EP2348518B1 - Verfahren zur herstellung gesinterter seltenerdmagneten - Google Patents

Verfahren zur herstellung gesinterter seltenerdmagneten Download PDF

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Publication number
EP2348518B1
EP2348518B1 EP09824563.2A EP09824563A EP2348518B1 EP 2348518 B1 EP2348518 B1 EP 2348518B1 EP 09824563 A EP09824563 A EP 09824563A EP 2348518 B1 EP2348518 B1 EP 2348518B1
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EP
European Patent Office
Prior art keywords
cavity
earth magnet
rare
powder
sintered
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EP09824563.2A
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English (en)
French (fr)
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EP2348518A1 (de
EP2348518A4 (de
Inventor
Masato Sagawa
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Intermetallics Co Ltd
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Intermetallics Co Ltd
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Publication of EP2348518A4 publication Critical patent/EP2348518A4/de
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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 sintered rare-earth magnet, such as a sintered Nd-Fe-B magnet or sintered Sm-Co magnet.
  • Sintered rare-earth magnets are commonly used as permanent magnets capable of creating strong magnetic fields.
  • sintered Nd-Fe-B magnets are commonly used in motors for hybrid cars or electric vehicles, compact motors for hard-disk drives, large-sized industrial motors, power generators and other applications.
  • a sintered rare-earth magnet is used as the rotor and an electromagnet as the stator.
  • the electromagnet is operated to create a rotating magnetic field for revolving the rotor.
  • an eddy current is generated in the sintered rare-earth magnet, causing a loss of energy or overheating of the motor.
  • Patent Document 1 A technique for solving this problem is disclosed in Patent Document 1, in which a plurality of slits are formed on the surface of the sintered rare-earth magnet to prevent the generation of eddy currents.
  • a conventional technique for solving these problems is the grain boundary diffusion, which includes applying Dy and/or Tb to the surface of a sintered compact of Nd-Fe-B alloy containing neither Dy nor Tb and heating it to a temperature within a range from 700 to 1000 degrees Celsius, whereby Dy and/or Tb is transferred through the boundaries of alloy particles into deeper regions of the sintered compact to create a product containing Dy and/or Tb only in the vicinity of the surfaces of the alloy particles.
  • This technique has the effect of achieving a high coercive force while preventing a significant decrease in the maximum energy product as well as decreasing the usage of Dy and Tb.
  • Patent Document 2 discloses the technique of efficiently injecting Dy and/or Tb into the vicinity of the surfaces of alloy particles by forming slits on the surface of the sintered compact of an Nd-Fe-B alloy and diffusing Dy and/or Tb from those slits into the grain boundaries.
  • the slits are formed by a machining process using a cutter, wire saw or similar tool.
  • the use of a machining process inevitably increases the production cost since it requires a considerable amount of labor and time, with heavy consumption of the tool.
  • the slits created by such a machining process cannot be very thin and hence considerably lower the ratio of the actual volume of the magnet (i.e. the volume of the sintered portion) to its outside volume. As a result, the performance of the product as the magnet substantially deteriorates.
  • the alloy powder remaining in the slits cannot be easily removed. If a compact with an alloy powder remaining in the slits is heated for sintering, the alloy powder will partially clog the slits, compromising the effect of preventing the generation of eddy currents. Furthermore, Dy and/or Tb is prevented from sufficiently reaching deep regions in the grain boundary diffusion process.
  • the problem to be solved by the present invention is to provide an easy and inexpensive method for producing a sintered rare-earth magnet having cavities (e.g. slits or holes) for making the magnet less likely to be influenced from eddy currents and/or for performing the grain boundary diffusion process.
  • cavities e.g. slits or holes
  • a sintered rare-earth magnet having a cavity can be easily produced by a simple method including filling a powder of rare-earth magnet alloy into the powder-filling container together with a cavity-forming member and then removing the cavity-forming member before the rare-earth magnet alloy begins to be sintered.
  • no machining is necessary to create the cavity and a sintered rare-earth magnet having a cavity can be produced at a low cost.
  • the compression-molding and aligning of a rare-earth magnet alloy powder is achieved by filling the powder into a container and applying a magnetic field to the powder while compressing it.
