WO2022124344A1 - 永久磁石及びその製造方法、並びにデバイス - Google Patents

永久磁石及びその製造方法、並びにデバイス Download PDF

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WO2022124344A1
WO2022124344A1 PCT/JP2021/045177 JP2021045177W WO2022124344A1 WO 2022124344 A1 WO2022124344 A1 WO 2022124344A1 JP 2021045177 W JP2021045177 W JP 2021045177W WO 2022124344 A1 WO2022124344 A1 WO 2022124344A1
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permanent magnet
atomic
magnet according
crystal grain
thmn
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French (fr)
Japanese (ja)
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裕和 幕田
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Tokin Corp
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Tokin Corp
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Priority to CN202180082188.7A priority Critical patent/CN116568836A/zh
Priority to JP2022568315A priority patent/JP7731908B2/ja
Priority to US18/256,189 priority patent/US20240021349A1/en
Publication of WO2022124344A1 publication Critical patent/WO2022124344A1/ja
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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
    • H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • 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
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
    • H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
    • 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
    • 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
    • H01F41/0266—Moulding; Pressing
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • B22F2301/355—Rare Earth - Fe intermetallic alloys
    • 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
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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 permanent magnet, a method for manufacturing the same, and a device.
  • Permanent magnets with high residual magnetization and high heat resistance are required.
  • Candidates for such magnet materials include SmFe 12 -based compounds having a ThMn 12 -type tetragonal structure with high saturation magnetization and high Curie temperature.
  • Patent Document 1 describes an alloy containing a hard magnetic phase having a ThMn 12 -type rectangular structure and a non-magnetic phase as a permanent magnet having excellent saturation magnetization and coercive force and improved temperature characteristics of the coercive force. Permanent magnets are disclosed.
  • Patent Document 2 discloses a magnet material having a main phase composed of a ThMn 12 -type crystal phase and having a specific composition as a magnet material for enhancing saturation magnetization.
  • the present invention solves the above-mentioned problems, and an object of the present invention is to provide a permanent magnet having a ThMn 12 -type rectangular structure and a high coercive force, a method for manufacturing the same, and a device using the permanent magnet. And.
  • the permanent magnet according to the present invention is It has a composition represented by the following formula (1).
  • Equation (1) (R 1-x Zr x ) a (T 1- y My ) b B c
  • R is at least one selected from rare earth elements
  • T is at least one selected from the group consisting of Fe, Co
  • Ni M represents at least one selected from the group consisting of Al, Si, Ti, V, Cr, Mn, Cu, Hf, Nb, Mo, Ta, and W.
  • a, b and c each indicate an atomic%
  • One embodiment of the permanent magnet has a crystal grain composed of a main phase having a ThMn 12 type crystal structure and a crystal grain boundary, and the crystal grain boundary includes an amorphous phase.
  • 50 atomic% or more of the R is Sm.
  • T 50 atomic% or more of T is Fe.
  • One embodiment of the permanent magnet is a number in which a satisfies 5 ⁇ a ⁇ 8.
  • One embodiment of the above permanent magnet has a coercive force (Hcj) of 1.8 kOe or more.
  • the Curie temperature exceeds 400 ° C.
  • the ratio (atomic%) of the B element at the crystal grain boundaries is 10 times or more the ratio of the B element at the crystal grains.
  • the peak intensity corresponding to the 321 surface of the ThMn 12 type crystal structure ( IThMn12 ) and the peak intensity corresponding to the 110 surface of ⁇ -iron in the X-ray diffraction spectrum (I ThMn12) is 1.0 or less.
  • the method for manufacturing a permanent magnet according to the present invention is as follows.
  • the step (II) of quenching the molten metal at 10 2 to 107 K / sec to form an alloy and
  • the step (III) of crushing the alloy into powder and
  • the device according to the present invention is characterized by having the above-mentioned permanent magnet.
  • the present invention provides a permanent magnet having a ThMn 12 -type rectangular structure and a high coercive force, a method for producing the same, and a device using the permanent magnet.
