EP3431209A1 - Procédé et installation de fabrication d'un matériau de départ pour la fabrication d'aimants à terres rares - Google Patents

Procédé et installation de fabrication d'un matériau de départ pour la fabrication d'aimants à terres rares Download PDF

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Publication number
EP3431209A1
EP3431209A1 EP18182618.1A EP18182618A EP3431209A1 EP 3431209 A1 EP3431209 A1 EP 3431209A1 EP 18182618 A EP18182618 A EP 18182618A EP 3431209 A1 EP3431209 A1 EP 3431209A1
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EP
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Prior art keywords
rare earth
intermediate product
starting material
powdery
production
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EP18182618.1A
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German (de)
English (en)
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EP3431209B1 (fr
Inventor
Frank Winter
Hermann Sickel
Dr. Wilhelm Fernengel
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Netzsch Trockenmahltechnik GmbH
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Netzsch Trockenmahltechnik GmbH
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Priority to SI201831039T priority Critical patent/SI3431209T1/sl
Priority to EP23190243.8A priority patent/EP4268995A1/fr
Publication of EP3431209A1 publication Critical patent/EP3431209A1/fr
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • B07B13/003—Separation of articles by differences in their geometrical form or by difference in their physical properties, e.g. elasticity, compressibility, hardness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • B07B13/04—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices according to size
    • 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
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/0536—Alloys characterised by their composition containing rare earth metals sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • 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
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • 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
    • 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
    • H01F41/0266—Moulding; Pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C15/00—Disintegrating by milling members in the form of rollers or balls co-operating with rings or discs
    • B02C2015/002—Disintegrating by milling members in the form of rollers or balls co-operating with rings or discs combined with a classifier
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
    • B04C5/00—Apparatus in which the axial direction of the vortex is reversed
    • 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
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, 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
    • 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
    • B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/025—Making ferrous alloys by powder metallurgy having an intermetallic of the REM-Fe type which is not magnetic

Definitions

  • the present invention relates to a process for producing a raw material for the production of rare earth magnets, a raw material and a plant for producing a raw material for the production of rare earth magnets.
  • a permanent magnet is a piece of magnetizable material, such as iron, cobalt or nickel, which retains its static magnetic field without the need for electrical current flow (as opposed to electromagnets).
  • a permanent magnet can be generated by the action of a magnetic field on a ferromagnetic material.
  • rare earth magnets consisting essentially of ferrous metals (iron, cobalt, rare nickel) and rare earth metals (especially neodymium, samarium, praseodymium, dysprosium, terbium, gadolinium) exist. They are characterized by having at the same time a high magnetic remanence flux density and a high magnetic coercive field strength and thus a high magnetic energy density.
  • NiFeB neodymium, iron and boron
  • NdFeB neodymium, iron and boron
  • the temperature stability can be raised to over 200 ° C.
  • other alloy components such as cobalt are often added.
  • Permanent magnets are made of crystalline powder.
  • the magnetic powder is pressed into a mold in the presence of a strong magnetic field.
  • the crystals align with their preferred magnetization axis in the direction of the magnetic field.
  • the pellets are then sintered.
  • the pulverized constituents of the powder are joined or compacted by heating, but no or at least not all starting materials are melted.
  • the compacts often under elevated pressure - heated so that the temperatures remain below the melting temperature of the main components, so that the shape of the workpiece is maintained.
  • the outward effective magnetization is lost, because the thermal movement of the atoms leads to the largely antiparallel alignment of the elementary magnets in the crystals.
  • the orientation of the grains in the sintering composite is not lost, the parallel alignment of the elementary streams after cooling of the magnets can be restored by a sufficiently strong magnetizing pulse.
  • the magnetic powder is produced in particular by grinding the corresponding alloys or constituents, for example in fluid bed jet mills or similar grinding plants.
  • fluid bed jet mills in particular a defined Feinstvermahlung, although with exact Oberkornbegrenzung, but with not inconsiderable proportion of Feinstpumblen.
  • the crushing energy is provided by gas jets.
