EP0505348B1 - Matériau pour aimant permanant ou aimant permanant fritté et procédé de fabrication - Google Patents

Matériau pour aimant permanant ou aimant permanant fritté et procédé de fabrication Download PDF

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Publication number
EP0505348B1
EP0505348B1 EP92890055A EP92890055A EP0505348B1 EP 0505348 B1 EP0505348 B1 EP 0505348B1 EP 92890055 A EP92890055 A EP 92890055A EP 92890055 A EP92890055 A EP 92890055A EP 0505348 B1 EP0505348 B1 EP 0505348B1
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EP
European Patent Office
Prior art keywords
phase
hard magnetic
sintered
magnetic
permanent
Prior art date
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EP92890055A
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German (de)
English (en)
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EP0505348A1 (fr
Inventor
Adolf Dipl.-Ing. Diebold
Oskar Dr. Pacher
Siegfried Dr. Heiss
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Vacuumschmelze GmbH and Co KG
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Vacuumschmelze GmbH and Co KG
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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

Definitions

  • the invention relates to a sintered permanent magnet (material) containing 8 to 30 at.% Rare earths (SE), 2 to 28 at.% Boron (B), remainder iron (Fe) or iron and cobalt (Co) a hard magnetic component or with a hard magnetic phase of the Se 2 Fe 14 B type, it being possible for some of the Fe atoms to be replaced by Co atoms.
  • SE Rare earths
  • B Boron
  • Fe remainder iron
  • Co cobalt
  • Permanent magnets or permanent materials made essentially of an alloy of iron (Fe), optionally cobalt (Co), boron (B) and rare earth (SE) sintered, are preferably used when high coercive force, high remanence and / or large Energy product are required.
  • the component forming or containing the magnetic phase of the Se 2 Fe 14 B type, some of the Fe atoms being able to be replaced by Co atoms, is produced and pulverized by melt metallurgy, which powder, optionally mixed with additives, is pressed into a green compact in a magnetic field and this is sintered and the sintered body can optionally be subjected to at least one further heat treatment.
  • An SE-Fe-B permanent magnet material in which an alloy additive containing an element from the group of the heavy SE and / or SSE compounds, optionally with grain boundary additives, is added to the grain boundaries of the grains, which are formed from a magnetic phase is disclosed by EP-A-0395625.
  • a sintered magnet is known from WO-A-8902156, the structure of which is free of large Fe 4 NdB 4 grains and the composition of which is selected such that the material at sintering temperature is in a two-phase area, namely in a hard magnetic phase and an Nd-rich phase.
  • EP-A-0425469 relates to a sintered SE-Fe-B permanent magnet (material) in which the local concentration of the SE content increases essentially at the grain boundaries of the magnetic phase, that is to say that an inhomogeneous distribution of the SE content is given.
  • JP-62274046 a permanent magnet which consists of a sintered powder mixture which is formed from at least two types of powder.
  • Nd 2 Fe 14 B 6 i.e. a hard magnetic phase
  • Nd paramagnetic alloy of Nd 95 Fe 5 and / or Nd 15 F 77 B 8 and / or Nd 2 FeB 16 and / or Nd 2 Fe 7 B 6 mixed.
  • the invention has for its object to eliminate the disadvantages of the known SE, (FeCo), B - containing magnets (materials) and their manufacturing processes and to specify and create sintered permanent magnets, the high saturation magnetization, high coercive force and high energy product with good temperature stability and have a high Curie point at low manufacturing costs.
  • Another object of the invention is to make the height of the Curie point of the permanent magnets (materials) easily adjustable according to the requirements.
  • the hard magnetic component is formed from a plurality of magnetic phases which, as has been shown completely surprisingly, interact advantageously with one another. It is important here that one or more magnetic phases as the central phase or core phase are formed from surface-smoothed or diffusion-molded grains, whereby according to the latest findings, surface recrystallization can take place by diffusion and a further magnetic phase component is oriented towards the central phase as a peripheral phase or is attached to it assigns. As a result, a high proportion of magnetic volume in the material can be achieved and domain wall formation and / or domain wall displacement can be reduced, as a result of which an increase in the coercive force and consequently in the energy product occurs.
  • the paramagnetic intermediate or binding phase should have a higher concentration of SE than the magnetic phases and, if appropriate, inclusions and / or additives, as a result of which a further blocking of domain walls is accomplished.
