EP0848397B1 - Herstellungsverfahren für eine auf Eisen basierende weichmagnetische Komponente mit nanokristalliner Struktur - Google Patents

Herstellungsverfahren für eine auf Eisen basierende weichmagnetische Komponente mit nanokristalliner Struktur Download PDF

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Publication number
EP0848397B1
EP0848397B1 EP97402667A EP97402667A EP0848397B1 EP 0848397 B1 EP0848397 B1 EP 0848397B1 EP 97402667 A EP97402667 A EP 97402667A EP 97402667 A EP97402667 A EP 97402667A EP 0848397 B1 EP0848397 B1 EP 0848397B1
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EP
European Patent Office
Prior art keywords
temperature
magnetic
crystallization
heat treatment
annealing
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Expired - Lifetime
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EP97402667A
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English (en)
French (fr)
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EP0848397A1 (de
Inventor
Georges Couderchon
Philippe Verin
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Mecagis SNC
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Mecagis SNC
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Publication of EP0848397A1 publication Critical patent/EP0848397A1/de
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Anticipated expiration legal-status Critical
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Classifications

    • 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
    • H01F41/0213—Manufacturing of magnetic circuits made from strip(s) or ribbon(s)
    • H01F41/0226—Manufacturing of magnetic circuits made from strip(s) or ribbon(s) from amorphous ribbons
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/832—Nanostructure having specified property, e.g. lattice-constant, thermal expansion coefficient
    • Y10S977/833—Thermal property of nanomaterial, e.g. thermally conducting/insulating or exhibiting peltier or seebeck effect