  • magnetic powders which can be prepared by the methods known from the prior art, are chemically very reactive and, for this reason, react even at low oxygen concentrations with the oxygen or nitrogen from the environment. This can be accompanied by further processing of the magnetic powder powder fires. Also, the practice has shown that magnets, which are produced by means of magnetic powders known from the prior art, often can be very poorly oriented, whereby the remanence of the magnets produced from the already known magnetic powders is deteriorated. Such disadvantages may be associated in particular with or at a high percentage by volume of fines in the magnetic powder.
  • magnets produced from the magnetic powders already known from the prior art have an improved field stability or coercive field strength due to a high percentage by volume of coarse fraction.
  • the object of the invention is to further optimize the production of the starting mixture for the production of rare earth magnets in order to be able to produce improved rare earth magnets.
  • the invention relates to a method for producing a powdered and intended for the production of rare earth magnets starting material.
  • a first step of the method provides for comminuting an alloy comprising at least one rare earth metal, wherein a powdery intermediate product is formed from the alloy comprising at least one rare earth metal.
  • a further step provides for carrying out at least one particle size and / or density-oriented classification for the powdery intermediate product, wherein a fraction of the powdery intermediate product formed by means of the at least one classification forms the starting material intended for the production of rare earth magnets.
  • At least one dynamic classifier is provided for the method, which at least one dynamic classifier converts at least one particle size and / or density-based classification for the powdery intermediate product and in this case separates the fraction from the powdery intermediate product which contains the starting material intended for the production of rare earth magnets formed.
  • the powdery intermediate product is fed to at least one static separator.
  • the at least one static classifier of the powdery intermediate product separated portion to which at least one dynamic classifier are supplied, which at least one dynamic classifier which converts at least one particle size and / or density classification for the separated by means of the at least one static classifier from the powdery intermediate proportion and in this case the fraction of the proportion separates, which forms the intended for the production of rare earth magnets starting material.
  • the at least one dynamic sifter sifts the powdery intermediate product and also disperses, as a result of which the fraction is separated from the intermediate powder product which forms the starting material intended for the production of rare earth magnets.
  • the at least one dynamic sifter separates coarse material from the powdery intermediate product and that within a second particle size and / or density-oriented classification, the at least one dynamic classifier fines separated from the powdery intermediate.
  • a portion of the powdery intermediate product separated from the fine material and coarse material can provide the fraction which forms the starting material intended for the production of rare earth magnets.
  • Embodiments have proved useful in which the first particle size and / or density-oriented classification and the second particle size and / or density-based classification are performed via exactly one dynamic classifier.
  • the alloy comprising at least one rare earth element can in each case preferably be mechanically comminuted in two separate steps, the pulverulent intermediate product being formed from the comminution in separate steps.
  • the invention also relates to a provided for the production of rare earth magnets starting material, which by a method according to one of previously described embodiments.
  • a proportion of particles> 8 ⁇ m is ⁇ 2% by volume, in particular in a range between 0.1% by volume and 1% by volume and / or a proportion of particles ⁇ 2 ⁇ m is ⁇ 2% by volume and in particular in a range between 0, 05% by volume and 2% by volume.
  • a starting material is prepared as described above and that this starting material is introduced into the molds and pressed.
  • the invention also relates to a plant for producing a powdery and intended for the production of rare earth magnets starting material.
  • Features which have already been described above for various embodiments of the method can also be provided in the system described below and are therefore not mentioned redundantly. Also, features described below, which relate to various embodiments of the system according to the invention, may optionally be provided in the previously described method.
  • the plant for producing a powdery and intended for the production of rare earth magnets starting material comprises at least one crushing device, which is aligned to a production of a powdery intermediate product by comminution of an alloy comprising at least one rare earth metal.
  • the system comprises at least one separating device which can separate a fraction from the powdery intermediate product by means of at least one particle size and / or density-oriented classification or sighting, which forms the starting material intended for the production of rare earth magnets.
  • the at least one separating device comprises at least one dynamic sifter, which can separate the fraction from the powdery intermediate product by means of a particle size and / or density classification, which forms the starting material intended for the production of rare earth magnets.
