WO2005043558A1 - Procede de production d'un aimant de terre rare frittee - Google Patents

Procede de production d'un aimant de terre rare frittee Download PDF

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Publication number
WO2005043558A1
WO2005043558A1 PCT/JP2004/016010 JP2004016010W WO2005043558A1 WO 2005043558 A1 WO2005043558 A1 WO 2005043558A1 JP 2004016010 W JP2004016010 W JP 2004016010W WO 2005043558 A1 WO2005043558 A1 WO 2005043558A1
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Prior art keywords
powder
added
rare earth
sample
strength
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PCT/JP2004/016010
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English (en)
Japanese (ja)
Inventor
Makoto Iwasaki
Chikara Ishizaka
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Tdk Corporation
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Priority to JP2005515145A priority Critical patent/JP4033884B2/ja
Priority to US10/541,724 priority patent/US20060207689A1/en
Priority to EP04793118A priority patent/EP1679724A4/fr
Publication of WO2005043558A1 publication Critical patent/WO2005043558A1/fr

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    • 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
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F3/12—Both compacting and sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • C22C1/0441—Alloys based on intermetallic compounds of the type rare earth - Co, Ni
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • 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
    • 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

Definitions

  • the present invention relates to a method for producing a rare earth sintered magnet containing a rare earth element, a transition metal element and B (boron) as main components, and particularly to a method for producing a rare earth sintered magnet by powder metallurgy. And a technique for improving the strength of a compact before sintering.
  • Rare earth sintered magnets for example, NdFeB-based sintered magnets have advantages such as excellent magnetic properties! Nd, the main component, is abundant in resources and relatively inexpensive. Therefore, the demand has been increasing in recent years. Under these circumstances, research and development for improving the magnetic properties of NdFe-B based sintered magnets and improvement of the manufacturing method for manufacturing high quality rare earth sintered magnets (for example, Patent Document 1 and See Patent Document 2 etc.) etc. in various fields.
  • Patent Literature 1 a lubricant diluted with a specific organic solvent is mixed with an alloy powder so as to eliminate a decrease in the strength of a molded body due to the addition of a lubricant.
  • Patent Document 2 by changing the timing at which the lubricant is added, the wear of the crushing equipment is reduced while enjoying the effects such as improvement of the degree of orientation by the lubricant-added mash.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 9 3504
  • Patent Document 2 JP-A-2003-68551
  • a powder metallurgy method As a method for producing a rare earth sintered magnet, a powder metallurgy method is known, as described in the above-mentioned patent documents, and is widely used because it can be produced at low cost. ing.
  • a powder metallurgy method first, a raw material alloy ingot is roughly pulverized and finely pulverized to obtain a raw material alloy fine powder having a particle diameter of about several meters.
  • the raw material alloy fine powder thus obtained is subjected to magnetic field orientation in a static magnetic field, and press molding is performed in a state where a magnetic field is applied. After forming in a magnetic field, the formed body is sintered in the air or in an inert gas atmosphere, and further subjected to aging treatment.
  • the present invention has been proposed in view of such conventional circumstances, and has as its object to develop a technology capable of improving the strength of a compact without deteriorating the magnetic characteristics. It is an object of the present invention to provide a method for manufacturing a rare earth sintered magnet capable of manufacturing a rare earth sintered magnet excellent in gas characteristics with a high yield.
  • the present inventors have conducted various studies over a long period of time in order to achieve the above object. As a result, they came to the conclusion that the addition of metal powder (eg, A1 powder, Ni powder, Zr powder, Mn powder) to the raw material alloy fine powder was effective.
  • the present invention has been completed based on such findings, and R (R is one or more rare earth elements, where the rare earth element is a concept including Y), T (T is Fe Or one or two or more transition metal elements which essentially include Fe and Co) and a raw material alloy fine powder containing B, and in which a metal powder is added when producing a rare earth sintered magnet. It is characterized in that raw material alloy fine powder is formed and sintered.
  • the caroten metal powder is, for example, one or more of A1 powder, Ni powder, Zr powder, and Mn powder.
  • the strength of the compact is improved by adding the additional metal powder during the compaction of the raw material alloy powder.