  • the inventor of the present patent application discovered the fact that a sintered rare-earth magnet could be created by filling a rare-earth magnet alloy powder into a powder-filling container, aligning the rare-earth magnet alloy powder without compression-molding this powder, and heating the powder in a state of being held in the powder-filling container.
  • This technique is called a press-less method. Refer to JP-A 2006-019521 .
  • the press-less method since the press-less method is used, the cavity-forming member undergoes no pressure even if this member is put in the powder-filling container together with the rare-earth magnet alloy powder.
  • the particles of the rare-earth magnet alloy powder held in the powder-filling container magnetically attract each other.
  • the cavity-forming member since the cavity-forming member is removed after the aligning process, the cavity will not be destroyed when the cavity-forming member is removed.
  • the powder When the rare-earth magnet alloy powder is heated to higher temperatures in the sintering process, the powder begins to be sintered when its temperature exceeds a specific level (e.g. approximately 600 degrees Celsius for a sintered Nd-Fe-B magnet), after which the sintered compact shrinks as the sintering process continues. To avoid impeding this shrinkage, the cavity-forming member used in the present invention is removed before the rare-earth magnet alloy powder begins to be sintered.
  • a specific level e.g. approximately 600 degrees Celsius for a sintered Nd-Fe-B magnet
  • the removal of the cavity-forming member is performed before the sintering process is initiated. This is done in that it eliminates the necessity of considering the heat resistance of the cavity-forming member or the reactivity between the cavity-forming member and the rare-earth magnet alloy powder.
  • the aforementioned rare-earth magnet alloy is an alloy of a sintered Nd-Fe-B magnet
  • Dy and/or Tb can be diffused into the sintered compact by injecting a substance containing Dy and/or Tb into the cavity of the sintered compact obtained by the sintering process.
  • a plate-shaped member can be used as the cavity-forming member. If the grain boundary diffusion is of primary importance, a rod-shaped member may be used. In the latter case, a large number of rod-shaped cavity-forming members may be arranged in the form of a matrix, whereby Dy and/or Tb can be uniformly diffused from a large number of holes.
  • the cross-sectional shape of the rod-shaped cavity-forming member is not specifically limited; for example, it may be circular, quadrilateral or hexagonal.
  • a plate-shaped or rod-shaped cavity-forming member is used as the cavity-forming member, it is preferable to align the rare-earth magnet alloy powder in a magnetic field parallel to the cavity-forming member in the aligning process.
  • the particles of the rare-earth magnet alloy powder forms a chain-like structure extending in the direction parallel to the cavity-forming member. Therefore, even if the cavity-forming member is removed in this state, the chain-like structure will not be broken off and the cavity will remain undestroyed.
  • the rare-earth magnet alloy powder may be mixed with a binder when it is filled into the powder-filling container.
  • the binder include methyl cellulose, polyacrylamide, polyvinyl alcohol, paraffin wax, polyethylene glycol, polyvinyl pyrrolidone, hydroxypropyl cellulose, hydroxypropyl methylcellulose, ethyl cellulose, acetyl cellulose, nitrocellulose, and polyvinyl acetate resin. (Refer to JP-A 10-270278 .)
  • the rare-earth magnet alloy powder When the rare-earth magnet alloy powder is filled into the powder-filling container together with the cavity-forming member, it is possible to simultaneously put both the powder of rare-earth magnet alloy and the cavity-forming member into the powder-filling container or to separately and sequentially fill them into the container.
  • the cavity formed in the sintered compact by the production method according to the present invention is mechanically weak and rather fragile if left in its original state. Furthermore, the cavity may retain moisture and cause corrosion or mechanical destruction of the product.
  • an embedding member such as epoxy resin
  • the process of filling the embedding member is performed after the removal of the cavity-forming member. If the embedding member is an epoxy resin or similar material whose heat-resistant temperature is lower than the sintering temperature of the rare-earth magnet, the filling process is performed after the sintering process. If the diffusion process is additionally performed, the filling process is performed after the diffusion process.
  • the embedding member should desirably be made of an insulating material to prevent the influence of eddy currents.
  • a cavity can be formed by a simple method including filling a powder of rare-earth magnet alloy into a powder-filling container together with a cavity-forming member, aligning the powder in a magnetic field, and removing the cavity-forming member.
  • Embodiments of the method for producing a sintered rare-earth magnet according to the present invention are hereinafter described by means of Figs. 1-11 .