  • the permanent magnet of the present embodiment (hereinafter, also referred to as the permanent magnet) is characterized by having a composition represented by the following formula (1). Equation (1): (R 1-x Zr x ) a (T 1- y My ) b B c
  • R is at least one selected from rare earth elements
  • T is at least one selected from the group consisting of Fe, Co
  • Ni M represents at least one selected from the group consisting of Al, Si, Ti, V, Cr, Mn, Cu, Hf, Nb, Mo, Ta, and W.
  • a, b and c each indicate an atomic%
  • R in the formula (1) represents a rare earth element.
  • the rare earth element is a general term for elements including lanthanoids from La (lanthanum) to Lu (lutetium) and Sc (scandium) and Y (yttrium).
  • R contains one or more elements selected from the above rare earth elements.
  • a permanent magnet having high magnetic anisotropy and high coercive force can be obtained.
  • R preferably contains one or more selected from Sm, Pr, Nd, Ce, and La, and more preferably contains Sm.
  • 50 atomic% or more of R is preferably Sm, 80 atomic% or more is preferably Sm, and R is substantially Sm. More preferred.
  • This permanent magnet contains Zr in the range where the ratio (atomic%) of R and Zr is (1-x): x.
  • Zr in the range where the ratio (atomic%) of R and Zr is (1-x): x.
  • x may be 0.01 to 0.5, and more preferably 0.2 or less from the viewpoint of magnetic anisotropy and coercive force.
  • the total content ratio (a) of R and Zr with respect to the entire permanent magnet is 5 to 12 from the point that the ThMn 12 type crystal structure is the main phase. From the viewpoint of increasing the magnetization, a is preferably 10 or less, and more preferably 8 or less.
  • T in the formula (1) represents at least one selected from the group consisting of Fe, Co, and Ni.
  • Each element of T contributes to the magnetization of the permanent magnet.
  • T contains Fe.
  • T contains Co from the viewpoint of raising the Curie temperature and improving the heat resistance.
  • 50 atomic% or more of T is preferably Fe, and 60 atomic% or more is preferably Fe.
  • the ratio (atomic%) of Fe and Co is preferably 60:40 to 95: 5, and more preferably 70:30 to 80:20.
  • M in the formula (1) represents at least one selected from the group consisting of Al, Si, Ti, V, Cr, Mn, Cu, Hf, Nb, Mo, Ta, and W.
  • This permanent magnet contains M in the range where the ratio (atomic%) of T and M is (1-y): y.
  • y may be 0.01 or more, preferably 0.02 or more.
  • y may be 0.5 or less, preferably 0.1 or less.
  • the total content ratio (b) of T and M with respect to the entire permanent magnet can be expressed as 100- (a + c), and is 70 to 94 from the point that the ThMn 12 type crystal structure is the main phase. From the viewpoint of increasing the magnetization, b is preferably 75 or more, and more preferably 77 or more.
  • this permanent magnet contains B (boron) in an amount of 0.1 to 20 atomic%.
  • B boron
  • the B content ratio (c) is preferably 0.5 or more.
  • the amorphous phase is formed at the crystal grain boundaries by setting the content ratio (c) of B to 1 or more and preferably using the production method described later. The amorphous phase becomes a domain wall pinning site and increases the coercive force of the permanent magnet.
  • the content ratio (c) of B is preferably 1.2 or more, more preferably 1.5 or more.
  • the content ratio (c) of B is preferably 15 or less, more preferably 10 or less, from the viewpoint of suppressing the decrease in saturation magnetization.
  • the permanent magnet may contain unavoidable impurities as long as the effect of the present invention is exhibited.
  • the unavoidable impurities are elements that are inevitably mixed from the raw materials and the manufacturing process and are not included in the formula (1) (elements other than R, T, M, Zr, and B). Specific examples thereof include, but are not limited to, O, C, N, P, S, Sn and the like.
  • the ratio of unavoidable impurities in the permanent magnet is preferably 5 atomic% or less, more preferably 1 atomic% or less, still more preferably 0.1 atomic% or less, based on the total amount of the permanent magnet.
  • the content ratio of each element in this permanent magnet can be measured, for example, by using energy dispersive X-ray spectroscopy (EDX).
