WO2010052862A1 - Procédé de production d'aimant fritté aux terres rares et contenant de poudre pour production d'aimant fritté aux terres rares - Google Patents

Procédé de production d'aimant fritté aux terres rares et contenant de poudre pour production d'aimant fritté aux terres rares Download PDF

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Publication number
WO2010052862A1
WO2010052862A1 PCT/JP2009/005726 JP2009005726W WO2010052862A1 WO 2010052862 A1 WO2010052862 A1 WO 2010052862A1 JP 2009005726 W JP2009005726 W JP 2009005726W WO 2010052862 A1 WO2010052862 A1 WO 2010052862A1
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Prior art keywords
rare earth
forming member
powder
alloy powder
sintered magnet
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PCT/JP2009/005726
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English (en)
Japanese (ja)
Inventor
佐川眞人
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インターメタリックス株式会社
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Application filed by インターメタリックス株式会社 filed Critical インターメタリックス株式会社
Priority to EP09824563.2A priority Critical patent/EP2348518B1/fr
Priority to CN200980144520.7A priority patent/CN102209999A/zh
Priority to US13/127,402 priority patent/US20110250087A1/en
Priority to JP2010536662A priority patent/JP5690141B2/ja
Publication of WO2010052862A1 publication Critical patent/WO2010052862A1/fr

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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
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • 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
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • B22F2005/103—Cavity made by removal of insert
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • 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
    • H01F1/047—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
    • H01F1/0575—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 pressed, sintered or bonded together
    • H01F1/0577—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 pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F3/00—Cores, Yokes, or armatures
    • H01F3/10—Composite arrangements of magnetic circuits
    • H01F3/14—Constrictions; Gaps, e.g. air-gaps
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0273—Imparting anisotropy

Definitions

  • the present invention relates to a method for producing a rare earth sintered magnet such as an Nd—Fe—B based sintered magnet or an Sm—Co based sintered magnet.
  • Rare earth sintered magnets are widely used as permanent magnets that can generate a strong magnetic field.
  • Nd—Fe—B based sintered magnets are widely used in motors for hybrid vehicles and electric vehicles, small motors for hard disks, large motors for industrial use, and generators.
  • a rare earth sintered magnet is used as a rotor (rotor) and an electromagnet is used as a stator (stator), and the rotor rotates by forming a rotating magnetic field.
  • eddy currents are generated in the rare earth sintered magnet of the rotor, which causes problems such as energy loss and motor overheating.
  • Patent Document 1 describes that the generation of such eddy current is suppressed by providing a slit on the surface of the rare earth sintered magnet.
  • Nd-Fe-B magnets neodymium magnets
  • a sintered magnet is produced using an alloy powder in which a part of Nd is substituted with Dy and / or Tb.
  • this method has the disadvantages that Dy and Tb are expensive and rare, leading to an increase in cost and a decrease in stable supply, and a decrease in the maximum energy product.
  • the sintered body Dy and / or Tb is fed into the sintered body through the grain boundaries of the alloy particles therein, and Dy and / or Tb is injected only near the surface of the alloy particles (grain boundary diffusion method).
  • a high coercive force can be obtained, a reduction in the maximum energy product can be suppressed, and the amount of Dy and Tb used can be reduced.
  • Patent Document 2 a slit is provided on the surface of a sintered body of an Nd—Fe—B alloy, and Dy and / or Tb is diffused from the slit to achieve an efficiency near the surface of the alloy particle. It is often described that Dy and / or Tb is injected.
  • JP 2000-295804 A ([0009]-[0011]) JP 2007-053351 A ([0027]-[0028], [0033]-[0035])
  • slits are formed by mechanical processing using a cutting machine, a wire saw, or the like.
  • mechanical processing labor and time are required, and tool consumption is severe, so an increase in cost is inevitable.
  • the slit width cannot be made very small by mechanical processing, the ratio of the substantial volume (volume of the sintered body portion) to the external volume of the magnet is reduced, and the function as a magnet is substantially reduced. End up.