  • the effect is high when the additive metal powder is a plate-like metal powder. The reason for this is unknown, but it has been confirmed experimentally.
  • the magnetic property deterioration caused by the added metal powder is small!
  • the addition time of the added metal powder is arbitrary as long as it is after pulverizing the melt-formed raw material alloy and before forming, and may be, for example, either after coarse pulverization or after fine pulverization.
  • A1, Zr, Ni, Mn, etc. are also known as elements contained in rare earth sintered magnets, but in order to achieve the object of the present invention, they are added at the stage of melting and forming the raw material alloy. However, it is necessary to pulverize the melted and forged raw material alloy and then add it to the raw material alloy powder as A1 powder, Zr powder, Ni powder, Mn powder or the like.
  • the strength of the compact before sintering can be improved, and the compact can be easily formed. Can be suppressed. Therefore, it is possible to reduce a decrease in yield due to cracks or chipping of the compact, and it is possible to efficiently manufacture a rare earth sintered magnet. Further, according to the present invention, it is possible to manufacture a rare earth sintered magnet having excellent magnetic properties such as coercive force and residual magnetic flux density without deteriorating the magnetic properties of the sintered rare earth magnet. is there.
  • FIG. 1 is a flowchart showing an example of a process for producing a rare earth sintered magnet.
  • FIG. 2 is a flowchart showing another example of the manufacturing process of the rare earth sintered magnet.
  • FIG. 3 is a schematic perspective view illustrating a method of measuring bending strength.
  • FIG. 4 is a micrograph of spherical A1 powder.
  • FIG. 5 is a micrograph of plate-like A1 powder.
  • the rare earth sintered magnet to be manufactured mainly includes a rare earth element, a transition metal element, and boron.
  • the magnet composition may be arbitrarily selected according to the purpose.
  • RTB (R is a concept of one or more rare earth elements, where the rare earth element includes Y. T is one or two or more of Fe or a transition metal element essential for Fe and Co. (Where B is boron.)
  • B is boron.
  • the composition be such that 40% by mass, 0.5-4.5% by mass of boron B, and the balance be transition metal element T.
  • R is a rare earth element, that is, one or more selected from the group consisting of Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb and Lu.
  • Nd is preferable as the main component because Nd is abundant in resources and relatively inexpensive.
  • Dy increases the anisotropic magnetic field, and is effective in improving the coercive force Hcj.
  • an additional element M to obtain an R—TB—M based rare earth sintered magnet.
  • the additional element M include Al, Cr, Mn, Mg, Si, Cu, C, Nb, Sn, W, V, Zr, Ti, Mo, Bi, and Ga.
  • One or more species can be selected and added.
  • the addition amount of these additional elements M is preferably 3% by mass or less in consideration of magnetic properties such as residual magnetic flux density. If the amount of the additive element M is too large, the magnetic properties may be deteriorated.
  • the present invention is not limited to these compositions, and it is needless to say that the present invention can be applied to all conventionally known compositions of rare earth sintered magnets!
  • FIG. 1 shows an example of a process for producing a rare earth sintered magnet by powder metallurgy.
  • This manufacturing process basically consists of an alloying step 1, a coarse pulverizing step 2, a fine pulverizing step 3, a forming step in a magnetic field 4, a sintering and aging step 5, a processing step 6, and a surface treatment step 7. Is done.
  • a coarse pulverizing step 2 a fine pulverizing step 3
  • a forming step in a magnetic field 4 a sintering and aging step 5
  • a processing step 6 and a surface treatment step 7.
  • Is done In order to prevent oxidization, most of the steps up to sintering were performed in vacuum. It is preferable to perform the reaction in a medium or in an inert gas atmosphere (such as a nitrogen atmosphere or an Ar atmosphere).
  • a metal or an alloy as a raw material is blended according to the magnet composition, melted in a vacuum or an inert gas, for example, an Ar atmosphere, and alloyed by forming.
  • a strip casting method continuous production method in which molten high-temperature liquid metal is supplied onto a rotating roll to continuously produce an alloy thin plate is preferable in terms of productivity and the like. It is not limited to that.
  • a raw material metal alloy
  • pure rare earth elements, rare earth alloys, pure iron, ferroboron, and alloys thereof can be used.
