WO2010146680A1 - 磁性粉末の製造方法及びその製造装置 - Google Patents

磁性粉末の製造方法及びその製造装置 Download PDF

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Publication number
WO2010146680A1
WO2010146680A1 PCT/JP2009/061076 JP2009061076W WO2010146680A1 WO 2010146680 A1 WO2010146680 A1 WO 2010146680A1 JP 2009061076 W JP2009061076 W JP 2009061076W WO 2010146680 A1 WO2010146680 A1 WO 2010146680A1
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Prior art keywords
magnetic powder
metal
hard magnetic
chamber
producing
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PCT/JP2009/061076
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English (en)
French (fr)
Japanese (ja)
Inventor
宮本典孝
大村真也
真鍋明
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トヨタ自動車株式会社
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Priority to PCT/JP2009/061076 priority Critical patent/WO2010146680A1/ja
Priority to CN200980159907.XA priority patent/CN102804296B/zh
Priority to JP2011519359A priority patent/JP5267665B2/ja
Priority to EP09846173.4A priority patent/EP2444984B1/de
Publication of WO2010146680A1 publication Critical patent/WO2010146680A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • B22F1/17—Metallic particles coated with metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
    • 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
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/003—Apparatus, e.g. furnaces
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/08—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/086—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together sintered

Definitions

  • the present invention relates to a method for manufacturing magnetic powder and an apparatus for manufacturing the same, and more particularly, to a method for manufacturing magnetic powder suitable for manufacturing a sintered magnet having excellent magnetic properties and an apparatus for manufacturing the same.
  • Permanent magnets obtained by sintering magnetic powder such as Nd—Fe—B system have been widely used in recent years due to their excellent magnetic properties. Permanent magnets such as Nd 2 Fe 14 B system in which such powder is sintered as the range of application of magnets has expanded to respond to environmental problems, including home appliances, industrial equipment, electric vehicles, and wind power generation. There is a demand for higher performance.
  • the magnitude of the residual magnetic flux density and the coercive force can be given.
  • increasing the residual magnetic flux density of an Nd—Fe—B based sintered magnet can be achieved by increasing the volume fraction of the Nd 2 Fe 14 B compound and improving the degree of crystal orientation.
  • Various process improvements have been made to achieve this.
  • the coercive force in order to increase the coercive force, it can be achieved by various approaches, such as a method of refining crystal grains, a method using a composition alloy with an increased amount of Nd, or a method of adding an effective element. Can do.
  • the most common technique is to increase the coercive force by using a composition alloy in which a part of Nd is substituted with Dy or Tb. Specifically, by substituting these elements for Nd in the Nd 2 Fe 14 B compound, the anisotropic magnetic field of the compound increases, thereby increasing the coercive force.
  • Tb can be cited as a rare earth element that exhibits the same effect as Dy for the purpose of achieving a high coercive force, but the abundance of Tb is much lower than Dy.
  • the coercive force of Nd—Fe—B based sintered magnets has been significantly improved compared to the early stage of development by adding such a trace amount of elements and searching for heat treatment conditions. Accordingly, in view of such an improvement effect, it is unavoidable to reduce the amount of Dy or Tb added as a trace element.
  • a technique is employed in which Dy and Tb are concentrated only at the grain boundaries of the magnet or in the vicinity thereof.
  • a two-alloy method is proposed in which a powder in which Dy and Tb are contained in a larger amount than the main phase (Nd 2 Fe 14 B) and a powder in which these elements are not mixed are sintered in advance (for example, a patent) Reference 1).
  • a method is proposed in which a fluorine compound such as Dy or Tb is applied to the surface of a sintered magnet, and Dy or Tb is diffused and penetrated into grain boundaries near the surface by heat treatment (for example, Patent Documents). 2).
  • the particle size of hard magnetic powders for sintering rare earth magnets at present is about 3 to 5 ⁇ m, and these transition elements (transition metals) and the like are magnetic powders having a thickness of several nanometers to several tens of nanometers. It is extremely difficult to uniformly coat around.
  • rare earth metals easily react with moisture, and basically, it is difficult to coat rare earth metals around powders in a wet environment.
  • magnetic powders of about 3 to 5 ⁇ m tend to agglomerate with each other and form solidified particles with these dozens of magnetic powders, and the surface of each magnetic powder can be uniformly coated with transition elements. It's not easy.
  • this hard magnetic powder due to the nature of rare earth metal, it is a fine powder with a particle size of 3-5 ⁇ m. It is difficult to avoid surface oxidation of the powder. And when a sintered magnet is molded using magnetic powder whose surface has been oxidized, the magnetic properties are lowered. Moreover, even if it carries out by a dry type, the aggregation of the magnetic powder mentioned above cannot be avoided.