  • the problem to be solved by the present invention is to easily and inexpensively manufacture a rare earth sintered magnet having voids such as slits and holes for making it less susceptible to eddy currents and / or performing grain boundary diffusion treatment. It is to provide a method that can.
  • the rare earth sintered magnet manufacturing method according to the present invention made to solve the above problems is as follows. a) a filling step of filling a powder filling container with a rare earth magnet alloy powder together with a gap forming member; b) an alignment step of aligning the rare earth magnet alloy powder in a magnetic field; c) a sintering step of sintering the rare earth magnet alloy powder by heating the rare earth magnet alloy powder together with the powder-filled container; In this order, d) removing the void forming member after the orientation step and before the rare earth magnet alloy powder starts to be sintered; Thus, a rare earth sintered magnet having voids is manufactured.
  • a rare earth magnet alloy powder is filled in a powder-filled container together with a void forming member, and the void forming member is simply removed before the rare earth magnet alloy powder starts sintering.
  • a magnet can be manufactured easily. Therefore, in the present invention, it is not necessary to perform mechanical processing to form a void, and a rare earth sintered magnet having a void can be manufactured at low cost.
  • a rare earth sintered magnet when a rare earth sintered magnet is manufactured, in many cases, a rare earth magnet alloy powder is filled in a container and a magnetic field is applied while compressing and compression molding and orientation are performed.
  • the inventor of the present application fills the powder-filled container with the rare-earth magnet alloy powder, orients the rare-earth magnet alloy powder without performing compression molding, and heats the powder-filled container as it is. It was found that a rare earth sintered magnet can be obtained by the pressless method (see JP 2006-019521 A). In the present invention, since the pressless method is used, even if the void forming member is placed in the powder-filled container together with the rare earth magnet alloy powder, the void forming member is not subjected to pressure.
  • the rare earth magnet alloy powder particles filled in the powder-filled container are magnetically attracted by the orientation in the magnetic field.
  • the void forming member since the void forming member is removed after the alignment step, the void does not collapse when the void forming member is removed.
  • the sintering starts when the temperature exceeds a predetermined temperature (for example, about 600 ° C. for a Nd—Fe—B based sintered magnet), Thereafter, as the sintering proceeds, the sintered body contracts.
  • a predetermined temperature for example, about 600 ° C. for a Nd—Fe—B based sintered magnet
  • the removal of the void forming member is preferably performed before the sintering step in that it is not necessary to consider the heat resistance of the void forming member and the reactivity between the void forming member and the rare earth magnet alloy powder.
  • the void forming member can be removed before sintering starts by raising the temperature for sintering.
  • the rare earth magnet alloy is an Nd-Fe-B sintered magnet alloy
  • a substance containing Dy and / or Tb is injected into the voids of the sintered body obtained by the sintering step. By heating, Dy and / or Tb can be diffused in the sintered body.
  • a plate material may be used for the gap forming member.
  • a bar material can also be used.
  • Dy and / or Tb can be uniformly diffused from a large number of holes by arranging a large number of rod-shaped void forming members in a matrix.
  • the cross-sectional shape of the rod-shaped void forming member is not particularly limited, such as a circle, a quadrangle, or a hexagon.
  • the gap forming member When a plate-like or rod-like gap forming member is used as the gap forming member, it is desirable to orient the rare earth magnet alloy powder in a magnetic field in a direction parallel to the gap forming member in the orientation step. Thereby, since the particles of the rare earth magnet alloy powder are connected in a chain shape in a direction parallel to the gap forming member, even if the gap forming member is removed in this state, the chain connection is not interrupted and the gap is not broken.
  • the rare earth magnet alloy powder and the binder may be mixed and filled in the powder filling container.
  • the binder methyl cellulose, polyacrylamide, polyvinyl alcohol, paraffin wax, polyethylene glycol, polyvinyl pyrrolidone, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, acetyl cellulose, nitrocellulose, vinyl acetate resin, or the like can be used (Japanese Patent Laid-Open No. Hei 10). -270278).
  • the rare earth magnet alloy powder and the gap forming member When filling the powder-filled container with the rare earth magnet alloy powder together with the gap forming member, the rare earth magnet alloy powder and the gap forming member may be placed in the powder filled container at the same time. May be put in.
