WO2022163407A1 - Nd-Fe-B積層焼結磁石およびその製造方法 - Google Patents
Nd-Fe-B積層焼結磁石およびその製造方法 Download PDFInfo
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- WO2022163407A1 WO2022163407A1 PCT/JP2022/001412 JP2022001412W WO2022163407A1 WO 2022163407 A1 WO2022163407 A1 WO 2022163407A1 JP 2022001412 W JP2022001412 W JP 2022001412W WO 2022163407 A1 WO2022163407 A1 WO 2022163407A1
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- sintered
- magnet
- thin plate
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- magnets
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- 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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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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
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/05—Use of magnetic field
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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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
- B22F2301/355—Rare Earth - Fe intermetallic alloys
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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
Definitions
- the present invention relates to Nd-Fe-B laminated sintered magnets, particularly Nd-Fe-B laminated sintered magnets used in large motors and generators such as the main motors of electric vehicles, and a method for producing the same.
- the Nd-Fe-B sintered magnet was invented by the inventors of the present application in 1982 (JP-B-61-3424).
- Applications include computer HDDs (hard disk drives), magnetic head drive motors (VCM: voice coil motors), high-end speakers, headphones, electrically assisted bicycles, golf carts, and permanent magnet magnetic resonance diagnostic equipment (MRI). etc.
- VCM magnetic head drive motors
- MRI permanent magnet magnetic resonance diagnostic equipment
- Nd-Fe-B sintered magnets have high magnetic properties, they have the disadvantage of poor temperature characteristics, and the temperature characteristics of coercive force are particularly important.
- temperature rise due to coil current cannot be avoided.
- a reverse magnetic field acts from the motor armature, irreversible demagnetization occurs in the permanent magnets when the temperature rises and the coercive force decreases. Therefore, in order to prevent irreversible demagnetization, the coercive force must be increased in advance.
- Nd-Fe-B sintered magnets in order to improve their properties such as coercive force, we developed additional elements (Patent No. 1606420, etc.), heat treatment (Patent No. 1818977, etc.), grain size control (Patent No. 1662257, etc.). etc.) have been clarified, but the most effective way to improve the coercive force was the addition of heavy rare earth elements (Dy, Tb) (Patent No. 1802487). However, if a large amount of the heavy rare earth element is used, the coercive force will surely increase, but the saturation magnetization will decrease and the maximum energy product will decrease. In addition, since Dy and Tb are scarce resources and expensive, it is difficult to cover electric vehicles and industrial/domestic motors, which are expected to be in great demand.
- Dy and Tb are scarce resources and expensive, it is difficult to cover electric vehicles and industrial/domestic motors, which are expected to be in great demand.
- Nd-Fe-B sintered magnets in which the magnets are divided and laminated, are used to reduce loss due to eddy current generation during operation, suppress heat generation in the magnets, and reduce the temperature rise of the magnets.
- Coupling magnets have been proposed.
- Dy fluoride powder was applied to a Nd-Fe-B sintered magnet with a thickness of 5 mm and heated at 900°C for 1 hour in Ar for grain boundary diffusion treatment.
- An IPM motor equipped with a rotor manufactured in this manner is proposed in Japanese Unexamined Patent Application Publication No. 2011-78268.
- Nd-Fe-B sintered magnets Another important background technology is the magnet powder molding orientation technology for manufacturing Nd-Fe-B sintered magnets.
- Magnet makers around the world manufacture Nd-Fe-B sintered magnets by the magnetic mold press method. That is, magnet alloy powder is oriented in a mold to which a magnetic field is applied, pressure-molded, and the oriented green compact is sintered to produce a sintered magnet.
- a lamellar magnet is produced by mechanically cutting a block-shaped magnet after making a large chunk of the magnet.
- the present inventors have developed and proposed a "PressLess Process (PLP)" (see Patent Document 1 below).
- PLP PressureLess Process
- the magnet alloy fine powder is densely packed in a filling container (hereinafter referred to as a "mold”).
- a filling container hereinafter referred to as a "mold”
- the mold is conveyed to a sintering furnace.
- a thin plate magnet is produced by filling magnet alloy powder in a mold with a shallow, large-area dish-shaped cavity, orienting it, and then sintering it.
- the orientation direction of the thin plate magnet is perpendicular to the main surface of the thin plate. direction.
- NPLP method which is a further improvement of the above “PLP method” was also proposed by the inventors of the present application (see Patent Document 2 below).
- NPLP method a mold is filled with an appropriate density to form an oriented packed compact of magnet alloy fine powder oriented in a magnetic field, then the outer wall member of the mold is removed and transferred to a base plate for sintering. It is carried into the sintering furnace.
- the cavity in the mold is divided into narrow cavities by a plurality of partition plates, and the narrow cavities partitioned by the partition plates are filled with magnet alloy powder. The mold is then covered and a magnetic field is applied to orient the magnetic alloy powder.
- the magnetic field application direction is the direction perpendicular to the main surface of the narrow cavity.
- the above PLP and NPLP methods have established a technology for directly manufacturing thin plate-like Nd-Fe-B sintered magnets without machining.
- the orientation direction of the magnet that is, the magnetization direction is perpendicular to the main surface of the thin plate.
- the Nd-Fe-B sintered magnets used in the main motor will keep the best magnetic properties while reducing the cost to the utmost limit. and Tb are desired to be reduced to the limit allowed by resources.
- the Nd-Fe-B magnets used in EVs (Electric Vehicles) and HEVs (Hybrid Electric Vehicles) contain a certain amount of Dy and Tb, and production costs are not sufficiently reduced.
- Nd-Fe-B sintered magnets for EVs and HEVs do not have sufficient Dy and Tb reductions and cannot be manufactured at a low cost. It is from.
- the only way to make thin plate magnets of Nd-Fe-B sintered magnets is to cut out thin magnets from block magnets by machining with a cutting wheel or wire saw. At this time, the thin plate magnet is cut so that the direction of easy magnetization is within the main surface of the thin plate. Cutting out such a thin plate magnet from a block magnet requires high processing costs and produces a large amount of chips, resulting in a large loss of material.
- Silicon steel sheets which are core materials used in motors, are punched into a predetermined shape with a thickness of 0.5 mm or less and laminated in order to reduce overcurrent loss that occurs during motor operation.
- Nd-Fe-B sintered magnets which are used in the same motor, could be thinly punched out and used to reduce eddy current loss as much as possible, which would be desirable, but this is not possible. Therefore, the Nd-Fe-B sintered magnets used in the main motors of electric vehicles are used as split magnets with a thickness of about 5 mm, as in the above-mentioned known example (Japanese Unexamined Patent Application Publication No. 2011-78268).
- Magnets with a thickness of 5 mm are machined from a large block of magnets (called block magnets), which incurs processing costs and costs due to lower material yields. Moreover, the effect of reducing eddy current loss is insufficient with a laminate having a thickness of about 5 mm.
- Each thin plate-shaped magnet forming a laminated magnet is called a "unit magnet”.
- the eddy current loss is reduced compared to a non-laminated block magnet, but it is still not sufficiently reduced.
- the eddy current loss generated in the motor is expected to be greatly reduced if the thickness of the unit magnet is thinner than 5 mm, for example 3 mm or less, and laminated magnets are used.
- Making a unit magnet is too costly to be put into practical use due to the great processing cost and the loss of material as chips, that is, the reduction in material yield.
- Nd-Fe-B magnets Another disadvantage of not being able to thin Nd-Fe-B magnets is that when a thick magnet is subjected to grain boundary diffusion treatment, Tb and Dy do not spread throughout the magnet, resulting in uneven coercive force within the magnet. is what you can do. Even if the magnet is divided into 5 mm-thick magnets and grain boundary diffusion treatment is applied to the divided unit magnets as in the above known example, it is difficult to obtain a uniform grain boundary diffusion effect to the inside of the magnet. When these are stacked and mounted in a motor, there is inherent non-uniformity in the coercive force within the magnet. This will remain a weakness of the motor in electric vehicles.
