EP1514282B1 - Matiere composite en poudre magnetique douce, ses procedes de production et d'utilisation - Google Patents

Matiere composite en poudre magnetique douce, ses procedes de production et d'utilisation Download PDF

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Publication number
EP1514282B1
EP1514282B1 EP03704253A EP03704253A EP1514282B1 EP 1514282 B1 EP1514282 B1 EP 1514282B1 EP 03704253 A EP03704253 A EP 03704253A EP 03704253 A EP03704253 A EP 03704253A EP 1514282 B1 EP1514282 B1 EP 1514282B1
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EP
European Patent Office
Prior art keywords
powder
soft
composite material
starting mixture
magnetic powder
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
EP03704253A
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German (de)
English (en)
Other versions
EP1514282A1 (fr
Inventor
Adnan Okumus
Waldemar Draxler
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.)
Robert Bosch GmbH
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Robert Bosch GmbH
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Filing date
Publication date
Application filed by Robert Bosch GmbH filed Critical Robert Bosch GmbH
Publication of EP1514282A1 publication Critical patent/EP1514282A1/fr
Application granted granted Critical
Publication of EP1514282B1 publication Critical patent/EP1514282B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/33Magnets 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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin

Definitions

  • the invention relates to a soft magnetic powder composite material, a method for producing such a material and its use according to the preamble of the independent claims.
  • a sintered soft magnetic composite and a method for its preparation in which forms in a starting mixture of a soft magnetic composite after heat treatment, a ferromagnetic starting component as the main component and a starting ferrite component as a minor component.
  • the second starting component forms a grain boundary phase after the heat treatment of the starting mixture to the composite.
  • the first starting component is for example a pure iron powder or a phosphated iron powder
  • the second starting component for example a ferrite powder, in particular a soft ferrite powder such as MnZn ferrite or NiZn ferrite.
  • the proportion of iron powder in the starting mixture is 95 to 99 weight percent, the proportion of ferrite powder 1 to 25 weight percent.
  • Object of the present invention was to provide a soft magnetic powder composite material having the highest possible magnetic saturation polarization and magnetic permeability in combination with the highest possible specific electrical resistance, and in particular the properties of the composite according to DE 199 60 095 A1 improved.
  • the soft magnetic powder composite according to the invention has the advantage over the prior art that it has a magnetic saturation polarization of more than 1.85 Tesla, in particular 1.90 Tesla to 2.05 Tesla, and that it is one over the prior art has significantly increased specific electrical resistance of more than 1 ⁇ m, in particular from 5 ⁇ m to 15 ⁇ m. As a rule, the specific electrical resistance is about 10 ⁇ m.
  • the soft magnetic powder composite according to the invention has a bending strength of more than 120 MPa, measured on cylindrical samples.
  • the edge rupture strength of components made of this material in the form of Switzerland Gurgnettöpfen for injectors is over 45 kN, and the resulting soft magnetic powder composite material is also temperature resistant to at least 400 ° C and resistant to fuel. In this respect, it is very well suited to the production of fast-switching solenoid valves, as they are needed in the bieseleinspritzung in motor vehicle engines.
  • the inventive method for producing the soft magnetic powder material is advantageous that the pressing by adding a pressing aid to the starting mixture, such as a Microwachs, can be facilitated, and that the properties of the powder composite obtained very easily on the gas atmosphere and the temperature program during debindering or the heat treatment can be adjusted.
  • a pressing aid such as a Microwachs
  • the soft ferrite powder used is a MnZn ferrite powder, a NiZn ferrite powder or a mixture of both powders.
  • the pure iron powder used, iron alloy powder or the phosphated iron powder is preferably used more advantageously have an average grain size of the powder particles between 30 ⁇ m and 150 ⁇ m, while the grain size of the inserted Soft ferrite powder, on the other hand, is advantageously significantly smaller and has an average of less than 20 ⁇ m.
  • the average particle size of the soft ferrite powder particles used is preferably less than 5 ⁇ m, in particular less than 1 ⁇ m.
  • the starting material is a starting mixture consisting of a pure iron powder or a phosphated iron powder and a soft ferrite powder.
  • iron alloy powders such as FeCr powder or FeCo powder may also be used.
  • Phosphated iron powder is preferably used, since it achieves the best electrical properties of the powder composite.
  • the starting mixture may also be admixed with a pressing aid, such as a microwax, which is removed again in the course of a subsequent heat treatment of the starting mixture for the production of the soft magnetic powder composite material.
  • a pressing aid such as a microwax
  • the proportion of the pressing aid in the starting mixture is 0% by mass to a maximum of 0.8% by mass.
  • the starting mixture consists of at least 99.4 mass% of a pure iron powder or a phosphated iron powder and 0.1 mass% to 0.6 mass% of a soft ferrite powder.
  • the proportion of the pure iron powder or of the phosphated iron powder is preferably more than 99.5% by mass, in particular 99.7% by mass to 99.8% by mass.
  • the proportion of the soft ferrite powder is preferably less than 0.5 mass%, in particular 0.1 mass% to 0.3 mass%.
  • the soft ferrite powder used is preferably a manganese-zinc ferrite (MnZnOFe 2 O 3 ) or a nickel-zinc ferrite (NiZnO-Fe 2 O 3 ) or a mixture of both powders. Preference is given to using phosphated iron powder or phosphated pure iron powder and one of these two soft-ferrite powders.
  • the pure iron powder or the phosphated iron powder has an average particle size of the powder particles of 50 .mu.m to 100 .mu.m.
  • the particle size of the soft-ferrite powder used is preferably well below 20 ⁇ m, preferably below 5 ⁇ m. For example, it is in the range between 0.5 .mu.m to 2 .mu.m, in particular 1 .mu.m.
  • the composition of the starting mixture which essentially consists of the pure iron powder or the phosphated iron powder and the soft ferrite powder, depending on the intended use of the material obtained on a variation of the composition of the material, on the one hand more emphasis on the highest possible magnetic Saturation polarization and the highest possible magnetic permeability, ie ⁇ max greater than 800, or on the other hand more weight can be placed on the highest possible specific electrical resistance.
  • the above-described powders are first prepared as described in the form of a starting mixture, this is mixed and then compacted by means of a press under elevated pressure and brought into the desired shape. Subsequently, the green bodies thus produced are debinded in a furnace in an inert gas atmosphere, for example a nitrogen atmosphere, or an oxygen-containing gas atmosphere.
  • an inert gas atmosphere for example a nitrogen atmosphere, or an oxygen-containing gas atmosphere.
  • the compressed starting mixture is heated in the oven to a temperature of 400 ° C to 500 ° C and held there for a period of 10 minutes to 1 hour.
  • the temperature during debinding depends mainly on the pressing aid used, ie the micro wax used. In this respect, it may also be below the explained 400 ° C, for example in the range of 220 ° C to 300 ° C.
  • a further heat treatment of the debindered, compressed starting mixture takes place in an oxidizing gas atmosphere at a temperature of 410 ° C. to 500 ° C. in an oven.
  • the compact is heated in the oven to this temperature and held there for a period of 20 minutes to 400 minutes, for example, 200 minutes.
  • the gas atmosphere in the furnace is, for example, air.
  • a soft magnetic powder composite is obtained in which the soft ferrite powder used is at least substantially in the grain boundary phase, i. the soft ferrite powder particles surround the iron powder particles used in the powder composite.
  • the pressing aid used during the manufacturing process facilitates the compaction and shaping of the starting mixture during pressing.
  • the densification of the starting mixture in the die under elevated pressure is preferably carried out by uniaxial pressing at a pressure of preferably 500 MPa to 1000 MPa.
  • magnetic valves produced with the soft magnetic powder composite according to the invention under general conditions of use in the diesel injection of motor vehicles are unrestricted fuel and temperature resistant. Furthermore, they have a very good mechanical strength both in terms of bending strength and edge breakage resistance.