  • Solution treatment may be performed as necessary for the purpose of eliminating solidification segregation.
  • the temperature is maintained at 700 to 1500 ° C. for 1 hour or more in a vacuum or Ar atmosphere.
  • the alloy may be a single alloy having almost the final magnet composition, or a plurality of alloys having different compositions may be mixed so as to have the final magnet composition. Mixing may be performed in any process of alloying, raw material coarse powder, and raw material fine powder.
  • a thin plate or ingot of the raw material alloy prepared above is pulverized until the particle size becomes about several hundreds / zm.
  • a stamp mill, a jaw crusher, a brown mill or the like can be used as a pulverizing means.
  • the coarse pulverizing step 2 may be constituted by a plurality of steps combining a plurality of pulverizing means.
  • FIG. 2 shows an example in which the coarse pulverizing step 2 includes two steps, a hydrogen pulverizing step 2a and a mechanical coarse pulverizing step 2b.
  • the hydrogen pulverizing step 2a is a step in which hydrogen is occluded in the manufactured raw material alloy, and pulverization is performed in a self-disintegrating manner by utilizing the fact that the amount of hydrogen occlusion varies depending on the phase. Thereby, it can be crushed to a particle size of about several mm.
  • the mechanical coarse pulverizing step 2b is a step of pulverizing using a mechanical method such as a brown mill as described above, and the raw material alloy pulverized to a size of about several mm by the hydrogen pulverizing step 2a.
  • the powder is ground to a particle size of several hundreds; In order to improve the coarse pulverizability, it is effective to perform the coarse pulverization in combination with the hydrogen pulverization step.
  • the mechanical coarse crushing step 2b can be omitted.
  • a pulverizing assistant is usually added to the coarsely pulverized raw alloy powder.
  • the grinding aid for example, a fatty acid compound or the like can be used.
  • a rare earth sintered magnet having good magnetic properties can be obtained.
  • the addition amount of the grinding aid is preferably 0.03 to 0.4% by mass. When the grinding aid is added within this range, the amount of residual carbon after sintering can be reduced, which is effective in improving the magnetic properties of the rare earth sintered magnet.
  • a fine pulverizing step 3 is performed.
  • the fine pulverizing step 3 is performed using, for example, a jet mill.
  • the conditions for the fine pulverization can be appropriately set according to the air-flow type pulverizer to be used.
  • the raw material alloy powder is finely pulverized until the average particle diameter becomes about 110 m, for example, 3-6 m.
  • Jet mills release high-pressure inert gas (for example, nitrogen gas) from a narrow nozzle to generate a high-speed gas flow, which accelerates the powder particles and causes the particles to collide with each other.
  • the target ⁇ ⁇ is a method of crushing by generating collision with the container wall. Jet mills are generally classified into jet mills using a fluidized bed, jet mills using a vortex, jet mills using an impinging plate, and the like.
  • the raw material alloy fine powder is formed in a magnetic field.
  • the raw material alloy fine powder obtained in the fine pulverization step 3 is filled in a mold in which an electromagnet is arranged, and is formed in a magnetic field with a crystal axis oriented by applying a magnetic field.
  • the molding in a magnetic field may be either vertical magnetic field molding or horizontal magnetic field molding. This molding in a magnetic field may be performed, for example, in a magnetic field of 800 to 1500 kAZm at a pressure of about 130 to 160 MPa.
  • sintering and aging treatment are performed. That is, after the raw alloy fine powder is compacted in a magnetic field, the compact is sintered in a vacuum or an inert gas atmosphere.
  • the sintering temperature needs to be adjusted according to various conditions such as composition, pulverization method, difference in particle size and particle size distribution, etc. This is preferred.
  • the obtained sintered body is preferably subjected to an aging treatment.
  • This aging treatment is an important step in controlling the coercive force Hcj of the obtained rare earth sintered magnet.
  • the aging treatment is performed in an inert gas atmosphere or in a vacuum.
  • two-stage aging treatment is preferred.
  • the temperature is kept at about 800 ° C for 11 to 13 hours.
  • the temperature is kept at about 550 ° C for 11 to 13 hours.
  • a second quenching step for quenching to room temperature is provided. Since the coercive force Hcj is greatly increased by the heat treatment at around 600 ° C, when performing the aging treatment in one stage, the aging treatment at around 600 ° C may be performed.
