EP0502397B1 - Procédé de fabrication d'un matériau magnétiquement doux à base de fer à haute magnétisation de saturation et à structure de graines ultrafine - Google Patents

Procédé de fabrication d'un matériau magnétiquement doux à base de fer à haute magnétisation de saturation et à structure de graines ultrafine Download PDF

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Publication number
EP0502397B1
EP0502397B1 EP92103081A EP92103081A EP0502397B1 EP 0502397 B1 EP0502397 B1 EP 0502397B1 EP 92103081 A EP92103081 A EP 92103081A EP 92103081 A EP92103081 A EP 92103081A EP 0502397 B1 EP0502397 B1 EP 0502397B1
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EP
European Patent Office
Prior art keywords
powder
main component
process according
component
heat treatment
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.)
Expired - Lifetime
Application number
EP92103081A
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German (de)
English (en)
Other versions
EP0502397A2 (fr
EP0502397A3 (en
Inventor
Christian Dr. Kuhrt
Ludwig Dr. Schultz
Kurt Dipl.-Ing. Schnitzke
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Siemens AG
Siemens Corp
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Siemens AG
Siemens Corp
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Publication of EP0502397B1 publication Critical patent/EP0502397B1/fr
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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
    • H01F1/12—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 soft-magnetic materials
    • H01F1/14—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 soft-magnetic materials metals or alloys
    • H01F1/20—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • 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
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
    • 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
    • H01F1/12—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 soft-magnetic materials
    • H01F1/14—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 soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
    • 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
    • H01F1/12—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 soft-magnetic materials
    • H01F1/14—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 soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15341—Preparation processes therefor
    • H01F1/1535—Preparation processes therefor by powder metallurgy, e.g. spark erosion