Definitions

  • the present invention relates to the manufacture of magnetic components in soft magnetic alloy based on iron having a nanocrystalline structure.
  • Nanocrystalline magnetic materials are well known and have been described, in particular, in European patent applications EP 0 271 657 and EP 0 299 498. These are iron-based alloys, containing more than 60 at% (atoms%) of iron, copper, silicon, boron, and possibly at least one element taken among niobium, tungsten, tantalum, zirconium, hafnium, titanium and molybdenum, cast in the form of amorphous ribbons and then subjected to a treatment which causes extremely fine crystallization (the crystals have less 100 nanometers in diameter). These materials have magnetic properties particularly suitable for the manufacture of soft magnetic cores for electrotechnical devices such as earth leakage circuit breakers.
  • hysteresis (Br / Bm ⁇ 0.5), i.e. a coated hysteresis cycle (Br / Bm ⁇ 0.3); Br / Bm being the ratio of remanent magnetic induction to magnetic induction Max.
  • Round hysteresis cycles are obtained when treatment thermal consists of a simple annealing at a temperature between 500 ° C and 600 ° C.
  • the lying hysteresis cycles are obtained when the treatment thermal includes at least one annealing under magnetic field, this annealing can be the annealing intended to cause the formation of nanocrystals.
  • Nanocrystalline ribbons, or more precisely, magnetic components produced with these ribbons have a drawback which limits their use. This drawback is insufficient stability of the magnetic properties when the temperature rises above room temperature. This stability insufficient results in unreliability of circuit breaker operation differentials fitted with such magnetic cores.
  • the object of the present invention is to remedy this drawback by providing a means for manufacturing magnetic cores from material nanocrystalline having magnetic properties whose temperature stability is significantly improved.
  • the thermal relaxation treatment can be a maintenance for a time between 0.1 and 10 hours, at a temperature between 250 ° C and 480 ° C.
  • the relaxation heat treatment can also consist of a progressive heating from room temperature to a temperature greater than 450 ° C, at a heating rate between 30 ° C / hour and 300 ° C / hour between 250 ° C and 450 ° C.
  • At least one annealing constituting the heat treatment can be carried out under magnetic field.
  • This process applies more particularly to soft magnetic alloys with iron base having a nanocrystalline structure, the chemical composition of which is such that Si ⁇ 14%.
  • the alloy may have low levels of impurities provided by raw materials or resulting from production.
  • the amorphous ribbon is obtained in a manner known per se by solidification very fast liquid alloy, poured, for example, on a cooled wheel.
  • the magnetic core blanks are also manufactured known in itself, by winding the ribbon on a mandrel, cutting it and fixing its end by a welding point, in order to obtain small toroids of rectangular section.
  • the blanks are first subjected to a so-called "relaxation" annealing, at a temperature below the temperature of onset of crystallization of the amorphous strip, and preferably between 250 ° C and 480 ° C, then an annealing of crystallization which may or may not be carried out under magnetic field, and possibly be followed by annealing at lowest temperature under magnetic field.
  • This annealing of relaxation had for advantage of significantly reducing the sensitivity of magnetic properties nuclei at temperature.
  • the inventors have also found that the annealing of relaxation prior to crystallization annealing had the added benefit of reduce the dispersion of the magnetic properties of the nuclei observed on mass production.
  • the crystallization annealing is intended to precipitate in the matrix amorphous nanocrystals of size less than 100 nanometers, preferably between 10 and 20 nanometers. This very fine crystallization makes it possible to obtain the desired magnetic properties.
  • the crystallization annealing consists of a maintaining at a temperature higher than the temperature at the start of crystallization and lower than the onset temperature of the secondary phases which deteriorate the magnetic properties.
  • the annealing temperature of crystallization is between 500 ° C and 600 ° C, but it can be optimized for each ribbon, for example, by determining by tests the temperature which leads to maximum magnetic permeability.
  • the annealing temperature of crystallization can then be chosen equal to this temperature, or, better, be chosen to be about 30 ° C higher.
  • crystallization annealing can be carried out under a transverse magnetic field.
  • the crystallization treatment can also be supplemented by annealing at a temperature below the crystallization start temperature, for example towards 400 ° C, carried out under transverse magnetic field.
  • the heat treatment of the blanks magnetic component include a relaxation annealing, a crystallization possibly carried out under magnetic field, and, possibly, an additional annealing carried out under magnetic field.
  • the relaxation annealing which precedes the crystallization annealing, and which can be performed both on the amorphous tape itself and on the component blank magnetic, can consist in maintaining a constant temperature during a time which preferably should be between 0.1 and 10 hours.
  • This annealing can also consist of a gradual rise in temperature, which precedes, by example, crystallization annealing, and which must be done at a rate of rise in temperature between 30 ° C / h and 300 ° C / h, at least between 250 ° C and 450 ° C; preferably the rate of temperature rise should be around 100 ° C / h.
  • the series of blanks of magnetic cores A2 and B2 have, for comparison, been treated in accordance with the prior art by a single crystallization annealing for 3 hours at 530 ° C.
  • the maximum magnetic permeability at 50 Hz was measured at different temperatures between - 25 ° C and + 100 ° C, and it was expressed as a% of the maximum magnetic permeability at 50 Hz at 20 ° C.
  • the first example relates to toroidal magnetic cores produced from ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73.5 Si 13.5 B 9 Cu 1 Nb 3 . After quenching on a wheel, it was checked by X-ray that the ribbon was completely amorphous. The ribbon was then separated into three sections, one, A, remained as it was, the other two, B and C, were subjected to relaxation annealing, for one, B, 1 hour at 400 ° C, for the other, C, 1 hour at 450 ° C.
  • the second example relates to toroidal magnetic cores produced from ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73 Si 15 B 8 Cu 1 Nb 3 .
  • ribbons 20 ⁇ m thick and 10 mm wide obtained by direct quenching on a cooled wheel, of an alloy of composition (in at%) Fe 73 Si 15 B 8 Cu 1 Nb 3 .
  • the ribbon two batches of 300 toroids with an internal diameter of 11 mm and an external diameter of 15 mm were produced using automatic winding machines. The batches were then treated in ovens with neutral atmosphere. A control batch A was only subjected to a 1 hour crystallization annealing at 530 ° C.
  • the second batch was treated in accordance with the invention: a relaxation annealing of 1 hour at 400 ° C. was first carried out, then a crystallization annealing of 1 hour at 530 ° C.
  • the toroids were put in a box

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Thin Magnetic Films (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Powder Metallurgy (AREA)

Claims (6)