  • the at least one separating device comprises at least one static separator to which the powdery intermediate product can be fed.
  • the at least one static classifier and the at least one dynamic classifier can communicate with one another in such a way that a portion separated from the supplied intermediate product by means of the at least one static classifier can be fed to the at least one dynamic classifier.
  • the at least one dynamic safety can then optionally separate from the added fraction the fraction which forms the starting material intended for the production of rare earth magnets.
  • the at least one dynamic sifter is designed for sifting and dispersing the supplied powdery intermediate product.
  • the at least one comminution device comprises two successive comminution machines which are each designed for preferably mechanical comminution of the alloy comprising at least one rare earth metal and cooperate with one another to produce the powdery intermediate of the alloy comprising at least one rare earth element.
  • the starting material that can be produced in the context of the methods described above or by means of the plant described above can essentially comprise particles of a target size range and hardly have any contamination with particles smaller than particles of a target size range. These are also referred to below as Feinstpiety. Furthermore, the starting material produced in the context of the previously described processes or by means of the plant described above can essentially have hardly any contamination with particles which are larger than the particles of the target size range. These are also referred to below as coarse particles.
  • a starting material which essentially comprises only particles with a size within the target size range in a substantially homogeneous mixture.
  • the starting material which can be produced by the previously described method or by means of the system described above, embodiments in which the starting material has particles in the target size range between 1 ⁇ m and 10 ⁇ m, in particular in a target size range between 2 ⁇ m and 8 ⁇ m, have proved successful.
  • an alloy comprising at least one rare earth metal
  • it can not be avoided in practice that a proportion of microparticles smaller than the target size range is produced.
  • a starting material prepared in the context of the preceding processes or by means of the plant described above contains ⁇ 2% by volume of very fine particles, in particular ⁇ 1% by volume. Furthermore, it can be provided that the starting material produced in the context of the preceding processes or by means of the plant described above comprises ⁇ 2% by volume of coarse particles, in particular ⁇ 1% by volume.
  • the starting material prepared in the context of the previously described process or by means of the plant described above essentially or predominantly contains particles in the target size range between 2 ⁇ m and 8 ⁇ m, a proportion of particles whose size is above 8 ⁇ m being ⁇ 2 Volume percent is, in particular in a range between 0.1 volume percent and 1 volume percent and wherein a proportion of particles whose size is less than 2 microns is ⁇ 2 percent by volume, in particular in a range between 0.05 percent by volume and 2 percent by volume.
  • the at least one dynamic classifier already mentioned above and embodied as part of the method according to the invention or the system according to the invention may comprise a classifying rotor.
  • a rotational speed of the classifying rotor can optionally be controlled or regulated as a function of a desired particle size distribution for the starting material to be produced.
  • a control and / or regulating unit may be provided, which communicates with the at least one dynamic classifier.
  • An algorithm can be stored on the control and / or regulating unit, via which the control and / or regulating unit independently regulates or controls a rotational speed of the classifying rotor formed as a component of the at least one dynamic classifier, taking into account the particular particle size distribution desired for the starting material to be produced ,
  • At least one static separator may optionally be formed by at least its cyclone classifier.
  • the at least one cyclone classifier may possibly already achieve a reduction in the proportion of ultrafine particles.
  • the ultrafine portions which are inevitably always present in such a powdery intermediate product, thus have a disadvantageous effect on the properties of the rare earth magnets produced therefrom in many respects.
  • the pulverulent intermediate product which may have already been partially freed of fine particles by way of the at least one static classifier, is subjected to at least one further classifying process, implemented by at least one dynamic classifier.
  • the pulverulent intermediate product is first dispersed and then a classification according to particle size and / or density for the dispersed powdery intermediate product is carried out.
  • This dispersion and classification according to particle size and / or density can be performed in exactly one dynamic sifter. Fine particles and / or coarse particles can then be separated from the powdery intermediate product via the at least one dynamic classifier or via the exactly one dynamic classifier.