  • Special magnetic properties of the material are achieved if the grains of the central or core phase have a diameter of 10 to 100 ⁇ m and the magnetic peripheral phase or phases are or are attached to the grains in a shell-like manner.
  • the RE portion in the magnetic phases is essentially formed by light rare earths (LSE), in particular Nd, and the RE portion in the intermediate or binding phase contains heavy rare earths (SSE), particularly high levels become Magnetic characteristics of the magnet reached.
  • LSE light rare earths
  • SSE heavy rare earths
  • the invention further relates to a method for producing rare earth (SE) containing (s), magnetically aligned (s), sintered (s) permanent magnet (s) according to claim 1, its base material or starting material by melt metallurgy is produced, this or this is essentially ground into powder, mixed with additives, pressed into a green body and the green body is sintered and annealed. According to the invention, such a method is characterized by the characterizing features of claim 8.
  • the advantages of the invention consist in particular in that at least two magnetic phase-forming base materials or starting materials with different chemical compositions and therefore different magnetic properties are produced, comminuted into powders and mixed, as a result of which an interaction of the base materials which has a favorable influence on the magnetic characteristics can be achieved.
  • a basic material is comminuted to powder with smaller particle sizes or to fine powder, which shows an earlier softening or plasticity during the sintering of the green compact pressed under magnetic field alignment and produces particularly good contact with the particles or grains of the coarse powder. This is important for the effect of the diffusion treatment or annealing, the phase boundaries being designed to be correspondingly favorable.
  • the SE concentration of the base materials is dimensioned higher than that of the magnetic phase of type SE 2 (FeCo) 14 B, the compositions SE 16 (FeCo) 77 B 7 , SE 15 (Feco) having been found. 77 B 8 and SE 14 (FeCo) 80 B 6 are particularly suitable. If at least one base material is alloyed with Co and the iron portion of the magnetic phase is substituted by up to 40% with Co, particularly good temperature stability and high Curie temperatures of the magnets can be achieved.
  • the SE portion of the base materials is essentially formed by LSE, the remanence and the energy product are increased.
  • one or more base materials are comminuted into coarse powder with a grain diameter of 10 to 100 ⁇ m, preferably 10 to 60 ⁇ m, in particular 15 to 30 ⁇ m, and at least one further base material is ground to fine powder with a particle diameter of 0.5 to 8 ⁇ m, in particular from 3 to 8 ⁇ m, different co-contents in the coarse and fine powder further improving the magnetic characteristics.
  • compounds of SSE such as, for example, Dy 2 O 3 and / or borides, for example Fe 2 B, and / or metals, for example Al, and / or oxides, for example A 12 O 3 and / or SE oxides are introduced, in particular the powders are mechanically alloyed with these substances, domain wall formation and domain wall displacement are further reduced and higher coercive forces are achieved.
  • a particularly important feature of the invention is a diffusion treatment of the sintered magnet (s) (material), which is advantageously carried out at a temperature below the sintering temperature and expediently in the pendulum annealing process, because the grain surfaces of the coarse powder are smoothed and a microstructure-oriented on the smoothed grain surfaces essentially shell-like accumulation of the phase formed by the fine powder is brought about, which brings about a significant improvement in the magnetic characteristics.
  • s sintered magnet
  • FIG. 1 and 2 show schematically the sequence of manufacture of permanent magnet materials according to the invention.
  • Table 1 shows compositions of the base materials with stoichiometric parameters.
  • Table 2 shows the compositions and the magnetic characteristics of reference magnets (materials) with the designation V1 to V7.
  • Tables 3a and 3b under numbers 1 to 23 list permanent magnets (materials) according to the invention.
  • high magnetic characteristics at an elevated Curie temperature are achieved by the construction with a plurality of differently composed magnetic phases with diffusion molded grains and deposits.
  • Table 1 Base material Range Nd 16 (Fe 1-x Co x ) 77 B 7 A Nd 15 (Fe 1-x Co x ) 77 B 8 B Nd 14 (Fe 1-x Co x ) 80 B 6 C. (Nd 1-y Dy y ) 16 Fe 77 B 7 D (Nd 1-y Dy y ) (Fe 1-x Co x ) 78 B 6 E No. Basic magnetic phase Magnetic values Ref. Troubles Vert.

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)
  • Soft Magnetic Materials (AREA)
  • Magnetic Ceramics (AREA)

Claims (17)

