EP3055870B1 - Procédé de fabrication d'un aimant permanent - Google Patents

Procédé de fabrication d'un aimant permanent Download PDF

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Publication number
EP3055870B1
EP3055870B1 EP14777023.4A EP14777023A EP3055870B1 EP 3055870 B1 EP3055870 B1 EP 3055870B1 EP 14777023 A EP14777023 A EP 14777023A EP 3055870 B1 EP3055870 B1 EP 3055870B1
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Prior art keywords
particle size
particles
separation
magnetic material
grinding
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German (de)
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EP3055870A1 (fr
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Branislav Zlatkov
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Volkswagen AG
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Volkswagen AG
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/023—Hydrogen absorption
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
    • 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
    • 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 invention relates to a method for producing a permanent magnet, in particular a method for producing a powder of the magnetic starting material for magnet production.
  • the invention further relates to a permanent magnet produced by the method and to an electric machine comprising at least one such permanent magnet.
  • rare earth alloys of the type SE-TM-B or SE-TM are predominantly used, where SE is a rare-earth element, TM is an iron-group transition metal (Fe, Co, Ni) and B is boron ,
  • Typical manufacturing processes include the process steps of pulverizing the magnetic raw material, pressing / solidifying the powder into a green part with or without external magnetic field to form a desired shape, sintering the green part for further densification (high temperature treatment), optionally tempering (heat or low temperature treatment) for stress relief and for stabilization of the structure in the magnetic body and magnetization in a magnetic field. Sometimes different process stages are combined with each other and the order is varied.
  • the pulverization of the magnetic starting material usually comprises several stages. For example, a melt of the alloy is poured into ingots (so-called ingots), mechanically broken and subjected to one or more milling stages. It is also known to process the alloy melt with the method of strip casting to a rapidly cooled band with a polycrystalline structure, which is subsequently further broken and ground. Furthermore, the method of the Hydrogen embrittlement (English: Hydrogen Decrepitation, HD process) is known, in which the material is pressurized with hydrogen, so that it interstitially penetrates into the material and leads to the formation of microcracks in the material during its subsequent release. As a result, the subsequent grinding time can be reduced. (A different process - the so-called HDDR process (for Hydrogenation Disproportionation Desorption Recombination ) -, however, uses the temporary formation of metal hydrides and their subsequent desorption to improve the structural phases of the magnetic material and the magnetic properties.
  • HDDR process for Hydrogenation Disproportionation Desorption Recomb
  • a method for producing a sintered rare earth magnet by first preparing from a melt of the rare earth magnet material, for example Nd 2 Fe 14 B, in a single roll or two roll process a rapidly cooled ("quenched") polycrystalline ribbon obtained by the cooling process - Forms on both sides of a Nd-rich phase having a lower melting point than Nd 2 Fe 14 B.
  • the strip is pulverized and subjected to low-temperature sintering at a temperature corresponding to the melting point of the Nd-rich phase. This is intended to prevent coarsening of the crystallites contained in the polycrystalline phase and having an average particle size of 10 to 200 nm.
  • EP 0 416 595 A2 describes a rare earth magnet manufacturing process in which a solidified melt of the magnetic material is first refracted and then milled with liquid nitrogen in a disc or impact mill to produce particle sizes of at most 400 microns. This is followed by hydrogenation of the material and re-milling in a liquid hydrocarbon to obtain particle sizes of at most 40 microns, typically 2.7 to 3.5 microns.
  • the powder thus obtained becomes the purpose its passivation is controlled oxidized, shaped, oriented in a magnetic field, pressed and sintered.
  • US 5,382,303 describes a method for producing a magnet in which an SM-Co type magnetic material is melted, cast and crushed and then subjected to a coarse grinding process in liquid nitrogen to obtain particle sizes of at most 600 ⁇ m. Finally, a fine grinding step is carried out, in which the powder is further milled together with a liquid hydrocarbon in a friction or ball mill up to a maximum particle size of 40 microns, especially from 3.8 to 4.6 microns. After removal of the hydrocarbon and passivation of the powder, it is compressed in a magnetic field and the green part thus obtained is sintered.