- the Nd-Fe-B sintered magnets currently used in main motors for EVs are Nd-Fe-B sintered magnets containing 2-3% or more of Tb and Dy in the base material. is used, but Tb and Dy are contained only in small amounts in rare earth ores.
- the amount of Tb and Dy used be kept within the limit of the components contained in monazite and bastenacite, which are known as abundant rare earth ores. , the limit is 0.5% of Nd-Fe-B magnet weight.
- an object of the present invention is to provide an Nd-Fe-B laminated sintered magnet that is magnetically uniform and has high magnetic properties.
- Another object of the present invention is to manufacture a laminated magnet consisting of ultra-thin (e.g., thickness of 3 mm or less, preferably 2.5 mm or less) unit magnets without a cutting process after sintering Nd-Fe-B sintered magnets. It is also to provide a method that can be done.
- the inventors have determined the following 1) to 7): 1) In order to minimize the eddy current loss generated in the magnet, the thickness of the unit magnet of the laminated magnet should be 3 mm or less (preferably 2.5 mm or less), and the number of layers should be 4 or more, preferably 10 or more. as a laminate, 2) In order to reduce the machining cost to the utmost limit, the PLP method or NPLP method is diverted to form a Nd 2 Fe 14 B tetragonal compound in the c-axis direction in the main surface of the Nd-Fe-B thin plate-shaped sintered magnet. (Direction of easy magnetization) Oriented Nd-Fe-B thin plate sintered magnets are made directly without machining.
- Adhering unit magnets with a thickness of 3 mm or less produced by diverting the PLP method or NPLP method with an adhesive or pressing them by a hot press method to produce a laminated magnet.
- the unit magnet is subjected to grain boundary diffusion treatment to increase the coercive force.
- the grain boundary diffusion treatment is performed either before or after laminating the unit magnets.
- the surface layer containing a large amount of Nd generated during the production of the unit magnet is not completely removed, but at least a portion is left.
- the thickness of the unit magnet should be 3 mm or less in order to make the grain boundary diffusion effect uniform and strong throughout the magnet. 7) In order to increase the coercive force of the magnet to be produced, in the PLP or NPLP method, fine powder with an average particle size of 3 ⁇ m or around is used, The present invention has been completed by finding that the above problems can be solved.
- the present invention has the following configurations.
- a method for manufacturing an Nd-Fe-B laminated sintered magnet in which Nd-Fe-B thin plate-like sintered magnets are laminated via a high electrical resistance layer After supplying and filling the alloy powder into a mold having a structure partitioned by a plurality of partitions arranged at regular intervals, a magnetic field is applied in a direction parallel to the main surfaces of the cavities partitioned by the partitions. By applying voltage to orient the alloy powder and then sintering, the c-axis direction of the Nd 2 Fe 14 B tetragonal compound is aligned with the Nd-Fe-B thin plate sintered without performing a cutting step.
- the Nd-Fe-B thin plate-like sintered magnets are mutually interposed with a compound powder or alloy powder containing Dy and/or Tb interposed between the Nd-Fe-B thin plate-like sintered magnets.
- a plurality of the Nd-Fe-B thin plate sintered magnets are stacked and fixed in an injection mold, and then resin is injected into the mold to bond and mold.
- the Nd-Fe-B thin plate-like sintered magnet After feeding and filling alloy powder into a mold partitioned by a plurality of partitions arranged at regular intervals, the mold is oriented in a magnetic field in a direction parallel to the main surfaces of the cavities partitioned by the partitions. , Then, a method of conveying the mold as it is to a sintering furnace and sintering it, or After powdering and filling alloy powder into a mold having a structure partitioned by a plurality of partition plates arranged at regular intervals and having side walls divided into two or more sections to produce a filled compact.
- a magnetic field is applied in the direction of the main surface of the filled molded body to orient the alloy powder in the filled molded body to produce an oriented filled molded body; Any one of [1] to [9], wherein the oriented and filled compact is taken out from the mold and the taken out oriented and filled compact is sintered.
- Nd-Fe-B lamination sintering characterized by being a laminate obtained by laminating four or more layers of Nd-Fe-B thin plate-like sintered magnets with a thickness of 3 mm or less by adhesion or hot press crimping. magnet.
- the Nd-Fe-B thin plate sintered magnet is subjected to grain boundary diffusion treatment, and the Nd-Fe-B thin plate sintered magnet is adhered with an adhesive or pressed by hot pressing.
- the effects of the present invention are as follows. (1) After sintering the Nd--Fe--B sintered magnet, it is possible to produce a laminated magnet consisting of ultra-thin unit magnets without a cutting step. Therefore, it is possible to industrially produce laminated magnets composed of extremely thin unit magnets without producing a large amount of chips in the cutting process and without an expensive cutting process. (2) Nd-Fe-B laminated sintered magnets with magnetic uniformity and high magnetic properties can be industrially produced.
- FIG. 2 is a schematic diagram showing each step of the NPLP method (New-Press Less Process method) used in the production method of the present invention.
- FIG. 2 is a view showing a preferred example of a mold (used in Example 1) used in the production method of the present invention, showing a state when the mold is filled with alloy powder, and the upper view is a plan view. In the drawing on the lower side, the direction of the magnetic field during the orientation process is indicated by arrows together with the structure in the AA cross section in the drawing on the upper side.
- 1 is a photograph showing the appearance of a unit magnet produced in Example 1 of the present invention and a laminate produced by laminating them by hot pressing.
- FIG. 10 is a diagram showing a method of applying GBD (grain boundary diffusion) paste between unit magnets (processing-less sintered base materials), laminating them, and pressing them in Example 2;
- GBD grain boundary diffusion
- the present invention is a method for producing an Nd-Fe-B laminated sintered magnet in which Nd-Fe-B thin plate-like sintered magnets are laminated via a high electrical resistance layer.
- a schematic diagram of the NPLP method used in the manufacturing method is shown.
- a mold having a structure partitioned by a plurality of partition plates arranged at regular intervals is assembled, and alloy powder (magnetic alloy powder) is fed into the mold.
- the alloy powder is oriented by applying a magnetic field, and then sintered so that the c-axis direction of the Nd 2 Fe 14 B tetragonal compound changes to the Nd-
- a Nd-Fe-B thin plate-like sintered magnet that is oriented in the main surface of the Fe-B thin plate-like sintered magnet, has a high degree of orientation of 90% or more, and has a thickness of 3 mm or less.
- the cavities in the mold are separated by a plurality of partition plates arranged at regular intervals (preferably 1 mm to 5 mm, more preferably 1 mm to 3.5 mm), as shown in Figure 1.1.
- a mold having a structure divided into narrow cavities is prepared, and alloy powder is filled into a plurality of narrow cavities (cavities) separated by partition plates (mold assembly/powder filling). At this time, the packing density of the alloy powder is preferably 3.4 to 3.8 g/cc.
- FIG. 2 shows a structure that has a side wall (outer wall member) that is divided into two or more parts used in the manufacturing method of the present invention, and that the side wall of the mold can be removed after filling the alloy powder.
- a side wall outer wall member
- FIG. 2 shows a structure that has a side wall (outer wall member) that is divided into two or more parts used in the manufacturing method of the present invention, and that the side wall of the mold can be removed after filling the alloy powder.
- the structure of the mold used in the present invention is not limited to this, and a mold having a structure in which the side wall cannot be removed may be used.
- a plurality of cavities 5 are formed by arranging a plurality of partition plates 3 at regular intervals inside the mold formed from four side plates 1 and a bottom plate 2. Magnetic poles 4 are arranged perpendicularly to the partition plate 3 on the top side and the bottom side of the mold, respectively.
- the magnetic pole 4 is made of a ferromagnetic or ferrimagnetic substance, and has the effect of uniformizing the magnetic field applied to the alloy powder and aligning the orientation direction thereof. If it is made with , there is no need to remove it during sintering.
