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 PDF

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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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Prior art keywords
sintered
magnet
thin plate
laminated
magnets
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PCT/JP2022/001412
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English (en)
French (fr)
Japanese (ja)
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眞人 佐川
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NDFEB Corp
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NDFEB Corp
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Priority to CN202280010037.5A priority Critical patent/CN116762147A/zh
Priority to US18/259,203 priority patent/US20240079179A1/en
Priority to JP2022578247A priority patent/JP7576862B2/ja
Priority to EP22745630.8A priority patent/EP4287226A4/en
Priority to KR1020237025676A priority patent/KR102721666B1/ko
Publication of WO2022163407A1 publication Critical patent/WO2022163407A1/ja
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    • 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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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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CN116721860A (zh) * 2023-08-08 2023-09-08 乳源瑶族自治县力强磁铁制品有限公司 一种钕铁硼电机磁体生产用烧结工艺及专用设备
JP2024016680A (ja) * 2022-07-26 2024-02-07 Ｎｄｆｅｂ株式会社 ネオジム積層焼結磁石
WO2025057759A1 (ja) * 2023-09-11 2025-03-20 日本特殊陶業株式会社 積層磁石及びモーター
WO2025057760A1 (ja) * 2023-09-11 2025-03-20 日本特殊陶業株式会社 積層磁石及びモーター
WO2025057758A1 (ja) * 2023-09-11 2025-03-20 日本特殊陶業株式会社 積層磁石及びモーター
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WO2025109656A1 (ja) * 2023-11-20 2025-05-30 Ｎｄｆｅｂ株式会社 ネオジム積層焼結磁石

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