  • a magnetic powder and a magnet bonded with resin will be described.
  • the magnetic powder is produced by grinding at ambient temperature or cryogenic temperatures, for example by means of liquid nitrogen or liquid argon, in an inert atmosphere as a nanostructured material.
  • the ground powder is pressed cold at room temperature with a binder resin. This is followed by a heat treatment to cure the binder resin.
  • CN 1 479 326 A In an example, the cryogenic milling of a magnetic powder in liquid nitrogen is described. After completion of the milling, the nitrogen is removed. A block of magnetic material is prepared by sintering the magnetic powder in an ammonia gas atmosphere at 600 ° C.
  • the invention is based on the object to provide a method for producing a permanent magnet, in which a magnet having improved magnetic properties, in particular higher coercive field strength, as well as an increased mechanical strength is obtained.
  • the invention thus comprises a combination of cryogenic grinding (also referred to below as cryogenic grinding) and cryogenic separation (also referred to below as cryogenic separation) of the magnetic material.
  • cryogenic grinding also referred to below as cryogenic grinding
  • cryogenic separation also referred to below as cryogenic separation
  • the magnetic material is in the form of a suspension in liquid nitrogen.
  • the cryogenic grinding in liquid nitrogen avoids heating of the millbase due to the low temperature of the liquid nitrogen (77 K).
  • agglomeration and welding of the particles is prevented and thus enables the production of particularly small particle sizes.
  • the presence of liquid nitrogen thus allows an extension of the grinding time to achieve the desired extremely small particle size.
  • the subsequent step of separating (classifying) also takes place in liquid nitrogen. Thus, agglomeration of the particles is also counteracted in this step.
  • the separation allows obtaining a smaller grain size distribution, excluding and removing particles having particle sizes above the predetermined upper particle size. Due to the small particle size distribution, a denser and more uniform spherical packing is achieved in the finished magnet. As a result, a higher mechanical strength and a higher coercive force of the magnet is obtained.
  • Separating is understood to mean a process in which a particulate starting material having a certain particle size distribution (Usually, according to a Gaussian distribution) a fraction is obtained, which has a smaller (narrower) particle size distribution than the starting material. In other words, a particle fraction is separated and precipitated at the upper and / or lower end of the original particle size distribution.
  • the separation comprises at least one separation of a particle fraction with particle sizes above the predetermined maximum particle size so that the target fraction contains exclusively particles whose particle sizes are smaller than or equal to the maximum particle size.
  • particle size refers to the so-called equivalent diameter, which takes into account the fact that the particles generally have no exactly spherical shape. For example, a particle that can happen just a square hole of a screen with an edge length of 1 micron, regardless of its geometric shape, an equivalent diameter (“particle size”) of 1 micron.
  • any lower or upper particle sizes can be separated in the step of cryogenic separation, for example particle sizes ⁇ 4 ⁇ m.
  • particle sizes ⁇ 4 ⁇ m For the production of permanent magnets, however, smaller particle sizes, especially in the nanometer range, are desirable in order to obtain better magnetic properties.
  • particles are separated which have a predetermined maximum particle size of ⁇ 500 nm, in particular ⁇ 400 nm, preferably ⁇ 350 nm and more preferably ⁇ 300 nm the use of sieves with corresponding mesh sizes of 500 nm, 400 nm, 350 nm and 300 nm, respectively.
  • particles separated by a sieve with a mesh size of 350 nm have a particle size of ⁇ 350 nm at 100% by mass. Due to the small particle size of at most 500 nm, the particles have sizes in the range of magnetic domains, that is to say they are so-called single-domain particles. The limitation of the particle sizes on the size of magnetic domains leads to permanent magnets with a particularly high coercive force.
  • the lower particle size of the separated particles is limited in the step of cryomilling, so that, for example, particles having a particle size in the range of> 2 to 4 ⁇ m are separated.
