WO2015121913A1 - 希土類永久磁石及び希土類永久磁石の製造方法 - Google Patents
希土類永久磁石及び希土類永久磁石の製造方法 Download PDFInfo
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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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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- 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
- H01F1/0536—Alloys characterised by their composition containing rare earth metals 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
- 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
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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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
Definitions
- a powder sintering method is generally used conventionally.
- the powder sintering method first, magnet powder obtained by pulverizing raw materials by a jet mill (dry pulverization) or the like is manufactured. Thereafter, the magnet powder is put into a mold and press-molded into a desired shape. Then, it is manufactured by sintering the solid magnet powder formed into a desired shape at a predetermined temperature (for example, 1100 ° C. for Nd—Fe—B magnets) (for example, Japanese Patent Laid-Open No. 2-266503).
- a predetermined temperature for example, 1100 ° C. for Nd—Fe—B magnets
- permanent magnets are magnetically oriented by applying a magnetic field from the outside in order to improve magnetic characteristics.
- a magnet powder is filled into a mold at the time of press molding, and a magnetic field is applied to orient the magnetic field, and then pressure is applied to form a compacted compact.
- a magnet was molded by applying pressure in an atmosphere to which a magnetic field was applied. Accordingly, it is possible to form a molded body in which the easy magnetization axis direction of each magnet particle constituting the permanent magnet is aligned with the magnetic field application direction.
- the C-axis (easy axis of magnetization) of more magnet particles is aligned in the same direction for the magnet particles constituting the permanent magnet by the magnetic field orientation ( That is, increasing the degree of orientation is important.
- magnet powder is molded by green sheet molding, since there is a binder on the particle surface, the frictional force at the time of orientation is increased, and the orientation of the particles is reduced compared to powder molding, so magnetic field orientation is performed. There is a problem that becomes difficult.
- the present invention has been made to solve the above-described conventional problems, and provides a rare earth permanent magnet and a rare earth permanent magnet manufacturing method in which the magnetic properties of the permanent magnet are improved by increasing the density of the magnet.
- the purpose is to do.
- a rare earth permanent magnet includes a step of pulverizing a magnet raw material into magnet powder, a step of generating a mixture in which the pulverized magnet powder and a binder are mixed, and the mixture.
- a step of magnetic field orientation by applying a magnetic field a step of calcining the magnetically oriented mixture in a non-oxidizing atmosphere, and a step of sintering by maintaining the calcined mixture at a firing temperature.
- the density is 95% or more.
- the rare earth permanent magnet according to the present invention is characterized in that, in the magnetic field orientation step, the mixture is formed into a sheet shape and then magnetically oriented in the sheet shape mixture.
- the mixture formed into a sheet shape is heated and magnetic field orientation is performed by applying a magnetic field to the heated mixture.
- the mixture is formed into a long sheet shape, and in the step of magnetic field orientation, an in-plane direction, a length direction, and an in-plane direction of the mixture formed into a long sheet shape
- the magnetic field is oriented by applying a magnetic field to the direction and the width direction or the direction perpendicular to the sheet surface.
- the mixture in the step of calcining the mixture, the mixture is heated to a set temperature at a predetermined heating rate in a non-oxidizing atmosphere, and then the set temperature is set. By holding for a certain time, the binder is scattered and removed.
- the rare earth permanent magnet manufacturing method according to the present invention is characterized in that the set temperature is a binder decomposition temperature.
- the method for producing a rare earth permanent magnet according to the present invention is characterized in that the rate of temperature rise is 2 ° C./min or less.
- the method for producing a rare earth permanent magnet according to the present invention is characterized in that, in the magnetic field orientation step, the mixture is formed into a sheet shape and then magnetically oriented in the sheet shape mixture.
- the method for producing a rare earth permanent magnet according to the present invention is characterized in that when the mixture is formed into a sheet, the mixture is heated and melted and formed into a sheet.
- the mixture formed in a sheet shape is heated and a magnetic field is applied to the heated mixture. It is characterized by doing.
- the density of the rare earth permanent magnet is set to 95% or more. It is possible to prevent the magnetic properties from being greatly deteriorated by the air gap without forming the air gap inside the magnet.
- the mixture is heated up to a set temperature at a predetermined heating rate in a non-oxidizing atmosphere, and then held at the set temperature for a certain period of time, whereby the binder is scattered. Therefore, the carbon contained in the mixture can be removed stepwise as the temperature changes during calcination.
- the rare earth permanent magnet according to the present invention since the binder is scattered and removed by maintaining the mixture at a binder decomposition temperature for a certain period of time in a non-oxidizing atmosphere, even when a binder is added, the magnet The amount of carbon contained therein can be reduced in advance. As a result, it is possible to suppress the precipitation of ⁇ Fe in the main phase of the magnet after sintering, to densely sinter the entire magnet, and to prevent the coercive force from being lowered.
