WO2008023731A1 - Permanent magnet and process for producing the same - Google Patents
Permanent magnet and process for producing the same Download PDFInfo
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- WO2008023731A1 WO2008023731A1 PCT/JP2007/066272 JP2007066272W WO2008023731A1 WO 2008023731 A1 WO2008023731 A1 WO 2008023731A1 JP 2007066272 W JP2007066272 W JP 2007066272W WO 2008023731 A1 WO2008023731 A1 WO 2008023731A1
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- sintered magnet
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- permanent magnet
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- sintered
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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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
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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
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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
- H01F1/06—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 in the form of particles, e.g. powder
- H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Definitions
- the present invention relates to a permanent magnet and a method for producing the permanent magnet, and in particular, a permanent magnet having high magnetic properties obtained by diffusing Dy and Tb in the grain boundary phase of an Nd Fe B-based sintered magnet, and the permanent magnet.
- the present invention relates to a magnet manufacturing method.
- Nd Fe B-based sintered magnets are inexpensively manufactured by combining iron and Nd and B elements that are inexpensive, abundant in resources, and can be stably supplied. In addition, it has high magnetic properties (the maximum energy product is about 10 times that of ferrite magnets), so it is used in various products such as electronic equipment. In recent years, it has been used for motors and generators for hybrid cars. Adoption is also progressing.
- the Curie temperature of the sintered magnet is as low as about 300 ° C, the temperature may rise above a predetermined temperature depending on the usage condition of the product to be used. There is a problem of demagnetization.
- the sintered magnet when used in a desired product, the sintered magnet may be processed into a predetermined shape, and this processing may cause defects (cracks, etc.) or distortions in the crystal grains of the sintered magnet. This causes a problem that the magnetic properties are significantly deteriorated.
- Patent Document 1 Arranged in a processing chamber in a state mixed with a B-based sintered magnet, heating the processing chamber evaporates the rare earth metal, sorbs the evaporated rare earth metal atoms to the sintered magnet, and further, this metal atom. Is diffused in the grain boundary phase of the sintered magnet, thereby introducing a uniform and desired amount of rare earth metal to the sintered magnet surface and the grain boundary phase to improve or recover the magnetization and coercivity. (Patent Document 1).
- Dy and Tb are larger than Nd! /, And have 4f electron magnetic anisotropy. It is known to greatly improve anisotropy.
- Dy or Tb is added during the production of sintered magnets, D Since y and Tb have a ferrimagnetic structure with spin orientation opposite to Nd in the main phase crystal lattice, the magnetic field strength, and hence the maximum energy product showing the magnetic properties, is greatly reduced. For this reason, it is proposed that Dy and Tb are introduced by the above-described method, and in particular, Dy and Tb are uniformly introduced into the grain boundary phase.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2004-296973 (see, for example, the description of claims) Disclosure of the Invention
- Dy and Tb are also present on the surface of the sintered magnet (that is, a thin film of Dy and Tb is formed on the surface of the sintered magnet).
- the metal atom is supplied, the metal atoms deposited on the surface of the sintered magnet are recrystallized, causing a problem that the surface of the sintered magnet is remarkably deteriorated (surface roughness is deteriorated).
- the rare earth metal melted when the metal evaporation material is heated directly adheres to the sintered magnets, thereby forming thin films and protrusions. Inevitable.
- the average composition of the surface of the sintered magnet adjacent to the thin film becomes a rare earth-rich composition of Dy or Tb.
- the liquid phase temperature decreases and the sintered magnet surface melts (that is, the main phase melts and the amount of liquid phase increases).
- the vicinity of the surface of the sintered magnet melts and collapses, and unevenness increases.
- Dy penetrates excessively into the crystal grains with a large amount of liquid phase, and the maximum energy product and residual magnetic flux density, which show magnetic properties, are further reduced.
- a thin film or protrusion is formed on the surface of the sintered magnet and the surface is deteriorated (the surface roughness is not good).
- a finishing process post-process
- the first object of the present invention is to effectively diffuse and maintain Dy and Tb in the grain boundary phase without deteriorating the surface of the NdFeB-based sintered magnet. It is an object of the present invention to provide a method for producing a permanent magnet that can effectively improve or recover the magnetic force and does not require a post-process.
- a second object of the present invention is a permanent magnet in which Dy and Tb are efficiently diffused only in the grain boundary phase of an Nd Fe—B-based sintered magnet having a predetermined shape, and have high magnetic properties and strong corrosion resistance. Is to provide.
- the method of manufacturing a permanent magnet according to claim 1 is the same or other methods in which an iron-boron rare earth-based sintered magnet is disposed in a processing chamber and heated to a predetermined temperature.
- the metal evaporation material consisting of at least one of Dy and Tb placed in the processing chamber is evaporated, and the amount of the evaporated metal atoms supplied to the sintered magnet surface is adjusted to attach the metal atoms. It is characterized in that atoms are diffused into the grain boundary phase of the sintered magnet before a thin film made of a metal evaporation material is formed on the surface of the sintered magnet.
- the metallic nuclear power S composed of at least one of vaporized Dy and Tb is supplied and attached to the surface of the sintered magnet heated to a predetermined temperature.
- the sintered magnet was heated to a temperature at which an optimum diffusion rate could be obtained, and the supply amount of Dy and Tb to the surface of the sintered magnet was adjusted. It is sequentially diffused into the grain boundary phase of the sintered magnet.
- the supply of Dy and Tb to the surface of the sintered magnet and the diffusion of the sintered magnet to the grain boundary phase are carried out in a single process. Therefore, the permanent magnet surface is prevented from being deteriorated (surface roughness is deteriorated), and in particular, excessive diffusion of Dy and Tb in the grain boundary near the sintered magnet surface is suppressed.
- the surface state of the permanent magnet is substantially the same as the state before the above-described treatment is performed, and a separate post-process is unnecessary.
- Dy and Tb are diffused and uniformly distributed in the grain boundary phase of the sintered magnet, so that the grain boundary phase contains a rich phase of Dy and Tb (a phase containing 5 to 80% of Dy and Tb).
- Dy and Tb diffuse only near the surface of the crystal grains.
- a permanent magnet having high magnetic properties in which the magnetization and coercive force are effectively improved or recovered can be obtained.
- defects (cracks) occur in the crystal grains near the surface of the sintered magnet during the processing of the sintered magnet, a rich phase of Dy and Tb is formed inside the crack, resulting in magnetization and coercive force. Can be recovered.
- the processing chamber is placed under a reduced pressure of 800-; Heating to a temperature in the range of C is preferred. According to this, by setting the temperature in the processing chamber to the range of 800 to 1050 ° C, the supply amount of metal atoms to the sintered magnet surface where the vapor pressure of the metal evaporation material is low is suppressed.
- the sintered magnet is heated to a temperature at which the diffusion rate increases, so that the Dy atoms attached to the surface of the sintered magnet become crystal grains of the sintered magnet before forming a thin film composed of Dy on the surface of the sintered magnet. It is diffused in the field phase and spreads uniformly.
- the temperature of the processing chamber is lower than 800 ° C, the vapor pressure that can supply Dy atoms to the surface of the sintered magnet does not reach so that Dy diffuses and spreads uniformly in the grain boundary phase. In addition, the diffusion rate of Dy atoms adhering to the surface of the sintered magnet to the grain boundary layer becomes slow.
- the temperature exceeds 1050 ° C the vapor pressure of Dy increases and Dy atoms in the vapor atmosphere are excessively supplied to the surface of the sintered magnet.
- Dy may be excessively diffused in the crystal grains. If Dy is excessively diffused in the crystal grains, the maximum energy product and residual magnetic flux density are further reduced because the magnetization in the crystal grains is greatly reduced. Become.
- the processing chamber is in a range of 900 to 1150 ° C under reduced pressure. It is preferable to heat to the inside temperature.
- the Tb nuclear power S attached to the surface of the sintered magnet diffused into the grain boundary phase of the sintered magnet before the thin film made of Tb was formed on the surface of the sintered magnet, and evenly spread, There is a Tb-rich phase in the grain boundary phase, and Tb diffuses only near the surface of the crystal grain, and as a result, a permanent magnet with high magnetic properties in which magnetization and coercive force are effectively improved or recovered can get.
- an iron boron rare earth sintered magnet is disposed in the processing chamber, and the sintered magnet is heated within a range of 800 to 1100 ° C to perform the same or other processing.