  • the dispersion of the intermediate product and the renewed separation of very fine particles and / or coarse particles are carried out within a single device, in particular within a single dynamic classifier. Due to the high chemical reactivity of possibly present in high concentration in the powdery intermediate fine particles, the only dynamic classifier if necessary, convert a dispersion and / or screening under a protective gas atmosphere.
  • a protective gas for example, helium, argon, nitrogen or the like. Use.
  • the at least one formed as a component of the alloy rare earth metal may be formed for example by iron and / or boron.
  • the alloy comprising at least one rare earth metal may be an NdFeB alloy.
  • a starting material can be produced from this alloy comprising at least one rare earth metal, which essentially comprises only particles in the target size range between 1 ⁇ m to 10 ⁇ m, preferably between 2 ⁇ m to 8 ⁇ m.
  • the starting mixture preferably comprises ⁇ 95% by volume, in particular ⁇ 98% by volume, of particles in the target size range, which target range is set from 2 ⁇ m to 8 ⁇ m.
  • the plant already described may comprise an apparatus for the coarsening of an alloy comprising at least one rare earth element.
  • a coarse powder fraction optionally formed from the alloy comprising at least one rare earth metal with the aid of the coarse comminution device can optionally be ground into a fine powder fraction in a fine comminution device optionally formed as part of the plant, the fine powder fraction forming the powdery intermediate product.
  • the device for fine comminution may be formed as a fluid bed jet mill.
  • FIG. 1 schematically shows process steps for the production of a starting material AM for the production of rare earth magnets.
  • R rare earth metal
  • Fe iron
  • B boron in the desired proportions.
  • an NdFeB alloy becomes a so-called neodymium magnet used.
  • an alloy of the elements in the desired proportions must first be prepared. This alloy is subjected to coarse milling in a first step. For example, in a mechanical Mahlanalage or by embrittlement with hydrogen. In particular, particles with a size of up to a few mm are produced.
  • the coarse particles gP are chemically stable in contrast to the particles fP of the fines described below and can also be oriented well in magnetic fields, they have negative effects on the counter-field stability of the magnet because these coarse particles gP are already magnetized in the case of small magnetic opposing fields and thus worsen the opposing field stability (or coercivity) of the entire magnet. For this reason, it is advantageous to further reduce the proportion of coarse particles gP in the starting mixture for the production of sintered permanent magnets.
  • the fP particles of the fines are chemically very reactive and react with the oxygen or nitrogen from the environment even at the lowest oxygen concentrations. These fine particles fP can cause spontaneous powder fires in the further processing of the powder.
  • a further disadvantage of the very fine particles fP is that these fine powder particles can only be orientated very poorly in the usually available magnetic fields and pressing devices (about 10-20 kOe in size) and therefore impair the remanence of the magnets produced therefrom. For this reason, ultrafine fractions, in particular particles with a diameter of ⁇ 1-2 ⁇ m, are removed from the fine powder fraction fPF in a fourth or additional process step.
  • the mixture is passed through a cyclone which entrains the very fine fraction via a suitable gas stream and thereby separates it from the mixture.
  • the intermediate ZP educated. However, this still contains a not inconsiderable proportion of up to 10% of very fine particles smaller than 1 ⁇ m to 2 ⁇ m.
  • the intermediate product ZP is subjected to at least one further classifying process in order to obtain undesired very fine particles fP or coarse particles gP or fines fP and coarse particles gP and thus further improve the homogeneity of the particles in the target size ZG, in particular in order to obtain as starting material AM a powder mixture which essentially comprises only particles having particle sizes in a target range of between approximately 2 ⁇ m to 8 ⁇ m, since these particles are the magnetic point of view represent the best powder fraction. All further steps, which in terms of time to the step after paragraph 4, are connected, with the aid of a dynamic classifier 10 (see. FIGS. 2 and 3 ) or a high-performance classifier.
  • the particles with the target size ZG between 2 ⁇ m and 8 ⁇ m are chemically sufficiently stable so that they do not cause any additional oxidation in the normal production process. In addition, they can be well oriented with the usual magnetic fields. They thus contribute significantly to achieving a high remanence of the produced magnets and are therefore desirable, necessary and useful.