  • Figs. 1 and 2 show the first embodiment of the present invention.
  • the method according to the first embodiment uses a mold (powder-filling container) 10 and a cavity-forming member 14 shown in Fig. 1 .
  • the mold 10 which is designed for creating a plate-shaped magnet, has a rectangular-parallelepiped receiving section 11, into which a powder of rare-earth magnet alloy is to be filled.
  • This receiving section 11 has an opening on its upper side, thus allowing the filling of the rare-earth magnet alloy powder and removal of a sintered rare-earth magnet after the sintering process.
  • a lid 13 for closing this opening is attached thereto.
  • the lid 13 has two insertion openings 131 extending parallel to each other in the longitudinal direction of the rectangular-parallelepiped receiving section 11. Each insertion opening 131 allows the insertion of a plate-shaped cavity-forming member 14, which is slightly smaller than the insertion opening 131 in both width and length. Examples of the materials available for the cavity-forming member 14 include various kinds of metal, carbon and plastic (which do not need to be heat-resistant in the present embodiment). There are two cavity-forming members 14 standing on a plate-shaped attachment base 15, with the same interval as the two insertion openings 131.
  • a rare-earth magnet alloy powder 19 is filled in the receiving section 11 ( Fig. 2(a) ).
  • the rare-earth magnet alloy powder 19 in a pure form may be used, or a binder may be mixed with the rare-earth magnet alloy powder 19.
  • the filling density should preferably be within a range from 40 to 50 % of the true density of the rare-earth magnet alloy powder.
  • the lid 13 is attached to the mold 10, and the cavity-forming members 14 are inserted through the insertion openings 131 into the rare-earth magnet alloy powder 19 held in the receiving section 11 ( Fig. 2(b) ).
  • the mold 10 is set into a magnetic-field generation coil 17, and a pulsed magnetic field parallel to the cavity-forming members 14 (and perpendicular to the lid 13) is applied to align the rare-earth magnet alloy powder 19 ( Fig. 2(c) ).
  • the strength of this magnetic field should be within a range from 3 to 10 T, and more preferably from 4 to 8 T.
  • the lid 13 should be securely pressed onto the mold 10 to prevent the rare-earth magnet alloy powder 19 from escaping.
  • the cavity-forming members 14 are pulled out from the rare-earth magnet alloy powder 19 and the insertion openings 131 ( Fig. 2(d) ).
  • slit-shaped cavities 18 are formed in the compact of the rare-earth magnet alloy powder 19.
  • the fine particles of the powder magnetically attract each other and hence will barely fall into the cavities 18.
  • the rare-earth magnet alloy powder 19 in a state of being held in the receiving section 11 is heated ( Fig. 2(e) ).
  • a sintered rare-earth magnet having slit-shaped cavities is obtained.
  • water and other substances that are inevitably present in the rare-earth magnet alloy powder 19 vaporize, and the generated gas is discharged through the insertion openings 131 to the outside of the mold.
  • the slits can be created at a much lower cost than in the case of performing machine work using a wire saw or similar tool after the sintering process. Furthermore, a narrow slit that cannot be created by machining can be created. The obtained slits are completely free from any unwanted matter (e.g. residual powder inside the slits) which lowers the functionalities of the slits. Thus, a high-quality slit can be obtained.
  • Figs. 3 and 4 show the second embodiment of the present invention.
  • the method according to the second embodiment uses a mold 20 shown in Fig. 3 and a cavity-forming member 24 shown in Fig. 4 .
  • the mold 20 has a receiving section 21 to which a lid 23 can be attached.
  • a difference from the first example exists in that two insertion openings 221 are formed in the bottom of the mold 20. No insertion opening is formed in the lid 23.
  • the cavity-forming members 24 fixed to a cavity-forming member attachment base 25 can be inserted into the insertion openings 221.
  • the method for producing a sintered rare-earth magnet according to the second embodiment is hereinafter described by means of Fig. 4 .
  • the cavity-forming members 24 are inserted into the insertion openings 221 of the mold 20 ( Fig. 4(a) ).
  • a rare-earth magnet alloy powder 29 is filled in the receiving section 21, and the lid 23 is attached ( Fig. 4(b) ).
  • the insertion of the cavity-forming member and the filling of the rare-earth magnet alloy powder are performed in reverse order as compared to the first embodiment.