- the magnetic poles 4 are useful and desirable for improving the quality of the sintered body by aligning the orientation directions of the magnetic particles in the sintered body. .
- the mold is covered as shown in Figure 1-2, and a magnetic field H is applied in the direction of the arrow (from top to bottom) to orient the alloy powder filled in the cavity of the mold. to obtain an oriented filling compact.
- the magnetic field application direction is the direction in the main surface of the oriented filling compact (that is, the vertical direction), and the pulse magnetic field using the air-core coil can apply a stronger magnetic field than the static magnetic field using the electromagnet. .
- the crystal axes of the particles constituting the powder can be aligned in one direction, thereby improving the magnetic properties after sintering.
- the c-axis direction of the Nd 2 Fe 14 B tetragonal compound is oriented in the main surface of the Nd-Fe-B thin plate-like sintered magnet, and the degree of orientation is 90% or more.
- Nd-Fe-B thin plate-shaped sintered magnets having a degree of hardness and a thickness of 3 mm or less are produced. It is 3 tesla or more, and 3.5 tesla or more is required to obtain a high orientation with a ratio of remanent magnetization to saturation magnetization of 93% or more, and 4 tesla or more is necessary to obtain a high orientation of 95% or more.
- the charge stored in the capacitor bank is normally discharged in a short period of time, and a large current is passed through the normal conducting air-core coil to generate a high magnetic field. It is between
- the waveform of the pulse current may be a DC (one-way) pulse waveform or an AC decay waveform.
- pulsed magnetic fields having both DC pulse and AC pulse waveforms may be combined, or a high current may be passed through a high-temperature superconducting air-core coil to generate a high magnetic field.
- the magnetic field may be applied for 1 second or longer. However, considering the efficiency of the process, it is preferable that the magnetic field is applied for 10 seconds or less.
- a plurality of Nd--Fe--B sheet-like sintered magnets in which the c-axis direction of the Nd 2 Fe 14 B tetragonal compound is oriented in the main plane can be produced directly without machining.
- the sintering temperature and sintering time in the sintering step are appropriately determined based on the composition and particle size of the alloy powder.
- the sintering temperature is about 900-1100° C., and the typical sintering time is about 10-40 hours including the heating time.
- the production method of the present invention includes a step of laminating a plurality of (preferably four or more layers) of the Nd-Fe-B thin plate-shaped sintered magnets obtained above.
- the thin plate-like sintered magnets may be laminated by adhering to each other with an adhesive, or may be laminated by hot pressing.
- the following two types of modes can be mentioned as modes for crimping by hot pressing.
- At least 4 or more layers (for example, 10 or more layers) of thin-layer unit magnets are hot-pressed at a high temperature of 700°C or higher to produce a laminated magnet.
- At least 4 layers e.g.
- Nd- A method when laminating a plurality of (at least four layers) Nd-Fe-B thin plate sintered magnets to produce an Nd-Fe-B laminated magnet, simply Nd- A method may be used in which an adhesive such as epoxy resin is applied to the Fe--B thin plate sintered magnets to bond the unit magnets together for lamination. may be fixed in a mold in a layered state, and then a resin may be injected into the mold for adhesion.
- an adhesive such as epoxy resin
- the adhesive works to increase the electrical resistance between the layers.
- neodymium oxide can be applied to the thin plate magnets before hot pressing. It is valid.
- Tb or Dy oxide or fluoride powder is applied to the surface of the thin-plate magnet and hot-pressed, these powders not only act on the grain boundary diffusion effect of the magnet, but also increase the electrical resistance between the thin-plate magnets. was confirmed to work.
- the term "high electrical resistance layer” refers to an oxide film formed on the surface of a thin plate magnet, an adhesive to be applied, or the compound described above. , oxides formed on the surface of the thin plate, fluorides and oxides of Tb and Dy, or mixtures and reaction products of resin and silicon grease applied before hot pressing. These coated materials and reaction products formed during hot pressing act as a high electrical resistance layer. It is desirable that such a high electrical resistance layer be as thin as possible and have a high electrical resistivity.
- the thickness of the high electrical resistance layer is desirably 0.1 mm or less, more preferably 0.05 mm or less.
- the electrical resistance value measured with electrodes attached to both end faces of the laminated magnet is equal to the electrical resistance value measured with electrodes attached to both end faces of a single unlaminated magnet of the same size. is preferably 5 times or more, more preferably 10 times or more, and most preferably 100 times or more.
- each of the Nd-Fe-B thin plate-like sintered magnets is coated with a compound powder or alloy powder containing Dy and/or Tb. It is preferable to bond the Nd--Fe--B sheet-like sintered magnets to each other after the grain boundary diffusion treatment.
- the Nd-Fe-B thin plate-like sintered magnet is prepared by interposing a compound powder or alloy powder containing Dy and/or Tb between the Nd-Fe-B thin plate-like sintered magnets. are bonded or pressed together, and then subjected to grain boundary diffusion treatment.
- the compound powder or alloy powder containing Dy or Tb is suspended in an organic solvent such as ethyl alcohol and applied to the unit magnet.
- the coating amount is such that the heavy rare earth metal component contained in the coated powder is 0.5% or less of the weight of the unit magnet.
- Preferred compound powders or alloy powders containing Dy and/or Tb in the present invention include R 2 O 3 , R 4 O 7 , RF 3 where Dy and Tb are represented as R, or RF 3 and LiF (fluorine lithium compound), and the like.
- Preferred examples are hydride powder obtained by hydrogenating and pulverizing alloys of Dy and/or Tb with metal elements such as Fe, Ni and Al, or rare earth hydride powder represented by RH ⁇ .
- metal hydrides become dehydrogenated metal and alloy powders when heated to high temperatures above 800°C.
- the bonding layer it is desirable for the bonding layer to have a high electrical resistance, so the metal powder or metal hydride powder is used as a mixed powder with the aforementioned rare earth oxide or rare earth fluoride powder for forming the bonding layer.
- the present inventors have found that ultra-thin sintered magnets with a thickness of 3 mm or less, preferably 2.5 mm or less, and even thinner, up to a thickness of 0.8 mm can be obtained. It was confirmed that a magnet can be produced. Then, it was confirmed that a laminated magnet can be produced by laminating the sintered thin plate magnets thus produced without machining.
- Nd-Fe-B magnets are made into thin-plate magnets by cutting or machining by grinding using a whetstone. The cutting and grinding processes are very costly and generate a large amount of chips, resulting in a reduction in material yield. According to the manufacturing method of the present invention, a unit magnet can be manufactured without cutting or grinding, and the unit magnets manufactured in this way can be stacked to manufacture a laminated magnet.
- a laminated sintered magnet obtained by laminating four or more layers of Nd--Fe--B thin plate sintered magnets produced by the production method described above can be used, for example, in main motors of electric vehicles.
- the laminated sintered magnet of the present invention has a structure in which a plurality of Nd-Fe-B thin plate sintered magnets of the same quality are laminated.
- Nd-Fe-B thin plate sintered magnets need to be laminated, but for convenience when loading the magnets into the motor, it is preferable to laminate 4 or more layers.
- a practical number of layers is 10 or more.
- NPLP method new pressless process method in which the oriented filling compact is removed from the mold by separating, and the oriented filling compact taken out is sintered. Either method can be used.
- the Nd-Fe-B thin plate sintered magnet is produced using the PLP method or the NPLP method.
- a thin plate magnet can be obtained directly without going through a cutting process. Therefore, in the case of the Nd--Fe--B thin sheet sintered magnet produced by using the production method of the present invention, there is no degradation of magnetic properties due to machining, which has been well known in the past.
- the PLP method described in the present invention is shown in Japanese Patent No. 4391897, etc.
- the NPLP method is shown in Japanese Patent No. 6280137.
- the magnetization direction is perpendicular to the main surface (plate surface) of the magnet. , in the thickness direction of the magnet.