  • the small particle size distribution also leads to a high packing density and especially regular packing of the particles in the finished permanent magnet, whereby particularly high mechanical strength and high coercive field strengths are achieved.
  • the representation of particle fractions with defined upper and lower particle sizes can be done in a simple manner by successive use of two (or more) sieves. For example, in order to separate a particle fraction whose particle sizes are from 100% by mass in the range from> 200 nm to ⁇ 300 nm, screening is first carried out with a sieve having a mesh size of 300 nm, with particles> 300 nm retained on the sieve and be separated.
  • the fraction passed through the first sieve with a particle size of ⁇ 300 nm is sieved through a second sieve with a mesh size of 200 nm, whereby particles ⁇ 200 nm pass through the second sieve.
  • the fraction retained by this sieve has exclusively particle sizes in the range of> 200 nm to ⁇ 300 nm.
  • the particles retained in the separation step with a particle size above the predetermined upper and / or lower particle size are returned to the preceding milling step.
  • the valuable magnetic material is processed practically lossless and ensures a high material yield.
  • the particle sizes obtained in the step of cryomilling are freely adjustable via the process parameters, in particular by the selected milling time. It is preferably provided that at least 50% by mass, in particular at least 70% by mass and particularly preferably at least 80% by mass, of the particles obtained by the milling have a particle size of at most 500 nm, in particular of at most 400 nm, preferably of at most 350 nm and preferably at most 300 nm. This has the advantage that a large part of the material used in the separation step already has the desired maximum particle size and passes through the subsequent separation step. The desired particle sizes can be adjusted but also other grinding parameters.
  • the steps of grinding and separating are linked together in such a way that the suspension of the magnetic material subjected to the grinding step is fed to the separation step.
  • the suspension of ground magnetic material and liquid nitrogen obtained from the milling step is passed without further material preparation into a device used for the separation step.
  • the cryogenic grinding is carried out in a ball mill.
  • the balls of the mill provide a high surface through which efficient heat removal occurs, thereby further suppressing the agglomeration of the particles.
  • other grinding devices in which suspensions can be processed are also usable within the scope of the invention.
  • the separation preferably takes place in a vibrating screen device.
  • Schwingsiebvorraumen comprise at least one horizontally arranged sieve, which is set on a swing axis in vibration. Vibrating screen devices are particularly well suited for the processing of suspensions.
  • the separation comprises the use of several serially connected screening stages with screens which have smaller mesh sizes.
  • particles with comparatively large particle sizes are removed in the upstream screening stages, and smaller particle diameters are sorted out by the downstream screening stages.
  • the use of multiple screening stages of different mesh size, in particular in continuous process management, allows a shortening of the sieving time.
  • the series connection of several screening stages can be particularly easily implemented in a Schwingsiebvorraum.
  • FIG. 1 shows a flow chart for visualizing a process flow for producing a powder of a magnetic material according to a first embodiment of the invention.
  • the starting material of the process is a magnetic material (hereinafter also referred to as magnetic material) which has at least one element of the rare earths (also called rare earths) and at least one element of the iron group (Fe, Co, Ni).
  • magnetic material which has at least one element of the rare earths (also called rare earths) and at least one element of the iron group (Fe, Co, Ni).
  • it is a rare earth alloy of the type SE-TM-A or SE-TM type, wherein SE is a rare earth element, TM is an iron group transition metal (Fe, Co, Ni) and A is an element of III.
  • Main group of the Periodic Table of the Elements in particular boron (B).
  • B boron
  • an Nd-Fe-B alloy or an Sm-Co alloy is used.
  • step S1 of FIG. 1 First, a melt of the magnetic material is processed by means of a strip casting to a thin strip. In this case, the melt is poured onto a rotating cooled roller, the melt solidifies abruptly.
  • the obtained thin tape of the magnetic material has a polycrystalline nano-structure. This is on the left side of the FIG. 2 using the example of the rare earth alloy Nd 2 Fe 14 B shown. It is It can be seen that the crystals of this alloy are enclosed by a neodymium-rich alloy phase, which is formed by the quenching of the alloy.
