EP0597582A1 - Matériau en poudre pour aimant à base de terre-rare - Google Patents
Matériau en poudre pour aimant à base de terre-rare Download PDFInfo
- Publication number
- EP0597582A1 EP0597582A1 EP93307756A EP93307756A EP0597582A1 EP 0597582 A1 EP0597582 A1 EP 0597582A1 EP 93307756 A EP93307756 A EP 93307756A EP 93307756 A EP93307756 A EP 93307756A EP 0597582 A1 EP0597582 A1 EP 0597582A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- powder
- grain size
- hereinafter referred
- magnet
- rare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
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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
- H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
Definitions
- the present invention relates to a rare-earth magnet powder material excellent in an isotropy, which comprises any of the rare-earth elements including Y (hereinafter referred to as "R”), Fe or a component in which part of the Fe is substituted by Co (hereinafter referred to as "T”) and B as the main components, and further containing one or more of Si, Ga, Zr, Nb, Mo, Hf, Ta, W, Al, Ti and V (hereinafter referred to as "M”) in an amount of from 0.001 to 5.0 atomic %, of which the main phase is an R2T14B-type intermetallic compound phase.
- R rare-earth elements
- T Co
- M Ti and V
- the present inventors therefore carried out studies with a view to manufacturing an R-Fe-B-M magnet powder with better magnetic anisotropy than that of conventional ones, and manufacturing magnets better in magnetic anisotropy than conventional ones with the use of this R-Fe-B-M magnet powder, and the following discoveries were made.
- the grain size of anisotropic R-Fe-B-M magnet powders having the recrystallized fine aggregate structure of the R2T14B-type intermetallic compound phase of an average recrystallization grain size of from 0.05 to 20 ⁇ m obtained through conventional H2 occlusion and dehydrogenation exerts an important effect on the magnetic properties of bonded magnets and full-density magnets made from them.
- the present invention was developed on the basis of these discoveries and provides a rare-earth magnet powder material excellent in anisotropy, having an average grain size within a range of from 5 to 200 ⁇ m, in the form of an R-T-B-M anisotropic magnet material powder, comprising R, T and B as the main components, further containing M in an amount of from 0.001 to 5.0 atomic % and having an average recrystallization grain size of from 0.05 to 20 ⁇ m.
- the powder should have an average grain size of from 5 to 200 ⁇ m because an average grain size of under 5 ⁇ m is not desirable as it leads to a lower iHc of bond magnets and full-density magnets made and an average grain size of over 200 ⁇ m results on the other hand in a lower magnetic anisotropy in such magnets.
- part of Fe may be substituted by Cr, Mn, Ni, Cu or Zn, and part of B may be substituted by C, N or O.
- an alloy having a chemical composition comprising 11.6% Nd, 0.5% Pr, 11.8% Co, 6.5% B, 0.1% Zr and the balance Fe (atomic %) was melted in an Ar gas atmosphere, and cast into an ingot.
- This ingot was homogenized in an Ar atmosphere by holding it at a temperature of 1,130°C for 30 hours, and then crushed to blocks each having a side of up to 20 mm.
- the block was caused to occlude hydrogen by heating it from room temperature to 750° C in an hydrogen atmosphere under 1 atm.
- Hydrogen occlusion was caused by holding the block at 750°C for one hour while maintaining the hydrogen atmosphere of 1 atm. to accelerate phase transformation.
- the block was further heated to 850°C. held at 850°C for one hour, and was forcedly caused to release hydrogen until a 1 x 10 ⁇ 1 vacuum atmosphere was achieved to accelerate phase transformation.
- the block was then cooled in Ar gas.
- samples of an anisotropic magnet powder material of the present invention Nos. 1 to 7 and comparative samples of anisotropic magnet material powder (hereinafter referred to as "comparative samples") Nos. 1 and 2 were prepared.
