EP2219195A1 - Matériau composite magnétique doux à haute résistance obtenu par compaction/combustion et son procédé de fabrication - Google Patents

Matériau composite magnétique doux à haute résistance obtenu par compaction/combustion et son procédé de fabrication Download PDF

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EP2219195A1
EP2219195A1 EP08847585A EP08847585A EP2219195A1 EP 2219195 A1 EP2219195 A1 EP 2219195A1 EP 08847585 A EP08847585 A EP 08847585A EP 08847585 A EP08847585 A EP 08847585A EP 2219195 A1 EP2219195 A1 EP 2219195A1
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Prior art keywords
soft
magnetic
oxide
heat treatment
compaction
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German (de)
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EP2219195A4 (fr
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Yoshihiro Tanaka
Masahisa Miyahara
Koichiro Morimoto
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Diamet Corp
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Diamet Corp
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    • 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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
    • C22C33/0207—Using a mixture of prealloyed powders or a master alloy
    • C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
    • 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
    • H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin

Definitions

  • the present invention relates to a high-strength soft-magnetic composite material obtained by compaction and heat treatment, which is used as a material of various types of electromagnetic circuit components of motors, actuators, reactors, transformers, choke cores, magnetic sensor cores or the like, and to a production method thereof.
  • the present application claims priority on Japanese Patent Application No. 2007-289774, filed on November 7, 2007 , the content of which is incorporated herein by reference.
  • soft-magnetic sintered materials produced by sintering iron powder, Fe-Al iron-based soft-magnetic alloy powder, Fe-Ni iron-based soft-magnetic alloy powder, Fe-Cr iron-based soft-magnetic alloy powder, Fe-Si iron-based soft-magnetic alloy powder and Fe-Si-Al iron-based soft-magnetic alloy powder (referred as soft-magnetic metal particles hereinafter) have conventionally been know.
  • this type of soft-magnetic sintered material has high magnetic flux density, it has the problem of having a low specific electrical resistance and hence poor high frequency characteristics. To improve the high frequency characteristics by increasing the specific electrical resistance, it has been proposed using soft-magnetic materials or the like that are bonded by water glass or low melting glass (see Patent Document 1 or Patent Document 2).
  • a composite soft-magnetic sintered material including a soft-magnetic metal particle phase and a grain boundary phase surrounding the soft-magnetic metal particle phase, wherein the grain boundary phase includes a ZnO phase having the hexagonal crystal structure, an Fe and Zn mixed oxide phase having the cubic crystal structure, and a glass phase (see Patent Document 3).
  • the ZnO phase having the hexagonal crystal structure is dispersed contacting to the soft-magnetic metal particle phase.
  • the Fe and Zn mixed oxide phase having the cubic crystal structure is dispersed contacting to the ZnO phase.
  • the glass phase is dispersed in between the Fe and Zn mixed oxide phases having the cubic crystal structure, and contacting with the Fe and Zn mixed oxide phase.
  • a method for producing compacted magnetic materials comprising, mixing Mg-containing iron powders coated with a Mg-containing ferrite film deposited by a chemical method such as chemical plating or a coating method, with low melting glass powders, molding by compaction, and heating, is known (see Patent Document 4).
  • One of the problems in the composite soft-magnetic sintered material described in Patent Document 3 is that the mixed oxide phase including Fe and Zn decomposes if it was heated at a temperature higher than 600°C, If the heat treatment was performed at 600°C or lower temperature, glass powers would not be melted, and thereby making it difficult to enhance adhesion between the soft-magnetic metal particle phases and hindering production of a high-strength soft-magnetic composite compaction-heat treated material.
  • the surface of the soft-magnetic metal particles is coated with Mg-containing ferrite film by a chemical method.
  • This chemically formed ferrite film is not stable and subjected to transformation, resulting reduction of insulating properties and poor adherence of the film to the surface of soft-magnetic metal particles. Therefore, even if the Mg-containing iron oxide-coated powder is press-formed with low melting glass followed by heat treatment, it does not guarantee reliable production of a high-strength soft-magnetic composite compaction-heat treated material.
  • an object of the present invention is to provide a high-strength soft-magnetic composite material by compaction and heat treatment, which can be subjected to a stress-relief annealing process retaining a high specific electrical resistance and low coercivity. It is achieved by an MgO coating that has high heat resistance properties, allowing a heat treatment process at a temperature higher than 600°C, for example at 700°C.
  • another object of the present invention is to provide a high-strength soft-magnetic composite material by compaction and heat treatment, which has high bending strength. It is achieved by forming strong bonding between soft-magnetic metal particles by filling the interface connecting the soft-magnetic metal particles with a grain boundary layer of low melting glass or metal oxide containing iron oxide mainly consisted of Fe 3 O 4 .