  • the present invention has been made in view of the above-described problems, and the magnetic properties of a sintered magnet can be improved by uniformly coating the surface of a hard magnetic powder with a metal such as a transition metal. It aims at providing the manufacturing method of a powder, and the manufacturing apparatus of a magnetic powder.
  • the inventors have made extensive studies and as a principle of attaching a metal such as a transition metal to the surface of the hard magnetic powder, pay attention to the thermophoresis phenomenon and use this phenomenon. As a result, a new finding has been obtained that a small amount of metal can be uniformly attached (coated) to the surface of the magnetic powder.
  • the present invention is based on the inventors' new knowledge, and a method for producing a magnetic powder according to the present invention includes a step of aerosolizing a hard magnetic powder with an inert gas, and a metal under an inert gas atmosphere. Heating and vaporizing, and attaching the vaporized metal to the surface of the aerosolized hard magnetic powder.
  • an aerosol of hard magnetic powder is generated, and the aerosolized hard magnetic powder is dispersed in an inert gas (aerosol). Then, vaporized metal is attached to the surface of the dispersed magnetic powder in an inert gas atmosphere. At this time, the vaporized metal, that is, the vapor particles of the metal has a higher temperature than the hard magnetic powder. Since there is a large thermal gradient between the hard magnetic powder and the vapor particles, the vapor particles having a higher temperature than the hard magnetic powder exert a force (thermophoretic force) to be attracted to the hard magnetic powder having a lower temperature. . As a result, the vapor particles are densely and firmly adsorbed (coated) on the surface of the magnetic powder. In addition, since the vaporized metal (vapor particles) is several tens of nanometers and smaller than the hard magnetic powder, a small amount of vapor particles are uniformly distributed on the surface of the hard magnetic powder as compared with the conventional method. Can be attached.
  • aerosol refers to a substance in which a large number of hard magnetic powders are floated in a gas
  • aerosolization means that a number of hard magnetic powders are floated in a gas.
  • the “hard magnetic powder” according to the present invention is a powder that does not retain magnetization when a magnetic field is removed after applying a magnetic field, and is a powder for producing a permanent magnet.
  • the powder that remains magnetized even if the magnetic field is removed and the magnetized state is maintained is soft magnetic powder.
  • examples of the inert gas include He, N 2 , and Ar gases, and are particularly limited as long as they do not oxidize the hard magnetic powder and the vaporized metal (vapor particles). is not.
  • the deposition method is not particularly limited as long as the vaporized metal can be adhered to the surface of the aerosolized hard magnetic powder.
  • the aerosolized hard magnetic powder and the vaporized metal are carried in an air stream, and the vaporized metal is allowed to collide with the aerosolized hard magnetic powder.
  • the flow velocity of the vaporized metal air flow is more preferably equal to or higher than the flow velocity of the aerosolized hard magnetic powder.
  • the vaporized metal (vapor particles) is several tens of nanometers as described above, and when the vapor particles are carried in an air stream, compared to the hard magnetic powder. Almost accelerated. Thereby, the vaporized metal can be collided with the aerosolized hard magnetic powder with higher energy. In this way, the vapor particles can be more firmly and densely attached to the surface of the hard magnetic powder.
  • the aerosolized hard magnetic powder is placed on the airflow means that the aerosol of the hard magnetic powder itself is transported.
  • the metal to be attached to the hard magnetic powder for use in the method for producing the magnetic powder of the present invention is preferably a transition metal or an alloy metal thereof.
  • a more preferable transition metal is a rare earth metal (third transition element (4f transition element)), and among these, Dy, Tb, or Pr is more preferable. Since these rare earth metals are elements having a higher anisotropic magnetic field than other metals, the magnets produced thereby can improve the magnetic properties.
  • the metal to be deposited may be an alloy metal of Dy, Tb or Pr and Nd. These alloy metals are easy to dissolve into the grain boundaries as compared with Dy, Tb or Pr alone.
  • other metals to be deposited include Al, Cu, Zn, In, Si, P, S, Ti, V, Cr, Mn, Ni, Co, Ga, Ge, Zr, Nb, Mo, Pd, Examples thereof include Ag, Cd, Sn, Sb, Hf, Ta, W, and alloy metals thereof.
  • a highly anisotropic metal or a nonmagnetic metal is desirable, and Al and Cu are more preferable. Both Al and Cu are easily melted into a magnet during sintering, and can form a Nd-rich phase and a low-melting eutectic alloy to improve the wettability at the grain boundary. Since it can be made discontinuous, the magnetic properties can be improved.
  • the hard magnetic powder is not particularly limited as long as it can produce a permanent magnet by sintering.
  • R 2 Tm 14 (B, C) 1 series examples thereof include magnetic powder (R is a rare earth metal, Tm is a transition metal excluding the rare earth metal, etc.).
  • the rare earth metal include Sc, Y, La, Ce, Pr, Sm, Eu, Gd, Ho, Er, Yb, and Lu.
