EP0844628B1 - Herstellungsverfahren eines Magnetkernes aus weichmagnetischem nanokristallinen Material - Google Patents

Herstellungsverfahren eines Magnetkernes aus weichmagnetischem nanokristallinen Material Download PDF

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Publication number
EP0844628B1
EP0844628B1 EP97402396A EP97402396A EP0844628B1 EP 0844628 B1 EP0844628 B1 EP 0844628B1 EP 97402396 A EP97402396 A EP 97402396A EP 97402396 A EP97402396 A EP 97402396A EP 0844628 B1 EP0844628 B1 EP 0844628B1
Authority
EP
European Patent Office
Prior art keywords
magnetic
process according
soft magnetic
annealing
iron
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
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EP97402396A
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English (en)
French (fr)
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EP0844628A1 (de
Inventor
Philippe Verin
Georges Couderchon
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Mecagis SNC
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Mecagis SNC
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Publication of EP0844628A1 publication Critical patent/EP0844628A1/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)
    • 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
    • Y10S977/838—Magnetic property of nanomaterial

Definitions

  • the present invention relates to nanocrystalline magnetic materials intended, in particular, for the manufacture of magnetic circuits for apparatus electric.
  • 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.
  • Materials with a round hysteresis cycle may exhibit very high magnetic permeability, even higher than that of alloys of the type Classic permalloys. This very high magnetic permeability makes them, a priori, particularly suitable for the manufacture of magnetic cores for circuit breakers AC class differentials, i.e. sensitive to fault currents alternative. However, for such use to be possible, it is necessary that the magnetic properties of the nuclei are sufficiently reproducible to that mass production is satisfactory.
  • an amorphous magnetic alloy ribbon capable of being used to acquire a nanocrystalline structure.
  • the toroids thus obtained are then annealed in order to cause the formation of nanocrystals and, as a result, their confer the desired magnetic properties.
  • the annealing temperature which located around 500 ° C, is chosen so that the magnetic permeability of the alloy is maximum.
  • the magnetic cores thus obtained are intended for receive windings which generate mechanical stresses which deteriorate the magnetic properties of the nuclei.
  • the toroids are arranged in protective boxes with the interior of which they are wedged for example by foam rings.
  • this wedging of the toroids in their casing induces, by itself, low stresses which are detrimental to the excellent magnetic properties developed on the nucleus.
  • the use of a protective case although effective not always sufficient, and, after winding, the properties of the devices obtained by industrial production are degraded and too dispersed to be even acceptable for the intended use.
  • the object of the present invention is to remedy these drawbacks by proposing a means for mass production of magnetic cores of material nanocrystalline, having both magnetic permeability (relative permeability impedance at 50 Hz maximum) greater than 400,000 and a round hysteresis cycle, so that the dispersion of their magnetic properties is compatible with the use for mass production of class GFCIs AC.
  • This process applies to all soft magnetic alloys based on iron capable of exhibiting a nanocrystalline structure, and more particularly to alloys whose chemical composition comprises, in% atoms: Fe ⁇ 60% 0.5% ⁇ Cu ⁇ 1.5% 5% ⁇ B ⁇ 14% 5% ⁇ Si + B ⁇ 30% 2% ⁇ Nb ⁇ 4%
  • the chemical composition of the alloy may also include low contents of impurities provided by raw materials or resulting from development.
  • the amorphous ribbon is obtained in a manner known per se by solidification very fast liquid alloy.
  • Magnetic core blanks are fabricated also in a manner known per se by winding the ribbon on a mandrel, cutting it and fixing its end with a welding point, in order to obtain small tori of rectangular section.