- the mixture is heated to a set temperature at a rate of temperature increase of 2 ° C./min or less in a non-oxidizing atmosphere, and then maintained at the set temperature for a certain period of time. Since the baking treatment is performed, it becomes possible to remove carbon contained in the mixture stepwise with a gradual temperature change. Therefore, a high-density rare earth permanent magnet can be obtained without forming a large number of voids inside the magnet.
- the mixture of the magnet powder and the binder is formed into a sheet-like green sheet, thereby making it easier to form the final product and control the orientation direction. It is possible to make it happen. Also, productivity can be improved.
- the mixture is heated and melted and formed into a sheet shape, so that the permanent magnet can be formed with high dimensional accuracy. Further, even when the permanent magnet is thinned, it is possible to prevent the processing man-hours from increasing without reducing the material yield. Further, there is no risk of liquid deviation, that is, uneven thickness of the sheet during magnetic field orientation.
- the rare earth permanent magnet according to the present invention in the step of forming the mixture into a long sheet shape and magnetic field orientation, the in-plane direction and the length direction of the long sheet, the in-plane direction and the width direction, or the sheet surface Since the magnetic field is oriented by applying a magnetic field to the vertical direction, magnetic field orientation can be appropriately performed, and the magnetic characteristics of the permanent magnet can be improved. Further, if the application direction of the magnetic field is the in-plane direction and the length direction or the in-plane direction and the width direction of the long sheet, there is no possibility that the surface of the sheet is inverted when the magnetic field is applied. On the other hand, if the magnetic field is applied in a direction perpendicular to the sheet surface, a thin film anisotropic magnet with the C axis (easy magnetization axis) in the thickness direction can be obtained.
- the mixture is heated to a set temperature at a predetermined heating rate in a non-oxidizing atmosphere, and then held at the set temperature for a certain time. Since carbon is scattered and removed, the carbon contained in the mixture can be removed stepwise in accordance with the temperature change during calcination.
- the binder is scattered and removed by maintaining the mixture at a binder decomposition temperature in a non-oxidizing atmosphere for a certain period of time.
- the amount of carbon contained in the magnet can be reduced in advance. As a result, it is possible to suppress the precipitation of ⁇ Fe in the main phase of the magnet after sintering, to densely sinter the entire magnet, and to prevent the coercive force from being lowered.
- the mixture of the magnet powder and the binder is formed into a sheet-like green sheet, thereby forming the final product shape, controlling the orientation direction, and the like. It becomes possible to make it easier. Also, productivity can be improved.
- the molded mixture is heated and magnetic field orientation is performed by applying a magnetic field to the heated mixture. Even if it exists, the magnetic field orientation with respect to a mixture can be performed appropriately, and it becomes possible to improve the magnetic characteristic of a permanent magnet.
- the magnetic field is oriented by applying a magnetic field to the direction perpendicular to the sheet surface, the magnetic field can be properly oriented and the magnetic characteristics of the permanent magnet can be improved. Further, if the application direction of the magnetic field is the in-plane direction and the length direction or the in-plane direction and the width direction of the long sheet, there is no possibility that the surface of the sheet is inverted when the magnetic field is applied. On the other hand, if the magnetic field is applied in a direction perpendicular to the sheet surface, a thin film anisotropic magnet with the C axis (easy magnetization axis) in the thickness direction can be obtained.
- FIG. 1 is an overall view showing a permanent magnet 1 according to the present embodiment.
- the permanent magnet 1 is a thin-film permanent magnet having a thickness of, for example, 0.05 mm to 10 mm (for example, 1 mm).
- the permanent magnet 1 is manufactured by sintering a molded body (green body) obtained by molding a mixture obtained by mixing magnet powder and a binder as described later. And a green body is produced by shape
- a predetermined shape for example, sheet shape, block shape, final product shape, etc.
- the mixture is once formed into a sheet shape and then processed into a final product shape, productivity can be improved by producing in a continuous process, and molding accuracy can also be improved.
- a thin film sheet member having a thickness of 0.05 mm to 10 mm (for example, 1 mm) is used. Even in the case of a sheet shape, a large permanent magnet 1 can be manufactured if a plurality of sheets are laminated.
- polystyrene resin examples include polyisobutylene (PIB), which is a polymer of isobutylene, polyisoprene (isoprene rubber, IR), which is a polymer of isoprene, and polybutadiene (butadiene) that is a polymer of 1,3-butadiene.
- PIB polyisobutylene
- IR polyisoprene rubber
- IR isoprene rubber
- IR isoprene rubber
- butadiene butadiene
- thermoplastic resin that softens at 250 ° C. or lower, more specifically a thermoplastic resin having a glass transition point or a melting point of 250 ° C. or lower in order to appropriately perform magnetic field orientation. .