  • an oxidized soft-magnetic powder having an iron oxide film on the surface of the soft-magnetic powder is prepared by preheating Fe-based soft-magnetic powders in an oxidizing atmosphere. After addition of Mg powders to the oxidized soft-magnetic powders, and mixing them with a rolling granulation agitation mixer, the mixed powders are heated in an inert gas atmosphere or vacuum atmosphere. If it is needed, further oxidation treatment is carried out by heating in an oxidizing atmosphere.
  • a Mg-Fe-O ternary oxide deposition film containing at least (Mg, Fe)O as oxides among ones found in the Mg-Fe-O ternary system which are typified by (Mg, Fe)O and (Mg, Fe) 3 O 4 in the conventionally known MgO-FeO-Fe 2 O 3 system can be formed on the surface of a soft-magnetic powder particles.
  • Fe-based soft-magnetic metal particles and an Mg-containing oxide coating film coating the surface of the soft-magnetic metal particles can be formed with tight adhesion.
  • the Fe-based soft-magnetic iron particles with the Mg-containing oxide coating film are bonded on the surface side of the grain boundary layer containing a mixture of silicon resin, low melting glass or metal oxide component in the grain boundary layers thereof. Since iron oxide is dispersed and grown at the grain boundaries of joined portions, the surface side of the grain boundary layer and the Mg-containing oxide coating film can be adhered strongly. Because of the strong adhesion, a high-strength soft-magnetic composite compaction-heat treated material can be produced.
  • the Mg-containing oxide coating film can be placed around Fe-based soft-magnetic metal particles property, even after compaction molding, individual Fe-based soft-magnetic metal particles can be separated and insulated properly.
  • high specific electrical resistance can be achieved in the entire soft-magnetic composite compaction-heat treated material, and a soft-magnetic composite compaction-heat treated material with suppressed eddy current loss can be produced.
  • the surface layer portion where Fe-based soft-magnetic metal particles are joined on the surface side of the grain boundary layer has high strength, it contributes to strength of the entire soft-magnetic composite compaction-heat treated material.
  • the soft-magnetic composite material produced by compacting and heat treatment according to the present invention has high density, high strength, high specific electrical resistance and high magnetic flux density.
  • the soft-magnetic composite material produced by compacting and heat treatment of the present invention is superior in terms of having the characteristics of high strength, high magnetic flux density and low high-frequency iron loss. Therefore, it can be used as a material of various types of electromagnetic circuit components by taking advantage of these characteristics.
  • the Mg-containing oxide film consists mainly of (Mg, Fe)O, and as a low melting glass, any one of Bi 2 O 3 -B 2 O 3 , SnO-P 2 O 3 , SiO 2 -B 2 O 3 -ZnO, SiO 2 -B 2 O 3 -R 2 O and Li 2 O-ZnO can be utilized.
  • a metal oxide any one of Al 2 O 3 , B 2 O 3 , Sb 2 O 3 or MoO 3 can be utilized.
  • a soft-magnetic composite material that is produced by compacting and heat treatment having the superior characteristics described above, can be produced.
  • a surface layer portion contributing to improved strength can be formed by heat treatment in an oxidizing atmosphere. Because of the surface layer portion, a soft-magnetic composite compaction-heat treated material with high strength, high density, high specific electrical resistance and high magnetic flux density, can be produced.
  • a high-strength soft-magnetic composite material produced by compacting and heat treatment of the present invention can be used as, for example, a magnetic core, motor core, generator core, solenoid core, ignition core, reactor core, transformer core, choke coil core or magnetic sensor core of the electromagnetic circuit components.
  • electromagnetic circuit components with superior performance can be provided in applications mentioned above.
  • Electrical equipment utilizing electromagnetic circuit components include motors, generators, solenoids, injectors, electromagnetic valve actuators, inverters, converters, transformers, relays and magnetic sensor systems. Because of the present invention, efficiency and performance of the electrical equipments can be improved, and additionally it can contribute to down-sizing and reducing weight of these equipments.
  • Mg-containing oxide-coated soft-magnetic particles which is coated with an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O on the soft-magnetic metal particles, are prepared.
  • the soft-magnetic metal particles can be prepared with the following raw material powders by any of the subsequently described methods from (A) to (D).
  • the conventionally and commonly known iron powder, the insulated iron powder, the Fe-Al iron-based soft-magnetic alloy powder, the Fe-Ni iron-based soft-magnetic alloy powder, the Fe-Si-Al iron-based soft-magnetic alloy powder, the Fe-Co iron-based soft-magnetic alloy powder, the Fe-Co-V iron-based soft-magnetic alloy powder or the Fe-P iron-based soft-magnetic alloy powder can be preferably used. More specifically, the iron powder is preferably a pure iron powder.