- the metal evaporation material containing at least one of Dy and Tb installed in the room may be heated to evaporate, and the evaporated metal atoms may be supplied to the surface of the sintered magnet and adhered.
- the diffusion rate could be increased, and Dy and Tb adhering to the surface of the sintered magnet were successively converted into crystal grains of the sintered magnet. It is the power that is efficiently diffused into the field phase.
- the temperature of the sintered magnet is lower than 800 ° C, a diffusion rate that can be diffused to the grain boundary phase of the sintered magnet and spread uniformly cannot be obtained. There is a risk of forming a thin film of metal evaporation material.
- Dy and Tb enter the crystal grains that are the main phase of the sintered magnet, and as a result, the same as adding Dy and Tb when obtaining the sintered magnet, There is a risk that the magnetic field strength, and hence the maximum energy product showing the magnetic properties, may be greatly reduced.
- an iron-boron rare earth-based sintered magnet is disposed in the processing chamber, and the sintered magnet is heated to a predetermined temperature and then held in the same or another processing chamber.
- the metal evaporation material containing at least one of Dy and Tb is vaporized by heating within a range of 800 ° C to 1200 ° C, and the evaporated metal atoms are supplied to the surface of the sintered magnet for adhesion. May be. According to this, since the metal evaporation material is heated and evaporated in the range of 800 ° C to 1200 ° C, the Dy and Tb metal atoms can be applied to the sintered magnet surface according to the vapor pressure at that time. Is supplied.
- the heating temperature of the metal evaporation material is lower than 800 ° C, Dy and Tb metal atoms are dispersed on the surface of the sintered magnet S so that Dy and Tb are diffused and uniformly distributed in the grain boundary phase.
- the vapor pressure that can be supplied is not reached.
- the temperature exceeds 1200 ° C the vapor pressure of the metal evaporation material becomes too high, and metal atoms of Dy and Tb in the vapor atmosphere are excessively supplied to the surface of the sintered magnet S, resulting in a sintered magnet. There is a possibility that a thin film having a metal evaporation material force is formed on the surface.
- the sintered magnet and the metal evaporating material are arranged apart from each other, it may be possible to prevent the molten metal evaporating material from directly attaching to the sintered magnet when the metal evaporating material is evaporated.
- the total surface area of the sintered magnets installed in the processing chamber is increased.
- the ratio of the sum of the surface area of the metal evaporating material against is preferably set in a range from 1 X 10- 4 of 2 X 10 3.
- the evaporation amount at a constant temperature is increased or decreased by changing the specific surface area of the metal evaporation material disposed in the processing chamber, for example, the supply amount of Dy and Tb to the sintered magnet surface is increased or decreased. It is possible to easily adjust the supply amount to the surface of the sintered magnet without changing the configuration of the equipment, such as installing separate parts in the processing chamber.
- the inside of the processing chamber Prior to heating the processing chamber containing the sintered magnet, in order to remove dirt, gas and water adsorbed on the surface of the sintered magnet before diffusing Dy and Tb into the grain boundary phase, It is preferable that the inside of the processing chamber is held at a predetermined pressure.
- the processing chamber is depressurized to a predetermined pressure and then heated and held at a predetermined temperature.
- the oxide film on the surface of the sintered magnet is removed before Dy and Tb are diffused into the grain boundary phase.
- the sintering by plasma is performed prior to heating the processing chamber containing the sintered magnet. It is preferable to clean the magnet surface.
- the sintered magnet has an average crystal grain size in the range of 1 ⁇ m to 5 ⁇ m or 7 ⁇ m to 20 ⁇ m.
- the average grain size is 7 m or more, the rotational force during magnetic field forming increases, the degree of orientation is good, and the surface area of the grain boundary phase decreases, so that it adheres to the surface of the sintered magnet.
- Dy and Tb can be diffused efficiently, resulting in a permanent magnet with a very high coercivity.
- the average crystal grain size exceeds 25 11 m, the degree of orientation deteriorates due to an extremely large proportion of grains containing different crystal orientations at the grain boundaries, and as a result, the maximum energy of the permanent magnet is reduced. One product, residual magnetic flux density, and coercive force are reduced.
- the average grain size is less than 5 ⁇ If it is full, the proportion of single-domain grains increases, and as a result, a permanent magnet having a very high coercive force is obtained. As the average grain size becomes smaller, the grain boundaries become finer and more complex, so that Dy and Tb cannot be diffused efficiently.
- the sintered magnet preferably does not contain Co. Since conventional neodymium magnets require anti-corrosion measures, when adding at least one of the force S to which Co was added, Dy or Tb adhering to the surface of the sintered magnet, the crystal grains of the sintered magnet Since there is no intermetallic compound containing Co at the boundary, Dy and Tb metal atoms adhering to the surface of the sintered magnet can be efficiently diffused. In addition, the rich phase of Dy and Tb, which has extremely high corrosion resistance and weather resistance compared to Nd, is formed inside the defects (cracks) in the crystal grains near the surface of the sintered magnet during processing of the sintered magnet and the crystal grains. By being formed in the field phase, it becomes a permanent magnet having extremely strong corrosion resistance and weather resistance without using Co.
- the permanent magnet according to claim 15 has a sintered magnet of iron-boron-rare earth, and evaporates a metal evaporation material composed of at least one of Dy and Tb. Then, the supply amount of the evaporated metal atoms to the surface of the sintered magnet is adjusted to attach the metal atoms, and a thin film made of a metal evaporation material is formed on the sintered magnet surface. It is characterized by being previously diffused into the grain boundary phase of the sintered magnet.
- the sintered magnet preferably has an average crystal grain size in the range of 1 ⁇ m to 5 ⁇ m or 7 ⁇ m to 20 ⁇ m.
- the sintered magnet preferably does not contain Co! /, And is preferably a thing!
- the method for producing a permanent magnet according to the present invention can efficiently diffuse Dy and Tb into the grain boundary phase without deteriorating the surface of the sintered NdFeB-based magnet, thereby increasing the magnetization.
- the coercive force can be effectively improved or recovered, and the supply of Dy and Tb to the surface of the sintered magnet and the diffusion of the sintered magnet to the grain boundary phase are performed in a single process and the subsequent process Combined with the fact that they are no longer necessary, the effect is high productivity.
- the permanent magnet of the present invention has the effect of being high when it has high V, magnetic properties and strength / corrosion resistance.
- the permanent magnet M of the present invention is processed into a predetermined shape.
- the evaporated metal vapor V containing at least one of Dy and Tb is evaporated on the surface of the sintered Nd—Fe—B based sintered magnet S, and the evaporated metal atoms are adhered to the crystal grain boundaries of the sintered magnet S. It is produced by performing a series of treatments (vacuum steam treatment) that spread and uniformly spread to phases.
- the Nd-Fe-B-based sintered magnet S which is a starting material, is produced by a known method as follows. That is, Fe, B, and Nd are blended at a predetermined composition ratio, and an alloy of 0.05 mm to 0.5 mm is first manufactured by a known strip casting method. On the other hand, an alloy having a thickness of about 5 mm may be produced by a known centrifugal forging method. In addition, a small amount of Cu, Zr, Dy, Tb, Al or Ga may be added during blending. Next, the produced alloy is once pulverized by a known hydrogen pulverization step, and then finely pulverized by a jet mill pulverization step.
- the sintered magnet is manufactured by sintering under predetermined conditions. After sintering, the sintered magnet is subjected to a heat treatment for removing distortion of the sintered magnet S at a predetermined temperature (in the range of 400 ° C to 700 ° C) for a predetermined time (for example, 2 hours). For example, it may be possible to further improve the magnetic properties when vacuum vapor treatment is performed.
- the average crystal grain size of the sintered magnet S is in the range of 1 ⁇ m to 5 ⁇ m, or 7 ⁇ m to 20 ⁇ m. Try to be within range.
- the average grain size is 7 in or more, the rotational force during magnetic field forming increases and the degree of orientation increases, and the surface area of the grain boundary decreases, so that at least one of Dy and Tb can be reduced in a short time.
- a permanent magnet M that can diffuse efficiently and has a high coercive force is obtained.
- the average crystal grain size exceeds 25 m, the degree of orientation deteriorates because the proportion of grains containing different crystal orientations in one crystal grain becomes extremely large, and as a result, the maximum energy of the permanent magnet is reduced.
- One product, residual magnetic flux density, and coercive force are reduced.