  • transition metals excluding rare earth metals Al, Cu, Zn, In, Si, P, S, Ti, V, Cr, Mn, Ni, Co, Ga, Ge, Zr, Nb, Mo, Pd, Ag, Cd, Sn, Sb, Hf, Ta, W, etc. can be mentioned.
  • the hard magnetic powder is an Nd—Fe—B based magnetic powder. According to the present invention, such a magnetic powder has a higher holding force and excellent magnetic properties than other combinations.
  • the magnetic powder thus produced is suitable for use as a magnet by sintering.
  • An apparatus for producing a magnetic powder suitable for producing the above-described magnetic powder includes an aerosol chamber for aerosolizing a hard magnetic powder with an inert gas, a vapor generation chamber for heating and vaporizing a metal in an inert gas atmosphere, and the vaporized metal It is characterized by comprising: an attaching portion for attaching the metal to the surface of the aerosolized hard magnetic powder; and a discharge chamber for releasing the hard magnetic powder to which the metal is attached.
  • the hard magnetic powder can be aerosolized with an inert gas in the aerosol chamber, while the metal can be heated and vaporized in an inert gas atmosphere in the vapor generation chamber. Then, the vaporized metal can be adhered to the surface of the aerosolized hard magnetic powder at the adhesion portion, and the hard magnetic powder with the metal adhered can be discharged in the discharge chamber. At this time, the vaporized metal can be uniformly adsorbed on the surface of the hard magnetic powder dispersed in the aerosol by the thermophoretic phenomenon described above.
  • the apparatus for producing the magnetic powder according to the present invention is not particularly limited as long as the vaporized metal can be adhered to the surface of the aerosolized hard magnetic powder.
  • the adhering portion includes a main transfer pipe connected to the aerosol chamber, and a sub-transfer pipe connected to the vapor generation chamber,
  • the sub-transport pipe is connected to the main transport pipe so that the vaporized metal can adhere to the hard magnetic powder.
  • the aerosolized hard magnetic powder is carried by the main carrier tube on the air stream and conveyed toward the discharge chamber (the aerosol itself is conveyed toward the discharge chamber), and the sub-carrier tube is used for vaporization.
  • the converted metal (vapor particles) can be carried in an air stream and conveyed toward the discharge chamber.
  • the sub-transport pipe is connected to the main transport pipe so that the vapor particles can adhere to the hard magnetic powder, so that the vapor particles can collide with the aerosolized hard magnetic powder.
  • the number of the steam generation chambers is not particularly limited, but more preferably, the magnetic powder manufacturing apparatus according to the present invention includes the steam generation chamber and the sub-transport pipe connected to the steam generation chamber. And the plurality of sub-transport pipes are connected to the outer periphery of the main transport pipe at equal intervals.
  • a plurality of pairs of steam generation chambers and sub-transport pipes are provided, and each sub-transport pipe is connected (flighted) to the outer circumference of the main transport pipe at equal intervals.
  • Vapor particles can be uniformly and uniformly attached to the surface of the hard magnetic powder contained in the aerosol. Further, since different metals can be vaporized in the plurality of vapor generation chambers, a multifunctional magnetic powder can be produced.
  • the magnetic powder manufacturing apparatus more preferably includes a tube heating unit for heating the sub-transport tube.
  • a tube heating unit for heating the sub-transport tube.
  • the aerosol chamber and the steam generation chamber of the manufacturing apparatus are provided with a supply pipe for supplying the inert gas, and the supply pipe removes oxygen contained in the inert gas. More preferably, an oxygen removing device is provided.
  • the oxidation of the hard magnetic powder and the vapor particles can be suppressed by reducing the oxygen concentration contained in the inert gas.
  • vapor particles of rare earth metals are preferable because they are easily oxidized.
  • the magnetic properties of a sintered magnet using this powder can be improved by uniformly coating the surface of the hard magnetic powder with a metal such as a transition metal.
  • FIG. 1 It is a whole block diagram of the manufacturing apparatus of the magnetic powder which concerns on 1st embodiment. It is a schematic diagram of the magnetic powder manufactured by the manufacturing method of the magnetic powder which concerns on 1st embodiment.
  • FIG. 2nd embodiment (a) is a whole block diagram of the manufacturing apparatus of magnetic powder, (b) is b part shown to (a).
  • C) is an AA ′ cross-sectional view of (b).