  • Processing step 6 is a step of mechanically forming a desired shape.
  • the surface treatment step 7 is a step performed to suppress oxidation of the obtained rare earth sintered magnet, and for example, a plating film and a resin film are formed on the surface of the rare earth sintered magnet.
  • a metal powder added as a forming aid is added to the raw material alloy fine powder, and the raw alloy powder is formed in a magnetic field forming step 4.
  • any metal powder such as Al, Mn, Fe, Co, Ni, Cu, Zn, Zr, Ag, Sn, Bi and the like can be used, and one or more of these can be used. Select and use. Above all, it is preferable to add one or more of these powers, which are preferably selected from A1 powder, Ni powder, Zr powder, and Mn powder, as molding aids.
  • the timing of adding the added metal powder may be between the time when the raw material alloy is melt-formed and pulverized in the alloying step 1 and the pulverization is performed, and the time when it is formed in the magnetic field in the magnetic field forming step 4.
  • the timing of adding the added metal powder may be between the time when the raw material alloy is melt-formed and pulverized in the alloying step 1 and the pulverization is performed, and the time when it is formed in the magnetic field in the magnetic field forming step 4.
  • the fine pulverization step 3 addition time A in the figure
  • the coarse pulverization step 2 addition time B in the figure
  • the hydrogen grinding step 2a additional time C in the figure.
  • the timing of adding the added metal powder may be basically any of these, but it is more effective to add the force as the raw material alloy is crushed. The effect is most effective when it is added to the raw material alloy fine powder immediately before compaction. Therefore, for example, in the manufacturing process of FIG. 1, it is more effective to add after the fine grinding step 3 (addition time A) than after the coarse grinding step 2 (addition time B). high. Similarly, in the manufacturing process shown in FIG. 2, it is more effective to add after the mechanical coarse grinding step 2a (addition time B) than to add after the hydrogen grinding step 2a (addition time C). Furthermore, it is more effective to add it after the fine grinding step 3 (addition time A) than after the mechanical coarse grinding step 2a (addition time B). Yes.
  • the additive metal powder may be mixed by a known mixing method, and any method may be employed as long as it is uniformly mixed, such as a V mixer or a ribbon mixer.
  • the addition amount of the added metal powder is preferably 0.01% by mass or more with respect to the raw material alloy fine powder, and more preferably 0.02% by mass or more. If the amount of the added metal powder is less than 0.01% by mass, it is difficult to obtain a sufficient effect. However, in consideration of the deterioration of the magnetic characteristics, the content is preferably 0.5% by mass or less. If the amount of the added metal powder exceeds 0.5% by mass, the magnetic properties may be deteriorated.
  • the optimum addition amount of the added metal powder varies depending on the type of the added metal powder.
  • the optimum addition amount of the A1 powder is 0.15% by mass or more and 0.3% by mass or less.
  • the optimal addition amount of Ni powder is 0.02% by mass to 0.08% by mass.
  • the optimal amount of Zur powder added is 0.15% by mass to 0.3% by mass.
  • the optimum addition amount of the Mn powder is 0.02% by mass to 0.25% by mass.
  • the average particle size and the like of the added metal powder to be added are arbitrary.
  • the average particle size of the added metal powder to be used may be appropriately selected according to the particle size of the raw material alloy fine powder.
  • the average particle size of the added carometal powder is 50 ⁇ m or less, and more preferably 10 ⁇ m or less.
  • the effect is high when the additive metal powder to be used is in the shape of a plate having an arbitrary shape. Therefore, for example, it is preferable to use a flat metal powder having a predetermined thickness such as a scale. Such a plate-like powder can be easily identified by observing the powder with a microscope or the like, for example.
  • the thickness is arbitrary, and preferably the plate ratio is 2-15.
  • the plate surface diameter is preferably 50 / zm or less, more preferably 10m or less.
  • the thickness of the plate-like powder is more preferably 10 m or less, and more preferably 10 m or less.
  • the added metal powder added after the sintering is alloyed with the raw material alloy and taken in. If the added metal powder is not more than a predetermined amount, it does not affect the properties of the obtained rare earth sintered magnet.