- the manufacturing process of the thin plate magnet as a unit magnet that constitutes the laminated magnet is almost the same as the above-mentioned PLP method and NPLP method, but the manufacturing process of the thin plate magnet for use in the laminated magnet of the present invention.
- the magnetization direction in the process is the direction within the main surface of the magnet (the direction parallel to the main surface).
- an oxide film is formed on the surface of the thin plate magnets produced by the PLP method or the NPLP method, and this naturally formed oxide film is effective in increasing the electrical resistance between the thin plate magnets.
- the present inventors have found that the surface layer containing a large amount of Nd has the effect of suppressing deterioration of the magnetic properties of the thin plate magnet, and found that the coercive force of the magnet is reduced if this surface layer is removed. confirmed. Therefore, in the present invention, the surface layer containing a large amount of Nd generated during the sintering process is effectively used without being completely stripped off, and the surface of the Nd-Fe-B thin plate-shaped sintered magnet is covered with the sintering process. It is preferable to laminate the Nd--Fe--B thin plate-like sintered magnets while leaving at least a part of the surface layer containing a large amount of Nd generated therein.
- “during the sintering process” includes the process of raising the temperature, maintaining the sintering temperature, and cooling in the sintering furnace. It is presumed that the Nd-rich surface layer formed on the surface of the unit magnet is produced during this sintering process.
- a relatively large block of sintered magnet bodies was manufactured to manufacture a thin plate, and then a thin plate-shaped magnet was obtained mainly by cutting. do not have.
- the expression "without a cutting step” means that a thin plate-like sintered magnet is obtained directly, not by cutting the block sintered body.
- Nd-Fe-B sintered magnet in the present invention uses the well-known notation of "Nd-Fe-B", but it does not have only Nd, Fe, and B elements as constituent elements.
- Nd represents a rare earth element containing Y and Sc, specifically Y, Sc, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Yb and Lu, one or two of them Species and above.
- Nd, Pr, Dy, and Tb are preferably the main constituents.
- These rare earth elements including Y and Sc preferably account for 10 to 15 atomic percent, particularly 12 to 15 atomic percent, of the entire alloy.
- the content of B is preferably 3 to 15 atomic %, particularly 4 to 8 atomic %.
- W may be contained in 0 to 11 atomic %, particularly 0.1 to 5 atomic %.
- the balance is Fe and unavoidable impurities such as C, N, O, etc.
- Fe is preferably contained in an amount of 50 atomic % or more, particularly 65 atomic % or more. Also, part of Fe, for example 0 to 40 atomic %, especially 0 to 15 atomic % of Fe, may be replaced with Co.
- the Nd-Fe-B laminated sintered magnet of the present invention in which the Nd-Fe-B thin plate-shaped sintered magnets manufactured by the PLP method or the NPLP method are laminated by adhesion or pressure bonding (welding) by hot pressing, contains Nd
- the c-axis direction of the 2Fe14B tetragonal compound is oriented in the main plane of the Nd - Fe-B thin plate-like sintered magnet, and the degree of orientation (the value obtained by dividing the residual magnetic flux density Br by the saturation magnetization Js Nd-Fe-B thin plate sintered magnets with a high degree of orientation of 90% or more and a thickness of 3 mm or less are laminated, preferably 4 or more, particularly preferably 10 or more. It is characterized by being a laminated body.
- the Nd-Fe-B thin plate-like sintered magnet is subjected to grain boundary diffusion treatment, and the Nd-Fe-B thin plate-like sintered magnet is laminated by bonding with an adhesive.
- an adhesive layer is present between the Nd-Fe-B thin plate-like sintered magnets, which is formed by hot-pressing compound (e.g., oxide) powder or alloy powder containing Dy and/or Tb.
- hot-pressing compound e.g., oxide
- the Nd--Fe--B thin plate-shaped sintered magnets are laminated by being adhered to each other by this adhesive layer, and such an adhesive layer functions as a high electrical resistance layer.
- the above-mentioned high electrical resistance layers include the gaps between thin plate magnets, adhesive layers, oxide films or oxygen-rich films formed during the manufacturing of unit magnets, and Dy and Tb coatings applied for grain boundary diffusion treatment.
- a layer made of oxides, fluorides, or their altered substances does this.
- a Nd-Fe-B laminated sintered magnet consisting of ultra-thin unit magnets can be produced without a cutting step, and this laminated sintered magnet is magnetically uniform and has a high density. It has magnetic properties and is useful not only as a magnet for electric vehicles but also as a magnet for various industrial and domestic motors.
- Example 1 A mold as shown in FIG. 2 was produced.
- the material of this mold is stainless steel (SUS304), reference numeral 1 in FIG. 2 denotes a side plate, 2 a bottom plate, 3 a partition plate, 4 a magnetic pole, 5 a cavity, and 6 a lid.
- SUS304 stainless steel
- reference numeral 1 in FIG. 2 denotes a side plate, 2 a bottom plate, 3 a partition plate, 4 a magnetic pole, 5 a cavity, and 6 a lid.
- the SC alloy having the above composition was subjected to hydrogen pulverization and pulverized to an average particle size D50 of 3 ⁇ m by a nitrogen jet mill. This jet-milled powder was then packed into the mold shown in FIG. 2 at a packing density of 3.5 g/cm 3 .
- the mold was inserted into an orientation coil, and a pulse magnetic field of 4 Tesla was applied in the direction of the arrow in FIG. 2 to orient the alloy powder.
- the mold used this time has 28 cavities, and each cavity has a width (called a) of 18.2 mm, a height (called b) of 10.8 mm, and a gap width (called c) of 2.35 mm. be.
- Each cavity is separated by a partition plate, which is made of stainless steel and has a thickness of 0.5 mm.
- the total amount of alloy powder was 45.27 g, and 1.616 g was precisely weighed and supplied to each cavity. After that, the magnetic pole, the lid and the side plate were removed from the mold in order, and the alloy powder molded body including the partition plate was transferred to the carbon plate and loaded into the vacuum sintering furnace. In this way, an in-plane oriented thin plate magnet was produced.
- This thin plate magnet is a unit that constitutes a laminated magnet.
- the sintering conditions are as follows. After evacuating to 1 ⁇ 10 ⁇ 3 Pa or less, the temperature was raised to 400° C. at a heating rate of 1° C./min in vacuum, and then held at 400° C. for 9 hours. Further, the temperature was raised to 1000°C at a heating rate of 2°C/min, held at 1000°C for 3 hours, and then cooled in the furnace to obtain a thin Nd-Fe-B sintered magnet.
- the degree of orientation (Br/Js) of the unit magnet obtained by the above sintering was 95% or more, and it was confirmed that the degree of orientation was high.
- Tb 2 O 3 powder having an average particle size of 5 ⁇ m was applied to the upper and lower surfaces of the unit magnet immediately after sintering.
- the coating amount was 0.5% of the weight of the unit magnet, the powder was suspended in liquid paraffin, and the suspension was applied to the unit magnet.
- Fifteen unit magnets coated with the Tb 2 O 3 powder in this manner were stacked and hot-pressed to produce a laminated magnet.
- Fifteen of these unit magnets were laminated, loaded into a graphite split mold, and hot-pressed to produce the Nd--Fe--B laminated sintered magnet of the present invention.
- the hot press conditions were 750° C. and 40 MPa pressure in vacuum for 10 minutes.
- FIG. 3 shows a photograph showing the appearance of the unit magnets produced in Example 1 and a laminate produced by laminating them and producing them by hot pressing. After heat-treating the hot-press laminate thus produced at 800° C. for 1 hour and at 500° C. for 1 hour, a 7 mm square cube was cut out and subjected to magnetic measurement. Table 2 shows the results.
- Example 2 Five unit magnets prepared by the method of Example 1 were prepared, and TbF 3 powder (GBD paste) was placed between the unit magnets (processing-less sintered base materials) as shown in FIG. It was applied to the upper and lower surfaces of the unit magnet so that the Tb weight was 0.3% with respect to the total weight of the magnet.