- a long chain hydrocarbon when used for the binder, it is preferable to use a long chain saturated hydrocarbon (long chain alkane) that is solid at room temperature and liquid at room temperature or higher. Specifically, it is preferable to use a long-chain saturated hydrocarbon having 18 or more carbon atoms. Then, when the mixture of the magnetic powder and the binder is magnetically oriented as described later, the magnetic field orientation is performed in a state where the mixture is heated and softened at a temperature equal to or higher than the melting point of the long-chain hydrocarbon.
- a long chain saturated hydrocarbon long chain alkane
- the coarsely pulverized magnet powder 10 is finely pulverized by a wet method using a bead mill 11 or a dry method using a jet mill.
- the coarsely pulverized magnet powder 10 is finely pulverized in a solvent to a predetermined particle size (for example, 0.1 ⁇ m to 5.0 ⁇ m) and the magnet powder is dispersed in the solvent.
- the magnet powder contained in the solvent after the wet pulverization is dried by vacuum drying or the like, and the dried magnet powder is taken out.
- coarsely pulverized magnet powder is (a) in an atmosphere composed of an inert gas such as nitrogen gas, Ar gas, and He gas having substantially 0% oxygen content.
- finely pulverized by a jet mill in an atmosphere made of an inert gas such as nitrogen gas, Ar gas, and He gas having an oxygen content of 0.0001 to 0.5%, A fine powder having an average particle diameter of 0.7 ⁇ m to 5.0 ⁇ m.
- the oxygen concentration of substantially 0% is not limited to the case where the oxygen concentration is completely 0%, but may contain oxygen in such an amount that a very small amount of oxide film is formed on the surface of the fine powder. Means good.
- the mixture when the mixture is formed into a sheet shape, for example, hot melt coating that forms a sheet shape after heating a compound in which a magnet powder and a binder are mixed, or a slurry containing a magnet powder, a binder, and an organic solvent.
- hot melt coating that forms a sheet shape after heating a compound in which a magnet powder and a binder are mixed, or a slurry containing a magnet powder, a binder, and an organic solvent.
- slurry coating or the like that forms a sheet by coating the substrate on a substrate.
- an additive for promoting orientation may be added to the compound 12 in order to improve the degree of orientation in a magnetic field orientation step performed later.
- a hydrocarbon-based additive is used, and it is particularly preferable to use an additive having polarity (specifically, an acid dissociation constant pKa of less than 41).
- the addition amount of the additive depends on the particle diameter of the magnet powder, and it is necessary to increase the addition amount as the particle diameter of the magnet powder is smaller.
- the specific addition amount is 0.1 to 10 parts, more preferably 1 to 8 parts, with respect to the magnet powder.
- the additive added to the magnet powder adheres to the surface of the magnet particles and has a role of assisting the rotation of the magnet particles in the magnetic field orientation process described later.
- orientation is easily performed when a magnetic field is applied, and the easy magnetization axis directions of the magnet particles can be aligned in the same direction (that is, the degree of orientation can be increased).
- the frictional force at the time of orientation is increased and the orientation of the particles is lowered, so that the effect of adding the additive is further increased.
- magnet powder and a binder are dispersed in a large amount of organic solvent, and the slurry is placed on a support substrate 13 such as a separator. Apply. Then, the green sheet 14 of a long sheet shape is formed on the support substrate 13 by drying and volatilizing the organic solvent.
- the calendar roll method a certain amount of the compound 12 is charged into the gap between the two heated rolls, and the compound 12 melted by the heat of the roll is applied onto the support base 13 while rotating the roll.
- the support base material 13 for example, a silicone-treated polyester film is used.
- the green sheet is formed on the support substrate 13 by molding the compound 12 melted by extrusion molding or injection molding into a sheet shape and extruding the support substrate 13 instead of coating on the support substrate 13. 14 may be formed.
- the sheet thickness of the green sheet 14 after coating is measured, and the gap D between the die 15 and the support base 13 is feedback-controlled based on the measured value. desirable. Further, the fluctuation of the amount of the fluid compound 12 supplied to the die 15 is reduced as much as possible (for example, suppressed to fluctuation of ⁇ 0.1% or less), and the fluctuation of the coating speed is reduced as much as possible (for example, ⁇ 0. It is desirable to suppress the fluctuation to 1% or less. Thereby, it is possible to further improve the thickness accuracy of the green sheet 14.
- the green sheet 14 is first softened by heating the green sheet 14 that is continuously conveyed together with the support base material 13. Specifically, the green sheet 14 is softened until the viscosity becomes 1 to 1500 Pa ⁇ s, more preferably 1 to 500 Pa ⁇ s. Thereby, the magnetic field orientation can be appropriately performed.
- the surface of the green sheet 14 can be prevented from standing upright by setting the direction in which the magnetic field is applied to the in-plane direction. Moreover, it is preferable that the heat dissipation and solidification of the green sheet 14 performed after the magnetic field orientation is performed in a transported state. Thereby, the manufacturing process can be made more efficient.