  • the insulated iron powder is preferably a phosphate-coated iron powder, or a silicon oxide- or aluminum oxide-coated iron powder prepared by drying and heat treatment, after addition of and mixing with a wet solution such as a silica sol gel solution (silicate) or alumina sol gel solution to coat the surface of the iron powder.
  • the Fe-Al iron-based soft-magnetic alloy powder is preferably an Fe-Al iron-based alloy powder containing 0.1 to 20 % of Al, with residuals consisting Fe and inevitable impurities (for example, an alperm powder having a composition consisting of Fe and 15% ofAl).
  • the Fe-Ni iron-based soft-magnetic alloy powder is preferably a nickel-based soft-magnetic alloy powder containing 35 to 85 % of Ni, and further containing one or more than two elements from a group comprising, 5 % of Mo or less, 5 % of Cu or less, 2 % of Cr or less, and 0.5 % of Mn or less depending on necessity, with a residual consisting af Fe and inevitable impurities (for example, powder consisting of Fe and 49% Ni).
  • the Fe-Cr iron-based soft-magnetic alloy powder is preferably an Fe-Cr iron-based soft-magnetic alloy powder containing 1 to 20 % of Cr, and further containing one or more than two elements from a group comprising of 5 % of Al or less and 5 % of Ni or less depending on necessity, with the residual consisting of Fe and inevitable impurities.
  • the Fe-Si iron-based soft-magnetic alloy powder is preferably an Fe-Si iron-based soft-magnetic alloy powder containing 0.1 to 10 % of Si, with the residual consisting of Fe and inevitable impurities.
  • the Fe-Si-Al iron-based soft-magnetic alloy powder is preferably an Fe-Si-Al iron-based soft-magnetic alloy powder containing 0.1 to 10 % of Si and 0.1 to 20 % of Al, with the residual consisting of Fe and inevitable impurities.
  • the Fe-Co-V iron-based soft-magnetic alloy powder is preferably an Fe-Co-V iron-based soft-magnetic alloy powder containing 0.1 to 52 % of Co and 0.1 to 3 % of V, with the residual consisting of Fe and inevitable impurities.
  • the Fe-Co iron-based soft-magnetic alloy powder is preferably an Fe-Co iron-based soft-magnetic alloy powder containing 0.1 to 52 % of Co, with the residual consisting of Fe and inevitable impurities.
  • the Fe-P iron-based soft-magnetic alloy powder is preferably an Fe-P iron-based soft-magnetic alloy powder containing 0.5 to 1.0 % of P, with the residual consisting of Fe and inevitable impurities (in the following descriptions, % refers to % by weight (wet%)).
  • An average diameter of the of the soft-magnetic metal particles is preferably within the range of 5 to 500 ⁇ m.
  • One of the reasons for choosing this range is that if the average particle diameter is less than 5 ⁇ m, the compressibility of the powder decreases and the volume ratio of the soft-magnetic metal particles becomes low, thereby lowering the value of magnetic flux density, which is not desirable.
  • Another reason is that if the average particle diameter exceeds 500 ⁇ m, eddy current within the soft-magnetic metal particles increases and magnetic permeability at high frequencies decreases.
  • the material is further heated at a temperature of 50 to 400°C in an oxidizing atmosphere (room temperature refers to a temperature of 25°C in the following descriptions), and Mg-containing oxide-coated soft-magnetic metal particles (powder) with an oxide insulating film containing Mg on the surface of the soft-magnetic metal particles are produced.
  • room temperature refers to a temperature of 25°C in the following descriptions
  • Mg-containing oxide-coated soft-magnetic metal particles have considerably superior adhesiveness as compared with conventional Mg-containing oxide-coated soft-magnetic particles with a formed Mg ferrite film. Frequency of being damaged and exfoliation of the insulating coating on the Mg-containing oxide-coated soft-magnetic particles is kept low, even if a powder compact is produced by press forming.
  • a soft-magnetic composite compaction-heat treated material obtains a structure in which an Mg-containing oxide film is uniformly dispersed at a grain boundary and is not concentrated at a grain boundary triple junction.
  • the mixed powder prepared by mixing the oxidation-treated soft-magnetic metal particles with Mg powders and heated in an inert gas atmosphere or vacuum atmosphere at a temperature of 150 to 1100°C and pressure of 1 ⁇ 10 -12 to 1 ⁇ 10 -1 MPa it is preferable to heat the mixed powder under rallying motion.
  • an Mg-Si-containing oxide-coated soft-magnetic powder is prepared in which an Mg-Si-containing oxide film is formed on the surface of the soft-magnetic powder.