  • the blanks must then be subjected to a annealing treatment to precipitate nanocrystals in the amorphous matrix of size less than 100 nanometers. This very fine crystallization makes it possible to obtain desired magnetic properties, and thus transforming the core blank magnetic in magnetic core.
  • the inventors having unexpectedly found that the effect of the conditions annealing on the magnetic properties of the nuclei depended not only on the chemical composition of the alloy, but also, and not very controllably, special manufacturing conditions for each ribbon taken individually, before to carry out the annealing, the temperature Tm which determines, for an annealing of given duration, at the maximum magnetic permeability that it is possible to obtain on a torus made with the ribbon.
  • This temperature Tm is specific to each ribbon, it is therefore determined for each ribbon by tests that a person skilled in the art can do.
  • the annealing is carried out at a temperature T between Tm + 10 ° C and Tm + 50 ° C, and preferably between Tm + 20 ° C and Tm + 40 ° C, for a time between 0.1 and 10 hours, and, from preferably between 0.5 and 5 hours.
  • Temperature and time are two setting parameters for annealing partially equivalent. However, variations in the annealing temperature have a much stronger effect than variations in the duration of annealing, in particular at the ends of the admissible annealing temperature range. Also, the temperature is a relatively coarse adjustment parameter of the conditions of processing, time is a fine adjustment parameter.
  • the specific conditions of treatment are determined based on the intended use for the magnetic core.
  • each core is placed in a box protector, in which it is wedged, for example, with foam washers.
  • each core can be coated in a resin.
  • the annealing temperature is not equal to Tm, the magnetic permeability of nuclei is not maximum. However, the inventors have found that in doing so, one could obtain a sufficiently reliable permeability magnetic greater than 400,000. They also found that the nuclei obtained magnets were well suited for mass production of circuit breakers differentials, and, in particular, they were less sensitive to the effect of constraints winding.
  • Lot A was annealed at 505 ° C (Tm + 5 ° C) for 1 hour, in accordance with the prior art, lot B was annealed at 530 ° C (Tm + 30 ° C) for 3 hours, in accordance with the prior art to the invention, and batch C was annealed at 555 ° C (Tm + 55 ° C) for 3 hours, for comparison.
  • the mean and standard deviation of the magnetic permeability values were determined for each of the batches, on the one hand for the naked nuclei, and on the other hand for the cased nuclei, that is to say, subjected to light stresses due to the setting of the torus in its case.
  • lots B and C are more lower than the standard deviation of the magnetic permeability values of the nuclei magnetic, in case or not, of lot A.
  • the difference between lots A and B results that the magnetic cores in lot B are less sensitive to stresses mechanical than the magnetic cores in lot A.
  • the magnetic cores in lot C are a priori less sensitive to mechanical stresses than cores magnetic of batch B, but have permeabilities incompatible with the application.
  • the dispersion of the magnetic properties of the nuclei of batch B is lower than that of the nuclei of batch A, and because the sensitivity of these properties under mechanical stress is lower for lot B than for lot A, after winding the magnetic cores of lot B are well suited to use in class AC residual current devices, while the cores of the lot A are not reliably so.
  • the magnetic cores of lot C although having theoretically lower sensitivity to mechanical stresses than lot B cores, are not suitable for use in circuit breakers differentials, especially because they have insufficient magnetic permeability.
  • Such cores can be made by performing at least annealing under magnetic field.
  • Annealing under magnetic field can be either the annealing which has just been described and which is intended to cause the precipitation of nanocrystals, i.e. an additional annealing carried out between 350 and 550 ° C.
  • the cores thus obtained have, in the same way, a sensitivity to the stresses very low mechanical properties, which increases the reliability of mass production.