  1. Matériau pour aimant permanent ou aimant permanent fritté contenant 8 à 30 % atomiques de terres rares (SE), de 2 à 28 % atomiques de bore (B), le reste étant formé de fer (Fe) ou de fer et de cobalt (Co), avec une partie en matériau magnétique dur ou une phase magnétique dure du type Se2Fe14B, une partie des atomes de Fe pouvant être remplacée par des atomes de Co, caractérisé en ce que la partie en matériau magnétique dur intervient pour au moins 65 % en volume, et cette partie en matériau magnétique dur est constituée par au moins deux phases magnétiques dures ayant des compositions chimiques différentes, au moins une phase magnétique dure étant formée dans la structure frittée par des grains plus grossiers à surface lissée, en tant que phase centrale à laquelle est fixée au moins une autre phase magnétique dure en tant que phase périphérique et dont la(les) phase(s) paramagnétique(s) de liaison, qui relient les parties magnétiques dures des phases de ce matériau, possèdent une concentration plus élevée en SE par rapport à celle des phases magnétiques dures.
  2. Matériau pour aimant permanent ou aimant permanent fritté selon la revendication 1, caractérisé en ce que les grains à surface lissée de la ou des phases centrales magnétiques dures possèdent un diamètre compris entre 10 et 100 µm et de préférence entre 10 et 60 µm et notamment entre 15 et 30 µm.
  3. Matériau pour aimant permanent ou aimant permanent fritté selon la revendication 1 ou 2, caractérisé en ce que la ou les phases périphériques magnétiques dures s'appliquent essentiellement contre les coupures de grain à surface lissée de la ou des phases centrales magnétiques dures, et notamment s'y fixent selon une forme de coque.
  4. Matériau pour aimant permanent ou aimant permanent fritté selon l'une des revendications 1 à 3, caractérisé en ce que la ou les phases centrales magnétiques dures et/ou la ou les phases périphériques magnétiques dures possèdent différents éléments SE et/ou différentes concentrations de Co.
  5. Matériau pour aimant permanent ou aimant permanent fritté selon l'une des revendications 1 à 4, caractérisé en ce qu'au moins une phase centrale magnétique dure possède une concentration en Co supérieure à celle de la ou des phases périphériques magnétiques dures, qui sont de préférence pauvres en Co ou ne comportent pas de Co.
  6. Matériau pour aimant permanent ou aimant permanent fritté selon l'une des revendications 1 à 5, caractérisé en ce que les concentrations locales en Co au niveau des coupures de grain ou dans la zone des coupures de grain entre phases possédant des teneurs différentes en Co comportent des transitions brusques formées conformément à la cinétique de diffusion.
  7. Matériau pour aimant permanent ou aimant permanent fritté selon l'une des revendications 1 à 6, caractérisé en ce que la partie SE dans les phases magnétiques dures est formée essentiellement par des terres rares légères (LSE), notamment par du Nd, et que la ou les parties SE dans la ou les phases de liaison, qui peuvent contenir des additifs de borures et/ou d'oxydes et/ou de métaux, contiennent essentiellement des terres rares lourdes (SSE), notamment du Dy.
  8. Procédé pour fabriquer des aimants permanents frittés, contenant des terres rares (SE) et orientés magnétiquement et contenant 8 à 30 % atomiques de terres rares (SE), 2 à 28 % atomiques de bore (B), le reste étant formé de (Fe) ou de fer et de cobalt (Co) comportant une partie formant matériau magnétique dur ou une phase magnétique dure du type Se2Fe14B, une partie des atomes de Fe pouvant être remplacée par des atomes de Co, le matériau de base ou le matériau de départ de ces aimants étant fabriqué au moyen de la métallurgie à fusion, tous ces matériaux de base sont fragmentés essentiellement pour former une poudre, à laquelle on mélange des additifs et que l'on presse pour former un compact vert, que l'on fritte et que l'on soumet à un recuit, pour fabriquer des aimants permanents frittés selon l'une quelconque des revendications 1 à 7, caractérisé en ce qu'on fait fondre au moins deux matériaux de base ou deux matériaux de départ et qu'on les laisse se solidifier, auquel cas, pour au moins un matériau de base, on règle une composition chimique qui diffère de l'autre matériau de base et on fragmente les matériaux de base pour former une poudre, on exécute la fragmentation d'au moins un matériau de base pour former une poudre ayant des tailles de particules ou des diamètres de grains nettement plus faibles, à la suite de quoi on ajoute des additifs et on les mélange aux matériaux de base pulvérisés, puis on presse le mélange, comme cela est connu en soi, moyennant une orientation du champ magnétique pour former un compact vert, et on fritte ce dernier et on soumet le corps fritté à un traitement de recuit pour obtenir un lissage de surface des grains de la phase centrale.
  9. Procédé selon la revendication 8, caractérisé en ce qu'on fait fondre les matériaux de base possédant une concentration en SE supérieure à ce qui correspond à la phase magnétique du type Se2(FeCo)14B, et on fabrique les matériaux de base notamment avec des compositions correspondant à
    SE16(Fe,Co)77B7
    SE15(Fe,Co)77B8
    SE14(Fe,Co)80B6,
    l'expression (Fe,Co) désignant la partie de Fe, qui est éventuellement partiellement substituée par du Co.
  10. Procédé suivant la revendication 8 ou 9, caractérisé en ce qu'on allie au moins un matériau de base avec du Co et qu'on remplace la composante de fer jusqu'à 40 % par du Co.
  11. Procédé suivant l'une des revendications 8 à 10, caractérisé en ce que la partie de SE des matériaux de base est formée essentiellement par des terres rares légères (LSE).
  12. Procédé suivant l'une des revendications 8 à 11, caractérisé en ce qu'on fragmente un ou plusieurs matériaux de base pour former une poudre grossière ayant un diamètre de particules ou un diamètre de grains de 10 à 100 µm et de préférence de 10 à 60 µm et notamment de 15 à 30 µm, et qu'on broie au moins un autre matériau de base pour former une poudre fine avec un diamètre de grains de 0,5 à 8 µm, notamment de 3 à 8 µm.
  13. Procédé suivant l'une des revendications 8 à 12, caractérisé en ce qu'on fabrique le ou au moins un matériau de base, qui est fragmenté pour former une poudre grossière, comparativement au matériau de base ou à au moins un matériau de base, que l'on broie pour obtenir une poudre fine, avec différentes terres rares SE et/ou avec différentes teneurs en Co.
  14. Procédé suivant l'une des revendications 8 à 13, caractérisé en ce que l'on introduit, comme cela est connu en soi, des additifs sous forme solide et/ou liquide, par exemple des composés organa-métalliques, dans la poudre grossière et/ou dans la poudre fine des matériaux de base, notamment avant ou lors de leur broyage préalable ou de leur introduction en mélange, et qu'on les répartit de façon homogène dans le mélange de poudre.
  15. Procédé suivant l'une des revendications 8 et 14, caractérisé en ce que, comme cela est connu en soi, on ajoute, comme additifs, des composés de terres rares lourdes (SSE) et éventuellement de métaux, de borures par exemple de fer et/ou d'aluminium, des oxydes, par exemple du Al2O3, ou des oxydes de terres rares SE et analogues au(x) matériau(x) de base sous forme de poudre et qu'on les répartit de façon homogène.
  16. Procédé suivant l'une des revendications 8 ainsi que 14 et 15, caractérisé en ce qu'on fritte le compact vert formé par pressage avec le mélange de poudre homogène contenant des additifs, moyennant une orientation du champ magnétique et qu'ensuite on exécute un lissage de la surface, à une température inférieure à la température de frittage, de préférence lors du processus de recuit alternatif autour de cette température.
  17. Procédé suivant l'une des revendications 8 à 16, caractérisé en ce qu'on lisse la surface des grains de la ou des poudres grossières et qu'on oriente la microstructure au niveau des surfaces lissées des grains et qu'on applique, de préférence sous la forme d'une coque, la phase formée par la poudre fine.
EP92890055A 1991-03-18 1992-03-11 Matériau pour aimant permanant ou aimant permanant fritté et procédé de fabrication Expired - Lifetime EP0505348B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT596/91 1991-03-18
AT0059691A AT399415B (de) 1991-03-18 1991-03-18 Verfahren zur herstellung von seltene erden enthaltendem(n) permanentmagnet(-en) (-werkstoffen)