  • a composite soft-magnetic sintered material produced with the Mg-Si-containing oxide-coated soft-magnetic powder prepared according to this method surpasses a conventional compound soft-magnetic sintered material produced by compression-molding and sintering a mixture including a compound forming SiO and powders of MgCO 3 or MgO, in terms of density, bending strength, specific electrical resistance and magnetic flux density.
  • an Mg-Si-containing oxide-coated soft-magnetic powder is prepared in which an Mg-Si-containing oxide film is formed on the surface of the soft-magnetic powder.
  • the mixed powder After addition of an Mg powder, and after or during mixing of the Mg powder with the oxide-coated soft-magnetic powder, the mixed powder is heated at a temperature of 400 to 800°C in a vacuum atmosphere.
  • an Mg-containing oxide-coated soft-magnetic powder is prepared in which an Mg-containing oxide film is formed on the surface of the soft-magnetic powder.
  • the mixed powder After addition of a silicon monoxide powder, and after or during mixing of the silicon monoxide with the Mg-containing oxide-coated soft-magnetic powder, the mixed powder is heated at a temperature of 600 to 200°C in a vacuum atmosphere.
  • an Mg-Si-containing oxide-coated soft-magnetic powder is prepared in which an Mg-Si-containing oxide film is formed on the surface of the soft-magnetic powder.
  • a composite soft-magnetic sintered material produced with the Mg-Si-containing oxide-coated soft-magnetic powder prepared according to this method surpasses a conventional compound soft-magnetic sintered material produced by compression-molding and sintering a mixture including a compound forming SiO and powders of MgCO 3 or MgO, in terms of density, bending strength, specific electrical resistance and magnetic flux density.
  • the amount of the silicon monoxide powder added is preferably within the range of 0.01 to 1% by weight, and the amount of the Mg powder added is preferably within the range of 0.05 to 1% by weight.
  • the vacuum atmosphere is preferably a vacuum atmosphere at a pressure of 1 ⁇ 10 -12 to 1 ⁇ 10 -1 MPa.
  • the silicon monoxide (SiO) powder used in the aforementioned production method is made of an oxide having the highest vapor pressure among silicon oxides.
  • silicon oxide components are easily deposited on the surface of soft-magnetic metal particles by heating, and even if heated after mixing with silicon dioxide (SiO 2 ) having a low vapor pressure, a silicon oxide film with an adequate thickness might not be formed on the surface of the soft-magnetic metal particles.
  • the mixed powder is heated at a temperature of 600 to 1200°C in a vacuum atmosphere.
  • a silicon oxide film-coated soft-magnetic powder is prepared in which SiO x (where, x is 1 or 2) film is formed on the surface of the soft-magnetic powder. Further, after addition of Mg powders to the silicon oxide film-coated soft-magnetic powders and during mixing of them, an Mg-Si-containang oxide-coated soft-magnetic powder coated by an Mg-Si-containing oxide film that is made of Mg-Si-Fe-O, can be prepared by heating in a vacuum atmosphere.
  • the oxide-coated soft-magnetic powder can be prepared by forming an iron oxide film on the surface of a soft-magnetic powder by leaving soft-magnetic metal particles at a temperature of 25 to 500°C in an oxidizing atmosphere (such as in air). Because of this iron oxide film, the particles can be coated with SiO and/or Mg more effectively. If the oxide-coated soft-magnetic powder is heated at a temperature higher than 500°C in an oxidizing atmosphere during production of the oxide-coated soft-magnetic powder, the soft-magnetic metal particles aggregate, resulting in the formation of soft-magnetic metal particle aggregates, and sintering. These prevent an uniform surface oxidation, and therefore are not desirable. Therefore, the heating temperature during production of the oxide-coated soft-magnetic powder is defined to be from room temperature to 500°C. A more preferable temperature range is from room temperature to 300°C.
  • the oxidizing atmosphere is more preferably a dry oxidizing atmosphere.
  • the amount of SiO powder added to the oxide-coated soft-magnetic powders is limited to 0.01 to 1% by weight. If the added amount of the SiO powder is less than 0.01% by weight, the thickness of the silicon oxide film formed on the surface of the oxide-coated soft-magnetic powder is inadequate, thereby causing an insufficient amount of Si to be contained in the Mg-Si-containing oxide film. It prevents having an Mg-Si-containing oxide film with high specific electrical resistance, and thereby making this undesirable.
  • SiO x (where, x is 1 or 2) silicon oxide film formed is excessively thick. This might cause lower density of a soft-magnetic composite compaction-heat treated material, which is produced by compacting and heat treatment the prepared Mg-Si-cantaining oxide-coated soft-magnetic metal particles.