- the average crystal grain size is less than 511 m, the proportion of single-domain crystal grains increases, and as a result, a permanent magnet having a very high coercive force can be obtained. If the average grain size force is smaller than m, the grain boundaries become complicated and the time required for carrying out the diffusion process becomes extremely long, resulting in poor productivity.
- the metal evaporation material V includes Dy and Tb, which greatly improve the magnetocrystalline anisotropy of the main phase.
- an alloy containing at least one of these can be used.
- Nd, Pr, Al, Cu, Ga, and the like are included in order to further increase the coercive force.
- the metal evaporating material V may be blended at a predetermined mixing ratio, for example, an arc melting furnace may be used to obtain a butter-like alloy and placed in a processing chamber described later.
- a vacuum vapor processing apparatus 1 for carrying out the process, a turbo molecular pump, cryopump, a predetermined pressure via the evacuating means 11 such as a diffusion pump (e.g. 1 X 10_ 5 Pa) It has a vacuum chamber 12 that can be kept under reduced pressure.
- a box 2 comprising a rectangular parallelepiped box 21 having an upper surface opened and a detachable lid 22 on the upper surface of the opened box 21 is installed.
- a flange 22a bent downward is formed on the outer peripheral edge of the lid 22 over the entire circumference.
- the flange 22a A processing chamber 20 is defined which is fitted to the outer wall (in this case, no vacuum seal such as a metal seal is provided) and is isolated from the vacuum chamber 11.
- a predetermined pressure of the vacuum chamber 12 through the vacuum exhaust means 11 e.g., 1 X 10- 5 Pa
- the processing chamber 20 is substantially half orders of magnitude higher pressure than the vacuum chamber 12 (e.g., 5 X 10- 4 The pressure is reduced to Pa).
- the volume of the processing chamber 20 is set so that metal atoms in the vapor atmosphere are supplied to the sintered magnet S from a plurality of directions either directly or repeatedly in consideration of the mean free path of the evaporated metal material. Has been. Further, the wall thickness of the box portion 21 and the lid portion 22 is set so as not to be thermally deformed when heated by a heating means described later, and is made of a material that does not react with the metal evaporation material.
- the box 2 is made of, for example, Mo, W, V, Ta, or an alloy thereof (including rare earth-added Mo alloy, Ti-added Mo alloy, etc.), CaO, YO, or rare earth oxide.
- these materials are formed as a lining film on the surface of another heat insulating material.
- a placement portion 21a is formed at a predetermined height position from the bottom in the processing chamber 20 by arranging, for example, a plurality of wire rods made of Mo (for example, ⁇ 0.;! To 10 mm) in a lattice shape.
- This A plurality of sintered magnets S can be mounted side by side on the mounting portion 21a.
- the metal evaporation material V is appropriately disposed on the bottom surface, side surface, or top surface of the processing chamber 20.
- the vacuum chamber 12 is provided with a heating means 3.
- the heating means 3 is made of a material that does not react with the metal evaporation materials of Dy and Tb, similar to the box 2 .
- the heating means 3 is provided so as to surround the box 2 and is made of Mo having a reflective surface on the inside. It is composed of a heat insulating material and an electric heater disposed on the inside thereof and having a filament made of Mo. Then, the inside of the processing chamber 20 can be heated substantially uniformly by heating the box 2 with the heating means 3 under reduced pressure and indirectly heating the inside of the processing chamber 20 via the box 2.
- the production of the permanent magnet M in which the method of the present invention is performed using the vacuum vapor processing apparatus 1 will be described.
- the sintered magnet S produced by the above method is placed on the placement portion 21a of the box portion 21, and Dy that is a metal evaporation material V is placed on the bottom surface of the box portion 21 (thereby, the processing chamber 20). In which the sintered magnet S and the metal evaporation material are spaced apart).
- the box body 2 is installed in a predetermined position surrounded by the heating means 3 in the vacuum chamber 12 (see FIG. 2).
- a predetermined pressure e.g., 1 X 10- 4 Pa
- vacuum chamber 12 via the evacuation hand stage 11 is evacuated to vacuum to reach, (the processing chamber 20 is evacuated to nearly a half orders of magnitude higher pressures
- the heating means 3 is activated to heat the processing chamber 20.
- Dy installed on the bottom surface of the processing chamber 20 is heated to substantially the same temperature as the processing chamber 20 and starts to evaporate.
- Dy vapor atmosphere is formed.
- the sintered magnets S and Dy are arranged apart from each other, so the melted Dy does not directly adhere to the sintered magnet S in which the surface Nd-rich phase is melted.
- Dy atoms in the Dy vapor atmosphere are supplied to and adhered to the surface of the sintered magnet S heated to approximately the same temperature as Dy from a plurality of directions by direct or repeated collisions.
- Dy is diffused into the grain boundary phase of the sintered magnet S, and the permanent magnet M is obtained.
- the average composition of the sintered magnet surface S adjacent to the thin film becomes the Dy rich composition, and when the Dy rich composition is reached, the liquidus temperature is As a result, the surface of the sintered magnet S melts (that is, the main phase melts and the amount of liquid phase increases). As a result, the vicinity of the surface of the sintered magnet S melts and collapses, and the unevenness increases. In addition, Dy penetrates excessively into the crystal grains with a large amount of liquid phase, and the maximum energy product and residual magnetic flux density, which show magnetic properties, are further reduced.
- the surface area per unit volume (specific surface area) is small! /, And Balta-like (substantially spherical) Dy is used in the processing chamber 20; The amount of evaporation at a constant temperature was reduced.
- the heating means 3 is controlled so that the temperature in the processing chamber 20 is in the range of 800 ° C. to 1050 ° C., preferably 900 ° C. to 1000 ° C. (For example, when the processing chamber temperature is 900 ° C and 1000 ° C, the saturated vapor pressure of Dy is about 1 X 10 1 X 10- &).
- the total surface area of the sintered magnet S installed on the mounting portion 21a of the processing chamber 20 is used to diffuse Dy into the grain boundary phase. Is set so that the ratio of the total surface area of Balta-shaped Dy installed on the bottom of the processing chamber 20 is in the range of 1 X 10_ 4 2 X 10 3 . If the ratio is outside the range of 1 X 1CT 4 2 X 10 3 , a thin film of Dy or Tb may be formed on the surface of the sintered magnet S, and a permanent magnet with high magnetic properties cannot be obtained.
- the ratio was Sigma preferred is the range of 1 X 10_ 3 of 1 X 10 3, the ratio is more preferably ranges from 1 X 10- 2 1 of X 10 2.
- the ratio is more preferably ranges from 1 X 10- 2 1 of X 10 2.
- the Dy layer (thin film) is formed, it can be diffused efficiently and uniformly distributed in the grain boundary phase of the sintered magnet S (see Fig. 1). As a result, the surface of the permanent magnet M is prevented from deteriorating, and Dy is prevented from excessively diffusing into the grain boundary in the region close to the surface of the sintered magnet. (A phase containing 5 to 80% of Dy), and Dy diffuses only near the surface of the crystal grains, so that the magnetization and coercive force are effectively improved or recovered, and the finish Permanent magnet M with excellent productivity that does not require machining can be obtained
- Tb with low vapor pressure can be used in the heating temperature range (900 ° C ⁇ ; 1000 ° C range).
- the evaporation chamber may be heated in the range of 900 ° C. to 1150 ° C.
- the vapor pressure that can supply Tb atoms to the surface of the sintered magnet S is not reached.
- Tb diffuses excessively into the crystal grains, reducing the maximum energy product and residual magnetic flux density.
- the force S used to use a bulky metal evaporation material V having a small specific surface area in order to reduce the amount of evaporation at a constant temperature which is not limited to this, for example, in the box portion 21 It is possible to reduce the specific surface area by installing a saucer with a concave cross-section and storing granular or Balta-like metal evaporating material V in the saucer. Further, metal evaporating material V is accommodated in the saucer. Thereafter, a lid (not shown) having a plurality of openings may be attached.
- the sintered magnet S and the metal evaporating material V are disposed in the processing chamber 20 !, but the sintered magnet S and the metal evaporating material V are described.
- Can be heated at different temperatures for example, an evaporation chamber (other processing chamber: not shown) is provided in the vacuum chamber 12 separately from the processing chamber 20, and other heating means for heating the evaporation chamber
- the metal atoms in the vapor atmosphere are supplied to the sintered magnet in the processing chamber 20 through the communication path that connects the processing chamber 20 and the evaporation chamber. You may be made to do.