  • the powdery intermediate ZP is dispersed in order to produce the most homogeneous possible distribution of the different particles of the intermediate ZP.
  • molecular and magnetic forces of attraction between the particles are overcome and a subsequent re-sifting and separation of particles of the fines and / or particles of the coarse fraction following dispersing becomes possible.
  • a dynamic separator 10 see. FIGS. 2 and 3 ) or high-performance classifier.
  • the dispersed powdery intermediate product ZP is re-sighted and particles of the fines and / or particles of the coarse fraction are thereby removed. This produces an optimized separation of the finest and coarse particles to the desired particle target size ZG.
  • the fines content of particles smaller than 1 ⁇ m is reduced to less than 1%.
  • the coarse fraction of particles whose size is more than 10 .mu.m can also be reduced to a fraction of less than 1%.
  • This at least one additional classifying process is preferably carried out under a protective gas atmosphere, for example under helium, argon, or nitrogen, although this is not meant to be a conclusive list of possibilities.
  • a protective gas atmosphere for example under helium, argon, or nitrogen, although this is not meant to be a conclusive list of possibilities.
  • the protective gas atmosphere prevents spontaneous powder fires due to the finest particles fP.
  • the fifth and sixth process step or the two last process steps ie the dispersion and the separation of fines fP and / or the separation of coarse particles gP in a dynamic classifier 10 according to FIG FIGS. 2 and 3 be done together.
  • the intermediate product ZP dispersed in this way is passed through a classifier wheel 4, which is infinitely variable in speed, the separation of the particle sizes taking place either in target and coarse material or else in target material and fines.
  • the optimized prepareerraddesign ensures that with only one crusherrad 4 very high subtleties can be achieved even at high throughputs.
  • the ultrafine particles fP leave the classifying device 10 via the classifying wheel 4 installed with horizontal shaft 8 in the center of the classifying device or the dynamic classifier 10.
  • the coarse particles gP are rejected by the classifying wheel 4 and by the helically formed and with a dividing wall 5 provided machine housing 9 back discharged over the Grobgutaustritt 6 on the underside of the machine housing 9.
  • the discharge of the coarse particles gP can be regulated in the case of difficult separating tasks, and thus the cleanliness of the coarse particles gP can be influenced.
  • the particles of the target size ZP leave the dynamic sifter 10 via the coarse material outlet 6 together with the coarse material.
  • the ultrafine particles fP have been separated from the particles of the target size ZP and thus do not form part of the fraction leaving the dynamic sifter 10 via the coarse material outlet 6.
  • the regulation of the desired target particle size ZG takes place here in particular by regulating the gas flow of the process air VL and / or the speed of the classifier wheel 4.
  • a higher gas flow and / or a lower speed lead to a coarser product, while a lower gas flow and / or a higher Speed lead to a finer product.
  • the shows FIG. 3 the at least two Spaltgaszu exchangeen (11), these are necessary to the gap between Feingutastritt and the reformerrad (4) to flush with so-called cracked gas. But there are also versions with only one Spaltgaszuateung (11) possible.
  • This flushing prevents particles in the classifying wheel (4) and / or the gap between the fines outlet and the classifying wheel (4) from settling and clogging.
  • the rinsing takes place by means of a suitable fluid, in a preferred embodiment by means of inert gas.
  • FIG. 4 shows the particle size distribution in the intermediate ZP and in the starting material AM.
  • the particle size in ⁇ m is plotted against the proportion of the volume density of the respective mixture in% in the diagram.
  • a more homogeneous particle mixture in the starting material AM can be achieved by the additional process step of dispersing the intermediate product ZP and viewing with subsequent separation of very fine particles fP ⁇ 1 ⁇ m and / or coarse particles gP ⁇ 10 via a dynamic separator 10.
  • the proportion of fines amounts to fP ⁇ 1% of the volume density and in which the proportion of coarse particles gP also amounts to ⁇ 1% of the volume density.
  • the fractions of fine particles fP and coarse particles gP shown hatched are removed from the powdery intermediate product ZP.