  • the amount of Mg powder added is limited to 0.05 to 1% by weight. If the amount of Mg powder added is less than 0.05% by weight, the thickness of the Mg film formed on the surface of the oxide-coated soft-magnetic powder is inadequate, and consequently only an inadequate amount of Mg is incorporated in the Mg-Si-containing oxide film. Because of lack of adequate thickness of the Mg-Si-containing oxide film, having the amount of Mg powder less than 0.05 % is not desirable.
  • the amount of Mg powder added exceeds 1% by weight, the thickness of the formed Mg film becomes excessively thick, and the density of a soft-magnetic composite compaction-heat treated material obtained by compacting and heat treatment the resulting Mg-Si-containing oxide-coated soft-magnetic powder decreases, thereby making this undesirable.
  • adding and mixing SiO powder, Mg powder and a mixed powder of SiO powder and Mg powder to the oxide-coated soft-magnetic powder is carried out in a vacuum atmosphere at a temperature of 600 to 1200°C. Due to the low vapor pressure of SiO, even if a mixed powder is heated at a temperature below 600°C, a sufficiently thick SiO film or Mg-Si-containing oxide coating film cannot be obtained. On the other hand, if a mixed powder is mixed at a temperature above 1200°C, the soft-magnetic powder ends up sintering.
  • the heating atmosphere at that time is preferably a vacuum atmosphere at a pressure of 1 ⁇ 10 -12 to 1 ⁇ 10 -1 MPa. Moreover, heating the mixed powder in rolling motion is more preferable.
  • Soft-magnetic powder having an average particle diameter within the range of 5 to 500 ⁇ m is preferably used for the soft-magnetic metal particles used when preparing an oxide-coated soft-magnetic powder.
  • the reason for this is that if the average particle diameter is less than 5 ⁇ m, the compressibility of the powder decreases and the volume ratio of the soft-magnetic powder becomes low, thereby causing reduction of the magnetic flux density value and making this undesirable.
  • the average particle diameter exceeds 500 ⁇ m, eddy current of the soft-magnetic powder increases, causing reduction of its magnetic permeability at high frequencies. Oxidation treatment of the soft-magnetic metal particles makes them more susceptible to coating afterward.
  • Oxidation treatment is carried out by leaving the particles at a temperature of 150 to 500°C in an oxidizing atmosphere or at a temperature of 50 to 100°C in distilled water or pure water. In either case, a temperature below 50°C is not efficient. On the other hand, if the temperature is held above 500°C in an oxidizing atmosphere, sintering occurs, thereby making this undesirable.
  • the oxidizing atmosphere is preferably a dry oxidizing atmosphere.
  • a deposition film normally refers to a film in which vacuum-deposited or sputtered atoms composing a film are deposited on, for example, a substrate
  • a deposition film refers to a film in which iron oxide (Fe-O) and Mg of an Fe-based soft-magnetic powder with an iron oxide film are deposited on the surface of the Fe-based soft-magnetic metal particles accompanying reaction thereof.
  • the film thickness of the Mg-Fe-O ternary oxide deposition film formed on the surface of the Fe-based soft-magnetic metal particles is preferably within the range of 5 to 500 nm in order to achieve high magnetic flux density and high specific electrical resistance of a soft-magnetic composite compaction-heat treated material after powder compaction. If the film thickness is less than 5 nm, the specific electrical resistance of the compacted soft-magnetic composite compaction-heat treated material is not adequate and eddy current loss increases, thereby making this undesirable. If the film thickness exceeds 500 nm, the magnetic flux density of the compacted soft-magnetic composite compaction-heat treated material decreases, thereby making this undesirable.
  • the film thickness is more preferably within the range of 5 to 200 nm.
  • Mg-containing oxide-coated soft-magnetic particles produced according to the aforementioned method have an Mg-containing oxide film formed on the surface thereof.
  • This Mg-containing oxide film reacts with silicon oxide or aluminum oxide to form a complex oxide and a complex oxide with high resistance interposes between grain boundaries of the soft-magnetic powder.
  • a soft-magnetic composite compaction-heat treated material with high specific electrical resistance can be produced.
  • a soft-magnetic composite compaction-heat treated material having superior mechanical strength can be produced, since sintered powders are mediated by the silicon oxide or aluminum oxide. In this case, coercivity can be held to low level since the main body of the sintered materials comprises silicon oxide or aluminum oxide.
  • a soft-magnetic composite compaction-heat treated material having low hysteresis loss can be produced.
  • the aforementioned heat treatment is preferably carried out in an inert gas atmosphere or non-oxidizing atmosphere at a temperature of 400 to 1300°C.
  • main body refers to the component with the largest composite ratio in each composition.
  • a soft-magnetic composite coinpaction-heat treated material is produced using Mg-containing oxide-coated soft-magnetic particles produced in the manner described above according to the previously explained methods.