- the evaporation chamber is set to 700 ° C ⁇ ; 1050 ° C (700 ° C ⁇ ; 1050 ° C, the saturated vapor pressure of Dy is about 1 (X 10 1 X 10 1 Pa).
- the vapor pressure that can supply Dy to the surface of the sintered magnet S is not reached so that Dy diffuses in the grain boundary phase and spreads uniformly.
- the metal evaporation material V is mainly composed of Tb
- the evaporation chamber may be heated in the range of 900 ° C to 1200 ° C.
- the sintered magnet S and the metal evaporation material V can be heated at different temperatures as described above, the sintered magnet may be heated and held in the range of 800 to 1100 ° C. As a result, the diffusion rate can be increased, and Dy and Tb adhering to the surface of the sintered magnet can be effectively diffused sequentially into the grain boundary phase of the sintered magnet.
- the temperature of the sintered magnet is lower than 800 ° C, a diffusion rate that allows the sintered magnet to diffuse into the grain boundary phase of the sintered magnet and spread it uniformly cannot be obtained. There is a risk that a thin film made of On the other hand, at a temperature exceeding 1100 ° C, Dy and Tb enter the crystal grains that are the main phase of the sintered magnet, and the result is the same as when adding Dy and Tb to obtain the sintered magnet, There is a possibility that the magnetic field strength, and hence the maximum energy product showing the magnetic characteristics, may be greatly reduced.
- the vacuum chamber 12 is set in a predetermined manner via the vacuum exhaust means 11.
- pressure e.g., 1 X 10- 5 Pa
- the processing chamber 20 was reduced from the vacuum chamber 12 to approximately half orders of magnitude higher pressure (e.g., 5 X 10_ 4 Pa)
- the heating means 3 may be operated to heat the inside of the processing chamber 20 to, for example, 100 ° C. and hold it for a predetermined time.
- a plasma generating device (not shown) having a known structure for generating Ar or He plasma is provided in the vacuum chamber 12, and the surface of the sintered magnet S by plasma prior to processing in the vacuum chamber 12 is provided.
- the cleaning pre-processing may be performed.
- a known transfer robot is installed in the vacuum chamber 12, and after the lid 22 is finished in the vacuum chamber 12, You just have to wear it.
- the lid portion 22 is mounted on the upper surface of the box portion 21 to constitute the box body 2.
- the vacuum chamber 12 is isolated from the vacuum chamber 12.
- the processing chamber 20 can be decompressed as the pressure in the chamber 12 is reduced.
- the upper surface opening thereof is opened, for example, in Mo. It may be covered with a thin film.
- the processing chamber 20 may be sealed in the vacuum chamber 12 and may be configured to be maintained at a predetermined pressure independently of the vacuum chamber 12.
- the sintered magnet S has a low oxygen content! /, So that it expands to the grain boundary phase of Dy and Tb. Since the diffusion rate is increased, the oxygen content of the sintered magnet S itself may be 3000 ppm or less, preferably 2000 ppm or less, more preferably lOOOppm or less.
- the composition is 30Nd-1B-0.1Cu-2Co-bal.Fe, the sintered magnet S itself has an oxygen content of 500 ppm and an average grain size of 3 ⁇ m. m was processed into a cylindrical shape of ⁇ 10 X 5 mm. In this case, the surface of the sintered magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- Comparative Example 1 a conventional resistance heating type vapor deposition apparatus using a Mo board (VFR—200M / manufactured by ULVAC) was used to form a film on the same sintered magnet S as in Example 1 above. Processing was performed. In this case, it sets the Dy of 2g on Mo board, after reducing the pressure of the vacuum chamber to 1 X 10- 4 P a, flowing 150A current to Mo board, 30 minutes, was formed.
- FIG. 5 is a photograph showing the surface state of the permanent magnet obtained by performing the above treatment
- (a) is a photograph of the surface of the sintered magnet S (before treatment).
- the black and / or the portions such as the voids of the Nd-rich phase, which are the grain boundary phases, and the traces of degranulation are seen! /
- the black part disappears when the surface of the sintered magnet is covered with a Dy layer (thin film) (see Fig. 5 (b)).
- the film thickness of the Dy layer was measured, it was 40 m.
- Example 1 similar to the sintered magnet S before processing, black portions such as Nd-rich phase voids and degranulation marks are seen, which are substantially the same as the surface of the sintered magnet before processing. Status In addition, since there was a change in weight, it is understood that Dy is efficiently diffused into the grain boundary phase before the Dy layer is formed! / (See Fig. 5 (c)) .
- FIG. 6 is a table showing magnetic characteristics when the permanent magnet M is obtained under the above conditions.
- the magnetic characteristics of the sintered magnet S before processing are shown.
- the coercive force of the sintered magnet S before vacuum vapor treatment was 11.3 K0e, whereas in Example 1, the maximum energy product was 49.9 MG0e and the residual magnetic flux density was 14.3 kG. It can be seen that the coercive force is 23. IkOe and the coercive force is improved.
- the composition is 30Nd—1B—0.1Cu—2Co—bal.
- Fe the sintered magnet S itself has an oxygen content of 500 ppm and an average crystal grain size of 3 ⁇ m.
- m was processed into a shape of 40 ⁇ 40 ⁇ 5 (thickness) mm.
- the surface of the fired magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- the box 2 is made of Mo having a size of 200 X I 70 X 60 mm, and 30 sintered magnets S are arranged at equal intervals on the mounting portion 21a.
- Dy having a purity of 99.9% was used as the metal evaporation material, and a flat or granular material was placed on the bottom surface of the processing chamber 20 in a predetermined amount.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 925 ° C. Then, after the temperature of the processing chamber 20 reached 925 ° C., the above processing was performed in this state for 12 hours. Next, heat treatment was performed at a treatment temperature of 530 ° C and a treatment time of 90 minutes. Finally, the permanent magnet obtained by carrying out the above method was processed into a shape of ⁇ 10 X 5 mm by wire cutting.
- FIG. 7 shows the amount of Dy placed on the bottom surface of the processing chamber 20 so that the ratio of the total surface area of Dy to the total surface area of the sintered magnet S in the processing chamber 20 is increased or decreased.
- 6 is a table showing the magnetic characteristics of permanent magnets when and are changed. According to this,;! Used Balta shaped Dy of ⁇ 5 mm, as long as it is within the range the ratio is about 5 X 10- 5 to 1, before the thin film of Dy is formed on the surface of the sintered magnet S It can be seen that Dy can diffuse into the grain boundary phase. However, 20 to obtain a high coercive force of about kOe, it is necessary to increase the ratio from 1 X 10_ 4.
- Fe, B, Nd, Dy, Co, Al, Cu are blended in the above composition ratio to produce an alloy of 0.05 mm to 0.5 mm by a known strip casting method, and by a known hydrogen grinding process. Once pulverized, then finely pulverized by the jet mill pulverization process.
- the sintered magnet S is adjusted so that the average crystal grain size is in the range of 0. ⁇ to 25 Hm.
- the surface of the fired magnet S was finished to have a surface roughness of 50 ⁇ m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting portion 21a in the Mo box 2.
- Balta-shaped Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of 10 g was disposed on the bottom surface of the processing chamber 20.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 975 ° C. Then, after the temperature of the processing chamber 20 reaches 975 ° C, in this state;! ⁇ 72 hours, the above vacuum vapor treatment is performed, and then the heat treatment temperature is set to 500 ° C and the processing time is set to 90 minutes. A heat treatment was performed.
- FIG. 8 is a table showing the average value of the magnetic characteristics when a permanent magnet is obtained under the above conditions. According to this, when the average crystal grain size of the sintered magnet is;! ⁇ 5 H m, or 7 ⁇ 20 ⁇ m, the maximum energy product is 52MG0e or more, the residual magnetic flux density is 14.3kG or more, It can also be seen that a permanent magnet having a high magnetic property with a coercive force of 3 ⁇ 40 k0e or more was obtained.
- Example 4 As the Fe-B-Nd sintered magnet not containing Co, a composition having a composition of 27Nd-lB- 0.05Cu-0.05Ga-0.lZr-bal.Fe was used. In this case, Fe, B, Nd, Gu, Ga, and Zr are blended in the above composition ratio to prepare an alloy of 0.05 mm to 0.5 mm by a known strip casting method, and once by a known hydrogen grinding process. Grind and then finely pulverize by jet mill fine pulverization process. Next, the film was oriented in a magnetic field and formed into a predetermined shape with a mold, and then sintered under predetermined conditions, and processed into a 3 ⁇ 20 ⁇ 40 mm rectangular parallelepiped shape. Then, the surface of the sintered magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 10 sintered magnets S were placed at equal intervals on the mounting portion 21a in the Mo box 2.
