EP1061534A2 - Matériau composite magnétique doux déformable et son procédé de fabrication - Google Patents

Matériau composite magnétique doux déformable et son procédé de fabrication Download PDF

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Publication number
EP1061534A2
EP1061534A2 EP00119956A EP00119956A EP1061534A2 EP 1061534 A2 EP1061534 A2 EP 1061534A2 EP 00119956 A EP00119956 A EP 00119956A EP 00119956 A EP00119956 A EP 00119956A EP 1061534 A2 EP1061534 A2 EP 1061534A2
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EP
European Patent Office
Prior art keywords
composite material
silicon
material according
weight
compound
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.)
Withdrawn
Application number
EP00119956A
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German (de)
English (en)
Other versions
EP1061534A3 (fr
Inventor
Wilfried Aichele
Hans-Peter Koch
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
Original Assignee
Robert Bosch GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Robert Bosch GmbH filed Critical Robert Bosch GmbH
Publication of EP1061534A2 publication Critical patent/EP1061534A2/fr
Publication of EP1061534A3 publication Critical patent/EP1061534A3/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • H01F1/22—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 pressed, sintered, or bound together
    • H01F1/24—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 pressed, sintered, or bound together the particles being insulated
    • H01F1/26—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 pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
    • 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
    • H01F1/22—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 pressed, sintered, or bound together
    • H01F1/24—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 pressed, sintered, or bound together the particles being insulated
    • 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
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder

Definitions

  • the invention relates to a soft magnetic, mouldable Composite material that has soft magnetic properties Powder contains a non-magnetic coating have, as well as a method for its production.
  • Soft magnetic materials are required for the production of temperature, corrosion and solvent resistant magnetic components in the electronics sector and especially in electromechanics. These soft magnetic components require certain properties: they should have a high permeability ( ⁇ max ), a high magnetic saturation (B s ), a low coercive force (H c ) and a high specific electrical resistance ( ⁇ spec ). The combination of these magnetic properties with a high specific electrical resistance results in high switching dynamics, that is to say that the magnetic saturation and demagnetization of such a component take place within a short time.
  • EP 0 540 504 B1 discloses soft magnetic powders prepare with a plastic binder and thus through a Injection molding process to produce corresponding components.
  • the powder parts in injection moldable Composite materials limited to a maximum of 65% by volume.
  • the compression takes place in the case of axial pressing of free-flowing powders with almost no material flow.
  • the fill levels of these composite materials are typically at 90-98 vol%.
  • thermosetting resins for example epoxies or phenolic resins
  • thermosetting resins for example epoxies or phenolic resins
  • organic solvents for example Fuels for internal combustion engines
  • soluble are, or swell strongly.
  • the corresponding Composite components change their dimensions under these conditions, lose their strength and fail completely.
  • appropriate composite materials with high temperature and media resistance for example in organic solvents, especially fuels for internal combustion engines.
  • Another Problem have so far set the operating conditions for these components among which are both thermoplastics and thermosets no longer represent a suitable binder because they are otherwise would completely decompose.
  • Coating the soft magnetic powder with compounds of the boron or aluminum, which in pyrolysis in corresponding Skipping ceramics is another way solvent resistance and temperature resistance of the soft magnetic composite material and the material produced from it Increase molded parts.
  • the temperature after a shaping of the material is advantageously chosen so that the coating material is converted into a ceramic, metallic or even intermetallic end product. This results in a high magnetization and a temperature and solvent resistance achieved.
  • Silicon compounds selected from the group consisting of from binary hydrogen compounds of silicon, polydialkylsilanes, Carbosilanes, polysilazanes, alkoxyalkylsilanes, Alkyl polysiloxanes, alkyl silanols and compounds of alkylsilanols with elements of the first main group.
  • This ensures that a wide connection class of molecular precursor compounds of silicon can be used, which in pyrolysis to different Ceramics, both based on silicon-oxygen, or also on a silicon-nitrogen or silicon-nitrogen-oxygen basis to provide can and optimized according to the desired requirement profile are.
  • the applications of the component to be manufactured so can the corresponding ceramics that also one Influence on the magnetic field strength and the switching time which has soft magnetic connections. It is also possible to change the temperature range for the Choose application accordingly.
  • Soft magnetic powder boron compounds selected from the group consisting of borazole, pyridine or other ⁇ -donor borane adducts, for example borane-phosphine, borane-phosphinite, Borane-sulfur or borane-nitrogen adducts, Borosilazanes and polyborazanes are used, so that in simple way after the thermolysis different boron-containing Ceramics can be made available in a simple manner can
  • a polyazalane as an aluminum precursor compound to use, which in very small quantities of 0.2-2% by weight, based on the total weight can be. This makes aluminum-nitrogen ceramics as Coating for the soft magnetic powder produced, wherein the weight fraction of the soft magnetic powder especially is high.
  • the inorganic, or silicon, boron and organoaluminium compounds used for coating the soft magnetic powders which are predominantly polymeric in character, have good sliding or lubricating properties. After hardening, they thus represent a thermosetting binder, which is converted into a ceramic or into alloy additives for ferrous metals by subsequent thermal decomposition (pyrolysis). In connection with oxidation-sensitive magnetic materials, such as pure iron or pure nickel, the pyrolysis takes place under protective gas. In order to obtain composite bodies with a small proportion of pores, the volume shrinkage occurring during the pyrolysis must be small, which is ensured by the compounds used. Silicon hydrogen compounds (silicon hydrides) are one example.