  • an insulating binder in the form of a silicone resin, low melting glass or metal oxide is mixed with the Mg-containing oxide-coated soft-magnetic particles, which is produced with the aforementioned methods, followed by compaction molding using an ordinary method and heat treatment in an inert gas atmosphere or non-oxidizing atmosphere to produce a precursor of a soft-magnetic composite compaction-heat treated material.
  • the precursor is heat-treated at a temperature of 400 to 600°C in an oxidizing atmosphere such as a steam atmosphere or air, as subsequently described to produce an object of the present invention in the form of a soft-magnetic composite material obtained by compaction and heat treatment.
  • an oxidizing atmosphere such as a steam atmosphere or air
  • a defined amount of silicone resin or low melting glass including any of Bi 2 O 3 -B 2 O 3 , SnO-P 2 O 3 , SiO 2 -B 2 O 3 -ZnO, SiO 2 -B 2 O 3 -R 2 O and Li 2 O-ZnO is incorporated in the Mg-containing oxide-coated soft-magnetic particles, which is produced according to the aforementioned methods.
  • the amount of silicone resin that is incorporated can be within the range of 0.2 to 1.5% by weight.
  • the amount of low melting glass that is incorporated can be within the range of 0.05 to 3.0% by weight.
  • a defined amount of metal oxide is incorporated in the Mg-containing oxide-coated soft-magnetic particles, instead of the silicone resin or low melting glass.
  • the metal oxides include one or more than two metal oxides selected from the group consisting of aluminum oxide, boron oxide, vanadium oxide, bismuth oxide, antimony oxide and molybdenum oxide. These metal oxides are incorporated within the range of 0.05 to 1% by weight as Al 2 O 3 , B 2 O 3 , V 2 O 5 , Bi 2 O 3 , Sb 2 O 3 and MoO 3 , and are compacted and molded after mixing.
  • the resulting compact is then heat treated within a temperature range of 500 to 1000°C, and preferably 550 to 750°C, in a non-oxidizing atmosphere to produce a precursor of a soft-magnetic composite compaction-heat treated material, which is followed by heat-treating the precursor in an oxidizing atmosphere to produce a soft-magnetic composite material obtained by compaction and heat treatment.
  • a non-oxidizing atmosphere to produce a precursor of a soft-magnetic composite compaction-heat treated material
  • zinc stearate can also be used for the metal oxide.
  • atmospheres that can be selected for the heat treatment atmosphere include an inert gas atmosphere such as a nitrogen atmosphere, and a non-oxidizing atmosphere such as a hydrogen gas atmosphere.
  • heat treatment is carried out by heating within a temperature range of 400 to 600°C in an oxidizing atmosphere such as a steam atmosphere for the purpose of enhancing the bending strength or the like of the precursor of the soft-magnetic composite compaction-molded material.
  • an oxidizing atmosphere such as a steam atmosphere for the purpose of enhancing the bending strength or the like of the precursor of the soft-magnetic composite compaction-molded material.
  • coated soft-magnetic particles (powder) in the precursor in which an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O is coated and formed on the surface of soft-magnetic particles, and an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O present at the interface thereof, are transformed.
  • the transformation results in a structure in which a plurality of Mg-containing oxide-coated soft-magnetic particles are bonded each other through the interposing the grain boundary layer and the intended soft-magnetic composite material obtained by compaction and heat treatment is produced at the end.
  • the Mg-containing oxide-coated soft-magnetic particles comprises soft-magnetic metal particles and the Mg-containing oxide coating on the surfaces of the soft-magnetic metal particles.
  • the grain boundary layer comprises mainly of a silicon oxide containing an iron oxide (for example, a silicon oxide such as a silicone resin containing an iron oxide consisting mainly of Fe 3 O 4 or FeO), an oxide containing a low melting glass component, or an iron oxide containing Mg.
  • a steam atmosphere at 400 to 600°C can be preferably selected for the aforementioned oxidizing atmosphere
  • heat treatment can be carried out in condition with heating within the aforementioned temperature range in an oxidizing atmosphere such as air. If the temperature of the heat treatment conditions in the steam atmosphere is lower than 400°C, formation of Fe 3 O 4 is not promoted, thereby possibly resulting in deterioration of strength. On the other hand, if temperature of the heating conditions exceeds 600°C, strength can be also deteriorated due to formation and decomposition of FeO (4FeO ⁇ Fe 3 O 4 + Fe).
