339B2 (en) * 2008-12-18 2020-07-14 Arcelormittal France Industrial vapor generator for depositing an alloy coating on a metal strip
EP2386371A1 (fr) * 2010-05-12 2011-11-16 Otto Hauser Procédé et dispositif destinés à la fabrication de poudre de métal
CN111906323A (zh) * 2020-08-13 2020-11-10 中天上材增材制造有限公司 一种用于高效在线连续生产的气雾化装置及其方法
CN113579240A (zh) * 2021-07-30 2021-11-02 深圳市中金岭南科技有限公司 一种金属合金的离心雾化制备装置及锌合金的制备方法

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