  • the mold 20 is set into a magnetic-field generation coil 27, and a pulsed magnetic field parallel to the cavity-forming members 24 (and perpendicular to the lid 23) is applied to align the rare-earth magnet alloy powder 29 ( Fig. 4(c) ).
  • the cavity-forming members 24 are pulled out from the rare-earth magnet alloy powder 29 and the insertion openings 221 to form cavities 28 ( Fig. 4(d) ), and the rare-earth magnet alloy powder 29 in a state of being held in the receiving section 21 is sintered by heat ( Fig. 4(e) ).
  • Fig. 5 shows another example of the mold. Unlike the mold 10 shown in Fig. 1 in which the cavity-forming members 14 are fixed to the cavity-forming member attachment base 15 prepared separately from the lid 13, the cavity-forming members 14A in the present example are directly fixed to the lid 13A ( Fig. 5(a) ). If this lid 13A is used, the lid 13A is detached from the mold after the aligning process in order to remove the cavity-forming members 14.
  • the cavity-forming members are made of a material that liquefies or vaporizes at a temperature lower than the sintering temperature of the rare-earth magnet alloy powder, it is possible to remove the cavity-forming members, without pulling them out, by heating them together with the mold and rare-earth magnet alloy powder.
  • the cavity-forming members may be attached to the inside of the receiving section. Specific examples of the materials available for such a cavity-forming member include polyvinyl alcohol or other plastic materials that easily vaporize.
  • Fig. 5(b) shows one example in which cavity-forming members 14B stand at the bottom 12 of the receiving section 11.
  • the following description explains how to determine an appropriate thickness and interval of the cavity-forming members as well as an appropriate depth by which these members should be inserted into the rare-earth magnet alloy powder (which is hereinafter called the "insertion depth").
  • the cavity-forming members should be as narrow as possible.
  • the cavity-forming members should be as thin as possible.
  • the lower limit of the thickness of the cavity-forming member is approximately 0.05 mm.
  • the width of the slit to be eventually formed in the sintered compact will be approximately 0.04 mm.
  • the insertion depth it is preferable to increase this depth to improve the effect of reducing the eddy currents.
  • the depth is smaller than the magnet's thickness in the direction of the insertion depth preferably by 1 mm or more, and more preferably 2 mm or more.
  • the thickness of the cavity-forming member should be appropriately determined so that the volume ratio will be equal to or higher than 90 %.
  • the interval of the slits or the interval of the cavity-forming members, it is preferable to reduce this interval since the loss of energy due to the eddy currents generated in the magnet is proportional to the second power of the magnet size.
  • increasing the number of slits reduces the volume ratio of the magnet. Given these factors along with the aforementioned conditions relating to the thickness and insertion depth, the interval and number of the cavity-forming members should be determined so that the volume ratio will exceed the level where the required magnetic properties are obtained.
  • the cavity-forming member is too narrow, it is difficult to inject a substance containing Dy and/or Tb into the slit formed in the sintered compact. Therefore, it is preferable to form the slits with a width equal to or larger than 0.1 mm. If the interval of the slits is too large, the effect of grain boundary diffusion cannot extend over the entirety of the sintered magnet, causing the resulting product to have uneven magnetic properties.
  • the interval of the slits, or the interval of the cavity-forming members should preferably be equal to or smaller than 6 mm, and more preferably equal to or smaller than 5 mm.
  • the difference between this depth and the magnet's thickness in the direction of the insertion depth should preferably be equal to or smaller than 6 mm, and more preferably equal to or smaller than 5 mm.
  • the difference should preferably be equal to or larger than 1 mm, and more preferably equal to or larger than 2 mm.
  • the thickness, insertion depth, number and interval of the cavity-forming members should be determined so that the volume ratio of the product will exceed the level where the required magnetic properties are obtained.
  • Fig. 6 shows one example, in which a large number of rod-shaped cavity-forming members 34 are arrayed in rows and columns in the form of a matrix on a plate-shaped attachment base 35.
  • the use of such a large number of rod-shaped cavity-forming members 34 in the form of a matrix results in a sintered compact having a large number of fine pores (cavities).
  • Dy and/or Tb can be efficiently diffused through these fine pores into the sintered compact.
  • the diameter of the fine pores formed in the sintered compact should preferably be equal to or larger than 0.2 mm, and more preferably equal to or larger than 0.3 mm.