  • SYMBOLS 11 Hard magnetic powder supply source, 12 ... Powder supply piping, 13a ... Oxygen removal apparatus, 13b ... Oxygen removal apparatus, 16 ... Inert gas piping, 17 ... Inert gas piping, 18 ... Cooler, 20 ... Aerosol chamber, DESCRIPTION OF SYMBOLS 21 ... Aerosol production
  • Transport pipe 49 ... Nozzle section, 50 ... Release chamber, 53: Receiving section, 58 ... Inert gas pipe, 100 ... Magnetic powder production equipment, 100A ... Magnetic powder production equipment, AG ... Aerosol, P ... Hard magnetic powder, PV ... Magnetic powder, V ... Vapor particles (vaporized metal)
  • FIG. 1 is an overall configuration diagram of a magnetic powder manufacturing apparatus according to the first embodiment for suitably performing the magnetic powder manufacturing method according to the present invention.
  • FIG. 2 is a schematic view of a magnetic powder produced by the magnetic powder production method according to the first embodiment.
  • the magnetic powder manufacturing apparatus 100 includes at least an aerosol chamber 20, a vapor generation chamber 30, an attachment portion 40, and a discharge chamber 50.
  • the aerosol chamber 20 is a chamber for aerosolizing the hard magnetic powder with an inert gas, and the aerosol chamber 20 is provided with a jet mill or the like via the powder supply pipe 12 to supply the hard magnetic powder P into the chamber. It is connected to a hard magnetic powder supply source 11 having both a pulverizer and an air classifier.
  • the aerosol chamber 20 is provided with an aerosol generating unit 21 that aerosolizes the hard magnetic powder P supplied into the chamber, that is, generates an aerosol of the hard magnetic powder P below the chamber.
  • the aerosol generation unit 21 is connected to the inert gas pipe 16 and is disposed in the aerosol generation unit 21 so as to be able to release the inert gas G3 toward the bottom of the room in order to make the hard magnetic powder into an aerosol.
  • a plurality of discharge ports 21a are formed.
  • the aerosol generation unit 21 may be, for example, a mechanism used in the aerosol deposition technique.
  • a mechanism for stirring the hard magnetic powder P with the inert gas G3 or a container containing the hard magnetic powder P may be used.
  • a mechanism for swinging can be used.
  • the inert gas pipe 16 is connected with an oxygen removing device 13a for removing oxygen gas contained in the inert gas G3 and a gas cooler 18 for cooling the inert gas G3. Furthermore, the aerosol chamber 20 is connected to an inert gas pipe 17 that replaces the gas in the chamber with the inert gas G2, and the inert gas pipe 17 similarly contains oxygen gas contained in the inert gas G2. An oxygen removing device 13a for removal is connected.
  • the inside of the aerosol chamber 20 is set to be pressurized to a pressure (120,000 Pa or less) higher than that of the discharge chamber 50 described later by the inert gas G2, and the aerosol chamber 20 and the discharge chamber 50 are separated from each other. Due to the differential pressure, the aerosolized hard magnetic powder in the aerosol chamber 20 can be conveyed to the discharge chamber 50.
  • the inert gases G2, G3 supplied into the aerosol chamber 20 are gases such as He, N 2 , or Ar, and it is desirable that these gases have a purity of 99.999% or more.
  • the oxygen concentration in the gas is preferably at least 1.0 ⁇ 10 ⁇ 6 atmO 2 or less in terms of partial pressure.
  • the upper part of the aerosol chamber 20 is connected to a main transport pipe 41 that constitutes an adhesion portion 40 described later, and this main transport pipe 41 is a pipe that transports the aerosolized hard magnetic powder P.
  • the steam generation chamber 30 is a chamber for heating and vaporizing rare earth metals such as Dy, Tb, or Pr, and other transition metals.
  • Dy is used as the rare earth metal.
  • the steam generation chamber 30 includes a metal melting furnace 32 and a heating device 33 that heats and melts the metal in the metal melting furnace 32.
  • the heating device 33 is not particularly limited as long as the metal in the metal melting furnace 32 can be melted.
  • examples of the heating method include heat ray melting, high frequency melting, arc melting, laser heating melting, and electron beam melting.
  • the vapor generation chamber 30 is pressurized to a pressure higher than that of the discharge chamber 50, which will be described later, by the inert gas G 2, and is pressurized to a pressure equal to or higher than the pressure of the aerosol chamber 20.
  • a shutter for making the inside of the aerosol chamber 20 a sealed space may be provided.
  • the vaporized metal in the steam generation chamber 30 can be transported to the discharge chamber 50 due to the differential pressure between the steam generation chamber 30 and the discharge chamber 50.
  • the flight speed of the vaporized metal (evaporated particles) V flying in the sub-transport pipe 42 is higher than the flight speed of the hard magnetic powder P flying in the main transport pipe 41. Can also be faster.
  • the pressure of the steam generating chamber 30, the following inert gas atmosphere 120000Pa, the oxygen concentration of the gas it is desirable to at least 1.0 ⁇ 10 -8 atm0 2 or less at a partial pressure.
  • the aerosol chamber 20 and the vapor generation chamber 30 are connected to a vacuum exhaust system including a vacuum pump through an exhaust pipe 25. Thereby, the gas in the aerosol chamber 20 and the vapor generation chamber 30 can be easily replaced with the inert gas G2.