Definitions

  • the invention relates to a method for producing a soft magnetic, Fe-containing material with high saturation magnetization and an ultra-fine structure. Such a method is e.g. from "J. Appl. Phys.”, Vol. 64, No. 10, Nov. 1988, pages 6044 to 6046.
  • Soft-magnetic alloys based on Fe with an ultra-fine structure can be provided in particular for magnetic components in which minimal hysteresis losses and / or low eddy current losses are important in high-frequency applications.
  • Nanocrystalline Fe-Si-Nb-Cu-B alloys with average grain sizes of about 10 to 20 nm are known, which have excellent soft magnetic properties, ie a small coercive force H c of less than 0.01 A / cm and a high permeability.
  • the known alloy is obtained from rapidly solidified strips, which are initially amorphous and in which the nanocrystalline Fe-Si phase is eliminated as the main component by subsequent heat treatment above the crystallization temperature.
  • the glass former boron cannot be dispensed with in the production of such rapidly solidified amorphous ribbons. This limits the saturation magnetization of the soft magnetic material to values of approximately 1.2 to 1.3 T.
  • This object is achieved in that a starting powder from an Fe-containing main component of the material is ground and with such intensity until a powdery ground material is obtained from powder particles of the main component with an average grain size between 5 and 50 nm, and then the regrind is subjected to a heat treatment at a temperature below 600 ° C for a maximum of one hour.
  • the invention is based on the finding that numerous stresses and defects are introduced into the material by a grinding process, which causes an intensive cold deformation of the Fe-containing main component, which are due to magnetostrictive Effects act as Blochwand pinning centers and magnetically harden the material.
  • a heat treatment of the mechanically alloyed material is now carried out according to the invention at a temperature at which these tensions and defects heal, but excessive grain growth does not yet occur.
  • the advantages associated with this can be seen in particular in the fact that a nanocrystalline material of extremely small coercive field strength and high saturation magnetization can be obtained.
  • a starting powder can first of all be formed particularly advantageously from the Fe-containing main component of the material and 0.1 to 10 atom% of an Fe-free additional component, which shows practically no solubility in the main component in thermodynamic equilibrium.
  • This starting powder is then to be ground until a mixed powder of powder particles having the predetermined average grain size and consisting of the main component with the additional component embedded therein has formed as the ground material.
  • Such an additional component in the regrind of the main component advantageously supports the healing process with regard to the stresses and defects which are undesirably introduced into the material by the grinding. This takes place in that this additional component preferably precipitates at the grain boundaries in the final heat treatment and thus stabilizes the individual grains with regard to undesired grain growth, i.e. hindered this growth.
  • the invention is explained in more detail below using an exemplary embodiment, reference being made to the drawing.
  • the figure shows a diagram of the saturation magnetization of a material produced according to the invention.
  • Common soft magnetic materials which have a saturation magnetization M s of at least 1.3 T are preferably alloys which contain at least one further component in addition to the component Fe. At least one element from the group of the elements Co, Si, Al, Ni is preferably considered as a further component.
  • the percentage composition of the individual components is chosen from the point of view of the highest possible saturation magnetization and a small magnetocrystalline anisotropy and magnetostriction constants. From this point of view, for example, an approximate composition of the Fe component with about 42 atomic% Co, or about 22 atomic% Si, or about 70 atomic% Ni or about 25 atomic% Al can be regarded as favorable. This Fe component and the at least one further component form the main component of the material to be produced.
  • the main component can also be three-component or even higher component, whereby minor impurities of the elements with a respective proportion below 0.1 atom% should always be included.
  • at least one element from the group of the elements Ti, V, Nb, Ta, Cr, Mo, W, Mn, Al, Sb, Ge, Sn, Zr, Hf can be provided as the third component.
  • This third component can be selected, for example, from the point of view of the material's resistance to corrosion. In general, their proportion within the main component is less than 20 atom%, in particular less than 10 atom%.
  • an additional component with a proportion within the material of between 0.1 atom% and 10 atom% is provided for the production of the soft magnetic material.
  • the choice of material for this additional component is to be carried out such that, on the one hand, the additional component in the thermodynamic equilibrium of the overall system consisting of the main component and the additional component has practically no solubility in the Main component shows during the individual process steps.
  • the material of the additional component during heat treatment after the step of mechanically alloying the main and additional components on the surface of the individual grains of the main component is said to settle in a quasi-precipitation reaction.
  • the material of the additional component is in particular an element from the first or second group of the periodic table (Li, Na, K, Rb, Cs or Ca, Sr, Ba, Mg) or one of the elements Pb, Bi, In, Cu, Ag, Sn, Cd or Hg in question. Pb or Bi are particularly suitable.
  • the material system Fe-Co is selected as the main component for the exemplary embodiment.
  • the zero crossing of the magnetocrystalline anisotropy constant K 1, which must be as small as possible in order to achieve small H c values, is in this composition range (at about 42 atomic% Co).
  • elemental Fe and Co powders or powders made of an Fe-Co master alloy with a composition in the range of around 60 atomic% Fe and 40 atomic% Co are added together with some as the main component of the material to be produced %
  • Pb or Bi powder weighed out as Fe-free additional component The proportion of this additional component within the powder mixture thus composed should in particular be between 2 and 5 atomic%.
  • the individual powders of the constituents of the powder mixture involved should be sufficiently pure and in particular each have a purity of at least 99.5%.
  • This powder mixture forming the starting powder with predetermined, Generally customary particle sizes of their powdery constituents in the order of magnitude of the largest diameters between 1 »m and 1 mm are now placed in a suitable grinding device, as is known in principle from processes of" mechanical alloying "(see, for example,” Metal. “, Vol. 5, Aug. 1974, pages 1929 to 1934).
  • the starting powder is then subjected to the grinding process, for example in a planetary ball mill, with the aid of hardened steel balls in a container made of hardened steel, for example filled with H2 or Ar.
  • the grinding time t m of the grinding process depends in particular on the grinding parameters. Important parameters are the ball diameter, the number of balls and the materials used for the grinding device.
  • the grinding speed and the ratio of the steel balls to the amount of powder are further parameters that determine the necessary grinding time.
  • the spherical mass can be, for example, approximately 10 times the powder mass.
  • the starting powder is progressively converted into a mixed powder with particles consisting of an alloy of the main component Fe-Co with additional components arranged statistically distributed at their lattice sites Pb or Bi exist.
  • a grinding time of several hours in general more than 10 hours, for example from at least 60 hours, required.
  • the finely crystalline regrind to be obtained in this way is finally subjected to a special heat treatment under protective gas such as Ar or in a vacuum.
  • protective gas such as Ar or in a vacuum.
  • the temperature must not be too high and the heat treatment time must not be too long to avoid excessive grain growth. Therefore, the temperature must in any case be below 600 ° C, preferably below 400 ° C and in particular between about 150 ° C and 250 ° C.
  • the duration of the heat treatment may not be longer than one hour, although longer times are permissible at relatively low temperatures than at higher temperatures. The exact duration can be determined experimentally depending on the given temperature by observing the grain growth.
  • an additional component which precipitates on the individual grains during the final heat treatment can optionally be dispensed with and a significant reduction in the coercive field strength of the ground material can nevertheless be achieved by means of this heat treatment.
  • the magnetization M (in T) as a function of the applied field strength H (in kOe) is plotted in the diagram of the drawing.
  • a saturation magnetization M s of approximately 2.35 T can be achieved for this material.
  • the material is to be regarded as soft magnetic, since its coercive field strength is clearly below 10 A / cm.
  • the soft magnetic materials produced according to the invention can be processed further in a known manner. For example, compact the powder into a shaped body with a desired shape.
  • a plastic-bonded magnetic body can also be produced from the powder by casting with a plastic without a special compacting step.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Soft Magnetic Materials (AREA)
  • Paints Or Removers (AREA)
  • Hard Magnetic Materials (AREA)

Claims (9)