  • Silicon hydrides with multiple Si atoms can be melted and thus also serve as lubricants for the coated magnetic powders. Depending on the hydride used, they decompose into Si and H 2 at higher temperatures. When the temperature increases further, the Si alloys in a surface layer, for example with pure iron powder. The Fe-Si alloy layer has a higher electrical resistance and a lower melting point than pure iron. The iron powder particles coated with Fe-Si sinter together to form composite bodies with a higher electrical resistance than pure iron. An alternative to this is the deposition of high-purity silicon on iron powder particles by thermal decomposition of SiH 4 . The method is common in semiconductor manufacturing for the build-up of silicon layers and in the tempering of glasses. Low molecular weight silicon hydrides are self-igniting, so that all process steps take place under protective gas.
  • a silicon carbide ceramic according to the invention is used, for example prepared by pyrolysis of polydialkylsilanes. In Connection with powders from the series of ferrous metals the elimination of carbon-containing compounds in the Pyrolysis to carburize. Through annealing treatments in hydrogen-containing The atmosphere then becomes the metal of the Carbon content withdrawn again.
  • Precursor compounds for BN ceramics as coating material are pyrolyzed under an ammonia atmosphere.
  • RCP Cubbon RAPRA Review Report No. 76, Polymeric Precursors for Ceramic Materials, Vol. 7, No. 4, 1994.
  • Borazole B 3 N 3 H 6
  • B 3 N 3 H 6 which splits off under reduced pressure at 90 ° CH 2 and turns into a polymer analogous to polyphenylene, has proven to be particularly suitable for soft-magnetic composite materials with a ceramic coating.
  • the elimination of H 2 continues until the hexagonal modification of BN is reached at approx. 750 ° C.
  • the pyrolysis takes place only under protective gas, for example argon or nitrogen, and not in an ammonia atmosphere.
  • the resulting slight weight loss of 5.1% results in low shrinkage and thus a small pore volume in the combination of BN and the magnetic powder.
  • polyazalanes As a suitable starting material for the coating of magnetic powders with an aluminum nitride ceramic, polyazalanes were found. These were by thermal condensation of Diisobutylaluminum hydride synthesized with unsaturated nitriles, which leads to curable liquid polyazalanes. This was used to coat the magnetic powders.
  • the polyazalans also serve as a thermoset glide and binder, which after subsequent pyrolysis crosslinked to a non-melting solid at 200 ° C. and in the next process step completely under an inert atmosphere pyrolyzed to AlN.
  • Carbosilanes and polysilazanes have proven to be a suitable starting material for coating magnetic powders with a silicon nitride ceramic.
  • Silicon nitride Si 3 N 4 is formed by pyrolysis of these compounds in an ammonia atmosphere. Pyrolysis under protective gas produced a coating with silicon carbonitrides of the formula SiN x C y .
  • Glasses, enamels and glazes are combinations of metal and non-metal oxides of different compositions.
  • An embodiment for the production of glass-like coatings of soft magnetic powders is the use of silanes with several silanol groups which form polymers when water is added with the elimination of alcohol.
  • the product NH 2100 manufactured by Hüls is a not yet fully cross-linked, soluble and meltable polycondensate of trimethoxymethylsilane (CH 3 Si (OCH 3 ) 3 ) x and is an excellent precursor material for a glass-like coating of magnetic powders.
  • the electrical resistance drops to 5 ⁇ m (pure iron has 0.1 ⁇ m), while the bending strength increases to 80 N / mm 2 .
  • the iron-iron sintered bridges and the strength increase, while the specific electrical resistance continues to decrease.
  • the corresponding glasses or enamels are formed by adding further compounds which can be converted into glass-forming oxides. Their composition is selected with a view to good adhesion to the magnetic powder.
  • an addition of aluminum stearate serves both as a lubricant for removal from the press tool and after its thermal decomposition to Al 2 0 3 as a glass former.
  • phosphated iron powder (AB 100.32, Höganäs) is wetted in the kneader with a solution of 2.4 g of methylpolysiloxane prepolymer (NH 2100, Nünchritz chemical plant) in acetone. After adding a solution of 46.3 g sodium trimethylsilanolate in acetone, a gel coat forms around the iron particles. After the acetone has been evaporated in a kneader, 5 g of aluminum tristearate are added and this is melted at 140 ° C. while kneading. The aluminum tristearate acts as a lubricant and mold release agent during the subsequent axial pressing of the composite material.
  • the methylpolysiloxane prepolymer When the compacts are heated to 200 ° C under protective gas, the methylpolysiloxane prepolymer initially hardens. When the temperature is increased further to 800 ° C., all the products used pyrolyze and melt to about 40 g of a glass with the approximate composition 27 g Si0 2 , 12.8 g Na 2 O and 0.3 g A1 2 0 3 .
EP00119956A 1997-08-14 1998-08-11 Matériau composite magnétique doux déformable et son procédé de fabrication Withdrawn EP1061534A3 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19735271A DE19735271C2 (de) 1997-08-14 1997-08-14 Weichmagnetischer, formbarer Verbundwerkstoff und Verfahren zu dessen Herstellung
DE19735271 1997-08-14
EP98948761A EP0931322B1 (fr) 1997-08-14 1998-08-11 Materiau composite magnetique doux deformable et procede permettant de le produire