  • the adhering portion 40 is a portion for adhering the vaporized metal V to the surface of the hard magnetic powder P that has been aerosolized.
  • the attachment unit 40 includes a main transport pipe 41 connected to the upper part of the aerosol chamber 20 and a sub-transport pipe 42 connected to the upper part of the vapor generation chamber 30. Further, the adhering portion 40 forms a confluence portion 45 in which the sub conveying pipe 42 is connected to the main conveying pipe 41 so that the vaporized metal V can adhere to the hard magnetic powder P. Further, a nozzle portion 49 extending from below the discharge chamber 50 to the inside thereof is formed further downstream of the merge portion 45.
  • the discharge chamber 50 is a chamber for discharging (jetting) hard magnetic powder (magnetic powder) PV to which metal is adhered.
  • the discharge chamber 50 has such a size that the magnetic powder PV naturally falls without colliding with the indoor wall surface due to the differential pressure between the aerosol chamber 20 and the vapor generation chamber 30.
  • the discharge chamber 50 is provided with a receiving portion 53 for receiving the dropped magnetic powder PV.
  • the discharge chamber 50 is connected to the vacuum exhaust system via the exhaust pipe 25, whereby the discharge chamber 50 is connected to 1.0 ⁇ 10 ⁇ 6.
  • a vacuum of atm or less is desirable.
  • the aerosol chamber 20 and the steam generating chamber 30 it may be a room in an inert gas atmosphere, in this case, an inert gas, to an oxygen concentration of 1.0 ⁇ 10 -7 atm0 2 below Is effective.
  • the discharge chamber 50 is connected to a gas circulation system via a gas circulation pipe 54 in order to reuse the inert gas.
  • the aerosol chamber 20 and the vapor generation chamber 30 are evacuated, and an inert gas is introduced into these chambers through the oxygen removing device 13b, whereby these chambers are made an inert gas atmosphere.
  • the pressure in the aerosol chamber 20 and the vapor generation chamber 30 is 120,000 Pa or less
  • the oxygen concentration is 1.0 ⁇ 10 ⁇ 7 to 10 ⁇ 8 atmO 2 or less
  • the pressure in the vapor generation chamber 30 is the aerosol.
  • the pressure in the chamber 20 is increased.
  • the inside of the discharge chamber 50 is evacuated to a pressure lower than that of the aerosol chamber 20 and the vapor generation chamber 30. At this time, if there is a shutter in each chamber, this is used to achieve the set pressure.
  • an Nd—Fe—B system (Nd 2 Fe 14 B) classified into an average particle size of 1 to 10 ⁇ m from a hard magnetic powder supply source 11 such as a jet mill through a powder supply pipe 12.
  • the hard magnetic powder P is supplied into the aerosol chamber 20.
  • the inert gas G3 is cooled by the gas cooler 18, cooled to a temperature of about 20 ° C., and the cooled inert gas G3 is removed. Introduced into the aerosol generator 21.
  • the cooled inert gas G3 is discharged from the plurality of discharge ports 21a of the aerosol generating unit 21 toward the bottom of the aerosol chamber 20, and the hard magnetic powder P at the bottom is shaken and stirred, and the aerosol Floating in the chamber 20, an aerosol of magnetic particles is generated (the hard magnetic powder P is aerosolized).
  • the rare earth metal Dy disposed in the metal melting furnace 32 in the steam generation chamber 30 is heated by the heating device 33 to be vaporized.
  • the aerosolized hard magnetic powder P is transported in the main transport pipe 41 toward the discharge chamber 50 due to a differential pressure with the discharge chamber 50.
  • the vaporized metal (vapor particles) V is also transported in the sub transport pipe 42 toward the discharge chamber 50.
  • the hard magnetic powder P that has been aerosolized by the main transport pipe 41 is carried on the airflow and transported toward the discharge chamber 50 (the aerosol itself is transported toward the discharge chamber 50), and the sub-transport pipe By 42, the vapor particles V are carried on the airflow and conveyed toward the discharge chamber 50. And since the sub conveyance pipe 42 is connected to the main conveyance pipe 41 so that the vapor particle V can adhere to the hard magnetic powder P, the vapor particle V is converted into the vapor particle V at the junction 45 of the adhesion part. Can collide with.
  • the aerosolized hard magnetic powder P is cooled by the cooler 18, while the vapor particles V are vaporized by heating, and therefore, as shown in the schematic diagram of FIG. Vapor particles V having a size of about 1 nm to 100 nm can be attached to the surface of the hard magnetic powder P classified in the range of 1 to 10 ⁇ m.
  • the vapor particles V collide with the hard magnetic powder P due to its thermal motion under the condition that the hard magnetic powder P is suspended in the gas.