Claims (10)

  1. Verfahren zur Herstellung wenigstens eines Magnetkernes aus einer weichmagnetischen Legierung auf Eisenbasis mit einer nanokristallinen Struktur, dadurch gekennzeichnet, daß:
    mit der magnetischen Legierung ein amorphes Band hergestellt wird,
    die Glühtemperatur Tm bestimmt wird, die für das Band zur maximalen magnetischen Permeabilität führt,
    mit dem Band wenigstens ein Kernrohling hergestellt wird,
    und wenigstens ein Kernrohling wenigstens einem Glühen unterzogen wird, wobei dieses Glühen bei einer Temperatur T zwischen Tm + 10°C und Tm + 50°C während einer Haltezeit t zwischen 0,1 und 10 Stunden erfolgt, um die Bildung von Nanokristallen zu bewirken.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Haltezeit zwischen 0,5 und 5 Stunden beträgt.
  3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Glühtemperatur T zwischen Tm + 20°C und Tm + 40°C liegt.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis in Atom-% umfaßt: Fe ≥ 60% 0,1% ≤ Cu ≤ 3% 0% ≤ B ≤ 25% 0% ≤ Si ≤ 30%
    wenigstens ein Element, gewählt unter Niobium, Wolfram, Tantal, Zirconium, Hafnium, Titan und Molybdän, in Gehalten zwischen 0,1 und 30%,
       wobei der Rest Verunreinigungen sind, die aus der Verhüttung stammen, wobei die Zusammensetzung außerdem die Beziehung: 5% ≤ Si + B ≤ 30% erfüllt.
  5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis derart ist, daß: 15% ≤ Si + B ≤ 25%.
  6. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis derart ist, daß: 0,5% ≤ Cu ≤ 1,5%.
  7. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis derart ist, daß sie wenigstens ein Element, gewählt unter Niobium, Wolfram, Tantal, Zirconium, Hafnium, Titan und Molybdän, in einem Gehalt zwischen 2% und 5% enthält.
  8. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis derart ist, daß: 12% ≤ Si ≤ 17%.
  9. Verfahren nach Anspruch 8, dadurch gekennzeichnet, daß die chemische Zusammensetzung der weichmagnetischen Legierung auf Eisenbasis derart ist, daß: 0,5% ≤ Cu ≤ 1,5% 5% ≤ B ≤ 14% 15% ≤ Si + B ≤ 25% und der Gehalt an wenigstens einem Element, gewählt unter Niobium, Wolfram, Tantal, Zirconium, Hafnium, Titan und Molybdän, zwischen 2% und 4% beträgt.
  10. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß wenigstens ein Glühen in einem Magnetfeld durchgeführt wird.
EP97402396A 1996-10-25 1997-10-13 Herstellungsverfahren eines Magnetkernes aus weichmagnetischem nanokristallinen Material Expired - Lifetime EP0844628B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9612996A FR2755292B1 (fr) 1996-10-25 1996-10-25 Procede de fabrication d'un noyau magnetique en materiau magnetique doux nanocristallin
FR9612996 1996-10-25

Publications (2)

Publication Number Publication Date
EP0844628A1 EP0844628A1 (de) 1998-05-27
EP0844628B1 true EP0844628B1 (de) 2001-12-05

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EP97402396A Expired - Lifetime EP0844628B1 (de) 1996-10-25 1997-10-13 Herstellungsverfahren eines Magnetkernes aus weichmagnetischem nanokristallinen Material

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Country Link
US (1) US5922143A (de)
EP (1) EP0844628B1 (de)
JP (1) JPH10130797A (de)
KR (1) KR19980032982A (de)
CN (1) CN1134033C (de)
AT (1) ATE210332T1 (de)
AU (1) AU715096B2 (de)
CZ (1) CZ293222B6 (de)
DE (1) DE69708828T2 (de)
ES (1) ES2166516T3 (de)
FR (1) FR2755292B1 (de)
HK (1) HK1011578A1 (de)
HU (1) HU221412B1 (de)
PL (1) PL184054B1 (de)
SK (1) SK284075B6 (de)
TR (1) TR199701235A2 (de)
TW (1) TW354842B (de)
ZA (1) ZA979359B (de)

Cited By (1)

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DE10331883A1 (de) * 2003-07-14 2005-02-10 Vacuumschmelze Gmbh & Co. Kg Messverfahren und Messanordnung zum Messen von Strömen mit grossem Dynamikbereich