  • step S2 of the process with the known method of hydrogen embrittlement the material obtained by the strip casting is treated.
  • the polycrystalline magnetic material is exposed to a hydrogen atmosphere under high pressure, wherein the hydrogen is absorbed by the alloy material.
  • an alloy of the Nd-Fe-B type absorbs about 2.5% hydrogen.
  • the pressure under which the material is suddenly released whereby the hydrogen escapes.
  • This process is on the right side of the FIG. 2 clarified.
  • the neodymium-rich phase which surrounds the Nd 2 Fe 14 B crystals, microcracks occur which embrittle the material.
  • the cryogenic grinding of the brittle magnet material according to the invention takes place in step S3 of the method.
  • the process of cryogenic grinding is in a ball mill in FIG. 3 shown.
  • the ball mill 10 has a double-walled container 11, inside which a stirrer 12 is rotatably arranged. Inside the vessel 11 are also balls 13 made of a hard metal, such as stainless steel or Zr 20 .
  • the brittle magnetic material from step S2 which has a first mean particle size, is added in the form of a suspension 20 in liquid nitrogen into the vessel 11 of the ball mill 10.
  • the liquid nitrogen has a temperature of about 77 K.
  • FIG. 3 shows an enlarged view of two balls 13, between which particles 21 of the magnetic starting material are crushed by the forces prevailing between two balls 13 forces. This results in particles of the magnetic material having a second average particle size, which is smaller than the first average particle size of the material fed to the ball mill.
  • the liquid nitrogen wets the powder particles 21 of the magnetic material during milling and dissipates the resulting heat. This prevents agglomeration of the particles. Furthermore, the liquid nitrogen protects the powder surface Impurities and prevents in-contact of the pyrophoric magnetic material with atmospheric oxygen.
  • the grinding process is preferably carried out until at least 90% by mass of the powder material has a particle size of at most 500 nm, preferably of at most 300 nm.
  • the milling process parameters are chosen so that the desired particle size is obtained. They depend on the system used and the size of the system. For example, a speed of the stirrer is set from 150 to 1000 rpm and a grinding time of 1 to 12 hours.
  • step S4 cryogenic separation (classification) takes place following cryogenic grinding. This process is in FIG. 4 shown.
  • the separation device 30 shown here has a double-walled housing 31, which is charged with the suspension 20 obtained from the cryogenic grinding, consisting of the powder of the magnetic material and liquid nitrogen.
  • a plurality of vibrating screens 33 are arranged horizontally one above the other.
  • the mesh size of the sieves 33 decreases from top to bottom.
  • the sieves 33 are mechanically connected to a vertical swing axle 32.
  • the oscillating axis 32 is offset by a drive, not shown, in a vertical vibration, which is thus transmitted to the vibrating screens 33.
  • screens may be used which have sintered metallic wire nets.
  • so-called MEMS sieves for micro-electro-mechanicalstructure
  • the powder of the magnetic material supplied in the form of the suspension 20 first reaches the uppermost, coarsest sieve on which particles above the corresponding mesh size of the sieve, for example above 500 nm, are retained. Particles with particle sizes ⁇ 500 nm reach the next below sieve arranged, which has a slightly smaller mesh size than the top sieve, for example of 400 nm. On the second sieve thus particles in the range of> 400 nm to ⁇ 500 nm are retained. This process continues to the bottom sieve, which defines the desired maximum particle size, for example of 300 nm.
  • a valve 34 is thus the filtered and separated suspension 20, which contains only particle sizes preferably ⁇ 300 nm, drained and collected.
  • the fractions retained on the screens 33 become the above process step S3 of FIG returned cryogenic milling.
  • a cooling stage can be interposed.
  • step S4 the generated frictional heat is dissipated by the liquid nitrogen, thereby preventing agglomeration of the magnetic particles. Furthermore, the use in the form of the suspension in liquid N 2 allows the particle fractions retained on the sieves 33 to be returned to the step of cryogenic grinding without media breakage.