  • composition of the raw material alloy ND24. 5 mass 0/0, Pr6. 0 mass 0/0, Dyl. 8 mass 0/0, CoO
  • a metal or alloy as a raw material was blended so as to have the above-mentioned composition, and a raw material alloy thin plate was melted and manufactured by a strip casting method.
  • the obtained raw material alloy thin plate is pulverized with hydrogen, it is mechanically coarsely pulverized by a brown mill to obtain a raw material alloy coarse powder.
  • the grinding aid material alloy coarse powder were added Orein acid amide 0.1 wt 0/0.
  • the added metal powder was added to the raw material alloy fine powder and mixed in a mortar.
  • Each of the obtained powders was molded in a magnetic field to obtain a molded body having a predetermined shape.
  • the powder was molded at a molding pressure of 147 MPa in a magnetic field of 1200 kA Zm.
  • the direction of the magnetic field is perpendicular to the pressing direction.
  • the compact formed in a magnetic field was sintered and subjected to an aging treatment to prepare Sample 119.
  • the sintering was performed at a sintering temperature of 1030 ° C for 4 hours in a vacuum.
  • the aging was a two-stage aging treatment, with the first stage at 900 ° C for 1 hour and the second stage at 530 ° C for 1 hour.
  • the bending strength of the molded body formed by molding in a magnetic field was measured.
  • the bending strength was measured according to Japanese Industrial Standard JIS R 1601. That is, as shown in FIG. 3, the molded body 11 is placed on two round bar-shaped supports 12, 13, and the round bar-shaped support 14 is also arranged at the center position on the molded body 11. A load was applied.
  • the chip size of the molded body 11 was 20 mm X I 8 mm X 6 mm.
  • the direction to apply the bending force was the pressing direction.
  • the coercive force Hcj and the residual magnetic flux density Br were measured for each of the manufactured rare earth sintered magnets. The measurement was performed using a B—H tracer.
  • spherical A1 powder was used as the added metal powder, and the amount of the spherical A1 powder added was changed as shown in Table 1, to prepare Sample 11 to Sample 1-11.
  • Use Fig. 4 shows a micrograph of the spherical Al powder used.
  • the particle size of A1 powder used in Sample 11 and Sample 19 was 20 ⁇ m, and the particle size of Al powder used in Samples 10 and 11 was 40 ⁇ m.
  • Table 1 shows the amount of spherical A1 powder added, the magnet A1 composition, the bending strength of the compact (compact strength), and the magnetic properties (coercive force Hcj and residual magnetic flux density Br) of each sample.
  • a rare-earth sintered magnet was prepared by changing the addition time of the spherical A1 powder.
  • the amount of spherical A1 powder added was 0.20% by mass.
  • the spherical A1 powder was added after hydrogen pulverization (sample 1 12), after coarse pulverization by a brown mill (sample 1 13), and after fine pulverization by a jet mill (sample 1-14).
  • a sample (Sample 115) was also prepared in which A1 was added to the alloy composition in an amount equivalent to the amount of spherical A1 powder added.
  • the strength and magnetic properties (coercive force Hcj and residual magnetic flux density Br) were measured in the same manner. Table 2 shows the results.
  • the difference in magnetic properties between the case where A1 powder was added as an additive metal powder and the case where it was added as an alloy composition was investigated.
  • the prepared samples were sample 1 16 with the raw material alloy A1 composition being 0.2% by mass and the amount of spherical A1 powder added being 0% by mass.
  • Sample 1-17 with an amount of 0.2% by mass
  • Sample 1-18 with a raw alloy A1 composition of 0% by mass and an addition amount of spherical A1 powder of 0.2% by mass, and a 0% mass of the material alloy A1 % Of the spherical A1 powder and 0% by mass.
  • Sample 116 is the same as Sample 11
  • Sample 1-17 is the same as Sample 1-6.
  • Table 3 shows the composition of the raw material alloy A1, the amount of A1 powder added, the strength of the compact, the coercive force Hcj, and the residual magnetic flux density Br of each sample.
  • Sample A20 was prepared by adding plate-like A1 powder as an additive metal powder in the amount shown in Table 4.
  • FIG. 5 shows a micrograph of the plate-like A1 powder used.