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US6960860B1 (en) * 1998-06-18 2005-11-01 Metglas, Inc. Amorphous metal stator for a radial-flux electric motor
EP1129459B1 (de) * 1998-11-13 2004-06-02 Vacuumschmelze GmbH Verwendung eines magnetkerns für einen stromwandler, verfahren zur herstellung eines magnetkerns und stromwandler mit einem magnetkern
KR100606515B1 (ko) * 1998-11-13 2006-07-31 바쿰슈멜체 게엠베하 운트 코. 카게 변류기에 사용하기에 적합한 자기 코어, 상기 자기 코어의 제조 방법 및 상기 자기 코어를 구비한 변류기
DE10134056B8 (de) * 2001-07-13 2014-05-28 Vacuumschmelze Gmbh & Co. Kg Verfahren zur Herstellung von nanokristallinen Magnetkernen sowie Vorrichtung zur Durchführung des Verfahrens
CN100372033C (zh) * 2005-06-23 2008-02-27 安泰科技股份有限公司 漏电保护器用抗直流偏磁互感器磁芯及其制造方法
DE102005034486A1 (de) * 2005-07-20 2007-02-01 Vacuumschmelze Gmbh & Co. Kg Verfahren zur Herstellung eines weichmagnetischen Kerns für Generatoren sowie Generator mit einem derartigen Kern
US20070273467A1 (en) * 2006-05-23 2007-11-29 Jorg Petzold Magnet Core, Methods For Its Production And Residual Current Device
DE502007000329D1 (de) * 2006-10-30 2009-02-05 Vacuumschmelze Gmbh & Co Kg Weichmagnetische Legierung auf Eisen-Kobalt-Basis sowie Verfahren zu deren Herstellung
US8012270B2 (en) * 2007-07-27 2011-09-06 Vacuumschmelze Gmbh & Co. Kg Soft magnetic iron/cobalt/chromium-based alloy and process for manufacturing it
US9057115B2 (en) * 2007-07-27 2015-06-16 Vacuumschmelze Gmbh & Co. Kg Soft magnetic iron-cobalt-based alloy and process for manufacturing it
US8699190B2 (en) 2010-11-23 2014-04-15 Vacuumschmelze Gmbh & Co. Kg Soft magnetic metal strip for electromechanical components
DE102010060740A1 (de) 2010-11-23 2012-05-24 Vacuumschmelze Gmbh & Co. Kg Weichmagnetisches Metallband für elektromechanische Bauelemente
CN102496450B (zh) * 2011-12-28 2017-03-15 天津三环奥纳科技有限公司 一种超微晶铁芯强磁退火工艺及其专用设备
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
CN102875024A (zh) * 2012-10-19 2013-01-16 张家港市清大星源微晶有限公司 高导磁率的微晶材料
KR101470513B1 (ko) * 2013-07-17 2014-12-08 주식회사 아모그린텍 대전류 직류중첩특성 및 코어손실 특성이 우수한 연자성 코어 및 그의 제조방법
FR3017750B1 (fr) * 2014-02-18 2016-03-04 Tronico Ligne de transmission mise en œuvre au sein d'une canalisation du type comprenant un tube de cuvelage et un tube de production, avec utilisation de rouleaux de materiau magnetique.
KR102203689B1 (ko) * 2014-07-29 2021-01-15 엘지이노텍 주식회사 연자성 합금, 이를 포함하는 무선 전력 송신 장치 및 무선 전력 수신 장치
CN106521287A (zh) * 2016-11-16 2017-03-22 黄忠波 一种纳米晶软磁合金材料及制备方法
CN111593273A (zh) * 2020-05-29 2020-08-28 唐山先隆纳米金属制造股份有限公司 一种新型软磁合金材料

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Publication number Priority date Publication date Assignee Title
DE10331883A1 (de) * 2003-07-14 2005-02-10 Vacuumschmelze Gmbh & Co. Kg Messverfahren und Messanordnung zum Messen von Strömen mit grossem Dynamikbereich
US7358716B2 (en) 2003-07-14 2008-04-15 Vacuumschmelze Gmbh & Co. Kg Measuring method and measuring arrangement for measuring currents with a large dynamic range
DE10331883B4 (de) * 2003-07-14 2018-01-18 Vacuumschmelze Gmbh & Co. Kg Messverfahren und Messanordnung zum Messen von Strömen mit grossem Dynamikbereich

Also Published As

Publication number Publication date
HUP9701672A3 (en) 2002-03-28
KR19980032982A (ko) 1998-07-25
TR199701235A3 (tr) 1999-10-21
TW354842B (en) 1999-03-21
US5922143A (en) 1999-07-13
AU4102997A (en) 1998-04-30
HK1011578A1 (en) 1999-07-16
ES2166516T3 (es) 2002-04-16
ZA979359B (en) 1998-05-12
FR2755292A1 (fr) 1998-04-30
PL184054B1 (pl) 2002-08-30
AU715096B2 (en) 2000-01-13
DE69708828T2 (de) 2002-06-20
HUP9701672A2 (hu) 1999-06-28
TR199701235A2 (xx) 1999-10-21
SK284075B6 (sk) 2004-09-08
DE69708828D1 (de) 2002-01-17
ATE210332T1 (de) 2001-12-15
HU9701672D0 (en) 1997-12-29
CN1188317A (zh) 1998-07-22
SK144597A3 (en) 1998-05-06
FR2755292B1 (fr) 1998-11-20
CZ293222B6 (cs) 2004-03-17
CN1134033C (zh) 2004-01-07
HU221412B1 (en) 2002-09-28
CZ337297A3 (cs) 1999-01-13
EP0844628A1 (de) 1998-05-27
PL322808A1 (en) 1998-04-27
JPH10130797A (ja) 1998-05-19

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