- the magnetic field application device 30 using a pole piece or the like includes two ring-shaped coil portions 31 and 32 arranged in parallel so that the central axes are the same, and the coil portion 31. , 32 and two substantially cylindrical pole pieces 33, 34 respectively disposed in the ring holes, and are spaced apart from the conveyed green sheet 14 by a predetermined distance.
- the thickness exceeds 1 mm.
- a liquid material having high fluidity such as a slurry containing an organic solvent by a general slot die method or doctor blade method without using hot melt molding
- the thickness exceeds 1 mm.
- foaming due to vaporization of the organic solvent contained in the slurry or the like during drying becomes a problem.
- the drying time is prolonged to suppress foaming, the magnet powder is settled, and accordingly, the density distribution of the magnet powder is biased with respect to the direction of gravity, which causes warping after firing. Therefore, in the molding from the slurry, the upper limit value of the thickness is substantially regulated, so it is necessary to mold the green sheet with a thickness of 1 mm or less and then laminate it.
- the green sheet 14 subjected to the magnetic field orientation is punched into a desired product shape (for example, a fan shape shown in FIG. 1), and a formed body 40 is formed.
- a non-oxidizing atmosphere in which the molded body 40 is pressurized to atmospheric pressure, or a pressure higher or lower than atmospheric pressure (for example, 1.0 Pa or 1.0 MPa).
- atmospheric pressure or a pressure higher or lower than atmospheric pressure (for example, 1.0 Pa or 1.0 MPa).
- a binder decomposition temperature in a mixed gas atmosphere of an inert gas and an inert gas a temperature satisfying a condition equal to or higher than the thermal decomposition temperature of the additive if an additive that promotes orientation is added
- the calcining process is performed by holding for 5 hours.
- the supply amount of hydrogen during calcination is set to 5 L / min.
- an organic compound such as a binder can be decomposed into a monomer by a depolymerization reaction or the like and scattered to be removed. That is, so-called decarbonization for reducing the amount of carbon in the molded body 40 is performed.
- the calcining treatment is performed under the condition that the carbon content in the molded body 40 is 2000 ppm or less, more preferably 1000 ppm or less. Accordingly, the entire permanent magnet 1 can be densely sintered by the subsequent sintering process, and the residual magnetic flux density and coercive force are not reduced.
- the binder decomposition temperature is determined based on the analysis result of the binder decomposition product and decomposition residue. Specifically, a temperature range is selected in which decomposition products of the binder are collected, decomposition products other than the monomers are not generated, and products due to side reactions of the remaining binder components are not detected even in the analysis of the residues. Although it varies depending on the kind of the binder, it is set to 200 ° C. to 900 ° C., more preferably 400 ° C. to 600 ° C. (for example, 450 ° C.).
- the heating rate is reduced as compared with a case where a general magnet is sintered.
- the temperature rising rate is set to 2 ° C./min or less (for example, 1.5 ° C./min). Therefore, when performing the calcining treatment, as shown in FIG. 7, the temperature is increased at a predetermined temperature increase rate of 2 ° C./min or less, and after reaching a preset temperature (binder decomposition temperature), Calcination is performed by holding at the set temperature for several hours to several tens of hours.
- the carbon in the molded body 40 is not removed rapidly but is removed in stages, so that the density of the sintered permanent magnet is increased ( That is, it is possible to reduce the air gap in the permanent magnet. And if a temperature increase rate shall be 2 degrees C / min or less, the density of the permanent magnet after sintering can be made 95% or more, and a high magnet characteristic can be anticipated.
- NdH 3 (high activity) in the molded body 40 produced by the calcination treatment is changed stepwise from NdH 3 (high activity) ⁇ NdH 2 (low activity).
- the activity of the molded body 40 activated by the calcination treatment is reduced.
- FIG. 8 is a schematic diagram showing a pressure sintering process of the compact 40 by SPS sintering.
- the compact 40 when performing SPS sintering, first, the compact 40 is installed in the sintering die 41 made of graphite. The calcining process described above may also be performed in a state where the molded body 40 is installed in the sintering mold 41. Then, the compact 40 placed in the sintering die 41 is held in the vacuum chamber 42, and an upper punch 43 and a lower punch 44 made of graphite are set.
- the compound was produced by adding a binder to magnet powder. Polyisobutylene (PIB) was used as the binder. Furthermore, an additive for promoting orientation was also added to the compound. In addition, the addition amount of the binder and additive with respect to magnet powder was 4 parts, respectively. Further, the heated and melted compound was applied to the substrate by a slot die method to form an 8 mm thick green sheet.
- PIB Polyisobutylene
- Example 1 and Comparative Examples 1 and 2 The density [%] and the degree of orientation [%] of each magnet after sintering in Example 1 and Comparative Examples 1 and 2 were measured. Further, the residual magnetic flux density [kG] and the coercive force [kOe] were measured for each magnet of Example 1 and Comparative Examples 1 and 2.