  • the plate surface diameter of the plate-like A1 powder used was 40 ⁇ m and the thickness was 3 ⁇ m.
  • Table 4 shows the calorie content of the plate-like Al powder, the bending strength of the compact, and the magnetic properties (coercive force Hcj and residual magnetic flux density Br) of each sample.
  • the addition of the plate-like A1 powder has the effect of improving the transverse rupture strength of the molded article.
  • the effect is higher than when the granular A1 powder is added.
  • spherical Ni powder particle diameter 2 m
  • the amount of spherical Ni powder added was changed as shown in Table 1. 2-9 were prepared.
  • Table 6 shows the addition amount of spherical Ni powder, flexural strength (compact strength), and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of the compact in each sample.
  • the addition of the spherical Ni powder improves the bending strength of the molded body.
  • the improvement in the bending strength of the molded product peaks at around 0.05% by mass of the added amount of spherical Ni powder, and tends to decrease slightly with the added amount of more than that.
  • the magnetic properties the larger the amount of spherical Ni powder added, the better the magnetic properties, especially the coercive force Hcj. From these facts, it is understood that the addition amount of the spherical Ni powder is preferably set to 0.02% by mass or more, more preferably 0.02% by mass to 0.08% by mass.
  • a rare-earth sintered magnet was manufactured by changing the addition time of the spherical Ni powder.
  • the addition amount of the spherical Ni powder is 0.05% by mass.
  • the addition time of the spherical Ni powder was after pulverization with hydrogen (sample 2-10), after coarse pulverization with a brown mill (sample 2-11), and after fine pulverization with a jet mill (sample 2-12).
  • a sample (Sample 2-13) was also prepared in which Ni was added to the alloy composition in an amount equivalent to the amount of Ni powder added.
  • the flexural strength and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of these samples were measured in the same manner. Table 7 shows the results.
  • the addition of Ni powder can improve the strength of the compact in any case.
  • the effect increases as the powder is added later in the pulverization process. I have. That is, the improvement in the strength of the compact is larger in Sample 2-11 than in Sample 2-10.
  • the improvement in the strength of the compact is larger in Sample 2-12 than in Sample 2-11.
  • Sample 2-13 in which Ni was added to the alloy composition, had the same strength as that of Sample 2-1 to which no Ni powder was added, and no effect was observed on the strength of the compact.
  • Plate-like Ni powder was added as the added metal powder in the amount shown in Table 8 to prepare Sample 2-14 and Sample 2-2-2.
  • the plate-like Ni powder used had a plate surface diameter of 10 m and a thickness of 2 m.
  • Table 8 shows the addition amount of plate-like Ni powder, the bending strength of the compact, and the magnetic properties (coercive force Hcj and residual magnetic flux density Br) of each sample.
  • the addition of the plate-like Ni powder has the effect of improving the transverse rupture strength of the compact, and the effect is higher than that of the case where the granular Ni powder is added.
  • Rare earth sintered magnets were manufactured according to the above manufacturing method while changing the addition time of Zr powder.
  • plate-like Zr powder was used.
  • the plate surface diameter of the plate-like Zr powder is 15 m and the thickness is 3 ⁇ m.
  • the amount of Zr powder added was 0.20% by mass.
  • the addition time of plate-like Zr powder was after hydrogen grinding (Sample 3-10), after coarse grinding by Brown mill (Sample 3-11), and after fine grinding by jet mill (Sample 3-12).
  • a sample (Sample 3-13) was also prepared in which Zr was added to the alloy composition in an amount corresponding to the amount of Zr powder added.
  • the bending strength and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of these samples were measured in the same manner. Table 11 shows the results.
  • the addition of Zr powder can improve the strength of the compact in any case, but the effect increases as the powder is added later in the pulverization process. ing. That is, the improvement in the strength of the compact is larger in Sample 3-11 than in Sample 3-10. The improvement in the strength of the compact is larger in Sample 3-12 than in Sample 3-11. In Sample 3-13 in which Zr was added to the alloy composition, the strength of the compact was not different from that of Sample 3-1 in which Zr powder was not added, and no effect was observed in the strength of the compact.
  • Sample 3-14 and Sample 3-22 were prepared by adding plate-like Zr powder as the added metal powder in the amounts shown in Table 12.