  1. Procédé de fabrication d'un matériau magnétique doux, contenant du fer, présentant une saturation magnetique elevee et pourvu d'une structure granulométrique ultrafine, procédé caractérisé en ce qu'une poudre initiale, obtenue a partir d'un constituant principal ferreux du materiau, est broyee pendant la duree et avec l'intensité nécessaires pour obtenir une matière moulue pulvérulente formée de particules de poudre du constituant principal qui ont une grosseur moyenne de grain comprise entre 5 et 50 nm, et que la matière moulue est ensuite soumise à un traitement thermique durant au maximum une heure, à une température inférieure à 600°C.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on prévoit un constituant principal forme d'au moins deux elements.
  3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que la poudre initiale est formée de poudres obtenues à partir de chaque element respectif.
  4. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce que l'on prévoit, pour la poudre initiale, une poudre obtenue à partir d'un préalliage du constituant principal.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que l'on prévoit un constituant principal qui, en plus du fer, contient encore du cobalt et/ou du nickel et/ou du silicium et/ou de l'aluminium.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce qu'une poudre initiale est d'abord formee à partir du constituant principal ferreux du matériau et de 0,1 à 10 pourcents atomiques d'un constituant additionnel ne contenant pas de fer, lequel constituant additionnel ne présente, à l'équilibre thermodynamique, pratiquement aucune solubilite dans le constituant principal, que cette poudre initiale est ensuite broyée jusqu'à obtention d'une matière moulue qui est un mélange pulvérulent formé de particules de poudre dont le calibre est égal à la grosseur moyenne de grain prédéfinie et qui sont composées du constituant principal et du constituant additionnel ajouté dans celui-ci, et que, lors du traitement thermique consécutif de la matière moulue, le constituant additionnel se dépose, de préférence, sur les périphéries des grains individuels.
  7. Procédé selon la revendication 6, caractérisé en ce que la poudre initiale est formée a l'aide d'un constituant additionnel consistant en une poudre de l'un de ces éléments: Pb, Bi, Cu, Ag, Sn, Mg, Li, Na, K, Rb, Cs, Ca, Sr, Ba, Cd, Hg, In.
  8. Procédé selon l'une des revendications 1 a 7, caractérisé en ce que l'on prévoit un traitement thermique à une température inférieure à 400°C, de préférence comprise entre 150°C et 250°C.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que l'on prévoit une durée de broyage dépassant 10 heures et, de préférence, dépassant 60 heures.
EP92103081A 1991-03-06 1992-02-24 Procédé de fabrication d'un matériau magnétiquement doux à base de fer à haute magnétisation de saturation et à structure de graines ultrafine Expired - Lifetime EP0502397B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4107192 1991-03-06
DE4107192 1991-03-06

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EP0502397A2 EP0502397A2 (fr) 1992-09-09
EP0502397A3 EP0502397A3 (en) 1992-11-25
EP0502397B1 true EP0502397B1 (fr) 1995-05-03

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EP92103081A Expired - Lifetime EP0502397B1 (fr) 1991-03-06 1992-02-24 Procédé de fabrication d'un matériau magnétiquement doux à base de fer à haute magnétisation de saturation et à structure de graines ultrafine

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EP (1) EP0502397B1 (fr)
DE (1) DE59202056D1 (fr)
ES (1) ES2071361T3 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19610196A1 (de) * 1996-03-15 1997-09-18 Horst Dr Kleine Verfahren zur Herstellung von weichmagnetischen FeSi-Massekernen
DE10024824A1 (de) 2000-05-19 2001-11-29 Vacuumschmelze Gmbh Induktives Bauelement und Verfahren zu seiner Herstellung
DE10134056B8 (de) 2001-07-13 2014-05-28 Vacuumschmelze Gmbh & Co. Kg Verfahren zur Herstellung von nanokristallinen Magnetkernen sowie Vorrichtung zur Durchführung des Verfahrens
DE102006028389A1 (de) 2006-06-19 2007-12-27 Vacuumschmelze Gmbh & Co. Kg Magnetkern und Verfahren zu seiner Herstellung
KR101060091B1 (ko) 2006-07-12 2011-08-29 바쿰슈멜체 게엠베하 운트 코. 카게 자심의 제조방법과, 자심 및 자심을 지닌 유도소자
DE102007034925A1 (de) 2007-07-24 2009-01-29 Vacuumschmelze Gmbh & Co. Kg Verfahren zur Herstellung von Magnetkernen, Magnetkern und induktives Bauelement mit einem Magnetkern
US9057115B2 (en) 2007-07-27 2015-06-16 Vacuumschmelze Gmbh & Co. Kg Soft magnetic iron-cobalt-based alloy and process for manufacturing it
EP3613872A1 (fr) * 2018-08-21 2020-02-26 Siemens Aktiengesellschaft Procédé de fabrication d'une pièce structurelle pour un composant électrique ou électronique ainsi que pièce structurelle

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB466048A (en) * 1935-01-31 1937-05-21 Hans Vogt A process for making magnetic powder

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Publication number Publication date
EP0502397A2 (fr) 1992-09-09
DE59202056D1 (de) 1995-06-08
EP0502397A3 (en) 1992-11-25
ES2071361T3 (es) 1995-06-16

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