- Balta-shaped Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of 1 g was disposed on the bottom surface of the processing chamber 20.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 900 ° C. Then, after the temperature of the processing chamber 20 reached 900 ° C., the above-described vacuum vapor processing was performed at intervals of 4 hours in a range of 2 to 38 hours in this state. Next, heat treatment was performed at a treatment temperature of 500 ° C. and a treatment time of 90 minutes. The vacuum steam processing time (optimum vacuum steam processing time) at which the highest magnetic properties were obtained was determined.
- Comparative Examples 4a to 4c as a Fe-B-Nd sintered magnet containing Co, the composition was 27Nd-lCo-lB-0. 05Cu-0. 05Ga-0. LZr-bal.
- Example 4a 27Nd— 4Co — IB— 0. 05Cu-0. 05Ga-0. LZr-bal.
- Fe Comparative Example 4b
- Each sintered magnet of Fe was used.
- Fe, B, Nd, Co, Gu, Ga, Zr are blended in the above composition ratio, and an alloy of 0.05 mm to 0.5 mm is prepared by a known strip casting method, and then a known hydrogen pulverization is performed. It is pulverized once in the process, and then finely pulverized in the jet mill pulverization process.
- After magnetic orientation and forming into a predetermined shape with a mold it was sintered under predetermined conditions and processed into a 3 ⁇ 20 ⁇ 40 mm rectangular parallelepiped shape.
- the surface of the sintered magnet S has a surface roughness of 20 m or less. After finishing as described above, it was washed with acetone. Next, the above treatment was performed under the same conditions as in Example 4 to obtain the permanent magnets of Comparative Examples 4a to 4c and to obtain the optimum vacuum steam treatment time).
- FIG. 9 is a table showing the average value of magnetic properties and the evaluation of corrosion resistance of the permanent magnets obtained in Example 4 and Comparative Examples 4a to 4c. The magnetic properties before the vacuum vapor treatment of the present invention are also shown. In addition, a 100-hour saturated steam pressurization test (PCT: pressure tacker test) was conducted as a test to show corrosion resistance.
- PCT pressure tacker test
- the composition is 20Nd—5Pr—3Dy—IB—ICo— 0 ⁇ 2 Al-bal.
- Fe, sintered magnet S itself has an oxygen content of 3000 ppm and an average crystal A particle size of 4 m and processed into a shape of 20 ⁇ 40 ⁇ 2 (thickness) mm was used.
- Fe, B, Nd, Dy, Co, Al, Pr are blended in the above composition ratio, an alloy having a thickness of 5 mm is produced by a known centrifugal forging method, and once pulverized by a known hydrogen grinding process. Subsequently, it is pulverized by the jet mill pulverization process.
- sintering was performed under predetermined conditions to obtain a sintered magnet S.
- the surface of the fired magnet S was finished to have a surface roughness of 20 Hm or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- ten sintered magnets S are arranged at equal intervals on the placement portion 21a in the box 2.
- Dy with a purity of 99.9% is used as the metal evaporation material, and the total amount of lg Arranged on the bottom of 20.
- the pressure was reduced once the vacuum chamber to 1 X 10_ 4 Pa by operating the evacuating means (pressure in the treatment chamber 5 X 10- 3 Pa), the pressure in the processing chamber to 1 X 10- 2 Pa
- the above processing was performed for 12 hours in this state.
- the sintered magnet S and the metal evaporation material V were heated to substantially the same temperature.
- the heat treatment was performed at a treatment temperature of 500 ° C and a treatment time of 90 minutes.
- FIG. 10 shows the average value of the magnetic properties of the permanent magnet when the temperature of the processing chamber 20 is changed in the range of 750 ° C to 1100 ° C. / Is a table showing together with the sintered magnets of the case. According to this, it can be seen that at a temperature lower than 800 ° C, sufficient Dy atoms cannot be supplied to the sintered magnet surface S, and the coercive force cannot be effectively improved. On the other hand, at temperatures above 1050 ° C, it can be seen that the maximum energy product and residual magnetic flux density decreased due to excessive supply of Dy atoms. In this case, a Dy layer was formed on the surface of the sintered magnet.
- the temperature of the processing chamber 20 is set in the range of 800 ° C to 1050 ° C, the maximum energy volume is 50MG0e or more, the residual magnetic flux density is 14.3kG or more, and the coercive force is It can be seen that a permanent magnet having a high magnetic property of 22 k0e or more was obtained. In this case, there was no Dy layer formed on the surface of the sintered magnet, and there was a change in weight, so Dy was efficiently diffused into the grain boundary phase before the Dy layer was formed. I understand that.
- the composition is 20Nd—8Pr—3Dy—IB—ICo—0.2 Al-bal.
- Fe, sintered magnet S itself has an oxygen content of 3000 ppm and an average crystal A particle size of 4 m and processed into a shape of 20 ⁇ 40 ⁇ 2 (thickness) mm was used.
- Fe, B, Nd, Dy, Co, Al, Pr are blended in the above composition ratio, an alloy having a thickness of 10 mm is produced by a known centrifugal forging method, and once pulverized by a known hydrogen grinding process. Subsequently, it is pulverized by the jet mill pulverization process.
- sintering was performed under predetermined conditions to obtain a sintered magnet S.
- the surface of the fired magnet S was finished to have a surface roughness of 20 Hm or less, and then washed with acetone.
- the permanent magnet M is removed by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1. Obtained.
- ten sintered magnets S are arranged at equal intervals on the placement portion 21a in the box 2.
- Tb having a purity of 99.9% was used as the metal evaporation material, and the total amount of lg was disposed on the bottom surface of the processing chamber 20.
- FIG. 11 shows the average value of the magnetic properties of the permanent magnet when the temperature of the processing chamber 20 is changed in the range of 850 ° C to 1200 ° C. / Is a table showing together with the sintered magnets of the case. According to this, it can be seen that at a temperature lower than 900 ° C, sufficient Dy atoms cannot be supplied to the sintered magnet surface S, and the coercive force cannot be effectively improved. On the other hand, when the temperature exceeds 1150 ° C, it can be seen that the excess energy of Tb atoms decreases the maximum energy product and residual magnetic flux density, and also reduces the coercive force. In this case, a Tb layer was formed on the surface of the sintered magnet!
- the temperature of the processing chamber 20 is set in the range of 900 ° C to 1150 ° C, the maximum energy volume is 50MG0e or more, the residual magnetic flux density is 14.6kG or more, and the coercive force is It can be seen that a permanent magnet with a high magnetic property of 21k0e or more and 30k0e depending on the conditions was obtained. In this case, the Tb layer was not formed on the surface of the sintered magnet.
- Fe, B, Nd, Dy, Co, Al, Cu are blended in the above composition ratio to produce an alloy of 0.05 mm to 0.5 mm by a known strip casting method, and by a known hydrogen grinding process. Once pulverized, then finely pulverized by the jet mill pulverization process.
- the sintered magnet S is adjusted so that the average crystal grain size is in the range of 0. ⁇ to 25 Hm.
- the surface of the fired magnet S was finished to have a surface roughness of 20 ⁇ m or less, and then washed with acetone.
- the permanent magnet M is removed by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1. Obtained.
- 100 sintered magnets S are arranged at equal intervals on the mounting portion 21a in the Mo box 2.
- Balta-like Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of lg was arranged on the bottom surface of the processing chamber 20.
- the vacuum evacuation means is operated to temporarily depressurize the vacuum chamber to 1 X 10_ 4 Pa.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 975 ° C. Then, after the temperature of the processing chamber 20 reaches 975 ° C, in this state;! ⁇ 72 hours, the above vacuum vapor treatment is performed, and then the heat treatment temperature is set to 500 ° C and the processing time is set to 90 minutes. A heat treatment was performed.
- FIG. 12 is a table showing the magnetic characteristics as average values when permanent magnets are obtained under the above conditions. According to this, when the average crystal grain size of the sintered magnet is! ⁇ 5 m, or 7 ⁇ 20 111, the maximum energy product is 50MG0e or more, the residual magnetic flux density is 14.3kG or more, and it is maintained. It can be seen that a permanent magnet with a magnetic force of 30 k0e or higher and high magnetic properties of 36 k0e depending on the conditions was obtained.