  • the vapor particles V having a higher temperature than the hard magnetic powder P have a force so as to be attracted to the hard magnetic powder P having a low temperature. (Thermophoretic force) is exerted.
  • the vapor particles V are densely and firmly attached (coated) to the surface of the hard magnetic powder P.
  • the aerosolized hard magnetic powder P has a particle size on the order of several ⁇ m, and the vapor particles V have a particle size on the order of several tens of nm, the vapor particles V are smaller than the hard magnetic powder P. Therefore, it is easy to get on the airflow and is accelerated. That is, the flight speed of the vapor particles V is faster than the flight speed of the hard magnetic powder P due to the above-described differential pressure in each chamber and the size of the particles. Thereby, the vapor particles V can be densely and firmly attached to the surface of the hard magnetic powder P. In this way, the vapor particles V adhere to the surface of the hard magnetic powder P as shown in FIG.
  • the hard magnetic powder (hard magnetic powder coated with Dy particles) PV to which the vapor particles V adhere is discharged into the discharge chamber 50 through the nozzle portion 49, and the receiving portion 53 has a magnetic property.
  • Powder PV and vapor particles V are deposited. And these can be classified using an airflow classifier, and only magnetic powder PV can be obtained.
  • the magnetic powder (hard magnetic powder coated with Dy particles) PV thus obtained is molded at a predetermined pressure while being oriented in a magnetic field. Then, the compact can be sintered in a sintering furnace under an inert gas atmosphere, and then subjected to a predetermined heat treatment to produce a magnet.
  • the magnet obtained in this way can obtain a holding force more than conventional magnets by using a rare earth metal such as Dy slightly compared to the conventional magnets.
  • FIG. 4 is a diagram for explaining a magnetic powder production apparatus according to the second embodiment, (a) is an overall configuration diagram of the magnetic powder production apparatus, and (b) is a diagram of (a).
  • FIG. 2B is an enlarged view of a portion b
  • FIG. 3C is a cross-sectional view taken along line AA ′ of FIG.
  • the manufacturing apparatus according to the second embodiment is mainly different from the apparatus according to the first embodiment in that a plurality of steam generation chambers are provided and the configuration of the adhesion portion connected to these steam generation chambers. Is different. That is, the difference is that a plurality of sets of steam generation chambers and sub-transport pipes are provided. Only differences from the first embodiment will be described below.
  • the magnetic powder manufacturing apparatus 100 ⁇ / b> A includes three steam generation chambers 30, 30, 30.
  • Each steam generation chamber 30 has the same configuration as the steam generation chamber shown in the first embodiment.
  • the sub conveyance pipe 42 of 40 A of adhesion parts is connected to the upper part of the steam generation chamber 30.
  • Each sub-transport pipe 42 is connected to the main transport pipe 41 at the junction 45A so that the vaporized metal V can adhere to the hard magnetic powder P.
  • junction portion 45A three sub-transport pipes 42 are connected to the outer periphery of the main transport pipe 41 at equal intervals. As described above, in the junction 45A, the sub-transport pipes 42 are connected to the outer periphery of the main transport pipe 41 at equal intervals, so that the hard magnetic powder contained in the aerosol AG passing (flighting) the main transport pipe 41. Vapor particles V can be uniformly and uniformly attached to the surface of P.
  • a conveyance tube heater (tube heating unit) 44 is disposed. By heating these tubes with the transfer tube heater 44, it is possible to prevent the vapor particles V from adhering to the inner wall surfaces of these transfer tubes.
  • the discharge chamber 50 is connected to an inert gas pipe 58 that replaces the room gas with the inert gas G2, and the inert gas pipe 17 is similarly included in the inert gas G2.
  • An oxygen removing device 13b for removing the oxygen gas is connected. Thereby, the inert gas can be filled in the discharge chamber 50.
  • Example 1 Nd, Al, Fe, Cu having a purity of 99.5% or more and ferroboron are dissolved at high frequency in an Ar gas atmosphere, and then Nd is 13.5 atomic%, Al is 0.5 atomic%, and Cu is 0.3 A strip cast of an alloy consisting of atomic%, B of 5.8 atomic%, and the balance of Fe and inevitable impurities was manufactured. This alloy was occluded with hydrogen at 0.1 MPa, dehydrated at 520 ° C., cooled and sieved to produce Nd—Fe—B magnetic coarse powder (hard magnetic coarse powder) of 50 mesh or less.
  • the average particle size was pulverized to 4.2 ⁇ m with a jet mill, and the hard magnetic coarse powder was fed into an aerosol chamber of 1.0 ⁇ 10 ⁇ 6 atm Ar gas.
  • the oxygen was increased to a concentration of 1.0 ⁇ 10 ⁇ 11 atmO 2 with a zirconia oxygen pump.
  • the residual gas in the room was replaced with Ar gas having a reduced concentration.