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
EP98948761A Division EP0931322B1 (fr) 1997-08-14 1998-08-11 Materiau composite magnetique doux deformable et procede permettant de le produire

Publications (2)

Publication Number Publication Date
EP1061534A2 true EP1061534A2 (fr) 2000-12-20
EP1061534A3 EP1061534A3 (fr) 2000-12-27

Family

ID=7838976

Family Applications (2)

Application Number Title Priority Date Filing Date
EP00119956A Withdrawn EP1061534A3 (fr) 1997-08-14 1998-08-11 Matériau composite magnétique doux déformable et son procédé de fabrication
EP98948761A Expired - Lifetime EP0931322B1 (fr) 1997-08-14 1998-08-11 Materiau composite magnetique doux deformable et procede permettant de le produire

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP98948761A Expired - Lifetime EP0931322B1 (fr) 1997-08-14 1998-08-11 Materiau composite magnetique doux deformable et procede permettant de le produire

Country Status (5)

Country Link
US (1) US6537389B1 (fr)
EP (2) EP1061534A3 (fr)
JP (1) JP2001504283A (fr)
DE (2) DE19735271C2 (fr)
WO (1) WO1999009565A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004033135A1 (fr) * 2002-09-27 2004-04-22 Vacuumschmelze Gmbh & Co. Kg Piece moulee magnetique douce fabriquee selon un procede de metallurgie des poudres et presentant une grande permeabilite maximale, procedes de fabrication et utilisation associes

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DE19945619A1 (de) 1999-09-23 2001-04-19 Bosch Gmbh Robert Preßmasse und Verfahren zur Herstellung eines weichmagnetischen Verbundwerkstoffes mit der Preßmasse
US6702870B2 (en) * 2000-03-10 2004-03-09 Höganäs Ab Method for preparation of iron-based powder and iron-based powder
DE10106172A1 (de) * 2001-02-10 2002-08-29 Bosch Gmbh Robert Verfahren zur Herstellung eines Formteils aus einem weichmagnetischen Verbundwerkstoff
US7153594B2 (en) * 2002-12-23 2006-12-26 Höganäs Ab Iron-based powder
DE10331339A1 (de) * 2003-07-10 2005-02-03 Siemens Ag Elektromagnetisches Schaltgerät
JP2005133148A (ja) * 2003-10-30 2005-05-26 Mitsubishi Materials Corp 高強度および高比抵抗を有する複合軟磁性材の製造方法
US7494600B2 (en) * 2003-12-29 2009-02-24 Höganäs Ab Composition for producing soft magnetic composites by powder metallurgy
SE0303580D0 (sv) * 2003-12-29 2003-12-29 Hoeganaes Ab Composition for producing soft magnetic composites by powder metallurgy
KR100845392B1 (ko) 2004-06-23 2008-07-09 회가내스 아베 절연된 연자성 철계 분말 조성물용 윤활제
SE0401644D0 (sv) * 2004-06-23 2004-06-23 Hoeganaes Ab Lubricants for insulated soft magnetic iron-based powder compositions
US7416578B2 (en) * 2004-09-17 2008-08-26 Höganäs Ab Powder metal composition
JP4613622B2 (ja) * 2005-01-20 2011-01-19 住友電気工業株式会社 軟磁性材料および圧粉磁心
DE102006032517B4 (de) * 2006-07-12 2015-12-24 Vaccumschmelze Gmbh & Co. Kg Verfahren zur Herstellung von Pulververbundkernen und Pulververbundkern
JP5332408B2 (ja) * 2008-08-29 2013-11-06 Ｔｄｋ株式会社 圧粉磁心及びその製造方法
US8911663B2 (en) * 2009-03-05 2014-12-16 Quebec Metal Powders, Ltd. Insulated iron-base powder for soft magnetic applications
DE102013212866A1 (de) * 2013-07-02 2015-01-08 Robert Bosch Gmbh Gesinterter weichmagnetischer Verbundwerkstoff und Verfahren zu dessen Herstellung

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Publication number Priority date Publication date Assignee Title
WO2004033135A1 (fr) * 2002-09-27 2004-04-22 Vacuumschmelze Gmbh & Co. Kg Piece moulee magnetique douce fabriquee selon un procede de metallurgie des poudres et presentant une grande permeabilite maximale, procedes de fabrication et utilisation associes

Also Published As

Publication number Publication date
US6537389B1 (en) 2003-03-25
DE19735271C2 (de) 2000-05-04
DE59808444D1 (de) 2003-06-26
EP0931322B1 (fr) 2003-05-21
EP0931322A1 (fr) 1999-07-28
JP2001504283A (ja) 2001-03-27
WO1999009565A1 (fr) 1999-02-25
EP1061534A3 (fr) 2000-12-27
DE19735271A1 (de) 1999-02-25

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