  • the plate surface diameter of the used plate-like Zr powder was 15 m and the thickness was 3 ⁇ m.
  • Table 12 shows the addition amount of plate-like Zr powder, bending strength and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of each sample.
  • sample-like Zr powder 0.20% by mass of plate-like Zr powder was added as an additive metal powder.
  • the transverse rupture strength of the molded body was improved. Has improved.
  • the improvement in the bending strength of the molded product peaks at about 0.10% by mass of the added amount of Mn powder, and tends to slightly decrease with the added amount of Mn powder. Therefore, it is understood that the addition amount of the Mn powder is preferably set to 0.02% by mass or more, more preferably 0.02% by mass and 0.25% by mass.
  • Rare earth sintered magnets were manufactured according to the above manufacturing method by changing the addition time of the square Mn powder.
  • the addition amount of the square Mn powder is 0.10% by mass.
  • the time for adding the square Mn powder was after hydrogen grinding (sample 410), after coarse grinding with a brown mill (sample 411), and after fine grinding with a jet mill (sample 412).
  • a sample (Sample 413) was also prepared in which Mn was added to the alloy composition in an amount corresponding to the amount of added syrup of Mn powder.
  • the bending strength and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of these samples were also measured. Table 15 shows the results.
  • Sample 414 and sample 422 were prepared by adding plate-shaped Mn powder as the added metal powder in the amount shown in Table 16.
  • the thickness of the used plate-like Mn powder is as follows. The amount of plate-like Mn powder added to each sample, the flexural strength of the compact, and the magnetic properties (coercive force Hcj and residual magnetic flux density) Table 16 shows the degree (Br).
  • the addition of the plate-shaped Mn powder has the effect of improving the transverse rupture strength of the compact. The effect is higher than when the granular Mn powder is added. You can see.
  • sample 423 Sample 427 with different thicknesses of the plate-like Mn powder were prepared. Table 17 shows the thickness of plate-like Mn powder, flexural strength of the compact, and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of each sample.
  • the metal powder shown in Table 18 was used as the added metal powder.
  • Sample 5-1 and Sample 5-8 were prepared.
  • Table 18 shows the type, amount of metal powder, bending strength (compact strength), and magnetic properties (coercive force Hcj and residual magnetic flux density Br) of the compact in each sample.

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Abstract

L'objectif de cette invention est d'améliorer la résistance d'un article formé sans détérioration de ses caractéristiques magnétiques. L'invention concerne donc plus spécifiquement un procédé permettant de produire un aimant de terre rare frittée, dans lequel une fine poudre d'alliage brut contenant un élément de terre rare, un élément de transition et du bore sont frittés. La fine poudre d'alliage brut est ajoutée à une poudre métallique d'addition puis formée et frittée, la ou les poudres métalliques d'addition étant choisies dans le groupe comprenant, par exemple, une poudre Al, une poudre Ni, une poudre Zr, une poudre Mn, une poudre Fe, une poudre Co, une poudre Cu, une poudre Zn, une poudre Ag, une poudre Sn et une poudre Bi. Lorsque ce procédé comprend une étape de pulvérisation grossière consistant à pulvériser grossièrement un alliage de matériau brut et une étape de pulvérisation fine consistant en une pulvérisation fine, la poudre métallique d'addition est ajoutée après l'étape de pulvérisation fine ou après l'étape de pulvérisation grossière, dans une quantité égale ou supérieure à 0,01 % en masse. La poudre métallique d'addition possède de préférence la forme d'une plaque possédant une épaisseur égale ou inférieure à 10 νm.