  • the interval of the cavity-forming members 34 should preferably be equal to or smaller than 6 mm, and more preferably equal to or smaller than 6 mm, to diffuse Dy and/or Tb over the entirety of the sintered magnet.
  • the conditions to be considered for the insertion depth are the same as in the case of the plate-shaped cavity-forming member.
  • the diffusion process includes filling a powder containing Dy and/or Tb into the cavities 18 and then heating the filled powder ( Fig. 7 ).
  • the heating temperature is typically within a range from 700 to 1000 degrees Celsius.
  • the Dy/Tb-containing substance to be injected into the cavities may be a fluoride, oxide, acid fluoride or hydride of Dy or Tb, an alloy of Dy or Tb and another kind of metal, or a hydride of such an alloy.
  • the alloy of Dy or Tb and another kind of metal include alloys of Ty or Tb and an iron group transition metal (e.g. Fe, Co or Ni), B, Al or Cu.
  • the grain boundary diffusion process can be effectively performed by mixing the aforementioned substances in an organic or similar solvent to prepare a slurry, injecting this slurry into the cavities, and heating the slurry.
  • This slurry may be injected into the cavities only, or it may be additionally applied to the surface of the sintered compact. In latter case, the grain boundary diffusion takes place from both the cavities and the surface of the sintered compact.
  • the grain boundary diffusion process is performed by heating the sintered compact at 700 to 1000 degrees Celsius for one to twenty hours under vacuum or in an inert-gas atmosphere.
  • This grain boundary diffusion process uses only a small amount of Dy and/or Tb and yet can effectively increase the coercive force of the sintered Nd-Fe-B magnet without significantly decreasing its residual flux density even if the magnet has a substantially large thickness of 5 mm or larger.
  • the cavities are formed for both purposes of helping the grain boundary diffusion process and reducing the loss of energy due to eddy currents
  • an epoxy resin in a liquid state is injected into the cavities 18 and then cured at room temperature or by heat ( Fig. 8 ).
  • this embedding process can be performed before the sintering process. In the case of using an epoxy resin or similar adhesive resin, this process is performed after the sintering process. If the diffusion process is additionally performed, the embedding process is performed after the diffusion process.
  • a strip-cast alloy of an Nd-Fe-B rare-earth magnet was subjected to hydrogen pulverization and then a jet-mill process using nitrogen gas, to obtain a rare-earth magnet powder with an average particle size of 5 ⁇ m.
  • the composition of this rare-earth magnet powder ratio was Nd: 25.8%, Pr: 4.3%, Dy: 2.5%, Al: 0.23%, Cu: 0.1%, and Fe: the rest.
  • the average particle size of the rare-earth magnet powder was measured with a laser-type particle-size analyzer.
  • This powder was filled into the mold 10 of the first embodiment to an apparent density of 3.5 g/cm 3 , after which the lid 13 was put on the mold 10. Subsequently, the cavity-forming members 14 were inserted through the insertion openings 131. After the mold 10 was fixed in a magnetic-field generation coil, a pulsed magnetic field of 5 T was applied three times in the direction parallel to the cavity-forming members 14 and perpendicular to the bottom of the mold 10 so as to align the rare-earth magnet powder in the magnetic field. Subsequently, the cavity-forming members 14 were pulled out from the mold 10, and then the mold 10 was put into a sintering furnace.
  • the entire process from the filling of the powder to the putting of the mold into the furnace was carried out in an argon-gas atmosphere.
  • the sintering process was performed under vacuum at 1010 degrees Celsius for two hours.
  • the mold 10 and the lid 13 were made of carbon and the cavity-forming members 14 were made of non-magnetic stainless steel.
  • the thickness of the cavity-forming members 14 was 0.5 mm.
  • the sintered compact created by the previously described process had a density of 7.56 g/cm 3 , which is as high as the density of a sintered Nd-Fe-B magnet created by a normal pressing method.
  • the obtained sintered compact 31 ( Fig. 9 ) had the shape of a rectangular parallelepiped having a short-side length of 37 mm, a long-side length of 39 mm and a height of 8.6 mm, with two slits 32 extending parallel to the shorter sides and at an interval of 12 mm on the top face. No noticeable deformation in the outside shape of the sintered compact or the slits 32 was recognized.