- the orientation degree is measured by measuring Br (residual magnetic flux density) and Jmax (maximum magnetization) using a direct current magnetic flux meter (“TRF-5BH-25auto” manufactured by Toei Kogyo Co., Ltd., maximum applied magnetic field 25 kOe). , Br / Jmax was calculated.
- FIG. 9 shows a list of measurement results.
- the density of the permanent magnet greatly affects the magnet characteristics, and the permanent magnet of Example 1 having a higher density shows higher values for the residual magnetic flux density and the coercive force. If the density is 95% or more, sufficient magnetic properties can be exhibited. If the temperature increase rate of the calcining process is 2 ° C./min or less, a permanent magnet having a density of 95% or more can be obtained. Can be realized.
- the permanent magnet of Comparative Example 2 in which the additive for promoting orientation was not added, the effect of the additive for promoting orientation was not obtained, so that the orientation was completely performed even when a magnetic field was applied.
- the degree of orientation of an anisotropic magnet is higher, the magnet characteristics are improved. Therefore, as shown in FIG. 9, the permanent magnets of Example 1 and Comparative Example 1 also show higher values for the residual magnetic flux density and the coercive force.
- the magnetic field orientation is performed after the mixture of the magnet powder and the binder is once molded into a sheet shape.
- the magnetic field orientation may be performed after molding into a shape other than the sheet shape. For example, it may be molded into a block shape. Then, the block-shaped molded body oriented in the magnetic field is further processed to form a final product shape.
- resin long chain hydrocarbon or fatty acid ester is used as the binder, but other materials may be used.
- the Nd—Fe—B type magnet has been described as an example, but other magnets (for example, samarium type cobalt magnet, alnico magnet, ferrite magnet, etc.) may be used. Further, in the present invention, the Nd component is larger than the stoichiometric composition in the present invention, but it may be stoichiometric.
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Abstract
Description
先ず、本発明に係る永久磁石1の構成について説明する。図1は本発明に係る永久磁石1を示した全体図である。尚、図1に示す永久磁石1は扇型形状を備えるが、永久磁石1の形状は打ち抜き形状によって変化する。
本発明に係る永久磁石1はNd-Fe-B系の異方性磁石である。尚、各成分の含有量はNd:27~40wt%、B:0.8~2wt%、Fe(電解鉄):60~70wt%とする。また、磁気特性向上の為、Dy、Tb、Co、Cu、Al、Si、Ga、Nb、V、Pr、Mo、Zr、Ta、Ti、W、Ag、Bi、Zn、Mg等の他元素を少量含んでも良い。図1は本実施形態に係る永久磁石1を示した全体図である。