  • the gap provided in the sintered body by the manufacturing method according to the present invention is left as it is, the mechanical strength is low, and it is easy to break. In addition, accumulation of moisture in the voids may cause corrosion or mechanical damage. Therefore, by embedding an embedding member such as an epoxy resin in the gap, it is possible to increase the mechanical strength and prevent moisture from staying.
  • the embedding member is embedded after the gap forming member is removed. However, when the heat resistant temperature is lower than the sintering temperature of the rare earth magnet, such as an epoxy resin, it is performed after the sintering step. When performing the diffusion process, the embedded member is embedded after the diffusion process. In order to prevent the influence of eddy current, the embedded member is preferably insulative.
  • a powder-filled container is filled with rare-earth magnet alloy powder together with a gap forming member, and after being oriented in a magnetic field, the gap can be formed simply by removing the gap forming member and performing mechanical processing. Since there is no need, a rare earth sintered magnet having voids can be manufactured easily and at low cost.
  • the longitudinal cross-sectional view which shows the 1st example of the mold used by the rare earth sintered magnet manufacturing method concerning this invention, the lid
  • Schematic which shows the 1st example of the rare earth sintered magnet manufacturing method concerning this invention.
  • the longitudinal cross-sectional view which shows the 2nd example of the mold used with the rare earth sintered magnet manufacturing method concerning this invention, the lid
  • gap. 1 is a perspective view of a rare earth sintered magnet produced by the method of Example 1.
  • FIG. FIG. 5 is a longitudinal sectional view of a mold, a mold lid, and a gap forming member used in Example 3-1, and a top view of the mold lid.
  • FIGS. 1 and 2 show a first embodiment of the present invention.
  • the mold (powder filling container) 10 and the gap forming member 14 shown in FIG. 1 are used.
  • the mold 10 is used to obtain a flat magnet, and has a rectangular parallelepiped housing portion 11 filled with a rare earth magnet alloy powder.
  • An opening for taking out the rare earth sintered magnet after filling and sintering of the rare earth magnet alloy powder is provided in the upper portion of the accommodating portion 11, and a lid 13 is attached so as to close the opening.
  • the material of the mold 10 and the lid 13 for example, magnetic stainless steel, nonmagnetic stainless steel, or carbon (having heat resistance equal to or higher than the sintering temperature of the rare earth sintered magnet) can be used.
  • two insertion ports 131 extending in the longitudinal direction of the rectangular parallelepiped of the accommodating portion 11 are provided in parallel.
  • a plate-like gap forming member 14 having a slightly smaller width and length than that can be inserted into the insertion port 131.
  • various metals, carbon, and plastics heat resistance is not required in the present embodiment
  • the gap forming member 14 is erected on the plate-like gap forming member fixture 15 at the same interval as the two insertion ports 131.
  • the accommodating part 11 is filled with the rare earth magnet alloy powder 19 (a).
  • the rare earth magnet alloy powder 19 may be used as it is, or a binder may be mixed with the rare earth magnet alloy powder 19.
  • the filling density is desirably 40 to 50% of the true density of the rare earth magnet alloy.
  • the lid 13 is attached to the mold 10, and the gap forming member 14 is inserted into the rare earth magnet alloy powder 19 in the accommodating portion 11 from the insertion port 131 (b).
  • the mold 10 is placed in the magnetic field generating coil 17 and a pulsed magnetic field is applied parallel to the gap forming member 14 (perpendicular to the lid 13) to orient the rare earth magnet alloy powder 19 (c).
  • the strength of the magnetic field is 3 to 10T, preferably 4 to 8T.
  • the lid 13 is firmly pressed against the mold 10 to prevent the rare earth magnet alloy powder 19 from popping out.
  • the air gap forming member 14 is extracted from the rare earth magnet alloy powder 19 and the insertion port 131 (d). As a result, slit-like voids 18 are formed in the compact of the rare earth magnet alloy powder 19.