  • the slits 32 had a width of approximately 0.4 mm and a depth of 6.2 mm.
  • a metallic foil having a thickness of 0.3 mm was inserted into each slit 32. The result confirmed that none of these slits 32 was clogged or closed with foreign matter.
  • a sintered Nd-Fe-B magnet with slits was created by using the mold 20 and the cavity-forming members 24 of the second embodiment.
  • the powder needs to be filled into the mold 20 with the cavity-forming members 24 attached thereto.
  • the filling density was 3.6 g/cm 3 .
  • the lid 23 was put on the mold 20. Subsequently, the aligning process in the magnetic field and the removal of the cavity-forming members 24 were performed under the same conditions as in Example 1, and then the sintering process was performed under the same conditions as in Example 1.
  • the sintered compact was removed from the mold. Similar to the product created in Example 1, the obtained sintered compact had a high density and no deformation in its shape. The slits were also found to be high-quality slits free from clogging or closing. The outside shape of the sintered compact, the interval of the slits, the width and other sizes of each slit were approximately the same as those of Example 1.
  • a sintered compact with cavities was created by using the molds and cavity-forming members shown in Figs. 10 and 11 .
  • the mold 40 shown in Fig. 10 has a rectangular-parallelepiped receiving section 41 having square-shaped top and bottom sides.
  • a lid 43 can be attached to the top side.
  • This lid 43 has two insertion openings 431 for allowing the insertion of two plate-shaped cavity-forming members 44.
  • the mold used in the example shown in Fig. 11 is the same as this mold 40.
  • a lid 53 to be attached to the mold 40 in the latter example has four insertion openings 531 arranged in the form of a square, thus allowing the insertion of four rod-shaped cavity-forming members 54.
  • Example 3-1 a sintered compact with slits (Example 3-1) and a sintered compact with fine pores (Example 3-2) were created by using the cavity-forming members 44 and 54, respectively.
  • Both sintered compacts had a cubic outside shape with one side approximately measuring 11 mm.
  • the slits formed in the former sintered compact had a width of 0.4 mm and a depth of 5.9 mm, and were spaced by an interval of 3.3 mm.
  • the fine pores formed in the latter sintered compact had a diameter of 0.5 mm and a depth of 7.2 mm.
  • Example 1 Another sintered compact having a rectangular-parallelepiped shape with neither slits nor fine pores (Comparative Example 1) was also created under the same conditions as used in the present Example (and Example 1) except that the insertion and removal of the cavity-forming members 44 were omitted.
  • Each of the three types of sintered compacts was shaped into a cube with one side accurately measuring 10 mm by using a surface grinder. The obtained cubes were then subjected to alkaline cleaning, acid cleaning and pure-water cleaning processes followed by a drying process.
  • a grain boundary diffusion process using a Dy-containing alloy powder was performed as follows: Initially, a Dy-containing alloy having a composition by atomic ratio of Dy: 80%, Ni: 14%, Al: 4%, and other kinds metals and impurities: 2 % was pulverized to an average particle size of 9 ⁇ m with a jet mill to obtain a Dy-containing alloy powder. Next, this powder was mixed with ethanol by 50 % by weight and stirred. The obtained mixture was vacuum-impregnated into the slits of the sample of Example 3-1 and the fine pores of the sample of Example 3-2, and then dried. Subsequently, the Dy-containing powder was applied to the surface of each of the magnets of Examples 3-1, 3-2 and Comparative Example.
  • Comparative Example 1-1 was obtained by performing the aforementioned grain boundary diffusion process on the sintered compact of Comparative Example 1.
  • Comparative Example 1-2 was obtained by heating the sintered compact of Comparative Example 1, without any Dy-containing alloy powder applied to its surface, in the same manner as in the grain boundary diffusion process.
  • the samples of Examples 3-1 and 3-2 had higher coercive forces H cJ and higher squareness H k /H cJ of magnetization curves. Their coercive forces H cJ were also higher than that of the sample of Comparative Example 1-2, for which no grain boundary diffusion process was performed.