更に、バインダーに樹脂を用いる場合には、構造中に酸素原子を含まず、且つ解重合性のあるポリマーを用いるのが好ましい。また、後述のように磁石粉末とバインダーとの混合物を最終製品形状に成形する際に生じた混合物の残余物を再利用する為、及び成形された混合物を加熱して軟化した状態で磁場配向を行う為に、熱可塑性樹脂が用いられる。具体的には以下の一般式(1)に示されるモノマーから選ばれる1種又は2種以上の重合体又は共重合体からなるポリマーが該当する。
尚、バインダーに用いる樹脂としては、磁場配向を適切に行う為に250℃以下で軟化する熱可塑性樹脂、より具体的にはガラス転移点又は融点が250℃以下の熱可塑性樹脂を用いることが望ましい。
次に、本発明に係る永久磁石1の製造方法について図2を用いて説明する。図2は本実施形態に係る永久磁石1の製造工程を示した説明図である。
先ず、ビーズミル11等で微粉砕された磁石粉末にバインダーを混合することにより、磁石粉末とバインダーからなる粉末状の混合物(コンパウンド)12を作製する。ここで、バインダーとしては、上述したように樹脂や長鎖炭化水素や脂肪酸エステルやそれらの混合物等が用いられる。例えば、樹脂を用いる場合には構造中に酸素原子を含まず、且つ解重合性のあるポリマーからなる熱可塑性樹脂を用い、一方、長鎖炭化水素を用いる場合には、室温で固体、室温以上で液体である長鎖飽和炭化水素(長鎖アルカン)を用いるのが好ましい。また、脂肪酸エステルを用いる場合には、ステアリン酸メチルやドコサン酸メチル等を用いるのが好ましい。また、バインダーの添加量は、上述したように添加後のコンパウンド12における磁石粉末とバインダーの合計量に対するバインダーの比率が、1wt%~40wt%、より好ましくは2wt%~30wt%、更に好ましくは3wt%~20wt%となる量とする。
図3に示すようにスロットダイ方式に用いられるダイ15は、ブロック16、17を互いに重ね合わせることにより形成されており、ブロック16、17との間の間隙によってスリット18やキャビティ(液溜まり)19を形成する。キャビティ19はブロック17に設けられた供給口20に連通される。そして、供給口20はギアポンプ(図示せず)等によって構成される塗布液の供給系へと接続されており、キャビティ19には供給口20を介して、計量された流体状のコンパウンド12が定量ポンプ等により供給される。更に、キャビティ19に供給された流体状のコンパウンド12はスリット18へ送液されて単位時間一定量で幅方向に均一な圧力でスリット18の吐出口21から予め設定された塗布幅により吐出される。一方で、支持基材13はコーティングロール22の回転に伴って予め設定された速度で連続搬送される。その結果、吐出した流体状のコンパウンド12が支持基材13に対して所定厚さで塗布され、その後、放熱して凝固することにより支持基材13上に長尺シート状のグリーンシート14が成形される。
また、磁場配向した後に行うグリーンシート14の放熱及び凝固は、搬送状態で行うことが好ましい。それによって、製造工程をより効率化することが可能となる。
図6に示すように、加熱装置37は発熱体となる平板部材38の内部に略U字型の空洞39を形成し、空洞39内に所定温度(例えば100~300℃)に加熱された熱媒体であるシリコーンオイルを循環させる構成とする。そして、図4に示すホットプレート26の代わりに、加熱装置37をソレノイド25内においてグリーンシート14に対して上下一対に配置する。それによって、連続搬送されるグリーンシート14を、熱媒体により発熱された平板部材38を介して加熱し、軟化させる。尚、平板部材38はグリーンシート14に対して当接させても良いし、所定間隔離間させて配置しても良い。そして、軟化したグリーンシート14の周囲に配置されたソレノイド25によって、グリーンシート14の面内方向且つ長さ方向(図4の矢印27方向)に対して磁場が印加され、グリーンシート14に対して適切に均一な磁場を配向させることが可能となる。尚、図6に示すような熱媒体を用いた加熱装置37では、一般的なホットプレート26のように内部に電熱線を有さないので、磁場中に配置した場合であってもローレンツ力によって電熱線が振動したり切断される虞が無く、適切にグリーンシート14の加熱を行うことが可能となる。また、電流による制御を行う場合には、電源のON又はOFFで電熱線が振動することにより疲労破壊の原因となる問題が有るが、熱媒体を熱源とした加熱装置37を用いることによって、そのような問題を解消することが可能となる。
図8に示すようにSPS焼結を行う場合には、先ず、グラファイト製の焼結型41に成形体40を設置する。尚、上述した仮焼処理についても成形体40を焼結型41に設置した状態で行っても良い。そして、焼結型41に設置された成形体40を真空チャンバー42内に保持し、同じくグラファイト製の上部パンチ43と下部パンチ44をセットする。そして、上部パンチ43に接続された上部パンチ電極45と下部パンチ44に接続された下部パンチ電極46とを用いて、低電圧且つ高電流の直流パルス電圧・電流を印加する。それと同時に、上部パンチ43及び下部パンチ44に対して加圧機構(図示せず)を用いて夫々上下方向から荷重を付加する。その結果、焼結型41内に設置された成形体40は、加圧されつつ焼結が行われる。また、生産性を向上させる為に、複数(例えば10個)の成形体に対して同時にSPS焼結を行うことが好ましい。尚、複数の成形体40に対して同時にSPS焼結を行う場合には、一の空間に複数の成形体40を配置しても良いし、成形体40毎に異なる空間に配置するようにしても良い。尚、成形体40毎に異なる空間に配置する場合には、空間毎に成形体40を加圧する上部パンチ43や下部パンチ44は各空間の間で一体とする(即ち一体となっている一の上部パンチ43及び下部パンチ44を駆動させることにより各空間にある複数の成形体を同時に加圧できる)ように構成する。
(実施例1)