  • the powder particles are magnetically attracted by the orientation in the magnetic field, the powder hardly spills into the void 18. Thereafter, the rare earth magnet alloy powder 19 is heated while being filled in the accommodating portion 11 (e). Thereby, the rare earth sintered magnet which has a slit-shaped space
  • This method makes it possible to form slits at a much lower price than when mechanical processing is performed with a wire saw after sintering.
  • a slit having a smaller width than that in the case of performing mechanical processing can be formed, and a high-quality slit having no reduction in the function of the slit such as residual powder can be formed in the slit.
  • FIG. 3 and 4 show a second embodiment of the present invention.
  • the mold 20 and the gap forming member 24 shown in FIG. 3 are used.
  • the mold 20 has the same accommodating portion 21 as the mold 10 of the first embodiment and has a structure to which a lid 23 is attached.
  • the mold 20 is different in that two insertion ports 221 are provided at the bottom of the mold 20. This is different from the first example.
  • the lid 23 is not provided with an insertion port.
  • the gap forming member 24 attached to the gap forming member fixture 25 can be inserted into the insertion port 221 as in the first example.
  • a method for producing a rare earth sintered magnet according to the second embodiment will be described with reference to FIG.
  • the gap forming member 24 is inserted into the insertion port 221 of the mold 20 (a).
  • the accommodating portion 21 is filled with the rare earth magnet alloy powder 29 and the lid 23 is attached (b). Accordingly, the order of insertion of the air gap forming member and filling of the rare earth magnet alloy powder is reversed from the first embodiment.
  • the mold 20 is placed in the magnetic field generating coil 27, and a pulsed magnetic field is applied in a direction parallel to the gap forming member 24 (perpendicular to the lid 23) to orient the rare earth magnet alloy powder 29 (c).
  • the rare earth magnet alloy powder 29 is heated while being filled in the accommodating portion 21. To be sintered (e).
  • Fig. 5 shows another example of the mold.
  • the gap forming member 14 is attached to the gap forming member fixture 15 separately from the lid 13, but the gap forming member 14A may be directly attached to the lid 13A (FIG. 5 (a)). ).
  • the lid 13A is removed from the mold in order to remove the gap forming member 14 after the orientation step.
  • FIG. 5B shows an example in which a gap forming member 14 ⁇ / b> B is erected on the bottom 12 in the accommodating portion 11.
  • the thickness of the gap forming member according to the purpose, the interval, and the depth of insertion into the rare earth magnet alloy powder (hereinafter referred to as “insertion depth”) will be described.
  • the main purpose is to prevent the generation of eddy currents when using rare earth sintered magnets
  • the preferred width, insertion depth, number and interval of the gap forming members will be described.
  • the width of the slit formed in the sintered body should be as small as possible. Accordingly, the thickness of the gap forming member is preferably as small as possible.
  • the lower limit of the thickness of the gap forming member is about 0.05 mm.
  • the width of the slit formed in the sintered body is about 0.04 mm.
  • the insertion depth is preferably as deep as possible from the viewpoint of reducing eddy current loss, but considering the mechanical strength of the sintered body, it is 1 mm or more, preferably 2 mm or less smaller than the thickness of the magnet in the insertion depth direction. It is preferable.
  • the volume ratio of the magnet ratio of the volume of the portion where the magnet exists to the volume of the outer shape of the sintered magnet
  • the interval between the slits that is, the interval between the gap forming members is preferably shorter.
  • gap formation members are determined so that the predetermined magnetic characteristic may be obtained exceeding the volume ratio, considering the above-mentioned thickness and insertion depth.
  • the preferred width, interval, and insertion depth of the void forming member will be described. If the width of the gap forming member is too small, it becomes difficult to inject a substance containing Dy or Tb into the slit formed in the sintered body. Therefore, the slit width is preferably 0.1 mm or more. Also, if the slit spacing is too large, there will be a part where Dy and Tb diffusing from the slit will not reach, and the grain boundary diffusion effect will not spread throughout the sintered magnet, resulting in a magnet with non-uniform magnetic properties. End up.
  • the interval between the slits is preferably 6 mm or less, more preferably 5 mm or less.