- a Fe-B-Nd-based sintered magnet containing no Co was used with a composition of 28Nd-lB- 0.05Cu-0.05Ga-0.lZr-bal.Fe.
- Fe, B, Nd, Gu, Ga, and Zr are blended in the above composition ratio to prepare an alloy of 0.05 mm to 0.5 mm by a known strip casting method, and once by a known hydrogen grinding process. Grind and then finely pulverize by jet mill fine pulverization process.
- the film was oriented in a magnetic field and formed into a predetermined shape with a mold, and then sintered under predetermined conditions, and processed into a 3 ⁇ 20 ⁇ 40 mm rectangular parallelepiped shape. Then, the surface of the sintered magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 10 sintered magnets S were placed at equal intervals on the mounting portion 21a in the Mo box 2.
- Balta-shaped Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of 1 g was disposed on the bottom surface of the processing chamber 20.
- the vacuum evacuation means is operated to temporarily depressurize the vacuum chamber to 1 X 10_ 4 Pa.
- Comparative Examples 8a to 8c as a Fe-B-Nd-based sintered magnet containing Co, the composition was 28Nd-lCo-lB-0. 05Cu-0. 05Ga-0. LZr-bal.
- Example 8a 28Nd— 4Co — IB— 0. 05Cu-0. 05Ga-0. LZr-bal.
- Fe Comparative Example 8b
- Each sintered magnet of Fe was used.
- Fe, B, Nd, Co, Gu, Ga, Zr are blended in the above composition ratio, and an alloy of 0.05 mm to 0.5 mm is prepared by a known strip casting method, and then a known hydrogen pulverization is performed. It is pulverized once in the process, and then finely pulverized in the jet mill pulverization process.
- After magnetic orientation and forming into a predetermined shape with a mold it was sintered under predetermined conditions and processed into a 3 ⁇ 20 ⁇ 40 mm rectangular parallelepiped shape. Then, after finishing the surface of the sintered magnet S so as to have a surface roughness of 20 m or less, it was washed with acetone. Next, the above treatment was performed under the same conditions as in Example 8 to obtain the permanent magnets of Comparative Examples 8a to 8c and to obtain the optimum vacuum steam treatment time).
- FIG. 13 is a table showing the average value of magnetic properties and the evaluation of corrosion resistance of the permanent magnets obtained in Example 8 and Comparative Examples 8a to 8c. The magnetic characteristics before the vacuum vapor treatment of the present invention are also shown. In addition, a 100-hour saturated steam pressurization test (PCT: pressure tacker test) was conducted as a test to show corrosion resistance.
- PCT pressure tacker test
- the composition is 20Nd—5Pr—3Dy—IB—ICo— 0 ⁇ 2 Al-0.
- LCu-bal. Fe the average grain size is 7 m, 20 X 40 X 1 (thickness) mm was used.
- the surface of the fired magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- ten sintered magnets S are arranged at equal intervals on the mounting portion 21a of the Mo box 2, and at this time, the mounting portion 21a is heated or cooled to obtain the sintered magnet S itself. The temperature of can be changed.
- Dy with a purity of 99.9% was used as the metal evaporation material V, and particles with a diameter of 2 mm were placed on the bottom surface of the processing chamber 20 in a total amount of 5 g.
- Fig. 14 shows the average value of the magnetic properties of the permanent magnet when the permanent magnet is obtained by changing the temperature of the sintered magnet at a predetermined temperature in the processing chamber 20 (and thus the metal evaporation material V). It is a table to show. According to this, when the temperature in the processing chamber is 750 to 900 ° C, if the temperature of the sintered magnet is lower than 800 ° C, a high coercive force cannot be obtained, while the temperature of the sintered magnet is 1100 ° C. When C is exceeded, it can be seen that the maximum energy product and the residual magnetic flux density decrease with the coercive force.
- the Nd—Fe—B-based sintered magnet used had a composition of 25Nd—2Dy—IB—ICo—0.2A1—0.05 Cu-0. LNb-0. IMo-bal. It was processed into a rectangular parallelepiped shape of X 20 X 40 mm. In this case, Fe, B, Nd, Dy, Co, Al, Cu, Nb, and Mo After blending, an ingot is prepared by a known centrifugal forging method, and once pulverized by a known hydrogen pulverization step, then finely pulverized by a jet mill pulverization step.
- the sintered magnet 3 is placed so that the average crystal grain size is in the range of 0.5 111 to 25 111. Obtained.
- the oxygen content in the sintered magnet S was 50 ppm.
- the surface of the fired magnet S was finished so as to have a surface roughness of 50 m or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting portion 21a in the Mo box 2.
- an alloy of 50Dy50Tb was used as the metal evaporation material, and a 2 mm diameter granular material was placed on the bottom surface of the processing chamber 20 in a total amount of 5 g.
- the vacuum evacuation means is actuated to temporarily depressurize the vacuum chamber to 1 X 10_ 4 Pa.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 975 ° C. Then, after the temperature of the processing chamber 20 reaches 975 ° C., in this state;! ⁇ 72 hours, the above vacuum vapor treatment is performed, and then the heat treatment temperature is set to 400 ° C. and the processing time is set to 90 minutes. A heat treatment was performed.
- FIG. 15 is a table showing the magnetic characteristics as average values when permanent magnets are obtained under the above conditions. According to this, when the average crystal grain size of the sintered magnet is! ⁇ 5 m, or 7 ⁇ 20 111, the maximum energy product is 51.5MG0e or more, the residual magnetic flux density is 14.4kG or more, It can also be seen that a permanent magnet having a high magnetic property with a coercive force of 28 k0e or more was obtained.
- the composition is 21Nd-7Pr-1B- 0.
- Fe 05Cu-0. 05Ga-0. LZr-bal. Fe was used.
- Fe, B, Nd, Gu, Ga, Zr, and Pr are blended in the above composition ratio, and an alloy of 0.05 mm to 0.5 mm is manufactured by a known strip casting method, and then by a known hydrogen grinding process. Once pulverized, then pulverized by the jet mill pulverization process. Next, the film was magnetically oriented and molded into a predetermined shape with a mold, and then sintered under predetermined conditions to be processed into a 5 ⁇ 20 ⁇ 40 mm rectangular parallelepiped shape.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 10 sintered magnets S were placed at equal intervals on the mounting portion 21a in the Mo box 2.
- Balta-shaped Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of 1 g was disposed on the bottom surface of the processing chamber 20.
- the vacuum evacuation means is operated to temporarily depressurize the vacuum chamber to 1 X 10_ 4 Pa.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 950 ° C. Then, after the temperature of the processing chamber 20 reached 950 ° C., the above-described vacuum vapor processing was performed at intervals of 2 hours in a range of 2 to 38 hours in this state. Next, heat treatment was performed at a treatment temperature of 650 ° C. and a treatment time of 2 hours. The vacuum steam processing time (optimum vacuum steam processing time) at which the highest magnetic properties were obtained was determined.
- Comparative Examples 11a to 11c as a Fe-B-Nd-based sintered magnet containing Co, the composition was 21 Nd-7Pr-lCo-lB-0. 05Cu- 0. 05Ga- 0. lZr-bal. Fe (Comparative Example l la), 2 lNd-7Pr-4Co- lB-0. 05Cu— 0. 05Ga— 0. lZr-bal. Fe (Comparative Example l lb), 21Nd-7Pr-8Co- lB-0. 05Cu — 0. 05Ga— 0. lZr-bal. Fe (Comparative Example 11c) sintered magnets were used.
- FIG. 16 is a table showing an average value of magnetic characteristics and evaluation of corrosion resistance of the permanent magnets obtained in Example 11 and Comparative Examples 11a to 11c. The magnetic properties before the vacuum vapor treatment of the present invention are also shown.
- a saturated steam pressure test PCT: pressure tacker test
- PCT pressure tacker test
- the permanent magnet of Example 11 did not visually recognize the occurrence of cracks even though it did not contain Co, and had high corrosion resistance. It can be seen that a permanent magnet with a high coercivity of 20.5 k0e on average was obtained by short-time vacuum steam treatment.
- the composition is 20Nd—7Pr— 1B— 0 ⁇ 2A1-0. 05Ga
- Fe was caloeed into a 20 x 20 x 40 mm cuboid.
- Fe, B, Nd, Pr, Al, Ga, Zr, Sn are blended in the above composition ratio, an ingot is prepared by a known centrifugal forging method, and once ground by a known hydrogen grinding process, Finely pulverized by a jet mill.