  1. Verfahren zur Herstellung eines magnetischen Bauteils aus einer weichen magnetischen Legierung auf Eisenbasis mit einer nanokristalinen Struktur, deren chemische Zusammensetzung in Atomprozent umfasst: Fe ≥ 60%, 0,1% ≤ Cu ≤ 3%, 0% ≤ B ≤ 25%, 0% Si ≤ 30%, und mindestens ein Element, gewählt unter Niobium, Wolfram, Tantal, Zirkonium, Hafnium, Titan und Molybdän mit Gehalten zwischen 0,1% und 30%, wobei der Rest aus der Erzeugung resultierende Verunreinigungen sind und wobei die Zusammensetzung darüber hinaus die Beziehung 5% ≤ Si + B ≤ 30% erfüllt, gemäß dem:
    mit der magnetischen Legierung ein amorphes Band hergestellt wird;
    mit dem Band ein Rohling für ein magnetisches Bauteil hergestellt wird, indem das magnetische Band um einen Spulenkörper gewickelt wird, um einen Torus zu bilden;
    und das magnetische Bauteil einer Wärmebehandlung zur Kristallisation unterzogen wird, umfassend mindestens ein Kristallisationsglühen bei einer Temperatur zwischen 500°C und 600°C während einer Haltezeit zwischen 0,1 und 10 Stunden, um die Bildung von Nanokristallen hervorzurufen, dadurch gekennzeichnet, dass vor der Ausführung der Wärmebehandlung zur Kristallisation eine Wärmebehandlung zur Entspannung bei einer Temperatur unter der Temperatur des Beginns der Rekristallisation der amorphen Legierung durchgeführt wird.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Wärmebehandlung zur Entspannung ein Halten während einer Zeit zwischen 0,1 und 10 Stunden auf einer Temperatur zwischen 250°C und 480°C ist.
  3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Wärmebehandlung zur Entspannung in einer allmählichen Erwärmung von der Umgebungstemperatur bis auf eine Temperatur von über 450°C besteht, mit einer Erwärmungsgeschwindigkeit zwischen 30°C/Stunde und 300°C/Stunde zwischen 250°C und 450°C.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Kristallisationsglühen in einem Magnetfeld durchgeführt wird.
  5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass darüber hinaus ein zusätzliches Glühen im Magnetfeld bei einer Temperatur unter der Temperatur des Beginns der Kristallisation durchgeführt wird.
  6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass die chemische Zusammensetzung der Legierung derart ist, dass Si ≤ 14%.
EP97402667A 1996-12-11 1997-11-07 Herstellungsverfahren für eine auf Eisen basierende weichmagnetische Komponente mit nanokristalliner Struktur Expired - Lifetime EP0848397B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9615197 1996-12-11
FR9615197A FR2756966B1 (fr) 1996-12-11 1996-12-11 Procede de fabrication d'un composant magnetique en alliage magnetique doux a base de fer ayant une structure nanocristalline

Publications (2)

Publication Number Publication Date
EP0848397A1 EP0848397A1 (de) 1998-06-17
EP0848397B1 true EP0848397B1 (de) 2002-09-18

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Country Status (17)

Country Link
US (1) US5911840A (de)
EP (1) EP0848397B1 (de)
JP (1) JPH10195528A (de)
KR (1) KR19980064039A (de)
CN (1) CN1134034C (de)
AT (1) ATE224582T1 (de)
AU (1) AU731520B2 (de)
CZ (1) CZ293837B6 (de)
DE (1) DE69715575T2 (de)
ES (1) ES2184047T3 (de)
FR (1) FR2756966B1 (de)
HU (1) HU216168B (de)
PL (1) PL184208B1 (de)
SK (1) SK284008B6 (de)
TR (1) TR199701599A3 (de)
TW (1) TW561193B (de)
ZA (1) ZA9710780B (de)

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CN102543347B (zh) * 2011-12-31 2015-10-14 中国科学院宁波材料技术与工程研究所 一种铁基纳米晶软磁合金及其制备方法
CN102856031A (zh) * 2012-09-10 2013-01-02 任静儿 一种磁性粉末合金材料
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CN102912257A (zh) * 2012-10-19 2013-02-06 张家港市清大星源微晶有限公司 微晶材料
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Publication number Publication date
HUP9702383A2 (hu) 1998-07-28
TW561193B (en) 2003-11-11
ZA9710780B (en) 1998-06-12
US5911840A (en) 1999-06-15
DE69715575T2 (de) 2003-05-22
AU731520B2 (en) 2001-03-29
EP0848397A1 (de) 1998-06-17
HU216168B (hu) 1999-04-28
ES2184047T3 (es) 2003-04-01
HUP9702383A3 (en) 1998-08-28
CN1185012A (zh) 1998-06-17
TR199701599A2 (xx) 2000-07-21
PL184208B1 (pl) 2002-09-30
ATE224582T1 (de) 2002-10-15
KR19980064039A (ko) 1998-10-07
AU4519997A (en) 1998-06-18
SK284008B6 (sk) 2004-07-07
CZ293837B6 (cs) 2004-08-18
CZ398397A3 (cs) 1998-07-15
FR2756966A1 (fr) 1998-06-12
TR199701599A3 (tr) 2000-07-21
SK161897A3 (en) 1998-12-02
JPH10195528A (ja) 1998-07-28
HK1010938A1 (en) 1999-07-02
FR2756966B1 (fr) 1998-12-31
CN1134034C (zh) 2004-01-07
DE69715575D1 (de) 2002-10-24
PL323663A1 (en) 1998-06-22

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