  • the insertion depth is preferably 6 mm or less, more preferably 5 mm or less, with a difference from the thickness of the magnet in the insertion depth direction in order to spread the effect of grain boundary diffusion throughout the sintered magnet.
  • the difference is preferably 1 mm or more, preferably 2 mm or more.
  • the thickness, insertion depth, number and interval of the air gap forming member are determined so as to exceed the volume ratio at which predetermined magnetic characteristics are obtained.
  • a rod-like void forming member can also be used when grain boundary diffusion is the main purpose.
  • a large number of rod-shaped gap forming members 34 can be arranged in a matrix on the surface of a plate-like gap forming member fixture 35 in the vertical and horizontal directions.
  • a sintered body having a large number of pores (voids) can be produced by using a large number of void forming members 34 arranged in a matrix like this, and an Nd-Fe-B-based sintered material can be produced by a grain boundary diffusion method.
  • Dy and / or Tb can be efficiently diffused from the pores into the sintered body.
  • the thickness of the pores formed in the sintered body is preferably 0.2 mm or more, and more preferably 0.3 mm or more so that a substance containing Dy or Tb can be reliably injected.
  • the space between the gap forming members 34 is preferably 6 mm or less, and more preferably 5 mm or less in order to spread Dy and Tb throughout the sintered magnet.
  • the insertion depth is the same as in the case of the plate-shaped gap forming member described above.
  • the diffusion treatment is performed by heating the powder containing Dy and / or Tb after filling the voids 18 (FIG. 7).
  • the heating temperature may be 700 to 1000 ° C.
  • the Dy / Tb-containing material to be injected into the gap include Dy and Tb fluorides, oxides, oxyfluorides or hydrides, alloys of Dy and Tb with other metals, and hydrides of these alloys.
  • alloys of Dy and Tb and other metals include Fe group transition metals such as Fe, Co and Ni, and alloys of B, Al and Cu and Dy and Tb.
  • Grain boundary diffusion treatment is effectively performed by injecting a slurry obtained by mixing powder of these substances with an organic solvent into the void and heating.
  • These slurries may be injected only into the voids, but may be injected into the slits and pores and applied to the surface of the sintered body.
  • grain boundary diffusion can be caused from both the voids and the surface of the sintered body.
  • Grain boundary diffusion treatment is performed by heating the sintered body in which the slurry is injected into the void (or applied to the surface in addition thereto) at 700 to 1000 ° C. for 1 to 20 hours in a vacuum or in an inert gas. be able to.
  • the conductive component in the slurry blocks the void.
  • the amount of slurry to be injected is adjusted so as not to stutter.
  • an embedded member such as an epoxy resin is embedded in the gap in order to prevent a decrease in mechanical strength due to the presence of the gap and corrosion due to accumulation of moisture in the gap.
  • the epoxy resin is injected into the void 18 in a liquid state and then cured at room temperature or by heating (FIG. 8).
  • This embedding process can be performed before the sintering process depending on the material of the embedding member, but when an adhesive resin such as an epoxy resin is used, it is performed after the sintering process. In the case of performing diffusion processing, an embedding process is performed after the diffusion processing.
  • the strip cast alloy of Nd—Fe—B rare earth magnet was subjected to hydrogen crushing and jet mill treatment using nitrogen gas to obtain rare earth magnet powder having an average particle size of 5 ⁇ m.
  • the composition of the rare earth magnet powder is Nd: 25,8%, Pr: 4.3%, Dy: 2.5%, Al: 0.23%, Cu: 0.1%, Fe: balance.
  • the average particle size of the rare earth magnet powder was measured with a laser type particle size distribution meter.
  • the mold 10 was covered with a lid 13.
  • the gap forming member 14 was inserted from the insertion port 131.
  • the mold 10 is fixed in a magnetic field generating coil, and a rare earth magnet powder is oriented in the magnetic field by applying a 5T pulse magnetic field three times in a direction parallel to the gap forming member 14 and perpendicular to the bottom of the mold 10. .