- magnetic field orientation was performed to form a predetermined shape with a mold and sintered under predetermined conditions to obtain an average crystal grain size of 5 5 ⁇ .
- sintered magnets were obtained by rapid cooling after sintering (sample 1) and those subjected to heat treatment in the range of 400 ° C to 700 ° C for 2 hours after sintering (sample 2).
- the surface was finished and processed to have a surface roughness of 20 am or less, and then washed with acetone.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting portion 21a of the box 2 made of Mo, and Dy with a purity of 99.9% is used as the metal evaporation material V, and the diameter is 5 mm.
- the granular material was placed on the bottom surface of the processing chamber 20 in a total amount of 20 g.
- the operating the vacuum evacuation means once pressure of the vacuum chamber to 1 X 10_ 4 Pa in (pressure in the treatment chamber 5 X 10- 3 Pa), the heating temperature of the processing chamber 20 by the heating means 3
- the temperature was set to 900 ° C., and after the temperature of the processing chamber 20 reached a predetermined temperature, the above processing was performed in this state for 6 hours.
- the treatment temperature was set to a predetermined temperature, the treatment time was set to 2 hours, and heat treatment was performed.
- Fig. 17 shows that the temperature of the heat treatment after the vacuum steam treatment is changed in the range of 400 to 700 ° C, It is a table
- Sample 2 which was heat-treated after sintering, had a low coercive force of 12.1 kOe before being subjected to vacuum vapor treatment, but it was 18 k0e when the heat treatment was performed after vacuum vapor treatment. Therefore, it can be seen that a permanent magnet having a high coercive force of 26.5 k0e was obtained.
- Nd—Fe—B based sintered magnet the composition is 21Nd—7Pr— 1B— 0 ⁇ 2A1-0. 05Ga -0. LZr-0. IMo-bal. Fe, with average grain size force m A 20 x 20 x 40 mm cuboid was used.
- permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting part 21a of the box 2 made of Mo, and Dy having a purity of 99.9% is used as the metal evaporation material V, and the diameter is 10 mm.
- the granular material was placed on the bottom surface of the processing chamber 20 in a total amount of 20 g.
- the vacuum evacuation means is actuated to temporarily reduce the vacuum chamber to a predetermined degree of vacuum (the pressure in the processing chamber is approximately half orders of magnitude higher), and the heating temperature of the processing chamber 20 by the heating means 3 is increased.
- the temperature was set to 900 ° C., and after the temperature of the processing chamber 20 reached 900 ° C., the above treatment was performed in this state for 6 hours.
- the treatment temperature was set to 550 ° C., the treatment time was set to 2 hours, and heat treatment was performed.
- Fig. 18 shows the magnet of the permanent magnet when the pressure in the vacuum chamber 11 (adjustment of the degree of opening of the vacuum exhaust valve and the amount of Ar introduced into the vacuum chamber is adjusted as appropriate) is obtained. It is a table
- the composition is 20Nd—5Pr—3Dy—IB—ICo— 0 ⁇ 1 Al-0. 03Ga-bal. Fe, with an average grain size force of 5-25, 20 x 20 x 40mm shape What was processed into the shape was used. In this case, the surface of the fired magnet S was finished so as to have a surface roughness of 20 m or less, and then washed with acetone.
- an evaporation chamber communicating with the processing chamber 20 via the communication path is separately provided in the vacuum channel 12.
- a vacuum vapor processing apparatus (not shown) provided with other heating means for heating the evaporation chamber, a permanent magnet M was obtained by the above vacuum vapor processing.
- ten sintered magnets S are arranged at equal intervals on the mounting portion 21a of the Mo box 2, and the floor of the evaporation chamber having the same form as the Mo box 2 is placed on the floor.
- Dy with a purity of 99.9% was used as the metal evaporation material V, and particles with a diameter of lmm were placed in a total amount of 10g.
- FIG. 19 is a table showing the average value of the magnetic characteristics of the permanent magnet when the heating temperature of the evaporation chamber is changed and the permanent magnet is obtained at a predetermined temperature of the processing chamber 20 (and thus the sintered magnet). It is. According to this, when the temperature of the sintered magnet is in the range of 800 ° C to 1100 ° C, if the evaporation chamber is heated in the range of 800 ° C to 1200 ° C to evaporate Dy, the maximum It can be seen that a permanent magnet having a high magnetic property of about 27 k0e was obtained with an energy product of 47.8 MG 0e or more, a residual magnetic flux density of 14 kG or more, and a coercive force of about 15.9 k0e or more. .
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting portion 21a in the Mo box 2.
- an alloy of 50Dy50Tb was used as the metal evaporation material, and a granular material having a diameter of 2 mm was disposed on the bottom surface of the processing chamber 20 in a total amount of 5 g.
- the vacuum evacuation means is actuated to temporarily depressurize the vacuum chamber to 1 X 10_ 4 Pa.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 975 ° C. Then, after the temperature of the processing chamber 20 reaches 975 ° C., in this state;! ⁇ 72 hours, the above vacuum vapor treatment is performed, and then the heat treatment temperature is set to 400 ° C. and the processing time is set to 90 minutes. A heat treatment was performed.
- FIG. 20 is a table showing the magnetic characteristics as average values when permanent magnets are obtained under the above conditions. According to this, when the average crystal grain size of the sintered magnet is! ⁇ 5 m, or 7 ⁇ 20 111, the maximum energy product is 51.5MG0e or more, the residual magnetic flux density is 14.4kG or more, It can also be seen that a permanent magnet having a high magnetic property with a coercive force of 28 k0e or more was obtained.
- the composition is 21Nd-7Pr-1B- 0.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 10 sintered magnets S are equally spaced on the mounting portion 21a in the Mo box 2. I decided to leave myself. Further, Balta-shaped Dy having a purity of 99.9% was used as the metal evaporation material, and the total amount of 1 g was disposed on the bottom surface of the processing chamber 20.
- the vacuum chamber is temporarily depressurized to 1 X 10_ 4 Pa by operating the vacuum exhaust means.
- the heating temperature of the processing chamber 20 by the heating means 3 was set to 950 ° C. Then, after the temperature of the processing chamber 20 reached 950 ° C., the above-described vacuum vapor processing was performed at intervals of 2 hours in a range of 2 to 38 hours in this state. Next, heat treatment was performed at a treatment temperature of 650 ° C. and a treatment time of 2 hours. The vacuum steam processing time (optimum vacuum steam processing time) at which the highest magnetic properties were obtained was determined.
- Comparative Examples 16a to 16c as a Co-containing Fe—B—Nd sintered magnet, the composition was 21 Nd-7Pr-lCo-lB-0. 05Cu— 0. 05Ga— 0. lZr-bal. Fe (Comparative Example 16a), 2 lNd-7Pr-4Co-lB-0. 05Cu— 0. 05Ga— 0. lZr-bal. Fe (Comparative Example 16b), 21Nd-7Pr-8Co-lB-0. 05Cu— 0 05Ga— 0. lZr-bal. Fe (Comparative Example 16c) sintered magnets were used.
- FIG. 21 is a table showing the average value of magnetic characteristics and the corrosion resistance evaluation of the permanent magnets obtained in Example 16 and Comparative Examples 16a to 16c. The magnetic properties before the vacuum vapor treatment of the present invention are also shown.
- a saturated steam pressure test PCT: pressure tacker test
- PCT pressure tacker test
- the composition is 21Nd—7Pr—1B— 0 ⁇ 2A1-0. 05Ga -0. LZr-0. IMo-bal. A 20 x 20 x 40 mm cuboid was used.
- the permanent magnet M was obtained by the vacuum vapor treatment using the vacuum vapor treatment apparatus 1.
- 100 sintered magnets S are arranged at equal intervals on the mounting part 21a of the box 2 made of Mo, and Dy having a purity of 99.9% is used as the metal evaporation material V, and the diameter is 10 mm.
- the granular material was placed on the bottom surface of the processing chamber 20 in a total amount of 20 g.
- the vacuum evacuation means is actuated to once reduce the vacuum chamber to a predetermined degree of vacuum (the pressure in the processing chamber becomes approximately half a digit higher), and the heating temperature of the processing chamber 20 by the heating means 3 is increased.
- the temperature was set to 900 ° C., and after the temperature of the processing chamber 20 reached 900 ° C., the above treatment was performed in this state for 6 hours.