- each of these samples of the invention Nos. 1 to 7 and comparative samples Nos. 1 and 2 was compression-formed in a magnetic field into pressurized powder.
- This pressurized powder was set on a hot press to conduct hot pressing in vacuum at 790°C for ten minutes under a pressure of 1 ton/cm2 so that the direction of application of the magnetic field agreed with the direction of compression, and rapidly cooled in Ar gas to prepare an anisotropic full-density magnet.
- the magnetic properties of the resulting anisotropic full-density magnets are shown in Table 1.
- Table 1 reveal that the bonded magnets manufactured from the samples of the invention Nos. 1 to 7 having an average grain size within a range of from 5 to 200 ⁇ m show better magnetic properties than those of the bonded magnets manufactured from the comparative samples Nos. 1 and 2 having an average grain size outside the range of from 5 to 200 ⁇ m.
- an alloy having a chemical composition comprising 12.2% Nd, 17.2% Co, 7.0% B, 0.1% Zr, 0.5% Ga and the balance Fe (atomic %) was melted in an Ar gas atmosphere, and cast into an ingot.
- This ingot was homogenized in an Ar atmosphere by holding it at a temperature of 1,120°C for 40 hours, and then crushed to blocks each having a side of up to 10 mm.
- the block was caused to occlude hydrogen by heating it from the room temperature to 760°C in a hydrogen atmosphere under 1 atm.
- Hydrogen occlusion was caused by holding the block at 760°C for one hour while maintaining the hydrogen atmosphere of 1 atm. to accelereate phase transformation
- the block was further heated to 820°C, held at 820°C for one hour, and was forcedly caused to release hydrogen until a 1 x 10 ⁇ 1 vacuum atmosphere is achieved to accelerate phase transformation.
- the block was then cooled in Ar gas.
- the ingot after hydrogen occlusion and release had a recrystallized fine aggregate structure of the R2T14B-type intermetallic compound phase having an average recrystallization grain size of 0.3 ⁇ m.
- samples of the magnet powder of the present invent ion Nos. 8 and 9 were prepared.
- a sample of comparative magnet powder No. 3 was prepared.
- the prepared samples of the invention Nos. 8 and 9 had a coercive force, iHc, of 14,2 kOe, and the comparative sample No. 3 had a coercive force, iHc , of 14.6 kOe.
- Each of the samples of the invention Nos. 8 and 9 and the comparative sample No. 3 was mixed with 2.7 wt.% epoxy resin and compression-formed while making adjustment so as to give a density of 6.0 g/cm3 in an oriented magnetic field in to a pressurized powder .
- This pressurized powder was thermoset at 130°C for one hour to prepare an anisotropic bonded magnet.
- the magnetic properties of the prepared anisotropic bonded magnets are represented in a graph as shown in Fig.
- H F is the oriented magnetic field during forming in the magnetic field; and iHc is the coercive force of the powder
- B r /B r70 where B r is the remanent magnetization; and B r70 is the remanent magnetization in a magnetized field of 70 kOe
- each of these samples of the invention Nos. 8 and 9 and the comparative sample No. 3 was compression-formed in an oriented magnetic field into pressurized powder.
- the pressurized powder was set on a hot press and hot-pressed under vacuum at 800°C for ten minutes under a pressure of 1 ton/cm2 so that the direction of application of the magnetic field agreed with the direction of compression.
- the hot-pressed powder was then rapidly cooled in Ar gas to prepare an anisotropic full-density magnet.
- the magnetic properties of the prepared anisotropic full-density magnet are represented in a graph as shown in Fig. 2, with H F /iHc on the abscissa and B r /B r70 on the ordinate
- Figs. 1 and 2 suggest that use of the samples of the invention Nos. 8 and 9 having an average grain size of 50 ⁇ m and 150 ⁇ m, respectively, improves the degree of orientation in a low-orientation magnetic field having an iHc of up to 1.5 times and permits preparation of an anisotropic bond magnet and an anisotropic full-density magnet having sufficiently high properties, whereas use of the comparative sample No. 3 having an average grain size of 300 ⁇ m does not improve the degree of orientation in an oriented magnetic field having an iHc of up to 1.5 times, and does not give an anisotropic bonded magnet or an anisotropic full-density magnet having sufficiently high properties.