  • the gap forming member 14 was pulled out from the mold 10 and the mold 10 was placed in a sintering furnace. All steps from filling the powder to charging to the sintering furnace were performed in Ar gas. Sintering was performed in vacuum at 1010 ° C. for 2 hours.
  • the mold 10 and the lid 13 are made of carbon
  • the gap forming member 14 is made of nonmagnetic stainless steel
  • the thickness of the gap forming member 14 is 0.5 mm.
  • the density of the sintered body produced by the above-described process was 7.56 g / cm 3 , which was as high as that of the NdFeB sintered magnet produced by a normal pressing method.
  • the outer dimensions of the sintered body 31 are a rectangular parallelepiped having a length of 37 mm, a width of 39 mm, and a height of 8.6 mm, and two slits 32 are formed in the vertical direction at 12 mm intervals on the upper surface side (FIG. 9). In the sintered body and the slit 32, almost no distortion was observed.
  • the width of the slit 32 was about 0.4 mm, and the depth was 6.2 mm. Then, it was confirmed by a test in which a 0.3 mm metal foil was passed through the slit 32 to prevent any slit 32 from being clogged or blocked by foreign matter.
  • an NdFeB sintered magnet having a slit was produced by the mold 20 and the gap forming member 24 of the second embodiment.
  • the powder is filled in a state in which the gap forming member 24 is mounted on the mold 20.
  • care must be taken so that the powder is uniformly filled throughout the container 21.
  • the packing density was 3.6 g / cm 3 .
  • the lid 23 was put on, orientation in the magnetic field under the same conditions as in Example 1, the void forming member 24 was pulled out, and sintering was performed under the same conditions as in Example 1.
  • the sintered body taken out from the mold after sintering is a high-quality slit having high density and no distortion of the shape as in the case of the sintered body produced in Example 1, and the slit is also a good quality slit with no clogging or blocking. confirmed.
  • the dimensions of the sintered body, slit spacing, slit width, etc. were all the same as in Example 1.
  • a sintered body having voids (slits, pores) was produced using the mold and void forming member shown in FIGS.
  • the mold 40 shown in FIG. 10 has a rectangular parallelepiped accommodating portion 41 whose upper and lower surfaces are square, and a lid 43 can be attached to the upper surface.
  • the lid 43 is provided with two insertion openings 431 so that two plate-like gap forming members 44 can be inserted.
  • the same mold as the mold 40 is used.
  • the lid 53 attached to the upper surface of the mold 40 is provided with four insertion ports 531 in a square shape so that four rod-shaped gap forming members 54 can be inserted.
  • each sintered body has a slit using the gap forming member 44 (Example 3-1) and a sintered body having pores using the gap forming member 54 (implementing) Examples 3-2) were prepared respectively.
  • the outer shape of each sintered body is a cube having a side of about 11 mm.
  • those having slits had a slit width of 0.4 mm, a depth of 5.9 mm, and an interval of 3.3 mm.
  • the pore diameter was 0.5 mm and the depth was 7.2 mm.
  • a rectangular parallelepiped sintered body (Comparative Example 1) that has neither slits nor pores under the same conditions as in this example (and Example 1) without inserting and removing the gap forming member 44. ) was produced.
  • These three types of sintered bodies were processed with a surface grinder so that the cubes were exactly 10 mm on a side. Thereafter, the sample was subjected to various cleanings such as alkali cleaning, acid cleaning, and pure water cleaning, and then dried.
  • a Dy-containing alloy having an atomic ratio of Dy: 80%, Ni: 14%, Al: 4%, other metals / impurities: 2% is pulverized to an average particle size of 9 ⁇ m by a jet mill.
  • a contained alloy powder was prepared.
  • This Dy-containing alloy powder was mixed and stirred with ethanol at a mass ratio of 50%, vacuum impregnated into the slit of the sample of Example 3-1 and the pore of the sample of Example 3-2, and then dried.
  • a powder containing Dy was applied to the magnet surfaces of Example 3-1, Example 3-2 and Comparative Example by the barrel painting method (see JP-A-2004-359873).