  • FIG. 5 shows a flow diagram of a process sequence for the preparation of the magnetic powder according to a second embodiment of the invention. The procedure differs from that in FIG. 1 shown method only in the first two steps, while the inventive steps S3 and S4 are the same and will not be explained again.
  • the alloy melt is first poured into small-sized castings and solidified. These are then broken mechanically under protective gas, resulting in particles having an average particle size of, for example, 500 microns.
  • a further mechanical pulverization of the material takes place by conventional grinding in a protective gas atmosphere, for example in gaseous nitrogen or argon.
  • the coarse grinding S2 ' can be carried out for example in a jet mill (jet milling) or in a ball mill. Particle sizes of, for example, 3 to 5 ⁇ m are obtained.
  • These are further pulverized in the already explained steps S3 and S4 in order to obtain particle sizes of preferably at most 300 nm.
  • FIG. 6 shows by way of example a further process sequence, in which the in step S4 (off FIG. 1 or 5 ) powder is further processed into a permanent magnet.
  • step S5 compacting and shaping of the powder of the magnetic material takes place, for example, by pressing.
  • the pressing may be anisostatic in a mechanical pressing tool, with mechanical pressure being applied to the compact from one or two opposite spatial directions.
  • the pressing may be carried out isostatically by subjecting the powder to a high pressure of an inert gas atmosphere. In both cases, the pressing can be done in an external magnetic field, so that a magnetically anisotropic compact arises.
  • Result of the Compaction step S5 is a (magnetically isotropic or anisotropic) compact, which is also referred to as a green part.
  • a sintering of the green part takes place.
  • the green part is solidified at a temperature which is lower or the melting temperature of the magnetic material.
  • a temperature which is lower or the melting temperature of the magnetic material For example, for alloys of the NdFeB type, for example Nd 2 Fe 14 B, temperatures in the range of 1000 to 1150 ° C. are used.
  • the particles of the powder are further compressed and solidified, and enter into mechanical, in some cases materially bonded, bonds.
  • a non-magnetized (isotropic or anisotropic, depending on whether or not pressed in magnetic field) body is present since the Curie remains during sintering.
  • an optional tempering process follows, in which the magnet is subjected to a further thermal treatment (low-temperature treatment).
  • the aim of annealing is the reduction of residual stresses in the crystal structure.
  • a shaping treatment and / or surface treatment of the magnet takes place in order to give it a desired shape and dimension.
  • cutting techniques are used, such as grinding, cutting, milling, etc.
  • the final shape of the magnet is already determined in the compacting step S5, for example, a corresponding pressing tool, so that dispenses with machining or this can at least be reduced.
  • the magnet can be provided with a surface coating, for example of an epoxy resin or a metallic coating.
  • step S9 the magnet is magnetized in an external magnetic field in which the magnetic dipoles are magnetized, that is to say aligned.
  • the permanent magnet produced by the method according to the invention is characterized by small particle sizes on the order of magnetic domains, that is, it consists of so-called single-domain particles. In addition, it has a uniform particle size distribution, preferably in the range of 200 to 300 nm. As a result, the magnet is characterized by a high coercive field strength and a high temperature stability. Its good magnetic properties are not impaired by increased levels of rare earths, for example in the form of Dy or Tb, which are introduced by conventional processing steps (eg GBDP for grain boundary diffusion process).

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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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Claims (13)

  1. Procédé de fabrication d'un aimant permanent, dans lequel une poudre d'un matériau magnétique est fabriquée et la poudre de matériau magnétique est traité afin d'obtenir un aimant permanent, la fabrication de la poudre de matériau magnétique comprenant les étapes suivantes :
    - broyage d'une suspension de particules de matériau magnétique d'une première taille moyenne de particules dans de l'azote liquide afin d'obtenir des particules de matériau magnétique d'une deuxième taille moyenne de particules, qui est inférieure à la première taille moyenne de particules,
    caractérisé par
    - la séparation d'une suspension du matériau magnétique broyé dans de l'azote liquide, les particules d'une taille inférieure à une taille de particules supérieure prédéterminée étant séparées.