- the rare-earth magnet material powder excellent in anisotropy of the present invention having an average grain size within a range of from 5 to 200 ⁇ m, the degree of orientation in a low-orientation magnetic field of a coercive force, iHc , of up to 1.5 times is improved, and it is possible to manufacture an anisotropic rare-earth magnet having better magnetic properties than those of conventional ones in a low magnetic field output, thus providing industrially useful effects.
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP328805/92 | 1992-11-13 | ||
JP4328805A JPH06151137A (ja) | 1992-11-13 | 1992-11-13 | 異方性に優れた希土類磁石材料粉末 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0597582A1 true EP0597582A1 (fr) | 1994-05-18 |
EP0597582B1 EP0597582B1 (fr) | 1997-12-17 |
Family
ID=18214300
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP19930307756 Expired - Lifetime EP0597582B1 (fr) | 1992-11-13 | 1993-09-30 | Matériau en poudre pour aimant à base de terre-rare |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0597582B1 (fr) |
JP (1) | JPH06151137A (fr) |
DE (2) | DE69315807D1 (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5589009A (en) * | 1994-04-29 | 1996-12-31 | Crucible Materials Corporation | RE-Fe-B magnets and manufacturing method for the same |
CN113593799A (zh) * | 2020-04-30 | 2021-11-02 | 烟台正海磁性材料股份有限公司 | 一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6004407A (en) * | 1995-09-22 | 1999-12-21 | Alps Electric Co., Ltd. | Hard magnetic materials and method of producing the same |
DE10255604B4 (de) | 2002-11-28 | 2006-06-14 | Vacuumschmelze Gmbh & Co. Kg | Verfahren zum Herstellen eines anisotropen Magnetpulvers und eines gebundenen anisotropen Magneten daraus |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0304054A2 (fr) * | 1987-08-19 | 1989-02-22 | Mitsubishi Materials Corporation | Poudre magnétique terre rare-fer-bore et son procédé de fabrication |
EP0411571A2 (fr) * | 1989-07-31 | 1991-02-06 | Mitsubishi Materials Corporation | Poudre à base de terre rare pour aimant, méthode de préparation et aimant à liant |
-
1992
- 1992-11-13 JP JP4328805A patent/JPH06151137A/ja not_active Withdrawn
-
1993
- 1993-09-30 EP EP19930307756 patent/EP0597582B1/fr not_active Expired - Lifetime
- 1993-09-30 DE DE1993615807 patent/DE69315807D1/de not_active Expired - Fee Related
- 1993-09-30 DE DE1993615807 patent/DE69315807T4/de not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0304054A2 (fr) * | 1987-08-19 | 1989-02-22 | Mitsubishi Materials Corporation | Poudre magnétique terre rare-fer-bore et son procédé de fabrication |
EP0411571A2 (fr) * | 1989-07-31 | 1991-02-06 | Mitsubishi Materials Corporation | Poudre à base de terre rare pour aimant, méthode de préparation et aimant à liant |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5589009A (en) * | 1994-04-29 | 1996-12-31 | Crucible Materials Corporation | RE-Fe-B magnets and manufacturing method for the same |
CN113593799A (zh) * | 2020-04-30 | 2021-11-02 | 烟台正海磁性材料股份有限公司 | 一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
EP0597582B1 (fr) | 1997-12-17 |
DE69315807T4 (de) | 1999-04-22 |
DE69315807D1 (de) | 1998-01-29 |
DE69315807T2 (de) | 1998-07-16 |
JPH06151137A (ja) | 1994-05-31 |
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