実施例1はNd-Fe-B系磁石であり、合金組成はwt%でNd/Fe/B=32.7/65.96/1.34とする。また、磁石粉末にバインダーを添加することによりコンパウンドを作製した。バインダーとしてはポリイソブチレン(PIB)を用いた。更に、コンパウンドには、配向を助長する添加剤についても添加した。尚、磁石粉末に対するバインダーと添加剤の添加量は、それぞれ4部とした。また、加熱溶融したコンパウンドをスロットダイ方式により基材に塗工して8mm厚のグリーンシートを成形した。また、成形したグリーンシートを200℃に加熱したホットプレートにより5分間加熱するとともに、磁場配向は、グリーンシートに対して面内方向且つ長さ方向に12Tの磁場を印加することにより行った。そして、磁場配向後に所望の形状に打ち抜いたグリーンシートを水素雰囲気で仮焼し、その後、真空焼結で焼結した。仮焼処理の条件は昇温速度を1.5℃/minとし、450℃に到達した後に450℃で5時間保持とする。尚、他の工程は上述した[永久磁石の製造方法]と同様の工程とする。
仮焼処理の条件を、昇温速度を15℃/minとし、450℃に到達した後に5時間保持とした。他の条件は実施例1と同様である。
磁石粉末に対して配向を助長する添加剤を添加せずに、バインダーのみを添加することによりコンパウンドを作製した。バインダーとしてはポリイソブチレン(PIB)を用い、磁石粉末に対するバインダーの添加量は8部とした。他の条件は比較例1と同様である。
また、脱炭素の為にグリーンシートに対する仮焼処理を行った場合において、希土類永久磁石の密度を95%以上とすることによって、磁石の内部に空隙が形成されることなく、空隙によって磁石特性が大きく低下することを防止できる。
また、グリーンシート14を非酸化性雰囲気下で、所定の昇温速度で設定温度まで昇温した後に、設定温度に一定時間保持することにより、バインダーを飛散させて除去するので、仮焼する際の温度変化に伴ってグリーンシート14中に含まれる炭素を段階的に除去することが可能となる。
また、グリーンシート14を非酸化性雰囲気下でバインダー分解温度に一定時間保持することによりバインダーを飛散させて除去するので、バインダーを添加した場合であっても磁石内に含有する炭素量を予め低減させることができる。その結果、焼結後の磁石の主相内にαFeが析出することを抑え、磁石全体を緻密に焼結することが可能となり、保磁力が低下することを防止できる。
また、グリーンシート14を非酸化性雰囲気下で、2℃/min以下の昇温速度で設定温度まで昇温した後に、設定温度に一定時間保持することにより仮焼処理を行うので、グリーンシート14中に含まれる炭素を緩やかな温度変化に伴って段階的に除去することが可能となる。従って、磁石の内部に空隙が多数形成されることなく、高い密度の希土類永久磁石とすることが可能となる。
また、磁石粉末とバインダーの混合物をシート状のグリーンシートへと成形することによって、その後の最終製品形状への成形や配向方向の制御等をより容易に行わせることが可能となる。また、生産性についても向上させることが可能となる。
また、グリーンシート14は長尺シート状であって、磁場配向する工程では、グリーンシート14の面内方向且つ長さ方向、面内方向且つ幅方向又はシート面の垂直方向に対して磁場を印加することにより磁場配向するので、磁場配向を適切に行わせることができ、永久磁石の磁気特性を向上させることが可能となる。また、磁場の印加方向をグリーンシート14の面内方向且つ長さ方向又は面内方向且つ幅方向とすれば、磁場を印加する際に、グリーンシート14の表面が逆立つ虞もない。一方、磁場の印加方向をグリーンシート14のシート面に対して垂直方向とすれば、C軸(磁化容易軸)を厚さ方向とした薄膜の異方性磁石とすることが可能となる。
例えば、磁石粉末の粉砕条件、混練条件、成形条件、磁場配向工程、仮焼条件、焼結条件などは上記実施例に記載した条件に限られるものではない。例えば、上記実施例ではビーズミルを用いた湿式粉砕により磁石原料を粉砕しているが、ジェットミルによる乾式粉砕により粉砕することとしても良い。また、仮焼を行う際の雰囲気は非酸化性雰囲気であれば水素雰囲気以外(例えば窒素雰囲気、He雰囲気等、Ar雰囲気等)で行っても良い。
11 ジェットミル
12 コンパウンド
13 支持基材
14 グリーンシート
15 ダイ
25 ソレノイド
26 ホットプレート
37 加熱装置
40 成形体
Claims (16)
- 磁石原料を磁石粉末に粉砕する工程と、
前記粉砕された磁石粉末とバインダーとが混合された混合物を生成する工程と、
前記混合物に対して磁場を印加することにより磁場配向する工程と、
磁場配向された前記混合物を非酸化性雰囲気下で仮焼する工程と、
仮焼された前記混合物を焼成温度で保持することにより焼結する工程と、により製造され、
密度が95%以上であることを特徴とする希土類永久磁石。 - 前記混合物を仮焼する工程では、前記混合物を非酸化性雰囲気下で、所定の昇温速度で設定温度まで昇温した後に、前記設定温度に一定時間保持することにより、前記バインダーを飛散させて除去することを特徴とする請求項1に記載の希土類永久磁石。
- 前記設定温度は、バインダー分解温度であることを特徴とする請求項2に記載の希土類永久磁石。
- 前記昇温速度は、2℃/min以下であることを特徴とする請求項2又は請求項3に記載の希土類永久磁石。
- 前記磁場配向する工程では、前記混合物をシート状に成形した後に、シート状の前記混合物に磁場配向することを特徴とする請求項1乃至請求項4のいずれかに記載の希土類永久磁石。
- 前記混合物をシート状に成形する場合には、前記混合物を加熱溶融させてシート状に成形することを特徴とする請求項5に記載の希土類永久磁石。
- 前記磁場配向する工程では、シート状に成形された前記混合物を加熱するとともに、加熱された前記混合物に対して磁場を印加することにより磁場配向することを特徴とする請求項6に記載の希土類永久磁石。
