EP4227963A1 - Procédé de fabrication d'une matière magnétique et matière magnétique - Google Patents

Procédé de fabrication d'une matière magnétique et matière magnétique Download PDF

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Publication number
EP4227963A1
EP4227963A1 EP22155955.2A EP22155955A EP4227963A1 EP 4227963 A1 EP4227963 A1 EP 4227963A1 EP 22155955 A EP22155955 A EP 22155955A EP 4227963 A1 EP4227963 A1 EP 4227963A1
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EP
European Patent Office
Prior art keywords
lanthanide
salt
magnetic material
grains
mixture
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22155955.2A
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German (de)
English (en)
Inventor
Gotthard Rieger
Rolf Vollmer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens AG
Original Assignee
Siemens AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Siemens AG filed Critical Siemens AG
Priority to EP22155955.2A priority Critical patent/EP4227963A1/fr
Publication of EP4227963A1 publication Critical patent/EP4227963A1/fr
Pending legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

Definitions

  • the present invention relates to a method for producing a magnetic material according to patent claim 1 and a magnetic material according to patent claim 10.
  • Metallic high-performance magnets also have high magnetic losses when used with high frequencies.
  • such a material for example based on iron, boron and neodymium, is segmented by sawing and reassembled using a polymer binder to form a laminate.
  • a polymer binder to form a laminate.
  • laminate materials have good permanent magnetic properties, they are, as already mentioned, no longer suitable for use in high-load electrical machines due to the polymer bond (here in the laminate and not in the microstructure) at temperatures below 100 °C .
  • the object of the invention is to provide a method for producing a magnetic material and a magnetic material which, compared to the prior art, have a higher temperature resistance and also have better permanent magnetic properties.
  • the solution to the problem consists in a method for producing a magnetic material with the features of patent claim 1 and in a sintered, polymer-free magnetic material with the features of patent claim 10.
  • infiltration means the introduction of a fluid into an open-pored system.
  • the fluid including the solvent, can be gaseous, with the substance to be introduced condensing on the pore walls and being deposited there.
  • the infiltration of liquid media which is driven on the basis of capillary effects and capillary forces, preferably takes place.
  • the solvent is also liquid here.
  • the method described leads to a magnetic material that has exceptionally high permanent magnetic properties and at the same time shows a high temperature resistance of significantly more than 100 °C.
  • the use of a second lanthanide in the border areas between the existing grains, which already have an iron-boron alloy and a lanthanide contained therein, causes a significant increase in the permanent magnetic properties compared to pure iron-boron-lanthanide materials.
  • the salt which is also infiltrated with the second lanthanide into the pores of the porous preliminary body causes a reduction in the electrical conductivity compared to a purely metallic permanent magnet based on iron, boron and lanthanide, for example also iron, boron and neodymium.
  • the second lanthanide increases the magnetic properties and that the salt introduced with the second lanthanide reduces the electrical conductance in order to create high frequency stability.
  • the first lanthanide is neodymium.
  • Iron-boron-neodymium permanent magnets basically have very good permanent magnetic properties.
  • the second lanthanide, which is infiltrated in the porous preliminary body together with salt, preferably has a higher atomic number than the first lanthanide.
  • the elements dysprosium and terbium are suitable for this purpose, in particular in contrast to the first lanthanide neodymium. Mixtures or alloys of these elements can also be useful.
  • a salt that is soluble in the liquid phase of the second lanthanide and combines with it is advantageously used as the added salt that reduces the electrical conductance of the magnetic material. Therefore e.g. B. the oxide of dysprosium or terbium very well suited.
  • a fluoride can also be suitable as a salt, since fluorides can be easily dissolved in the liquid phase of the second lanthanide.
  • the salts calcium fluoride or neodymium fluoride are particularly suitable.
  • a further advantage of the invention is that, due to the process steps described, it is possible to use a grain size distribution which is between 100 and 300 micrometers. This preferably includes 80% of the grains of the magnetic powder present in the microstructure of the resulting material.
  • the particle size distribution is determined by sieve analysis.
  • the grain distribution in the microstructure of the magnetic material is analyzed by image analysis of a light micrograph of a micrograph of the magnetic material.
  • the element distribution within the grains is determined by a quantified EDX evaluation based on a scanning electron microscope evaluation of the micrograph.
  • Another component of the invention is a sintered, polymer-free magnetic material with the features of claim 10.
  • This has a microstructure that is between 60 vol% and 80 vol% lanthanide iron boron grains.
  • the grains have at least 80 at% iron and boron in their core. In their edge area, the grains contain more than 50 at% of a first lanthanide, which is present there in an increased concentration, in addition to the iron and boron.
  • the magnetic material is characterized by the fact that between the lanthanide-FeB grains there is an intermediate phase that contains more than 50 at% of a second element from the lanthanide series, i.e. a second lanthanide that has a higher atomic number than the first lanthanide , which is present in the grains. Furthermore, this intermediate phase contains a salt, with the electrical conductivity of the magnetic material being less than 10 S/m.
  • the magnetic material described has the same advantageous properties that have already been described with regard to the method for producing this magnetic material.
  • the introduction of the second lanthanide into the intermediate phase, together with the salt described, leads on the one hand to an increase in the permanent magnetic properties with a simultaneous reduction in the electrical conductance by the salt.
  • the permanent magnet itself, it is expedient to use neodymium as the first lanthanide element, which together with iron and boron results in a very good permanent magnet. Furthermore, it is expedient to use dysprosium or terbium or alloys thereof as the second lanthanide, which increases the magnetic properties even further.
  • the oxide of dysprosium and terbium, or a fluoride of calcium or dysprosium, are also particularly suitable for dissolving in the second lanthanide and bringing about a reduction in the electrical conductance there.