  • Ar gas whose gas temperature was adjusted to 20 ° C. by a cooler while the pressure in the chamber was 1.0 ⁇ 10 ⁇ 6 atm was used as the aerosol gas.
  • the Nd—Fe—B based magnetic powder in the room was agitated and agitated to aerosolize the Nd—Fe—B based magnetic powder (an Nd—Fe—B based magnetic particle aerosol was generated).
  • the vapor generation chamber similarly to the aerosol chamber, after the chamber was evacuated to 1.0 ⁇ 10 ⁇ 11 atm, the O 2 concentration was reduced to a concentration of 1.0 ⁇ 10 ⁇ 11 atmO 2 with a zirconia oxygen pump. Was replaced with Ar gas with reduced pressure, and the pressure in the room was 1.0 ⁇ 10 ⁇ 5 atm.
  • Dy has a melting point of 844 ° C. under a pressure environment of 1.0 ⁇ 10 ⁇ 5 atm.
  • the heater shown in FIG. 1 is set so that the temperature of at least the inner wall of the sub-transport pipe from the steam generation chamber shown in FIG. 1 to the adhering portion (region until the vapor metal is covered) becomes 844 ° C. or higher. And heated. This is to prevent the Dy nano vapor particles from adhering and laminating on the inner wall surfaces of the sub-transport pipe and the merging portion.
  • the discharge chamber was similarly evacuated to 1.0 ⁇ 10 ⁇ 11 atm, and then Ar 2 was reduced in O 2 concentration to 1.0 ⁇ 10 ⁇ 11 atmO 2 with a zirconia oxygen pump.
  • the interior of the chamber was replaced with gas, and the internal pressure was set to 1.0 ⁇ 10 ⁇ 7 atm.
  • the hard magnetic powder in the aerosol chamber flies through the main conveyance pipe and travels toward the discharge chamber due to the differential pressure between the aerosol chamber and the discharge chamber.
  • the Dy nano vapor particles in the vapor generation chamber also fly in the sub-transport pipe due to the differential pressure between the vapor generation chamber and the discharge chamber, and go to the discharge chamber.
  • the Dy nano vapor particles collide with or adsorb to the hard magnetic powder having a temperature lower than that, and adhere to cover the surface of the hard magnetic powder.
  • the Nd—Fe—B based magnetic powder has an average particle diameter of 4.2 ⁇ m in this example, and the Dy nano vapor particles have a diameter of about 20 nm. Since the diameter is about 200 times larger, the vapor particles are easier to ride on the airflow and are more easily accelerated. Then, when the above-mentioned differential pressures of the chambers are provided and the size of the particles is taken into consideration, the flight speed of the Dy nano-vapor particles up to the collision chamber and the discharge chamber is the flight speed of the Nd—Fe—B based magnetic powder. The relative speed is estimated to be 100 m / s or higher. Due to such a relative speed, the Dy nano vapor particles are densely adhered and coated on the surface of the Nd—Fe—B based magnetic powder.
  • the hard magnetic powder (magnetic powder) to which the Dy nano vapor particles are attached in this manner is discharged into the discharge chamber through the nozzle portion and allowed to cool, so that the Dy nano vapor particles attached to the hard magnetic powder are converted into the Dy nano particles. It was.
  • the magnetic powder and the Dy nanoparticles that did not adhere to the magnetic powder were deposited on the receiving part in the discharge chamber, and these were classified by an airflow classifier to obtain only the magnetic powder.
  • the hard magnetic powder coated with the Dy nanoparticles thus obtained was molded at a pressure of 100 MPa while being oriented in a magnetic field of 15 kOe in an Ar gas atmosphere of 1.0 ⁇ 10 ⁇ 11 atmO 2. It compacted in the mold. Next, this compact was put into a sintering furnace under an Ar gas atmosphere of 1.0 ⁇ 10 ⁇ 11 atmO 2 and sintered at 1067 ° C. for 2 hours. Furthermore, a heat treatment was performed under the treatment conditions of 820 ° C. for 5 hours, and subsequently, a heat treatment was performed for 520 ° C. for 1.5 hours to produce a magnet block.
  • the magnet block was processed into a size of 5 ⁇ 5 ⁇ 2 mm with a diamond cutter, and then subjected to magnetic measurement with a BH tracer (VSM (Lakeshore 7400)).
  • the measurement contents are residual magnetization Br, coercive force Hcj, and maximum energy product (BH) max.
  • the results are shown in Table 1 and FIGS.