Claims (10)

  1. Ein Verfahren zur Herstellung eines gesinterten Seltenerdmagneten mit einer Kavität durch Ausführen der folgenden aufeinanderfolgenden Prozesse:
    a) einen Füllprozess zum Füllen eines Pulvers von einer Seltenerdmagnetlegierung in einen Pulverfüllbehälter (10; 20; 40) durch gleichzeitiges Einbringen sowohl des Pulvers (19; 29) von Seltenerdmagnetlegierung als auch eines eine Kavität bildenden Glieds (14; 24; 34; 44; 54) in den Pulverfüllbehälter (10; 20; 40) oder durch separates und aufeinanderfolgendes Einbringen des Pulvers (19; 29) von Seltenerdmagnetlegierung und des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) in den Pulverfüllbehälter (10; 20; 40);
    b) einen Ausrichtprozess zum Ausrichten des Seltenerdmagnetlegierungspulvers (19; 29) in einem Magnetfeld; und
    c) einen Sinterprozess zum Sintern des Seltenerdmagnetlegierungspulvers (19; 29) durch Erhitzen des Seltenerdmagnetlegierungspulvers (19; 29) in einem Zustand, in dem es in dem Pulverfüllbehälter (10; 20; 40) gehalten ist,
    wobei das eine Kavität bildende Glied (14; 24; 34; 44; 54) entfernt wird, um die Kavität (18; 28) zu bilden, nachdem der Ausrichtprozess beendet ist und bevor das Seltenerdmagnetlegierungspulver (19; 29) zu sintern beginnt, und wobei eine Einsetztiefe des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) kleiner ist als die Dicke des Magneten in der Richtung der Einsetztiefe, d.h. kleiner als eine Tiefe des Pulverfüllbehälters (10; 20; 40).
  2. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach Anspruch 1, dadurch gekennzeichnet, dass das Entfernen des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) durchgeführt wird, bevor der Sinterprozess eingeleitet wird.
  3. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das eine Kavität bildende Glied (14; 24; 34; 44; 54) ein plattenförmiges Glied oder ein stabförmiges Glied ist.
  4. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach Anspruch 3, dadurch gekennzeichnet, dass in dem Ausrichtprozess das Seltenerdmagnetlegierungspulver (19; 29) in einem Magnetfeld parallel zu dem eine Kavität bildenden Glied (14; 24; 34; 44; 54) ausgerichtet wird.
  5. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach einem der Ansprüche 1-4, dadurch gekennzeichnet, dass in dem Füllprozess ein Binder zusammen mit dem Seltenerdmagnetlegierungspulver (19; 29) in den Pulverfüllbehälter (10; 20; 40) eingefüllt wird.
  6. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach einem der Ansprüche 1-5, dadurch gekennzeichnet, dass nach der Entfernung des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) ein Einbettungsglied in die Kavität (18; 28) eingefüllt wird.
  7. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach einem der Ansprüche 1-5, dadurch gekennzeichnet, dass:
    die Seltenerdmagnetlegierung eine Nd-Fe-B-Magnetlegierung ist; und
    ein Diffusionsprozess zum Eindiffundieren von Dy und/oder Tb in den gesinterten Presskörper durchgeführt wird durch Injizieren einer Dy und/oder Tb enthaltenden Substanz in die Kavität (18; 28) des gesinterten Presskörpers, der durch den Sinterprozess erhalten wird.
  8. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach Anspruch 7, dadurch gekennzeichnet, dass nach dem Diffusionsprozess ein Einbettungsglied in die Kavität (18; 28) eingefüllt wird.
  9. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach Anspruch 6 oder 8, dadurch gekennzeichnet, dass das Einbettungsglied aus einem isolierenden Material hergestellt ist.
  10. Das Verfahren zur Herstellung eines gesinterten Seltenerdmagneten nach einem der Ansprüche 1-9, dadurch gekennzeichnet, dass der Füllprozess umfasst: Einsetzen des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) in den Pulverfüllbehälter (10; 20; 40) durch eine Einsetzöffnung (131; 221; 431; 531) hindurch, welche entweder in dem Pulverfüllbehälter (10; 20; 40) oder in einem Deckel (13; 23; 53) des Pulverfüllbehälters (10; 20; 40) ausgebildet ist, und dass der Entfernungsprozess umfasst: Herausziehen des eine Kavität bildenden Glieds (14; 24; 34; 44; 54) aus der Einsetzöffnung (131; 221; 431; 531).
EP09824563.2A 2008-11-06 2009-10-29 Verfahren zur herstellung gesinterter seltenerdmagneten Not-in-force EP2348518B1 (de)

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