  • Comparative Example 1-1 is obtained by subjecting the sintered body of Comparative Example 1 to the above-mentioned grain boundary diffusion treatment, and Comparative Example 1-2 applies Dy-containing alloy powder to the sintered body of Comparative Example 1. Without doing so, only the heat treatment was performed in the same manner as in the grain boundary diffusion treatment.
  • Example 3-1 and Example 3-2 have a coercive force H cJ and a square shape of the magnetization curve as compared with the sample of Comparative Example 1-1 which has no slits or pores and was subjected to grain boundary diffusion treatment. It can be seen that the coercivity H k / H cJ is also high and the coercive force H cJ is higher than that of the sample of Comparative Example 1-2 in which the grain boundary diffusion treatment is not performed. According to this embodiment, even a large NdFeB sintered body that has not been effective in the grain boundary diffusion treatment so far, such as a 10 mm cube, uses the expensive method of slit formation after sintering according to the method of the present invention. It was shown that the coercive force can be increased by the grain boundary diffusion method by an inexpensive method.

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  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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  • Powder Metallurgy (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

L'invention porte sur un procédé pour produire facilement un aimant fritté aux terres rares qui comporte un vide, tel qu'une fente, pour réduire l'influence de courant de Foucault et/ou diffuser des joints de grain, à bas coût. Le procédé de production d'un aimant fritté aux terres rares est caractérisé par l'exécution, successivement dans l'ordre suivant : d'étapes de remplissage ((a), (b)) dans lesquelles un contenant de poudre (10) est rempli d'une poudre d'alliage d'aimant aux terres rares (19) conjointement avec un élément de formation de vide (14), d'une étape d'orientation (c) dans laquelle la poudre d'alliage d'aimant aux terres rares (19) est orientée dans un champ magnétique, et d'une étape de frittage (e) dans laquelle la poudre d'alliage d'aimant aux terres rares est frittée par chauffage du contenant de poudre (10) conjointement avec la poudre d'alliage d'aimant aux terres rares (19) contenue dans celui-ci, et l'exécution d'une étape d'enlèvement (d) dans laquelle l'élément de formation de vide est enlevé, après l'étape d'orientation mais avant le début du frittage de la poudre d'alliage d'aimant aux terres rares.
PCT/JP2009/005726 2008-11-06 2009-10-29 Procédé de production d'aimant fritté aux terres rares et contenant de poudre pour production d'aimant fritté aux terres rares WO2010052862A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP09824563.2A EP2348518B1 (fr) 2008-11-06 2009-10-29 Procédé de production d'aimant fritté aux terres rares
CN200980144520.7A CN102209999A (zh) 2008-11-06 2009-10-29 稀土类烧结磁体制造方法和稀土类烧结磁体制造用粉末填充容器
US13/127,402 US20110250087A1 (en) 2008-11-06 2009-10-29 Method for producing sintered rare-earth magnet and powder-filling container for producing such magnet
JP2010536662A JP5690141B2 (ja) 2008-11-06 2009-10-29 希土類焼結磁石製造方法及び希土類焼結磁石製造用粉末充填容器