  • the starting material AM produced in this way is particularly suitable for the production of sintered rare-earth magnets, since with these particle sizes of the starting material AM particularly good magnet values can be achieved.
  • this starting material AM for the production of permanent magnets high (improved) remanence values BR and a good (improved) opposing field stability HcJ as well as a significant improvement in the squareness of the demagnetization curve are achieved.
  • FIG. 5 shows a scanning electron micrograph of the powdery intermediate ZP
  • FIG. 6 shows a scanning electron micrograph of the starting material AM, as it can be produced in various embodiments of the method according to the invention and used for the production of rare earth magnets.
  • the intermediate ZP represents a highly inhomogeneous mixture of different particle sizes and in particular also contains a high proportion of fines FP
  • FIG. 6 clearly that the double-screened starting material AM mainly contains only particles of a target size ZG between 1 .mu.m and 10 .mu.m, preferably between 2 .mu.m and 8 .mu.m.

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  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
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EP18182618.1A 2017-07-19 2018-07-10 Procédé et installation de fabrication d'un matériau de départ pour la fabrication d'aimants à terres rares Active EP3431209B1 (fr)

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DE102018112406A1 (de) * 2018-05-24 2019-11-28 Netzsch Trockenmahltechnik Gmbh Verfahren und Anlage zur Herstellung eines Ausgangsmaterials für die Herstellung von Seltenerd-Magneten
CN109848030A (zh) * 2019-01-26 2019-06-07 南通理工学院 一种增材制造用原料筛选装置
DE102023210125A1 (de) 2023-10-16 2025-04-17 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein Verfahren zur Herstellung eines oder mehrerer Permanentmagneten sowie Permanentmagnet und dessen Verwendung

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JP2000317338A (ja) * 1999-05-11 2000-11-21 Nippon Pneumatic Mfg Co Ltd ジェット粉砕装置及びジェット粉砕方法
US20020129874A1 (en) * 2000-11-08 2002-09-19 Yuji Kaneko Rare earth magnet and method for producing the magnet
WO2007045320A1 (fr) * 2005-10-21 2007-04-26 Vacuumschmelze Gmbh & Co. Kg Poudres pour aimants a base d'elements de terres rares, aimants a base d’elements de terres rares et leurs procedes de fabrication
EP2273513A1 (fr) * 2008-03-31 2011-01-12 Hitachi Metals, Ltd. Aimant fritté de type r-t-b et son procédé de fabrication

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EP0414376A2 (fr) * 1989-07-24 1991-02-27 Shin-Etsu Chemical Co., Ltd. Méthode pour la préparation d'un aimant permanent de terre rare-fer-bore
JP2000317338A (ja) * 1999-05-11 2000-11-21 Nippon Pneumatic Mfg Co Ltd ジェット粉砕装置及びジェット粉砕方法
US20020129874A1 (en) * 2000-11-08 2002-09-19 Yuji Kaneko Rare earth magnet and method for producing the magnet
WO2007045320A1 (fr) * 2005-10-21 2007-04-26 Vacuumschmelze Gmbh & Co. Kg Poudres pour aimants a base d'elements de terres rares, aimants a base d’elements de terres rares et leurs procedes de fabrication
EP2273513A1 (fr) * 2008-03-31 2011-01-12 Hitachi Metals, Ltd. Aimant fritté de type r-t-b et son procédé de fabrication

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US20230271224A1 (en) 2023-08-31
DK3431209T3 (da) 2024-01-02
EP4268995A1 (fr) 2023-11-01
SI3431209T1 (sl) 2024-02-29
US11660639B2 (en) 2023-05-30
PL3431209T3 (pl) 2024-03-04
LT3431209T (lt) 2024-01-10
ES2966804T3 (es) 2024-04-24
FI3431209T3 (fi) 2023-12-21
CN109277577A (zh) 2019-01-29
EP3431209B1 (fr) 2023-09-20
DE102017116272A1 (de) 2019-01-24
RU2706258C1 (ru) 2019-11-15

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