- the treatment temperature was set to 550 ° C., the treatment time was set to 2 hours, and heat treatment was performed.
- Fig. 22 shows the magnet of the permanent magnet when the pressure in the vacuum chamber 11 (adjustment of the degree of opening of the vacuum exhaust valve and the amount of Ar introduced into the vacuum chamber is appropriately adjusted) is obtained. It is a table
- FIG. 1 is a diagram schematically illustrating a cross section of a permanent magnet manufactured according to the present invention.
- FIG. 2 is a diagram schematically showing a vacuum processing apparatus for performing the processing of the present invention.
- 3 A diagram schematically illustrating a cross section of a permanent magnet manufactured by a conventional technique.
- FIG. 5 is a magnified photograph of the surface of a permanent magnet produced by carrying out the present invention.
- FIG. 6 is a table showing the magnetic properties of the permanent magnet produced in Example 1.
- FIG. 7 is a table showing the magnetic characteristics of the permanent magnet produced in Example 2.
- FIG. 8 is a table showing the magnetic properties of the permanent magnet produced in Example 3.
- FIG. 9 is a table showing the magnetic characteristics of the permanent magnet produced in Example 4.
- FIG. 10 is a table showing the magnetic characteristics of the permanent magnet produced in Example 5.
- FIG. 11 is a table showing the magnetic properties of the permanent magnet produced in Example 6.
- FIG. 12 is a table showing the magnetic properties of the permanent magnet produced in Example 7.
- FIG. 13 is a table showing the magnetic properties of the permanent magnet produced in Example 8.
- FIG. 14 is a table showing the magnetic characteristics of the permanent magnet produced in Example 9.
- FIG. 15 is a table showing the magnetic properties of the permanent magnet produced in Example 10.
- FIG. 16 is a table showing the magnetic characteristics of the permanent magnet produced in Example 11.
- FIG. 17 is a table showing the magnetic properties of the permanent magnet produced in Example 12.
- FIG. 18 is a table showing the magnetic properties of the permanent magnet produced in Example 13.
- FIG. 19 is a table showing the magnetic characteristics of the permanent magnet produced in Example 14.
- FIG. 20 is a table showing the magnetic properties of the permanent magnet produced in Example 15.
- FIG. 21 is a table showing the magnetic properties of the permanent magnet produced in Example 16.
- FIG. 22 is a table showing the magnetic properties of the permanent magnet produced in Example 17.
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Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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CN2007800312872A CN101506919B (zh) | 2006-08-23 | 2007-08-22 | 永磁铁以及永磁铁的制造方法 |
DE112007002010T DE112007002010T5 (de) | 2006-08-23 | 2007-08-22 | Permanentmagnet und Herstellungsverfahren davon |
US12/438,057 US8257511B2 (en) | 2006-08-23 | 2007-08-22 | Permanent magnet and a manufacturing method thereof |
KR1020097004472A KR101425828B1 (ko) | 2006-08-23 | 2007-08-22 | 영구자석 및 영구자석의 제조방법 |
JP2008530940A JP5356026B2 (ja) | 2006-08-23 | 2007-08-22 | 永久磁石及び永久磁石の製造方法 |
US13/310,907 US20120086531A1 (en) | 2006-08-23 | 2011-12-05 | Permanent magnet and a manufacturing method thereof |
Applications Claiming Priority (8)
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JP2006-227122 | 2006-08-23 | ||
JP2006-227123 | 2006-08-23 | ||
JP2006227123 | 2006-08-23 | ||
JP2006227122 | 2006-08-23 | ||
JP2006-245302 | 2006-09-11 | ||
JP2006245302 | 2006-09-11 | ||
JP2006246248 | 2006-09-12 | ||
JP2006-246248 | 2006-09-12 |
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US13/310,907 Division US20120086531A1 (en) | 2006-08-23 | 2011-12-05 | Permanent magnet and a manufacturing method thereof |
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WO2008023731A1 true WO2008023731A1 (en) | 2008-02-28 |
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PCT/JP2007/066272 WO2008023731A1 (en) | 2006-08-23 | 2007-08-22 | Permanent magnet and process for producing the same |
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US (2) | US8257511B2 (ja) |
JP (1) | JP5356026B2 (ja) |
KR (1) | KR101425828B1 (ja) |
CN (1) | CN101506919B (ja) |
DE (1) | DE112007002010T5 (ja) |
TW (1) | TWI433172B (ja) |
WO (1) | WO2008023731A1 (ja) |
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JP2010129665A (ja) * | 2008-11-26 | 2010-06-10 | Ulvac Japan Ltd | 永久磁石の製造方法 |
JP2010245392A (ja) * | 2009-04-08 | 2010-10-28 | Ulvac Japan Ltd | ネオジウム鉄ボロン系の焼結磁石 |
EP2270822A1 (en) | 2009-07-01 | 2011-01-05 | Shin-Etsu Chemical Co., Ltd. | Rare earth magnet and its preparation |
US20110052799A1 (en) * | 2008-02-20 | 2011-03-03 | Hiroshi Nagata | Method of recycling scrap magnet |
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KR20220064920A (ko) | 2020-11-12 | 2022-05-19 | 신에쓰 가가꾸 고교 가부시끼가이샤 | 희토류 소결 자석의 제조 방법 |
KR20220066039A (ko) | 2019-09-20 | 2022-05-23 | 신에쓰 가가꾸 고교 가부시끼가이샤 | 희토류 자석의 제조 방법 |
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RU2458423C2 (ru) * | 2006-12-21 | 2012-08-10 | Улвак, Инк. | Постоянный магнит и способ его изготовления |
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CN105185498B (zh) | 2015-08-28 | 2017-09-01 | 包头天和磁材技术有限责任公司 | 稀土永磁材料及其制造方法 |
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US11254998B2 (en) | 2016-03-28 | 2022-02-22 | Hitachi Metals, Ltd. | Method for separating Dy and Tb from alloy containing both |
WO2017170347A1 (ja) * | 2016-03-28 | 2017-10-05 | 日立金属株式会社 | DyとTbを含む合金から両者を分離する方法 |
CN106782980B (zh) | 2017-02-08 | 2018-11-13 | 包头天和磁材技术有限责任公司 | 永磁材料的制造方法 |
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CN107424703B (zh) * | 2017-09-06 | 2018-12-11 | 内蒙古鑫众恒磁性材料有限责任公司 | 晶界扩散法制作烧结钕铁硼永磁的重稀土附着工艺 |
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TWI471875B (zh) * | 2008-10-08 | 2015-02-01 | Ulvac Inc | Materials for the production of evaporation materials |
JP2013237929A (ja) * | 2008-10-08 | 2013-11-28 | Ulvac Japan Ltd | 蒸発材料の製造方法 |
WO2010041416A1 (ja) * | 2008-10-08 | 2010-04-15 | 株式会社アルバック | 蒸発材料及び蒸発材料の製造方法 |
KR101456837B1 (ko) * | 2008-10-08 | 2014-11-04 | 가부시키가이샤 알박 | 증발 재료 및 증발 재료의 제조 방법 |
US9434002B2 (en) | 2008-10-08 | 2016-09-06 | Ulvac, Inc. | Evaporating material and method of manufacturing the same |
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RU2490367C2 (ru) * | 2008-10-08 | 2013-08-20 | Улвак, Инк. | Иcпаряющийся материал и способ его изготовления |
JP5348670B2 (ja) * | 2008-10-08 | 2013-11-20 | 株式会社アルバック | 蒸発材料 |
JP2010129665A (ja) * | 2008-11-26 | 2010-06-10 | Ulvac Japan Ltd | 永久磁石の製造方法 |
JP2010245392A (ja) * | 2009-04-08 | 2010-10-28 | Ulvac Japan Ltd | ネオジウム鉄ボロン系の焼結磁石 |
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TWI433172B (zh) | 2014-04-01 |
KR101425828B1 (ko) | 2014-08-05 |
CN101506919A (zh) | 2009-08-12 |
US8257511B2 (en) | 2012-09-04 |
US20100164663A1 (en) | 2010-07-01 |
CN101506919B (zh) | 2012-10-31 |
JPWO2008023731A1 (ja) | 2010-01-14 |
JP5356026B2 (ja) | 2013-12-04 |
KR20090048613A (ko) | 2009-05-14 |
US20120086531A1 (en) | 2012-04-12 |
DE112007002010T5 (de) | 2009-07-02 |
TW200822155A (en) | 2008-05-16 |
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