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JP2008-285007 2008-11-06
JP2008285007 2008-11-06

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JP2014146627A (ja) * 2013-01-25 2014-08-14 Aichi Elec Co 永久磁石および永久磁石製造方法
JP2014147151A (ja) * 2013-01-25 2014-08-14 Aichi Elec Co 永久磁石電動機
WO2015012412A1 (fr) * 2013-07-24 2015-01-29 Ｎｄｆｅｂ株式会社 Procédé de production d'aimant fritté aux terres rares et moule de frittage pour aimant fritté aux terres rares
KR101534706B1 (ko) * 2013-12-18 2015-07-07 현대자동차 주식회사 매입형 영구자석 동기모터
JP2015225965A (ja) * 2014-05-28 2015-12-14 大同特殊鋼株式会社 焼結磁石製造用モールド及び焼結磁石製造方法
JPWO2014148356A1 (ja) * 2013-03-18 2017-02-16 インターメタリックス株式会社 ＲＦｅＢ系焼結磁石製造方法及びＲＦｅＢ系焼結磁石
JPWO2014148355A1 (ja) * 2013-03-18 2017-02-16 インターメタリックス株式会社 ＲＦｅＢ系焼結磁石製造方法及びＲＦｅＢ系焼結磁石
CN107424703A (zh) * 2017-09-06 2017-12-01 内蒙古鑫众恒磁性材料有限责任公司 晶界扩散法制作烧结钕铁硼永磁的重稀土附着工艺

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JP6280137B2 (ja) * 2014-09-28 2018-02-14 Ｎｄｆｅｂ株式会社 希土類焼結磁石の製造方法及び当該製法にて使用される製造装置
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JP6627307B2 (ja) 2015-07-24 2020-01-08 大同特殊鋼株式会社 焼結磁石製造方法
WO2017104788A1 (fr) * 2015-12-16 2017-06-22 日立金属株式会社 Procédé d'analyse d'aimant fritté anisotrope et procédé de production d'aimant fritté anisotrope l'utilisant
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WO2023210842A1 (fr) * 2022-04-29 2023-11-02 주식회사 디아이씨 Procédé de fabrication d'aimant permanent aux terres rares
CN114823025B (zh) * 2022-05-10 2024-02-02 江西金力永磁科技股份有限公司 一种低涡流损耗钕铁硼磁体
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WO2011128383A1 (fr) 2010-04-15 2011-10-20 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de lithographie electronique avec correction de fins de lignes par insertion de motifs de contraste
JP2012125139A (ja) * 2010-09-29 2012-06-28 Hitachi Metals Ltd カップリング装置およびカップリング装置の製造方法
JP2013057434A (ja) * 2011-09-07 2013-03-28 Denso Corp マイクロチャネル熱交換器の製造方法
JP2014017956A (ja) * 2012-07-09 2014-01-30 Toyota Motor Corp 割断形成永久磁石及びその製造方法
US9928956B2 (en) 2012-07-09 2018-03-27 Toyota Jidosha Kabushiki Kaisha Permanent magnet and manufacturing method therefor
JP2014146627A (ja) * 2013-01-25 2014-08-14 Aichi Elec Co 永久磁石および永久磁石製造方法
JP2014147151A (ja) * 2013-01-25 2014-08-14 Aichi Elec Co 永久磁石電動機
JPWO2014148356A1 (ja) * 2013-03-18 2017-02-16 インターメタリックス株式会社 ＲＦｅＢ系焼結磁石製造方法及びＲＦｅＢ系焼結磁石
JPWO2014148355A1 (ja) * 2013-03-18 2017-02-16 インターメタリックス株式会社 ＲＦｅＢ系焼結磁石製造方法及びＲＦｅＢ系焼結磁石
WO2015012412A1 (fr) * 2013-07-24 2015-01-29 Ｎｄｆｅｂ株式会社 Procédé de production d'aimant fritté aux terres rares et moule de frittage pour aimant fritté aux terres rares
KR101534706B1 (ko) * 2013-12-18 2015-07-07 현대자동차 주식회사 매입형 영구자석 동기모터
US9825493B2 (en) 2013-12-18 2017-11-21 Hyundai Motor Company Interior permanent magnet synchronous motor
JP2015225965A (ja) * 2014-05-28 2015-12-14 大同特殊鋼株式会社 焼結磁石製造用モールド及び焼結磁石製造方法
CN107424703A (zh) * 2017-09-06 2017-12-01 内蒙古鑫众恒磁性材料有限责任公司 晶界扩散法制作烧结钕铁硼永磁的重稀土附着工艺
CN107424703B (zh) * 2017-09-06 2018-12-11 内蒙古鑫众恒磁性材料有限责任公司 晶界扩散法制作烧结钕铁硼永磁的重稀土附着工艺

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EP2348518A1 (fr) 2011-07-27
JP5690141B2 (ja) 2015-03-25
JPWO2010052862A1 (ja) 2012-04-05
CN105355415A (zh) 2016-02-24
EP2348518A4 (fr) 2015-02-25
EP2348518B1 (fr) 2016-08-24
CN102209999A (zh) 2011-10-05

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