- a stainless block having a weight of 5 kg was placed on the five laminates, placed in a vacuum furnace, and the laminate was heat-treated in vacuum at 900° C. for 10 hours. After that, heat treatment was performed at 500° C. for 1 hour.
- a 7 mm square thin plate was cut out from one of the unit magnets subjected to the above heat treatment, and the magnetic properties were measured. Table 3 shows the results.
- Example 3 Five unit magnets prepared in Example 1 were prepared and chamfered to remove burrs. Then, a long-curing two-liquid epoxy resin was evenly applied to both sides of each unit magnet using a spatula. After coating, five sheets were superimposed and a weight of about 500 g was placed thereon to cure. At this time, in order to shorten the curing time, it was placed in an oven at 90° C., held for 1 hour, and then taken out to produce the Nd—Fe—B laminated sintered magnet of the present invention.
- Example 4 Using the same alloy and the same powder as in Example 1, a unit magnet was produced in the same manner. A portion of this unit magnet was polished with sandpaper to a thickness of 0.1 mm. Then, all the magnets were subjected to a heat treatment in which they were held at 800°C for 1 hour and then quenched, and further held at 500°C for 1 hour and then quenched. Using these two types of unit magnets (polished and unpolished), laminated magnets were produced by laminating 5 sheets each by bonding with epoxy resin.
- the coercive force Hcj of the laminated magnet (comparative product) produced from the unit magnet with no mechanical processing is compared to the laminated magnet (comparative product) produced from the unit magnet with the entire surface polished. It was found that the product of the present invention was larger by 1 kOe or more.
- Nd-Fe-B thin plate magnets produced by the NPLP method have a surface layer rich in Nd, and this surface layer suppresses the magnetic deterioration of the crystal grains near the surface of the magnet. It is presumed that That is, in the normal method of manufacturing Nd-Fe-B sintered magnets by pressing, a thin plate magnet is produced by cutting out a large block magnet, so there is no Nd-rich surface layer on the surface of this thin plate magnet. Therefore, it is considered that the coercive force of the laminated magnet produced from the thin plate magnet obtained by cutting the block magnet is lower by about 1 kOe.
- This Example 4 proved that the Nd--Fe--B laminated magnet produced by the production method of the present invention is more advantageous in terms of magnetic properties than the laminated magnet produced by the conventional method.
- Example 5 Using the same Nd-Fe-B alloy powder as in Example 1, the width a and height b of the mold in FIG. Three types of unit magnets with thicknesses of 2 mm, 3 mm, and 5 mm were produced. Using these unit magnets and under the same conditions as in Example 1, a hot-press laminate was produced by stacking five unit magnets. Further, the same unit magnet was subjected to grain boundary diffusion treatment with TbF 3 under the same conditions as in Example 2 to produce unit magnets, and five of these were bonded with a resin to produce a laminated magnet. Table 4 shows the results of measuring the AC resistance values of these hot-pressed laminated magnets and resin-bonded laminated magnets.
- the AC resistance value was measured by winding a coil around each magnet for 50 turns and changing the frequency of the alternating magnetic field with a HIOKI IM3536LCR meter.
- Table 4 shows the results at a measurement current of 1 mA and a frequency of 30 kHz.
- Example 6 A unit magnet was produced from the SC alloy having the composition shown in Table 5 by the method of Example 1. An oxide film (high electrical resistance layer) is formed on the surface of this unit magnet by sintering, and this unit magnet is used to manufacture a laminated magnet in which 24 layers of unit magnets are stacked in the same manner as in Example 1. did. However, here, the laminated magnet was produced by hot-pressing 24 layers of the laminated body with nothing sandwiched between the unit magnets. The hot press conditions were a maximum temperature of 850°C, a maximum pressure of 65 MPa, and a holding time of 20 minutes. The obtained laminated magnet was subjected to aging treatment in vacuum at 800°C for 30 minutes and then at 520°C for 1 hour.