PCT/JP2004/016010 2003-10-31 2004-10-28 Procede de production d'un aimant de terre rare frittee WO2005043558A1 (fr)

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Cited By (6)

* Cited by examiner, † Cited by third party
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JP2007027428A (ja) * 2005-07-15 2007-02-01 Neomax Co Ltd 希土類焼結磁石及びその製造方法
WO2010113371A1 (fr) * 2009-03-31 2010-10-07 昭和電工株式会社 Alliage pour aimant permanent à terres rares de type r-t-b, procédé de fabrication d'aimant permanent à terres rares de type r-t-b, et moteur
WO2012029527A1 (fr) * 2010-09-03 2012-03-08 昭和電工株式会社 Alliage pour aimant permanent en terres rares à base de r-t-b, procédé de fabrication dudit aimant, et moteur
WO2012043139A1 (fr) * 2010-09-30 2012-04-05 昭和電工株式会社 Matériau d'alliage pour aimant permanent aux terres rares du système r-t-b, procédé de production d'un aimant permanent aux terres rares du système r-t-b et moteur électrique
JP2020120112A (ja) * 2019-01-28 2020-08-06 包頭天和磁気材料科技股▲ふん▼有限公司 サマリウムコバルト磁石およびその製造方法
CN112951534A (zh) * 2021-02-02 2021-06-11 包头市金蒙汇磁材料有限责任公司 一种烧结钕铁硼磁体及其制备方法

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JP5274781B2 (ja) * 2007-03-22 2013-08-28 昭和電工株式会社 Ｒ−ｔ−ｂ系合金及びｒ−ｔ−ｂ系合金の製造方法、ｒ−ｔ−ｂ系希土類永久磁石用微粉、ｒ−ｔ−ｂ系希土類永久磁石
CN104308146B (zh) * 2014-10-24 2017-05-03 合肥斯科尔智能科技有限公司 一种应用于金属粉打印工艺的原料回收系统

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007027428A (ja) * 2005-07-15 2007-02-01 Neomax Co Ltd 希土類焼結磁石及びその製造方法
JP4645336B2 (ja) * 2005-07-15 2011-03-09 日立金属株式会社 希土類焼結磁石及びその製造方法
WO2010113371A1 (fr) * 2009-03-31 2010-10-07 昭和電工株式会社 Alliage pour aimant permanent à terres rares de type r-t-b, procédé de fabrication d'aimant permanent à terres rares de type r-t-b, et moteur
JP2011021269A (ja) * 2009-03-31 2011-02-03 Showa Denko Kk Ｒ−ｔ−ｂ系希土類永久磁石用合金材料、ｒ−ｔ−ｂ系希土類永久磁石の製造方法およびモーター
WO2012029527A1 (fr) * 2010-09-03 2012-03-08 昭和電工株式会社 Alliage pour aimant permanent en terres rares à base de r-t-b, procédé de fabrication dudit aimant, et moteur
JP2012057182A (ja) * 2010-09-03 2012-03-22 Showa Denko Kk Ｒ−ｔ−ｂ系希土類永久磁石用合金材料、ｒ−ｔ−ｂ系希土類永久磁石の製造方法およびモーター
WO2012043139A1 (fr) * 2010-09-30 2012-04-05 昭和電工株式会社 Matériau d'alliage pour aimant permanent aux terres rares du système r-t-b, procédé de production d'un aimant permanent aux terres rares du système r-t-b et moteur électrique
JP2012079796A (ja) * 2010-09-30 2012-04-19 Showa Denko Kk Ｒ−ｔ−ｂ系希土類永久磁石用合金材料、ｒ−ｔ−ｂ系希土類永久磁石の製造方法およびモーター
CN103153504A (zh) * 2010-09-30 2013-06-12 昭和电工株式会社 R-t-b系稀土类永久磁铁用合金材料、r-t-b系稀土类永久磁铁的制造方法和电动机
CN103153504B (zh) * 2010-09-30 2015-04-29 昭和电工株式会社 R-t-b系稀土类永久磁铁用合金材料、r-t-b系稀土类永久磁铁的制造方法和电动机
US9601979B2 (en) 2010-09-30 2017-03-21 Showa Denko K.K. Alloy material for R-T-B system rare earth permanent magnet, method for producing R-T-B system rare earth permanent magnet, and motor
JP2020120112A (ja) * 2019-01-28 2020-08-06 包頭天和磁気材料科技股▲ふん▼有限公司 サマリウムコバルト磁石およびその製造方法
CN112951534A (zh) * 2021-02-02 2021-06-11 包头市金蒙汇磁材料有限责任公司 一种烧结钕铁硼磁体及其制备方法
CN112951534B (zh) * 2021-02-02 2023-03-24 包头市金蒙汇磁材料有限责任公司 一种烧结钕铁硼磁体及其制备方法

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