  • the iron oxide consisting mainly of Fe 3 O 4 grows in the steam atmosphere by diffusing in the silicone resin, it is inferred that Fe diffuses through minute cracks, which are formed during molding, and crystal grains composing the MgO film. It is interpreted that strength is improved because the diffusing Fe is oxidized in the heat treatment in the oxidizing atmosphere and then the grain boundary layer is filled with the increasing iron oxide, which is mainly consisted of Fe 3 O 4 , or in addition to Fe 3 O 4 , iron oxides including FeO in part fill the grain boundary layer.
  • connections between the Mg-containing oxide-coated soft-magnetic metal particles, which are comprised of the soft-magnetic metal particles and the Mg-containing oxide film coating the soft-magnetic metal particles, and the aforementioned low melting glass or the metal oxide are the connections through the surface side grain boundary layers, and they are formed by mixing, compacting and heat-treating.
  • the iron oxide present in the surface side grain boundary layer between the Mg-containing oxide-coated soft-magnetic particles is dispersed and grown as a result of the iron component thereof precipitating from the soft-magnetic metal particles at the grain boundary and forming an oxide.
  • the Mg-containing oxide adjacent to the surface side grain boundary layer is obtained from an Mg-containing oxide film provided on the Mg-containing oxide-coated soft-magnetic particles prior to the aforementioned mixing, compacting and heat treatment.
  • the surface side grain boundary layer that surrounds the Mg-containing oxide-coated soft-magnetic particles has a structure mainly consisting of silicon oxide containing iron oxide (for example, a silicon oxide such as a silicone resin containing iron oxide consisting mainly of Fe 3 O 4 or FeO), an oxide containing a low melting glass component, or an iron oxide containing Mg.
  • FIG. 1A shows the cross-sectional structure of an example of this type of soft-magnetic composite material obtained by compaction and heat treatment.
  • This example of a soft-magnetic composite compaction-heat treated material 10 is in the shape of a disc, and has a bilayer structure in which a surface layer portion 10a having a thickness of 2 to 4 mm is formed on the surface layer side (in the case of a density of 7.5 g/cm 3 ) and an inner layer portion 10b formed to the inside thereof
  • the thickness of the surface layer portion 10a is affected by the density of the finished product of the soft-magnetic composite compaction-heat treated material.
  • the thickness thereof is 2 to 4 mm in the case of a density of 7.5 glcm 3 as described above, in the case of a density of 7.0 g/cm 3 , the thickness increases up to a maximum of about 15 mm, and becomes a thickness of about 0.3 mm depending on whether the density is increased and heat-treatment conditions.
  • FIG. 1B shows an enlarged view of a portion of the surface layer portions.
  • an Mg-containing oxide film 2 is formed so as to cover the surface of an Fe-based soft-magnetic particle 1 resulting in the formation of an Mg-containing oxide-coated soft-magnetic particle, and a soft-magnetic composite compaction-heat treated material includes a plurality of the Mg-containing oxide-coated soft-magnetic particles being bonded each other through an interposing surface side grain boundary layer 5.
  • the soft-magnetic composite compaction-heat treated material 10 is produced by compacting, heat treatment and heat-treating a plurality of Mg-containing oxide-coated soft-magnetic particles
  • the Mg-containing oxide-coated soft-magnetic particles preferably have an irregular shape and the Mg-containing oxide film 2 is formed over their entire surface.
  • Each Mg-containing oxide-coated soft-magnetic particle is at least preferably covered with the Mg-containing oxide film so that overall specific electrical resistance of the soft-magnetic composite compaction-heat treated material does not decrease.
  • the grain boundary layer 5 at the grain boundary triple junction where three soft-magnetic particles 1 have gathered is thicker than the grain boundary layer 5 at another site as shown in FIG. 1B
  • the thickness of the Mg-containing oxide film 2 at certain portions thereof, or in the case there are certain portions where coating is inadequate do not cause a problem as long as the overall specific electrical resistance of the soft-magnetic composite compaction-heat treated material as claimed in the present invention is high.
  • the duration of heat treatment in a steam atmosphere or in air for producing the soft-magnetic composite compaction-heat treated material 10 can be suitably adjusted within a range of several minutes to several hours, the effect of improving strength tends to be saturated if heat treatment is carried out beyond that which is necessary.
  • an interposing grain boundary layer consisting mainly of silicon oxide containing iron oxide (for example, a silicon oxide such as a silicone resin containing iron oxide consisting mainly of Fe 3 O 4 or FeO)
  • an oxide containing a low melting glass component, or an iron oxide containing Mg is not formed throughout the entire thickness of the precursor.
  • This structure is formed at the portion with a thickness of 2 to 4 mm from the uppermost surface of the precursor in the case of a density of 7.5 g/cm 3 under ordinary heat treatment conditions.