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Abstract
Description
従来のプレス法では、次工程である焼結工程への搬送のために充分な強度を有する粉末圧縮成形体を作製する必要があるために、プレス法により、高配向された薄板状圧粉体を製造することは困難であった。これに対し、PLP法ではモールドごと粉末配向成形体を搬送することで、薄板状磁石が直接工業的に製造できるようになった。
その後、モールドにふたをして、磁界を印加して、磁石合金粉末を配向する。磁界印加方向は、狭い空洞の主面に垂直な方向である。その後、モールドと粉末成型配向体を焼結用台板に移し替える時にモールドの外壁を取り除き、モールド内部に形成された多層の粉末・仕切り板からなる粉末・仕切り板積層体だけを焼結台板上に残す。そして、この焼結台板上に残された粉末・仕切り板積層体を焼結炉の中で加熱することにより、複数の薄板状焼結体が製造される。
焼結磁石の製造に使用されるモールドは、ある程度の精度が要求される材質で作製されるが、1000℃以上の高温の焼結温度に何度も曝されると、モールドが消耗するため、PLP法ではモールドのコストがかかるという問題があったが、NPLP法の場合には、モールドを燒結炉内に入れないので、モールドコストの問題が解消される。
これらの理由により、現状のEV用主機モータに使われるNd-Fe-B焼結磁石には、基材中にTbやDyを2~3%以上入れた材質のNd-Fe-B焼結磁石が使われるが、TbやDyは希土類鉱石中に少ししか含まれない。
EV、HEVに使われるNd-Fe-B磁石において、TbやDyの使用量は、豊富な希土類鉱石として知られるモナザイトやバステナサイト中に含まれる成分限界内に抑えることが強く望まれており、その限界はNd-Fe-B磁石重量の0.5%である。
1)磁石内に発生する渦電流損失を極限まで下げるために、積層磁石のユニット磁石の厚さを3mm以下(好ましくは2.5mm以下)にし、積層数を4層以上、好ましくは10層以上の積層体とする、
2)機械加工コストを極限まで下げるために、PLP法またはNPLP法を転用して、Nd-Fe-B薄板状焼結磁石の主面内に、Nd2Fe14B正方晶化合物のc軸方向(磁化容易方向)が配向されたNd-Fe-B薄板焼結磁石を、機械加工なしに直接作る、
3)PLP法またはNPLP法を転用して作製された厚さ3mm以下のユニット磁石を接着剤により接着し、またはホットプレス法により圧着して、積層磁石を製作する、
4)ユニット磁石には必要に応じて、高保磁力化のために、粒界拡散処理を施す。粒界拡散処理は、ユニット磁石を積層する前、または積層化した後のどちらかで行う、
5)積層磁石の低コスト化のためと、積層磁石としての性能向上のために、ユニット磁石作製中に生成されたNdを多く含む表面層は全部はぎとらずに、少なくとも一部残した状態で、積層化または粒界拡散処理をする、
6)粒界拡散効果を磁石全体に均一に強く効かせるために、ユニット磁石の厚さを3mm以下にする、
7)製造する磁石の保磁力を高めるために、PLP法またはNPLP法において、平均粒径3μmまたはその前後の粒径の微細粉末を使用する、
ことによって、上記の課題が解決できることを見出して、本発明を完成した。
〔1〕Nd-Fe-B薄板状焼結磁石が高電気抵抗層を介して積層されてなるNd-Fe-B積層焼結磁石を製造する方法であって、
一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填した後、前記仕切り板により区切られた空洞の主面と平行な方向に磁界を印加して前記合金粉末を配向させ、その後、焼結を行うことにより、切断工程を行うことなく、Nd2Fe14B正方晶化合物のc軸方向が、前記Nd-Fe-B薄板状焼結磁石の主面内に配向され、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石を製造する工程、および
前記工程で得られたNd-Fe-B薄板状焼結磁石を複数枚積層する工程
を含むことを特徴とする、Nd-Fe-B積層焼結磁石の製造方法。
〔2〕前記Nd-Fe-B薄板状焼結磁石の表面に、前記焼結中に生成されたNdを多く含む表面層を少なくとも一部残したまま、前記Nd-Fe-B薄板状焼結磁石を積層することを特徴とする、〔1〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔3〕前記Nd-Fe-B薄板状焼結磁石を互いに接着して積層することを特徴とする、〔1〕または〔2〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔4〕前記Nd-Fe-B薄板状焼結磁石をホットプレスによって圧着することを特徴とする、〔1〕または〔2〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔5〕前記Nd-Fe-B薄板状焼結磁石のそれぞれにDyおよび/またはTbを含む化合物粉末または合金粉末を塗布して粒界拡散処理を施したあと、前記Nd-Fe-B薄板状焼結磁石を互いに接着することを特徴とする、〔1〕または〔2〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔6〕前記Nd-Fe-B薄板状焼結磁石の間に、Dyおよび/またはTbを含む化合物粉末または合金粉末を介在させた状態で、前記Nd-Fe-B薄板状焼結磁石を互いに接着または圧着して、その後、粒界拡散処理を施すことを特徴とする、〔1〕または〔2〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔7〕前記Nd-Fe-B薄板状焼結磁石を、接着剤を用いて互いに接着することを特徴とする〔3〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔8〕複数の前記Nd-Fe-B薄板状焼結磁石を射出成型金型内に積層した状態にて固定し、その後、当該金型内に樹脂を注入して接着し成形することを特徴とする〔3〕に記載のNd-Fe-B積層焼結磁石の製造方法。
〔9〕前記Nd-Fe-B薄板状焼結磁石を10層以上積層することを特徴とする〔1〕~〔8〕のいずれか1項に記載のNd-Fe-B積層焼結磁石の製造方法。
〔10〕前記Nd-Fe-B薄板状焼結磁石を、
一定間隔を開けて配列された複数の仕切り板により仕切られたモールド内に合金粉末を給粉・充填した後、前記仕切り板により区切られた空洞の主面と平行な方向に磁界中配向を施し、その後、モールドのまま焼結炉に搬送して焼結を行う方法、または、
2分割以上に分割された側壁を有し、一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填して充填成形体を作製した後、前記充填成形体の主面内の方向に磁界を印加し、該充填成形体内の合金粉末を配向させ配向充填成形体を作製し、その後、前記モールドの側壁を前記配向充填成形体から引き離して前記配向充填成形体を前記モールドから取り出し、取り出した前記配向充填成形体を焼結する方法
のいずれかの方法を用いて製造することを特徴とする〔1〕~〔9〕のいずれか1項に記載のNd-Fe-B積層焼結磁石の製造方法。
〔11〕Nd2Fe14B正方晶化合物のc軸方向が、前記Nd-Fe-B薄板状焼結磁石の主面内に配向されており、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石が4層以上、接着またはホットプレス圧着により積層された積層体であることを特徴とするNd-Fe-B積層焼結磁石。
〔12〕前記Nd-Fe-B薄板状焼結磁石に粒界拡散処理が施されており、該Nd-Fe-B薄板状焼結磁石が接着剤により接着され、またはホットプレスにより圧着されて積層されていることを特徴とする、〔11〕に記載のNd-Fe-B積層焼結磁石。
(1)Nd-Fe-B焼結磁石を焼結後、切断工程なしで、極薄のユニット磁石からなる積層磁石を製造することができる。そのため、切断工程による多量の切りくずを生成しないで、かつ高価な切断工程なしで、極めて薄いユニット磁石からなる積層磁石を工業的に生産できる。
(2)磁気的に均一で高い磁気特性を持つNd-Fe-B積層焼結磁石が工業的に生産できる。
本発明の製造方法における最初の工程では、一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールドを型組し、当該モールド内に合金粉末(磁石合金粉末)を給粉・充填した後、磁界を印加して前記合金粉末を配向させ、その後、焼結を行うことにより、切断工程を行うことなく、Nd2Fe14B正方晶化合物のc軸方向が、前記Nd-Fe-B薄板状焼結磁石の主面内に配向され、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石を製造する。
この工程においては、図1の1.に示されるような、モールド内の空洞が、一定間隔(好ましくは1mm~5mm、より好ましくは1mm~3.5mm)を開けて配置された複数の仕切り板によって狭い空洞に分割された構造を有するモールドを準備し、この仕切り板によって区切られた複数の狭い空洞(キャビティ)内に合金粉末を充填する(型組・粉末充填)。この際、合金粉末の充填密度は3.4~3.8g/ccであることが好ましい。