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Claims (13)

  1. Matériau composite magnétique doux en poudre constitué d'au moins 99,4 % en masse d'une poudre de fer pur, d'une poudre de fer phosphaté ou d'une poudre d'alliage de fer et de 0,05% en masse à 0,6 % en masse d'une poudre de ferrite douce.
  2. Matériau composite magnétique doux en poudre selon la revendication 1, caractérisé en ce que la poudre de ferrite douce est une poudre de ferrite au MnZn, une poudre de ferrite au NiZn ou un mélange de ces poudres.
  3. Matériau composite magnétique doux en poudre selon les revendications 1 ou 2, caractérisé en ce que la poudre de fer pur ou la poudre de fer phosphaté présente des particules d'une granulométrie comprise entre 30 µm et 150 µm.
  4. Matériau composite magnétique doux en poudre selon les revendications 1 ou 2, caractérisé en ce que la poudre de ferrite douce présente des particules d'une granulométrie moyenne inférieure à 20 µm.
  5. Matériau composite magnétique doux en poudre selon la revendication 4, caractérisé en ce que la granulométrie moyenne des particules de poudre est inférieure à 5 µm et en particulier inférieure à 1 µm.
  6. Matériau composite magnétique doux en poudre selon l'une des revendications précédentes, caractérisé en ce qu'il présente une polarisation de saturation supérieure à 1,85 Tesla et en particulier de 1,90 à 2,05 Tesla.
  7. Matériau composite magnétique doux en poudre selon l'une des revendications précédentes, caractérisé en ce qu'il présente une résistance électrique spécifique supérieure à 1 µΩ.m et en particulier de 5 µΩ.m à 15 µΩ.m.
  8. Procédé de fabrication d'un matériau composite magnétique doux en poudre selon l'une des revendications précédentes, qui présente les étapes suivantes :
    a) préparation d'un mélange initial d'une poudre de fer pur, d'une poudre de fer phosphaté ou d'une poudre d'alliage de fer et d'une poudre de ferrite douce,
    b) homogénéisation du mélange initial,
    c) compactage du mélange initial dans une presse sous haute pression,
    d) enlèvement du liant du mélange de départ compacté dans une atmosphère de gaz inerte ou dans une atmosphère de gaz contenant de l'oxygène et
    e) traitement thermique du mélange de départ compacté, dans une atmosphère de gaz oxydante et à une température de 410°C à 500°C.
  9. Procédé selon la revendication 8, caractérisé en ce qu'avant le mélange, un adjuvant de compression, en particulier une microcire, est ajouté au mélange de départ.
  10. Procédé selon la revendication 8, caractérisé en ce que la déliaison s'effectue à une température de 400°C à 520°C et pendant une durée de 10 minutes à 1 h.
  11. Procédé selon la revendication 8, caractérisé en ce que le traitement thermique est conduit pendant une durée de 20 min à 400 min.
  12. Procédé selon les revendications 8 ou 10,
    caractérisé en ce que l'enlèvement du liant est réalisé dans une atmosphère d'azote ou dans un mélange d'oxygène et d'azote, qui contient en particulier 5 % en volume à 30 % en volume d'oxygène, ou à l'air, pendant une durée de 10 min à 70 min.
  13. Utilisation d'un matériau composite magnétique doux en poudre selon l'une des revendications précédentes dans des soupapes magnétiques à commutation rapide, en particulier pour l'injection de diesel dans les moteurs à combustion interne.
EP03704253A 2002-06-06 2003-01-27 Matiere composite en poudre magnetique douce, ses procedes de production et d'utilisation Expired - Lifetime EP1514282B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10225154 2002-06-06
DE10225154A DE10225154B4 (de) 2002-06-06 2002-06-06 Weichmagnetischer Pulververbundwerkstoff, Verfahren zu dessen Herstellung und dessen Verwendung
PCT/DE2003/000211 WO2003105161A1 (fr) 2002-06-06 2003-01-27 Matiere composite en poudre magnetique douce, ses procedes de production et d'utilisation