  • the magnet material is particularly preferably characterized by a low porosity, with this in particular being less than 20 vol%.
  • the porosity is measured by mercury porosimetry.
  • FIG 1 is purely schematic the manufacturing process for producing a magnetic material 2, which at the end of the process chain figure 1 is shown.
  • a mixture 4 is first provided in any mixing device 48 , which comprises a magnetic powder 6 and a binder 10 .
  • This mixture is shaped into a porous preform 12 in a shaping process using any desired shaping device 42, shown here for example in the form of a uniaxial press.
  • any desired shaping device 42 shown here for example in the form of a uniaxial press.
  • isostatic pressing of the preliminary body 12 or an extrusion method could also be used.
  • the resulting preliminary body 12 thus has the binder 10 and the magnetic powder 6, wherein in a further step, a debinding step 14, in a debinding oven 44 at elevated temperature, for example at 220 ° C, the binder 10 is thermally decomposed and from the Pre-body 12 exits.
  • This process step is called debinding.
  • the formerly essentially dense preliminary body 12 has become a porous preliminary body 16 since the binder 10 previously contained has decomposed thermally or chemically and has escaped from the preliminary body 12 .
  • the porous preform 16 is now fed to an infiltration step.
  • a second mixture 18 is first provided, which includes a second lanthanide 20 and a salt 22, which are added together to a solvent 24, from which a solution 26 is formed.
  • the solution 26 is infiltrated into the porous preform 16 by capillary forces.
  • infiltration is to be understood broadly.
  • the description using a solvent is an exemplary, advantageous embodiment.
  • the lanthanide could also be brought to an appropriate melting temperature
  • the salt 22 could be dissolved in it and the open-pored preform 16 could be infiltrated with the second mixture in the liquid phase in a high-temperature process.
  • CVD or CVI chemical vapor deposition
  • an infiltrated preliminary body 30 is spoken of, which is sintered in a further process step, a heat treatment 28 in a heat treatment furnace 46 at a sintering temperature to form the magnetic material 2 .
  • the heat treatment 28 is preferably a diffusion-controlled sintering process in which there is preferably no liquid phase in the microstructure of a sintered body 52 (transitional state between infiltrated preliminary body 30 and magnetic material 2) during the process.
  • a diffusion-controlled sintering process in which there is preferably no liquid phase in the microstructure of a sintered body 52 (transitional state between infiltrated preliminary body 30 and magnetic material 2) during the process.
  • the sintered body 52 states of aggregation, which indeed have liquid phase fractions, but with the exchange of Materials between grains 32 diffusion processes dominate.
  • a microstructure 34 as shown in figure 3 is shown can be achieved.
  • FIG 3 a typical magnetic grain 32 of the magnetic powder 6 is first shown, which has an iron-boron (FeB) phase 36 in an inner region.
  • FeB iron-boron
  • an edge region 38 of the grain 32 there is a phase which is very strongly enriched with a first lanthanide, in particular neodymium.
  • the atomic proportion of the neodymium in the edge region 38 preferably has more than 50%.
  • 38 iron-boron atoms can also be present in the edge area. It has been found that a magnetic powder 6 designed in this way with the magnetic grains 32 and the edge region 38 rich in lanthanide described can produce a magnetic material 2 which has very good permanent magnetic properties.
  • Such grains usually have a grain diameter of between 100 ⁇ m and 300 ⁇ m (preferably 200 ⁇ m), whereby they preferably have a grain substructure (not shown graphically here) in the size range of 5 ⁇ m and 15 ⁇ m, which belongs to the good permanent-magnetic or Contribute to hard magnetic properties.
  • microstructure 34 is a result of the manufacturing process described, in particular through the infiltration of a porous preform 16 with a second lanthanide and a salt 22 and the subsequent diffusion-controlled sintering process 28.
  • the microstructure 34 shown is characterized in particular by the figure 2 described grains 32, which have an iron-boron core and are surrounded by a border area 38 rich in neodymium. Occasionally, the grains 32 are also connected to one another by the formation of sinter necks 50 . For the most part, however, there is an intermediate phase 40 between the grains 32 , which comprises the second lanthanide 20 and the salt 22 .
  • the second lanthanide 20 for example dysprosium or terbium, with a salt 22 of dysprosium or terbium or a calcium fluoride, dominates the intermediate phase 40.
  • dysprosium or terbium atoms also diffuse in the edge region 38 of the grains 32.
  • the iron-boron core of the grains 32 is replaced by neodymium and enriched with a heavier, higher atomic number lanthanide such as dysprosium or terbium, further enhancing the permanent magnetic properties of the iron-boron.
  • the porosity of the microstructure 34 or of the magnetic material 2 is very low; it is preferably below 20% by volume, particularly preferably below 10% by volume. Such a low porosity can be achieved in particular by the sintering process described.
  • the described microstructure 34 proves to be a typical microstructure that is achieved by a diffusion-controlled process. If the liquid phase were to dominate during production or during the sintering process, as is often the case in the prior art, then the microstructure would be dominated by melt phases.
  • the original grain 32 is only present in a slightly modified form with a higher degree of lanthanide enrichment in the edge region 38 .
  • grains 32 used to have a larger diameter than is usual in the prior art are expedient in the case of the described material 2 and the microstructure 34 for the grains 32 used to have a larger diameter than is usual in the prior art.
  • Grains 32 have a diameter between 100 and 300 microns, preferably between 150 and 250 microns. You are in accordance figure 2 advantageous shape with core area 36 and edge area 38 can be produced better.
  • a A grain 32 designed in this way leads to better permanent magnetic properties in the microstructure 34 or in the magnetic material 2 .
  • liquid phase sintering processes require the use of grains smaller than 20 microns. Such small grains, which are not shown here, lead to poorer magnetic properties.
  • Good hard magnetic magnet materials 2 which were produced by the method described or according to a microstructure figure 3 have a remanence B r of 1.1 T and a coercivity H c of about 2600 kA/m and an energy product (B ⁇ H) max of 225 kJ/m 3 in example A and a remanence B r in example B of 1.5 T and a coercivity Hc of about 1400 kA/m and an energy product (B ⁇ H) max of 410 kJ/m 3