図2に例示したモールドは、4枚の側板1と底板2から形成されたモールドの内部に複数の仕切り板3が一定間隔をあけて配置されることにより複数のキャビティ5が形成されており、モールドの上面側と底面側にはそれぞれ、仕切り板3と垂直に、磁極4が配置されている。この磁極4は、強磁性体またはフェリ磁性体物質からなり、合金粉末にかかる磁界を均一化して、その配向方向を揃える効果を有しており、鉄やケイ素鋼などの焼結により変形しない素材で作っておけば、焼結の際、取り外す必要がない。又、この磁極4は、焼結体中の磁性粒子の配向方向を揃えて、焼結体の品質向上に有用で望ましいが、磁極がなくても配向の乱れが無視できる場合には必要ではない。
本発明の製造方法では、Nd2Fe14B正方晶化合物のc軸方向が、Nd-Fe-B薄板状焼結磁石の主面内に配向されており、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石が製造されるが、このような薄板状焼結磁石を製造するための印加磁界の強さの望ましい範囲は3テスラ以上であり、飽和磁化に対する残留磁化の比率が93%以上の高配向を得るためには3.5テスラ以上、さらに95%以上の高配向を得るためには4テスラ以上が必要である。
本発明では、通常、コンデンサーバンクに貯めた電荷を短時間に放電して、常電導空芯コイルに大電流を流して高磁界を発生し、1回のパルス磁界の幅は通常1msから1秒までの間である。パルス電流の波形としては直流(一方向)のパルス波形でも、交流減衰波形でもよい。本発明では、直流パルスと交流パルスの両者の波形のパルス磁界を組み合わせてもよく、高温超電導空芯コイルに大電流を流して高磁界を発生してもよい。この際、超電導では、あまり短時間の電流変化は難しいので、1秒以上の磁界印加でもよい。しかし、工程の能率を考慮して、磁界を印加する時間は10秒以下であることが望ましい。
その後、図1の4.に示すようにして、焼結台板上の粉末・仕切り板積層体を焼結炉に入れて焼結を行うことにより、Nd-Fe-B薄板状焼結磁石の主面内に、Nd2Fe14B正方晶化合物のc軸方向が配向された複数のNd-Fe-B薄板状焼結磁石を直接、機械加工を行うことなく製造できる。
本発明では、焼結工程を行う際の焼結温度と焼結時間は、合金粉末の組成や粒径を元に適宜定められるが、Nd-Fe-B系焼結磁石の場合の典型的な焼結温度は900~1100℃程度であり、典型的な焼結時間は、昇温時間を含めて10~40時間程度である。
この際、ホットプレスによる圧着を行う場合の態様としては、次の2種類の態様が挙げられる。
(1)少なくとも4層以上(例えば10層以上)段積みした薄層ユニット磁石をホットプレスにより、700℃以上の高温で、単に圧着して積層磁石を作る。
(2)ホットプレス装置内に、少なくとも4層以上(例えば10層以上)段積みした薄層ユニット磁石を金型内に配置し、700℃以上の高温で、段積みした薄板状磁石を上下パンチにより圧縮して、薄層ユニット磁石を圧縮方向と垂直な方向に変形させて金型内面に押し付け、積層体の形状および寸法を整える。
本明細書における「高電気抵抗層」とは、薄板磁石の表面に形成されている酸化物膜や、塗布される接着剤や上記の化合物からなり、さらにホットプレス法で接着される場合には、薄板表面に形成された酸化物、TbやDyのフッ化物や酸化物、あるいはホットプレス前に塗布された樹脂やシリコングリスの混合物や反応生成物からなる。これらの塗布された物質やホットプレス中に形成される反応生成物が高電気抵抗層として働く。このような高電気抵抗層はできるだけ薄くて高電気抵抗率をもつことが望ましい。高電気抵抗層の厚さは、0.1mm以下が望ましく、0.05mm以下がさらに好ましい。そしてこれらの高電気抵抗層によって、積層磁石両端面に電極を付けて測定した電気抵抗値が、同じ大きさの積層していないひと固まりの磁石について両端面に電極を付けて測定した電気抵抗値の5倍以上が好ましく、10倍以上がさらに好ましく、100倍以上が最も好ましい。
又、本発明では、前記Nd-Fe-B薄板状焼結磁石の間に、Dyおよび/またはTbを含む化合物粉末または合金粉末を介在させた状態で、Nd-Fe-B薄板状焼結磁石を互いに接着または圧着し、その後、粒界拡散処理を施すことが好ましい。
この際、DyやTbを含む化合物粉末または合金粉末は、エチルアルコールなどの有機溶媒に懸濁させてユニット磁石に塗布する。塗布量は、塗布される粉末中に含まれる重希土類金属成分が、ユニット磁石の重量の0.5%以下とすることが資源的な観点から好ましい。又、上記の粒界拡散処理は、これらのDyやTbを含む化合物粉末を塗布したユニット磁石を重ねて真空中または不活性ガス中、800~900℃で、5~20時間加熱することにより行われ、その後、これらのユニット磁石を接着またはホットプレスによる圧着により、積層磁石を製作する。
DyやTbを含む化合物粉末を塗布したユニット磁石をホットプレスにより圧着して積層磁石を製作する場合には、粒界拡散効果を高めるため、ホットプレス後に、800~900℃で5~20時間の長時間加熱を行うことが好ましい。
本発明にて好ましい上記のDyおよび/またはTbを含む化合物粉末または合金粉末としては、DyやTbをRと表してR2O3、R4O7、RF3、あるいはRF3とLiF(フッ化リチウム)の混合物等が挙げられる。またDyおよび/またはTb とFe、Ni、Alなどの金属元素との合金が水素化されて粉砕された水素化物粉末、またはRHδで表される希土類水素化物の粉末も好ましい例である。これらの金属水素化物は、800℃以上の高温に加熱されると、脱水素された金属や合金粉末になる。積層磁石としては、接合層の電気抵抗が高いことが望ましいので、金属粉末または金属水素化物粉末は上述の、希土類酸化物や希土類フッ化物の粉末との混合粉末として、接合層形成に用いられる。
これまでの技術では、Nd-Fe-B磁石は、切断加工や、砥石を使った研削加工による機械加工により薄板状磁石が作られる。切断加工や、研削加工には多大なコストがかかる上に、多量の切りくずが発生して、材料歩留まりが低下することが問題であった。本発明の製造方法では、切断や研削加工を加えることなくユニット磁石を作ることができ、このようにして作ったユニット磁石を積層して、積層磁石を作ることができる。
本発明の積層焼結磁石は、同質のNd-Fe-B薄板焼結磁石が複数積層された構造を有するものであり、本発明が目的とする渦電流低減の効果を得るには、複数枚のNd-Fe-B薄板焼結磁石が積層される必要があるが、モータに磁石を装填するときの利便性から、積層枚数は4層以上が好ましく、電気自動車の主機モータ用としては、積層枚数は10層以上が実用的である。
この時、モータ運転中の渦電流損を減らすために、薄板焼結磁石どうしを、高電気抵抗層を介して積層する必要がある。高電気抵抗層の電気抵抗値は、電気絶縁に近い高抵抗である必要がないことが知られている。
a)一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填した後、前記仕切り板により区切られた空洞の主面と平行な方向に磁界中配向を施し、その後、モールドのまま焼結炉に搬送して焼結を行うプレスレスプロセス法(PLP法)、または、
b)2分割以上に分割された側壁を有し、一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填して充填成形体を作製した後、前記充填成形体の主面内の方向に磁界を印加し、該充填成形体内の合金粉末を配向させ配向充填成形体を作製し、その後、前記モールドの側壁を前記配向充填成形体から引き離して前記配向充填成形体を前記モールドから取り出し、取り出した前記配向充填成形体を焼結するニュープレスレスプロセス法(NPLP法)
のいずれかの方法を用いることができる。
そのため、本発明では、焼結工程中に生成されたNdを多く含む表面層を全部はぎ取ってしまわずに有効に活用し、Nd-Fe-B薄板状焼結磁石の表面に、その焼結工程中に生成された、Ndを多く含む表面層を少なくとも一部残したまま、Nd-Fe-B薄板状焼結磁石を積層することが好ましい。
また、本発明では、Nd-Fe-B薄板状焼結磁石の間に、Dyおよび/またはTbを含む化合物(例えば酸化物)粉末または合金粉末をホットプレス圧着して形成された接着層が存在し、この接着層によって、Nd-Fe-B薄板状焼結磁石が互いに接着されて積層されていることが好ましく、このような接着層は高電気抵抗層として機能する。
図2に示されるモールドを作製した。このモールドの材質はステンレス(SUS304)であり、図2中の符号1は側板であり、2は底板、3は仕切り板、4は磁極、5はキャビティ、6は蓋である。
そして、Nd-Fe-B焼結磁石を作製するための出発合金(ストリップキャスト合金=SC合金)として、以下の表1に記載される組成を有した合金粉末を準備した。
なお、今回使用したモールドは28個のキャビティを有し、各キャビティのサイズは幅(aと呼ぶ)18,2mm、高さ(bと呼ぶ)10.8mm、ギャップ幅(cと呼ぶ)2.35mmである。尚、各キャビティは仕切り板にて隔てられており、仕切り板はステンレス製で、厚さはいずれも0.5mmである。
上記の合金粉末を給粉する際、各キャビティに給粉される合金粉末の重量が均一になるように、個々のキャビティごとに秤量して、各キャビティに給粉した。
このようにして面内配向した薄板磁石を作製した。この薄板磁石は積層磁石を構成するユニットとなるものである。
上記の焼結によって得られたユニット磁石の配向度(Br/Js)は95%以上であり、高配向度を有していることが確認された。
このユニット磁石15枚を積層してグラファイト製の割型に装填し、ホットプレスを行い、本発明のNd-Fe-B積層焼結磁石を製造した。尚、割型の内寸は製品寸法を想定してa=16.0mm、b=7.2mmとした。ホットプレス条件は、真空中で、750℃、40MPaの加圧下で、10分間保持とした。