  • Example 2 A magnet block was manufactured in the same manner as in Example 1. The difference from Example 1 is that Nd, Al, Fe, Cu, Dy having a purity of 99.5% or more and ferroboron are dissolved at high frequency in an Ar gas atmosphere, and then Nd is 11.5 atomic% and Dy is , 5.0 atomic%, Al 0.5 atomic%, Cu 0.3 atomic%, B 5.8 atomic%, the balance being the only alloy strip cast made of Fe and inevitable impurities It is. Then, as in Example 1, the remanent magnetization Br, the coercive force Hcj, and the maximum energy product (BH) max of the manufactured magnetic block were measured. The results are shown in Table 1 and FIGS.
  • Example 1 A magnetic block was manufactured in the same manner as in Example 1. The difference from Example 1 is that the Dy vapor particles were not adhered. Specifically, the average particle size was pulverized to 4.2 ⁇ m with a jet mill, and the same conditions as in Example 1 were applied. A magnetic block was manufactured by sintering the magnetic powder after molding. Then, as in Example 1, the remanent magnetization Br, the coercive force Hcj, and the maximum energy product (BH) max of the manufactured magnetic block were measured. The results are shown in Table 1 and FIGS.
  • Example 2 A magnetic block was produced in the same manner as in Example 2. The difference from Example 2 is that Dy vapor particles were not adhered. Specifically, the average particle size was pulverized to 4.2 ⁇ m with a jet mill, and the hard particles were subjected to the same conditions as in Example 2. A magnetic block was manufactured by sintering the magnetic powder after molding. Then, as in Example 1, the produced magnetic remanent magnetization Br, coercive force Hcj, and maximum energy product (BH) max were measured. The results are shown in Table 1 and FIGS.
  • Example 3 A magnetic block was manufactured in the same manner as in Example 1. The difference from Example 1 is that Dy vapor particles are not adhered, and instead, the following Dy surface diffusion method is used. Specifically, the average particle size was pulverized to 4.2 ⁇ m with a jet mill, and this hard magnetic powder was molded under the same conditions as in Example 1.
  • the hard magnetic powder coated with the Dy nanoparticles thus obtained was molded at a pressure of 100 MPa while being oriented in a magnetic field of 15 kOe in an Ar gas atmosphere of 1.0 ⁇ 10 ⁇ 11 atmO 2. It compacted in the mold. Next, this compact was put into a sintering furnace under an Ar gas atmosphere of 1.0 ⁇ 10 ⁇ 11 atmO 2 and sintered at 1067 ° C. for 2 hours, and the magnet block was measured with a diamond cutter in a size of 5 ⁇ 5 ⁇ 2 mm. Processed into a magnet.
  • the magnet was immersed for 30 seconds while applying ultrasonic waves to a turbid liquid in which dysprosium fluoride with an average particle size of 10 ⁇ m was mixed with ethanol at a mass fraction of 50%, and placed in a vacuum desiccator. And dried for 30 minutes in an exhaust atmosphere. Further, the magnet covered with dysprosium fluoride was heat-treated at 800 ° C. for 10 hours in an Ar gas atmosphere, and further subjected to aging treatment at 510 ° C. for 1 hour to rapidly cool the magnet. Then, as in Example 1, the produced magnetic remanent magnetization Br, coercive force Hcj, and maximum energy product (BH) max were measured. The results are shown in Table 1 and FIGS.
  • Example 1 and Example 2 had higher coercive force and larger maximum energy product than those of Comparative Examples 1 to 3. This is considered due to the fact that Dy is uniformly and densely arranged at the grain boundaries of the particles made of magnetic powder.
  • the magnet of Comparative Example 2 has a low coercive force and a small maximum energy product in spite of having a large Dy content as compared with the magnet of Example 1, because Dy does not exist at the grain boundaries. It is thought that.
  • the magnet of Comparative Example 3 since Dy is not sufficiently diffused to the inside, it is considered that the coercive force is lower and the maximum energy product is smaller than that of the magnet of Example 1.

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JP2011061038A (ja) * 2009-09-10 2011-03-24 Toyota Central R&D Labs Inc 希土類磁石とその製造方法および磁石複合部材
JP2015086413A (ja) * 2013-10-29 2015-05-07 大陽日酸株式会社 複合超微粒子の製造方法

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JP6552283B2 (ja) * 2015-06-02 2019-07-31 Ｄｏｗａエレクトロニクス株式会社 磁性コンパウンド、アンテナおよび電子機器
CN106229102B (zh) * 2016-08-23 2019-05-31 南京工程学院 一种超细晶NdFeB永磁材料及其制备方法
DE102017215265A1 (de) * 2017-08-31 2019-02-28 Siemens Aktiengesellschaft Verfahren zur Herstellung eines Permanentmagneten, Permanentmagnet, elektrische Maschine, Medizingerät und Elektrofahrzeug
CN107876791A (zh) * 2017-10-27 2018-04-06 内蒙古盛本荣科技有限公司 生产粉体的装置及其方法
CN109954876B (zh) * 2019-05-14 2020-06-16 广东工业大学 一种抗氧化微纳铜材料的制备方法

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