  2. Procédé selon la revendication 1, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille ≤ 500 nm sont séparées.
  3. Procédé selon la revendication 2, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille ≤ 400 nm sont séparées.
  4. Procédé selon la revendication 3, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille ≤ 300 nm sont séparées.
  5. Procédé selon l'une des revendications précédentes, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille > 100 nm à ≤ 500 nm sont séparées.
  6. Procédé selon la revendication 5, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille > 100 nm à ≤ 400 nm sont séparées.
  7. Procédé selon la revendication 6, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille > 150 nm à ≤ 350 nm sont séparées.
  8. Procédé selon la revendication 7, caractérisé en ce que, dans l'étape de séparation, les particules avec une taille de 200 nm à ≤ 300 nm sont séparées.
  9. Procédé selon l'une des revendications précédentes, caractérisé en ce que les particules avec une taille supérieure à la taille de particules supérieure prédéterminée sont retournées de l'étape de séparation vers l'étape de broyage.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que les étapes de broyage et de séparation s'enchaînent entre elles de façon à ce que la suspension de matériau magnétique soumise à l'étape de broyage soit introduite dans l'étape de séparation.
  11. Procédé selon l'une des revendications précédentes, caractérisé en ce que le broyage a lieu dans un broyeur à billes.
  12. Procédé selon l'une des revendications précédentes, caractérisé en ce que la séparation a lieu à l'aide d'un dispositif de tamis vibrant.
  13. Procédé selon l'une des revendications précédentes, caractérisé en ce que la séparation comprend l'utilisation de plusieurs étages de tamisage avec des tailles de mailles de plus en plus petites.
EP14777023.4A 2013-10-10 2014-09-19 Procédé de fabrication d'un aimant permanent Active EP3055870B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201310220452 DE102013220452A1 (de) 2013-10-10 2013-10-10 Verfahren zur Herstellung eines Permanentmagneten sowie Permanentmagnet und elektrische Maschine mit einem solchen
PCT/EP2014/070047 WO2015051986A1 (fr) 2013-10-10 2014-09-19 Procédé de fabrication d'un aimant permanent, et aimant permanent ainsi que machine électrique équipée d'un tel aimant

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EP3055870A1 EP3055870A1 (fr) 2016-08-17
EP3055870B1 true EP3055870B1 (fr) 2019-11-13

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US20180166190A1 (en) * 2016-12-14 2018-06-14 Government Of The United States As Represented By The Secretary Of The Air Force Bulk anisotropic exchange-spring magnets and method of producing the same
DE102018112411A1 (de) 2018-05-24 2019-11-28 Netzsch Trockenmahltechnik Gmbh Verfahren und Anlage zur Herstellung eines Ausgangsmaterials für die Herstellung von Seltenerd-Magneten
CN109473271A (zh) * 2018-11-08 2019-03-15 浙江嘉兴南湖电子器材集团有限公司 一种磁体取向压制成型工艺
CN110090965B (zh) * 2019-06-10 2022-05-13 重庆理工大学 一种制备高矫顽力超细Sm2Co17磁粉的方法
CN111640566B (zh) * 2020-05-20 2021-09-21 杭州三炻磁性材料有限公司 恒压恒磁钐钴粉末压制的工艺方法
CN113546745B (zh) * 2021-06-22 2022-11-25 国家能源集团宁夏煤业有限责任公司 制备聚合物粉末的深冷粉碎装置和深冷粉碎方法

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WO2015051986A1 (fr) 2015-04-16
CN105612594B (zh) 2018-11-23
KR20160070788A (ko) 2016-06-20
DE102013220452A1 (de) 2015-04-30
CN105612594A (zh) 2016-05-25
EP3055870A1 (fr) 2016-08-17

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