  • EDX energy dispersive X-ray spectroscopy
  • the permanent magnet becomes a permanent magnet having a crystal grain having a main phase having a ThMn 12 type crystal structure and a crystal grain boundary serving as a boundary between the crystal grains.
  • This permanent magnet is excellent in stability, saturation magnetization, coercive force, and heat resistance of ThMn 12 type crystal structure.
  • B boron
  • the ratio (atomic%) of the B element at the crystal grain boundary can be 10 times or more the ratio of the B element of the crystal grain. This further improves the coercive force.
  • the permanent magnet has a coercive force (Hcj) of 1.8 kOe or more, preferably 2.0 or more.
  • Hcj coercive force
  • the permanent magnet can be obtained in which the Curie temperature exceeds 400 ° C.
  • the texture of the crystal grain boundaries can be observed using a scanning transmission electron microscope (STEM).
  • STEM scanning transmission electron microscope
  • the Curie temperature can be measured using a vibrating sample magnetometer (VSM).
  • the coercive force can be obtained from the JH curve obtained by using the DC magnetization characteristic analyzer.
  • the method for manufacturing a permanent magnet according to the present embodiment (hereinafter, also referred to as the present manufacturing method) is The step (I) of preparing a molten metal having the composition represented by the above formula (1) and The step (II) of quenching the molten metal at 10 2 to 107 K / sec to form an alloy, and The step (III) of crushing the alloy into powder and The step (IV) of molding the powder into a molded body and The step (V) of sintering the molded product to obtain a sintered body, and It has a step (VI) of heat-treating the sintered body and then quenching the sintered body.
  • the permanent magnet having a crystal grain consisting of a main phase having a ThMn 12 type crystal structure and a crystal grain boundary serving as a boundary between the crystal grains and having an amorphous phase at the crystal grain boundary is preferably used.
  • a molten metal having a composition represented by the above formula (1) is prepared (step (I)).
  • the method for preparing the molten metal may be prepared by obtaining a commercially available alloy having a desired composition, or may prepare an alloy by blending each element so as to have a desired composition. If there is a possibility that the element evaporates in the subsequent step, the composition after manufacturing the permanent magnet is adjusted so as to satisfy the above formula (1).
  • the prepared alloy is melted to make a molten metal.
  • the melting method may be appropriately selected from known melting means such as arc melting and high frequency melting.
  • the molten metal is rapidly cooled at 102 to 107 K / sec (step ( II )).
  • step ( II ) By quenching the molten metal at a cooling rate of 102 K / sec or more , an alloy in which the precipitation of ⁇ -Fe ( ⁇ -iron) is suppressed can be obtained.
  • ⁇ -Fe precipitation of ⁇ -Fe
  • an amorphous phase can be suitably formed at the grain boundary portion, and a permanent magnet having a high coercive force can be obtained.
  • the alloy after quenching may be further heat-treated for microstructure homogenization.
  • the quenching speed is preferably 10 3 to 106 K / sec.
  • the alloy is preferably flaky from the viewpoint of suppressing the precipitation of ⁇ -iron due to quenching.
  • the thickness of the flakes is preferably 1 to 100 ⁇ m, more preferably 20 to 90 ⁇ m, because it is easy to quench. Since the alloy contains boron, the viscosity is lowered, so that the thick flakes can be easily obtained when the molten metal is rapidly cooled by the meltspun method or the like.
  • the amount of ⁇ -iron can be evaluated, for example, by an X-ray diffraction spectrum. Specifically, the X-ray diffraction spectrum of a permanent magnet is measured using Cu K ⁇ characteristic X-rays, and the peak intensity (I ThMn12 ) of the peak corresponding to the 321 plane of the main phase ThMn 12 type crystal structure is obtained. , The degree of ⁇ -iron precipitation can be estimated from the intensity ratio (I ⁇ -Fe / I ThMn12 ) of the peak intensity (I ⁇ -Fe ) corresponding to the 110 planes of ⁇ -iron. As the peak intensity, the peak height minus the background is used, and the intensity ratio is preferably 1.0 or less, more preferably 0.8 or less. The lower the strength ratio is, the more preferable it is, and the lower limit is not particularly limited, but it is usually 0.001 or more.