Publications (2)

Publication Number Publication Date
EP0505348A1 EP0505348A1 (fr) 1992-09-23
EP0505348B1 true EP0505348B1 (fr) 1996-10-16

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Country Status (9)

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EP (1) EP0505348B1 (fr)
AT (2) AT399415B (fr)
CZ (1) CZ281163B6 (fr)
DE (1) DE59207356D1 (fr)
DK (1) DK0505348T3 (fr)
ES (1) ES2095454T3 (fr)
GR (1) GR3022263T3 (fr)
HU (1) HU216373B (fr)
PL (1) PL293878A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4331563A1 (de) * 1992-09-18 1994-03-24 Hitachi Metals Ltd Nd-Fe-B-Sintermagnete

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3729361A1 (de) * 1987-09-02 1989-03-16 Max Planck Gesellschaft Optimierung der gefuegestruktur des fe-nd-b-basis sintermagneten
AT393177B (de) * 1989-04-28 1991-08-26 Boehler Gmbh Permanentmagnet(-werkstoff) sowie verfahren zur herstellung desselben
AT393178B (de) * 1989-10-25 1991-08-26 Boehler Gmbh Permanentmagnet(-werkstoff) sowie verfahren zur herstellung desselben

Also Published As

Publication number Publication date
HUT62341A (en) 1993-04-28
CZ78492A3 (en) 1993-12-15
AT399415B (de) 1995-05-26
ATE144348T1 (de) 1996-11-15
HU9200889D0 (en) 1992-05-28
DE59207356D1 (de) 1996-11-21
PL293878A1 (en) 1992-10-19
EP0505348A1 (fr) 1992-09-23
DK0505348T3 (da) 1997-03-24
HU216373B (hu) 1999-06-28
ES2095454T3 (es) 1997-02-16
CZ281163B6 (cs) 1996-07-17
GR3022263T3 (en) 1997-04-30
ATA59691A (de) 1994-09-15

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