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
EP22155955.2A 2022-02-09 2022-02-09 Procédé de fabrication d'une matière magnétique et matière magnétique Pending EP4227963A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP22155955.2A EP4227963A1 (fr) 2022-02-09 2022-02-09 Procédé de fabrication d'une matière magnétique et matière magnétique

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP22155955.2A EP4227963A1 (fr) 2022-02-09 2022-02-09 Procédé de fabrication d'une matière magnétique et matière magnétique

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EP4227963A1 true EP4227963A1 (fr) 2023-08-16

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2043114A1 (fr) * 2006-11-30 2009-04-01 Hitachi Metals, Ltd. Aimant haute densité micro-cristallin r-fe-b et son procédé de fabrication
CN105976959A (zh) * 2016-07-14 2016-09-28 安徽万磁电子有限公司 一种铽钇离子注入的镀镍钕铁硼磁体及其制备方法
WO2017055170A1 (fr) * 2015-09-28 2017-04-06 OBE OHNMACHT & BAUMGäRTNER GMBH & CO. KG Procédé de fabrication d'un aimant permanent
WO2021071236A1 (fr) * 2019-10-07 2021-04-15 주식회사 엘지화학 Procédé de fabrication d'aimant fritté
DE102020211857A1 (de) * 2020-09-22 2022-03-24 Mimplus Technologies Gmbh & Co. Kg Verfahren zur Herstellung eines Permanentmagneten aus einem magnetischen Ausgangsmaterial

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2043114A1 (fr) * 2006-11-30 2009-04-01 Hitachi Metals, Ltd. Aimant haute densité micro-cristallin r-fe-b et son procédé de fabrication
WO2017055170A1 (fr) * 2015-09-28 2017-04-06 OBE OHNMACHT & BAUMGäRTNER GMBH & CO. KG Procédé de fabrication d'un aimant permanent
CN105976959A (zh) * 2016-07-14 2016-09-28 安徽万磁电子有限公司 一种铽钇离子注入的镀镍钕铁硼磁体及其制备方法
WO2021071236A1 (fr) * 2019-10-07 2021-04-15 주식회사 엘지화학 Procédé de fabrication d'aimant fritté
DE102020211857A1 (de) * 2020-09-22 2022-03-24 Mimplus Technologies Gmbh & Co. Kg Verfahren zur Herstellung eines Permanentmagneten aus einem magnetischen Ausgangsmaterial

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