  • the alloy pulverization method may be appropriately selected from conventionally known methods.
  • the alloy is coarsely pulverized by a known pulverizer such as a disc mill in an inert atmosphere. If the pulverizability is poor, the alloy may be subjected to hydrogen storage treatment in advance. The hydrogen storage treatment makes the alloy brittle and facilitates coarse crushing. Then, the coarsely pulverized product is further pulverized.
  • the fine pulverization may be dry pulverization or wet pulverization. Examples of the dry pulverization include a jet mill method. Further, examples of the wet pulverization include a wet ball mill method.
  • a lubricant for imparting lubricity to the powder may be added during grinding. Further, the mixture of the organic solvent and the fine powder after pulverization is dried in the inert gas.
  • the average particle size of the powder after pulverization makes it possible to shorten the sintering time in the sintering step described later, and the average particle size is preferably 1 to 10 ⁇ m from the viewpoint of producing a uniform permanent magnet. ..
  • the obtained powder is pressure-molded to obtain a molded product having a desired shape (step (IV)).
  • the relationship between the direction of the magnetic field and the pressing direction is not particularly limited, and may be appropriately selected according to the shape of the product and the like.
  • a parallel magnetic field press in which a magnetic field is applied in a direction parallel to the pressing direction can be used.
  • a right-angled magnetic field press in which a magnetic field is applied at right angles to the pressing direction.
  • the magnitude of the magnetic field is not particularly limited, and may be, for example, a magnetic field of 15 kOe or less, or a magnetic field of 15 kOe or more, depending on the intended use of the product. Above all, from the viewpoint of excellent magnetic characteristics, pressure molding in a magnetic field of 15 kOe or more is preferable. Further, the pressure at the time of pressure molding may be appropriately adjusted according to the size, shape and the like of the product. As an example, the pressure can be 0.5 to 2.0 ton / cm 2 .
  • the powder is pressure-molded in a magnetic field of 15 kOe or more at a pressure of 0.5 to 2.0 ton / cm 2 or less perpendicular to the magnetic field. Is particularly preferable.
  • the sintering temperature is preferably 950 to 1250 ° C, more preferably 950 to 1220 ° C.
  • the sintering time is preferably 20 to 240 minutes, more preferably 60 to 120 minutes.
  • the sintering step is preferably performed in a vacuum of 1000 Pa or less or in an inert gas atmosphere, and further, from the viewpoint of increasing the density of the sintered body, 1000 Pa or less, preferably 100 Pa or less. It is preferable to sinter in the vacuum of.
  • the obtained sintered body is continuously heat-treated.
  • a ThMn 12 -type crystal structure is formed and an Fe—B liquid phase component is generated at the grain boundary portion.
  • the heat treatment temperature is preferably 500 to 1180 ° C, more preferably 500 to 900 ° C.
  • heat-treating at 500 ° C. or higher it is easy to homogenize the structure, promote the formation of ThMn 12 type structure, and obtain the above liquid phase component.
  • by heat-treating at 1180 ° C. or lower it is possible to suppress an excessive increase in the amount of the liquid phase component and suppress deterioration of magnetic properties.
  • the heat treatment time can be, for example, 1 to 100 hours, preferably 5 to 50 hours.
  • process (VI) Amorphous phase is formed at the grain boundaries by quenching.
  • the quenching rate in the step (VI) may be 60 to 250 ° C./min, preferably 100 to 250 ° C./min.
  • the obtained sintered body may be further subjected to aging treatment, if necessary.
  • the permanent magnet having a crystal grain composed of a main phase having a ThMn 12 type crystal structure and a crystal grain boundary serving as a boundary between the crystal grains and having an amorphous phase at the crystal grain boundary is manufactured. be able to.
  • the present invention can further provide a device having the present permanent magnet.
  • a device having the present permanent magnet include watches, electric motors, various instruments, communication devices, computer terminals, speakers, video discs, sensors, and the like.