次に、この積層磁石の寸法を評価したところa=16.0mm、b=7.2mm、c'(積層厚み)=28.1mmであり、aおよびbの寸法は割型の内寸と同一であることから積層されたユニット磁石は、ホットプレス中に接合と同時に型内壁に向って変形し、内壁に到達した後に変形が停止したと考えられ、加工を一切加えることなく、設計通りの寸法を持つ積層一体化磁石を実現できることが判明した。
この実施例1で作製された、ユニット磁石と、これらを積層してホットプレスにより作製された積層体の外観を示す写真が、図3に示されている。
このようにして作製したホットプレス積層体を800℃で1時間、500℃で1時間熱処理したのち、7mm角の立方体を切り出して磁気測定を行った。その結果を表2に示す。
前記実施例1の方法で作製したユニット磁石を5枚準備し、図4に示されるようにして、ユニット磁石(加工レス焼結基材)間にTbF3粉末(GBDペースト)をユニット磁石5枚の全体重量に対してTb重量が0.3%になるようにユニット磁石上下面に塗布した。この5枚の積層体の上に、重さ5kgのステンレス製ブロックを載せて真空炉内に配置し、この積層体を真空中900℃で10時間熱処理した。その後、500℃で1時間の熱処理を行った。
上記の熱処理を行ったユニット磁石の1枚から7mm角の薄板を切り出し、磁気特性の測定を行った。その結果を表3に示す。
前記実施例1にて作製したユニット磁石を5枚用意し、バリ除去のための面取り加工を行ったのち、各ユニット磁石の両面に長時間硬化タイプの2液性エポキシ樹脂を均等にスパチュラにて塗布した上で5枚を重ね合わせて500g程度の重りを載せて硬化させた。この際、硬化時間を短縮するため90℃のオーブンに入れて1時間保持したのち取り出し、本発明のNd-Fe-B積層焼結磁石を製造した。
又、上記で作製した積層磁石の渦電流損失を測定した。比較のために、上記積層磁石と同一サイズの一体型磁石(ブロック状磁石)を併せて作製して同様に測定に供した。
更に、空芯コイル中央に供試磁石を置き、周波数100から50kHzの範囲で20mAの交流磁界を印加した場合のコイルの交流抵抗Rsを測定した。又、同一サイズの一体型磁石も同一条件にてコイルの交流抵抗Rsを測定し、両者を比較した。
その結果、作製した積層磁石は一体型磁石に対して、コイルの交流抵抗Rsが24.7%であることが判明し、大きな渦電流低減効果を示すことが確認された。
前記実施例1と同じ合金、同じ粉末を使って同じ方法でユニット磁石を作製した。このユニット磁石の一部はサンドペーパにより全面0.1mm研磨した。そして、全部の磁石について、800℃で1時間保持してから急冷し、さらに500℃で1時間保持してから急冷する熱処理を加えた。これら2種類のユニット磁石(研磨あり、研磨なし)を用いて、それぞれ5枚ずつ積層した積層磁石をエポキシ樹脂による接着によって作製した。
その結果、磁気特性の平均値は、全面研磨を行ったユニット磁石を積層して得られた積層磁石(比較品)については、残留磁束密度Br=14.1kGであり、保磁力Hcj=14.8kOeであった。一方、機械加工を行っていないユニット磁石を積層して得られた積層磁石(本発明品)については、Br=14.4kGで、Hcj=16.1kOeであった。両積層磁石のBrの差はあまりないが、保磁力Hcjについては、全面研磨したユニット磁石で作製した積層磁石(比較品)に比べて、機械加工を一切加えないユニット磁石で作製した積層磁石(本発明品)の方が1kOe以上大きいことが判明した。
この実施例4により、本発明の製造方法により作製されたNd-Fe-B積層磁石は、従来法により作製される積層磁石より磁気特性の面でも有利であることが立証された。
実施例1と同じNd-Fe-B合金粉末を使用し、図2のモールドで幅aと高さbは実施例1と同じで、ギャップ幅cだけを変えて、焼結後の焼結体厚みが2mm、3mm、5mmの3種類の厚みのユニット磁石を作製した。これらのユニット磁石を使用して、実施例1と同じ条件で、ユニット磁石5枚を重ねたホットプレス積層体を作製した。さらに、同じユニット磁石に実施例2と同じ条件で、TbF3による粒界拡散処理を施したユニット磁石を作製して、これを5枚、樹脂により接着して、積層磁石を作製した。
これらのホットプレス積層磁石、および樹脂接着積層磁石の交流抵抗値を測定した結果を表4に示す。交流抵抗値は各磁石の周囲にコイルを50ターン巻き、HIOKI製IM3536LCRメータで交番磁界の周波数を変化させながら測定した。測定電流1mA、周波数30kHzにおける結果を表4に示す。
表5に示す組成のSC合金から実施例1の方法で、ユニット磁石を作製した。このユニット磁石の表面には、焼結により酸化膜(高電気抵抗層)が形成されており、このユニット磁石を使用して実施例1の方法で24層のユニット磁石を重ねた積層磁石を作製した。ただし、ここではユニット磁石間には何も挟まない積層体24層をホットプレスすることにより積層磁石を作製した。ホットプレス条件は最高温度850℃、最大加圧力65MPa、保持時間20分であった。得られた積層磁石を真空中で800℃×30min.、引き続いて520℃×1時間時効処理を施した。
2 底板
3 仕切り板
4 磁極
5 キャビティ
6 蓋
Claims (12)
- Nd-Fe-B薄板状焼結磁石が高電気抵抗層を介して積層されてなるNd-Fe-B積層焼結磁石を製造する方法であって、
一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填した後、前記仕切り板により区切られた空洞の主面と平行な方向に磁界を印加して前記合金粉末を配向させ、その後、焼結を行うことにより、切断工程を行うことなく、Nd2Fe14B正方晶化合物のc軸方向が、前記Nd-Fe-B薄板状焼結磁石の主面内に配向され、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石を製造する工程、および
前記工程で得られたNd-Fe-B薄板状焼結磁石を複数枚積層する工程
を含むことを特徴とする、Nd-Fe-B積層焼結磁石の製造方法。 - 前記Nd-Fe-B薄板状焼結磁石の表面に、前記焼結中に生成されたNdを多く含む表面層を少なくとも一部残したまま、前記Nd-Fe-B薄板状焼結磁石を積層することを特徴とする、請求項1に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石を互いに接着して積層することを特徴とする、請求項1または2に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石をホットプレスによって圧着することを特徴とする、請求項1または2に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石のそれぞれにDyおよび/またはTbを含む化合物粉末または合金粉末を塗布して粒界拡散処理を施したあと、前記Nd-Fe-B薄板状焼結磁石を互いに接着することを特徴とする、請求項1または2に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石の間に、Dyおよび/またはTbを含む化合物粉末または合金粉末を介在させた状態で、前記Nd-Fe-B薄板状焼結磁石を互いに接着または圧着して、その後、粒界拡散処理を施すことを特徴とする、請求項1または2に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石を、接着剤を用いて互いに接着することを特徴とする請求項3に記載のNd-Fe-B積層焼結磁石の製造方法。
- 複数の前記Nd-Fe-B薄板状焼結磁石を射出成型金型内に積層した状態にて固定し、その後、当該金型内に樹脂を注入して接着し成形することを特徴とする請求項3に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石を10層以上積層することを特徴とする請求項1~8のいずれか1項に記載のNd-Fe-B積層焼結磁石の製造方法。
- 前記Nd-Fe-B薄板状焼結磁石を、
a)一定間隔を開けて配列された複数の仕切り板により仕切られたモールド内に合金粉末を給粉・充填した後、前記仕切り板により区切られた空洞の主面と平行な方向に磁界中配向を施し、その後、モールドのまま焼結炉に搬送して焼結を行う方法、または、
b)2分割以上に分割された側壁を有し、一定間隔を開けて配列された複数の仕切り板により仕切られた構造を有するモールド内に合金粉末を給粉・充填して充填成形体を作製した後、前記充填成形体の主面内の方向に磁界を印加し、該充填成形体内の合金粉末を配向させ配向充填成形体を作製し、その後、前記モールドの側壁を前記配向充填成形体から引き離して前記配向充填成形体を前記モールドから取り出し、取り出した前記配向充填成形体を焼結する方法
のいずれかの方法を用いて製造することを特徴とする請求項1~9のいずれか1項に記載のNd-Fe-B積層焼結磁石の製造方法。 - Nd2Fe14B正方晶化合物のc軸方向が、前記Nd-Fe-B薄板状焼結磁石の主面内に配向されており、配向度が90%以上の高配向度をもち、かつ厚さが3mm以下であるNd-Fe-B薄板状焼結磁石が4層以上、接着またはホットプレス圧着により積層された積層体であることを特徴とするNd-Fe-B積層焼結磁石。
- 前記Nd-Fe-B薄板状焼結磁石に粒界拡散処理が施されており、該Nd-Fe-B薄板状焼結磁石が接着剤により接着され、またはホットプレスにより圧着されて積層されていることを特徴とする、請求項11に記載のNd-Fe-B積層焼結磁石。
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