Publications (2)

Publication Number Publication Date
EP1514282A1 EP1514282A1 (fr) 2005-03-16
EP1514282B1 true EP1514282B1 (fr) 2009-04-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP03704253A Expired - Lifetime EP1514282B1 (fr) 2002-06-06 2003-01-27 Matiere composite en poudre magnetique douce, ses procedes de production et d'utilisation

Country Status (8)

Country Link
US (1) US7686894B2 (fr)
EP (1) EP1514282B1 (fr)
JP (1) JP2005536036A (fr)
CN (1) CN1331169C (fr)
AT (1) ATE429020T1 (fr)
AU (1) AU2003206641A1 (fr)
DE (2) DE10225154B4 (fr)
WO (1) WO2003105161A1 (fr)

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CN101777407B (zh) * 2010-03-26 2012-12-26 北京科源科金属材料有限公司 一种改进非晶粉芯导磁率及损耗的方法及依据此方法制备的复合粉芯
CN102528024B (zh) * 2012-01-20 2013-06-26 钢铁研究总院 一种软磁复合材料用绝缘铁粉的制备方法
CN103664159A (zh) * 2012-09-26 2014-03-26 比亚迪股份有限公司 一种镍锌铁氧体软磁材料及其制备方法
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DE102013200229B4 (de) 2013-01-10 2024-06-06 Robert Bosch Gmbh Verfahren zum Herstellen eines weichmagnetischen Verbundwerkstoffs
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CN104332266A (zh) * 2014-10-30 2015-02-04 安徽首文高新材料有限公司 一种耐高温铁粉芯的制备方法
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EP3354437A1 (fr) * 2017-01-25 2018-08-01 Continental Automotive GmbH Soupape de commutation électromagnétique et pompe haute pression à carburant
KR102311667B1 (ko) 2017-07-26 2021-10-13 현대자동차주식회사 Fe-Si 연자성 분말을 이용한 연자성체 제조방법
CN107818856A (zh) * 2017-10-31 2018-03-20 桂林市漓江机电制造有限公司 一种软磁粉末冶金材料及其制造方法
CN107818855A (zh) * 2017-10-31 2018-03-20 桂林市漓江机电制造有限公司 一种细晶粒软磁体复合材料及其制造方法
CN107799261A (zh) * 2017-10-31 2018-03-13 桂林市漓江机电制造有限公司 一种软磁体复合材料及其制造方法
CN111243813B (zh) * 2020-03-12 2021-10-15 钢铁研究总院 高电阻率钕铁硼永磁合金及其制备方法
EP3937347A1 (fr) * 2020-07-08 2022-01-12 Siemens Aktiengesellschaft Couche de matière pour un paquet de tôles d'une machine électrique
KR20220167986A (ko) 2021-06-15 2022-12-22 현대자동차주식회사 철계 혼합분말 제조장치 및 제조방법
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Also Published As

Publication number Publication date
US7686894B2 (en) 2010-03-30
ATE429020T1 (de) 2009-05-15
DE10225154A1 (de) 2004-01-15
JP2005536036A (ja) 2005-11-24
US20050217759A1 (en) 2005-10-06
WO2003105161A1 (fr) 2003-12-18
DE10225154B4 (de) 2012-06-06
CN1331169C (zh) 2007-08-08
AU2003206641A1 (en) 2003-12-22
CN1656575A (zh) 2005-08-17
EP1514282A1 (fr) 2005-03-16
DE50311421D1 (de) 2009-05-28

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