  • the permanent magnet of the present invention does not easily deteriorate its magnetic force even in a high environmental temperature, it can be used in an angle sensor, an ignition coil, a drive motor such as an HEV (Hybrid electric vehicle), etc. used in an automobile engine room. It can be suitably used.
  • Example 1 Each metal was weighed in a predetermined amount so as to have the composition shown in Table 1, and a mother alloy was obtained by high-frequency melting. The mother alloy was melted again at high frequency and rapidly cooled at 102 to 107 K / sec by the meltspun method to obtain alloy flakes having the thickness shown in Table 1. Next, it was roughly pulverized with a vibration mill and finely pulverized with a wet ball mill to obtain a raw material powder. This was formed into a green compact by pressing in a magnetic field. The green compact was sintered and continuously heat-treated. The sintering temperature was 1000 ° C. and the heat treatment temperature was 900 ° C. After the heat treatment, the permanent magnet of Example 1 was obtained by quenching.
  • Example 2 to 3 Permanent magnets of Examples 2 to 3 were obtained in the same manner as in Example 1 except that the composition and the heat treatment temperature were changed as shown in Table 1.
  • Example 5 Each metal was weighed in a predetermined amount so as to have the composition shown in Table 2, and the raw material alloy was prepared by high-frequency melting and quenching at 10 2 to 107 K / sec using a quenching thin band preparation device. This alloy was heat-treated at 800 to 1180 ° C. to homogenize the composition. After that, the alloy was heated in a hydrogen stream at a temperature of 200 to 600 ° C. to store hydrogen. The alloy was coarsely pulverized by a disc mill and finely pulverized by a ball mill in a 2-propanol solvent. Lubricant was added during fine grinding. This imparts lubricity to the powder and facilitates magnetic field orientation in the later molding process.
  • a slurry consisting of a solvent, a lubricant and fine powder was pressure-dried with nitrogen gas, and the obtained raw material powder was molded in a magnetic field.
  • the molded product was heated in a hydrogen stream and subjected to decarbonization heat treatment. After that, the temperature is raised by switching to vacuum, sintered at 1200 ° C. in an Ar atmosphere of 30 kPa, continuously heat-treated at 800 to 1180 ° C., and finally the sintered body is rapidly cooled to carry out Examples 4 to 5. Obtained a permanent magnet.
  • Comparative Example 4 Permanent magnets of Comparative Example 1 were obtained in the same manner as in Examples 4 to 5 except that the compositions of Examples 4 to 5 were changed as shown in Table 2.

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS64703A (en) * 1986-04-15 1989-01-05 Tdk Corp Permanent magnet and manufacture thereof
JPH01103805A (ja) * 1987-07-30 1989-04-20 Tdk Corp 永久磁石
JPH0851007A (ja) * 1995-07-17 1996-02-20 Tdk Corp 永久磁石およびその製造方法
JP2001189206A (ja) * 1999-12-28 2001-07-10 Toshiba Corp 永久磁石
JP2003213384A (ja) * 2001-11-09 2003-07-30 Hitachi Metals Ltd 永久磁石合金及びボンド磁石
JP2013254756A (ja) * 2010-08-30 2013-12-19 Hitachi Ltd 焼結磁石
JP2019039025A (ja) * 2017-08-22 2019-03-14 トヨタ自動車株式会社 磁性化合物及びその製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS64703A (en) * 1986-04-15 1989-01-05 Tdk Corp Permanent magnet and manufacture thereof
JPH01103805A (ja) * 1987-07-30 1989-04-20 Tdk Corp 永久磁石
JPH0851007A (ja) * 1995-07-17 1996-02-20 Tdk Corp 永久磁石およびその製造方法
JP2001189206A (ja) * 1999-12-28 2001-07-10 Toshiba Corp 永久磁石
JP2003213384A (ja) * 2001-11-09 2003-07-30 Hitachi Metals Ltd 永久磁石合金及びボンド磁石
JP2013254756A (ja) * 2010-08-30 2013-12-19 Hitachi Ltd 焼結磁石
JP2019039025A (ja) * 2017-08-22 2019-03-14 トヨタ自動車株式会社 磁性化合物及びその製造方法

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