- 前記混合物は長尺シート状に成形され、
前記磁場配向する工程では、長尺シート状に成形された前記混合物の面内方向且つ長さ方向、面内方向且つ幅方向又はシート面の垂直方向に対して磁場を印加することにより磁場配向することを特徴とする請求項5乃至請求項7のいずれかに記載の希土類永久磁石。 - 磁石原料を磁石粉末に粉砕する工程と、
前記粉砕された磁石粉末とバインダーとが混合された混合物を生成する工程と、
前記混合物に対して磁場を印加することにより磁場配向する工程と、
磁場配向された前記混合物を非酸化性雰囲気下で仮焼する工程と、
仮焼された前記混合物を焼成温度で保持することにより焼結し、密度が95%以上の希土類永久磁石を製造する工程と、を有することを特徴とする希土類永久磁石の製造方法。 - 前記混合物を仮焼する工程では、前記混合物を非酸化性雰囲気下で、所定の昇温速度で設定温度まで昇温した後に、前記設定温度に一定時間保持することにより、前記バインダーを飛散させて除去することを特徴とする請求項9に記載の希土類永久磁石の製造方法。
- 前記設定温度は、バインダー分解温度であることを特徴とする請求項10に記載の希土類永久磁石の製造方法。
- 前記昇温速度は、2℃/min以下であることを特徴とする請求項10又は請求項11に記載の希土類永久磁石の製造方法。
- 前記磁場配向する工程では、前記混合物をシート状に成形した後に、シート状の前記混合物に磁場配向することを特徴とする請求項9乃至請求項12のいずれかに記載の希土類永久磁石の製造方法。
- 前記混合物をシート状に成形する場合には、前記混合物を加熱溶融させてシート状に成形することを特徴とする請求項13に記載の希土類永久磁石の製造方法。
- 前記磁場配向する工程では、シート状に成形された前記混合物を加熱するとともに、加熱された前記混合物に対して磁場を印加することにより磁場配向することを特徴とする請求項14に記載の希土類永久磁石の製造方法。
- 前記混合物は長尺シート状に成形され、
前記磁場配向する工程では、長尺シート状に成形された前記混合物の面内方向且つ長さ方向、面内方向且つ幅方向又はシート面の垂直方向に対して磁場を印加することにより磁場配向することを特徴とする請求項13乃至請求項15のいずれかに記載の希土類永久磁石の製造方法。
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CN112820531A (zh) * | 2021-02-02 | 2021-05-18 | 贵州广播电视大学(贵州职业技术学院) | 一种带环形槽基座与永磁体的粘接装置及方法 |
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JPH01150303A (ja) * | 1987-12-08 | 1989-06-13 | Mitsubishi Steel Mfg Co Ltd | 磁気異方性焼結磁石及びその製造方法 |
JPH0677028A (ja) * | 1992-06-24 | 1994-03-18 | Sumitomo Special Metals Co Ltd | 射出成形法によるR−Fe−B系焼結磁石の製造方法 |
JP2013191611A (ja) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | 希土類永久磁石及び希土類永久磁石の製造方法 |
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JP5908246B2 (ja) * | 2011-09-30 | 2016-04-26 | 日東電工株式会社 | 希土類永久磁石の製造方法 |
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- 2014-02-12 JP JP2015562577A patent/JPWO2015121913A1/ja active Pending
- 2014-02-12 WO PCT/JP2014/053112 patent/WO2015121913A1/ja active Application Filing
- 2014-02-12 US US15/118,117 patent/US20170169922A1/en not_active Abandoned
Patent Citations (3)
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JPH01150303A (ja) * | 1987-12-08 | 1989-06-13 | Mitsubishi Steel Mfg Co Ltd | 磁気異方性焼結磁石及びその製造方法 |
JPH0677028A (ja) * | 1992-06-24 | 1994-03-18 | Sumitomo Special Metals Co Ltd | 射出成形法によるR−Fe−B系焼結磁石の製造方法 |
JP2013191611A (ja) * | 2012-03-12 | 2013-09-26 | Nitto Denko Corp | 希土類永久磁石及び希土類永久磁石の製造方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112820531A (zh) * | 2021-02-02 | 2021-05-18 | 贵州广播电视大学(贵州职业技术学院) | 一种带环形槽基座与永磁体的粘接装置及方法 |
CN112820531B (zh) * | 2021-02-02 | 2022-06-24 | 贵州广播电视大学(贵州职业技术学院) | 一种带环形槽基座与永磁体的粘接装置及方法 |
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