  • the steam atmosphere or other oxidizing atmosphere does not have an effect on the formation of the grain boundary layer throughout the entire thickness of the precursor, but rather the effect is limited to a region having a certain thickness from the uppermost surface of the precursor. Namely, since a pathway for the oxidizing atmosphere is obstructed by the formation of oxide at the grain boundary, the oxidizing atmosphere is unable to be supplied to the inside, thereby resulting in the formation of oxide occurring in a limited region from the surface.
  • an inner layer portion is formed in which Fe-based Mg-coated soft-magnetic alloy powder is bound by the inside grain boundary layer formed as a result of being heat-treated in a state in which the central portion thereof is either not affected or only slightly affected by the oxidizing atmosphere such as a steam atmosphere.
  • the Mg-containing oxide-coated magnetic particles are bonded by a grain boundary layer in which an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O has been heat-treated, and an inner grain boundary layer including a grain boundary layer consisting mainly of SiO 2 obtained by heat treatment a silicone resin.
  • the Mg-containing oxide-coated soft-magnetic particles are bonded on the side of this inner layer portion by a grain boundary layer obtained by heat-treating an Mg-Fe-O ternary oxide deposition film and an inside grain boundary layer including the heat treated product of a silicone resin, instead of a surface side grain boundary layer formed as a result of being affected by a steam atmosphere or other oxidizing atmosphere, strength of the inside structure becomes deteriorated compared to that of the surface layer portion.
  • the soft-magnetic composite compaction-heat treated material 10 which is the final product, retain sufficiently high strength.
  • the periphery of the Mg-containing oxide-coated soft-magnetic particles is coated with a surface side grain boundary layer or inside grain boundary layer, which is formed based on an Mg-Fe-O ternary oxide deposition film.
  • an Mg-containing oxide coating which is present around the soft-magnetic particles, magnetically isolates each soft-magnetic particle, and the soft-magnetic composite compaction-heat treated material, with high specific electrical resistance and low eddy current loss can be produced.
  • the soft-magnetic composite compaction-heat treated material 10 obtained according to the production method described above has high density, high strength, high specific electrical resistance and high magnetic flux density. Since this soft-magnetic composite compaction-heat treated material 10 has the characteristics of high magnetic flux density and low high-frequency iron loss, it can be used as a material of various types of electromagnetic circuit components by taking advantage of these characteristics.
  • the soft-magnetic composite compaction-heat treated material 10 obtained according to the production method described above is provided with a surface layer portion 10a in which soft-magnetic particles are bonded each other through an interposing surface side grain boundary layer containing a low melting glass component containing iron oxide consisting mainly of Fe 3 O 4 , or a surface side grain boundary layer consisting mainly of a metal oxide containing iron oxide consisting mainly of Fe 3 O 4 .
  • These surface side grain boundary layers are grown by heat treatment an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O and low melting glass or metal oxide present at the interface thereof in an oxidizing atmosphere.
  • each Mg-containing oxide-coated soft magnetic particle can be bonded properly, and even higher bending strength can be achieved.
  • a soft-magnetic composite material with high strength can be obtained by compaction and heat treatment.
  • the soft-magnetic composite compaction-heat treated material produced according to the present production method has superior characteristics provided in addition to the characteristics of high magnetic flux density and low high-frequency iron loss.
  • the minimum value of the thickness of the surface layer portion 10a in the soft-magnetic composite compaction-heat treated material 10 cannot be uniformly defined since it is affected by the size and density of the finished product.
  • a minimum thickness of 0.3 mm or more is preferable.
  • the thickness of the surface layer portion 10a is about 4 mm at a maximum even if temperature, duration and other parameters are controlled during heat treatment in an oxidizing atmosphere.
  • Heat treatment was carried out on a soft-magnetic powder (pure iron powder) having an average particle diameter of 100 ⁇ m at 220°C in air for 0 to 60 minutes.
  • the MgO film is proportional to the oxide film thickness formed during the heat treatment in air at 220°C of the previous stage.
  • the amount of Mg added is only required to be the minimum required amount, 0.1% by weight of Mg powder was incorporated in the iron powder, and Mg-containing oxide-coated soft-magnetic particles were produced by rolling with a rolling granulation agitation mixer.
  • the results of measuring the thickness of the Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O formed on the outer periphery of the Mg-containing oxide-coated soft-magnetic particles are shown in Table 1. Since the thickness of this film is proportional to the oxide film thickness formed by heat treatment in air as described above, samples having an MgO film thickness of 20 to 80 nm were used for the test samples.
  • Silicon resin was added to each of the MgO film thickness samples within the range of 0.3 to 1.5% as shown in Table 1, followed by heat treatment at the molding pressure and heat treatment conditions shown in Table 1. In addition, a sample was also prepared in which silicone resin was not added.
  • a precursor of a soft-magnetic composite compaction-heat treated material comprised of an Mg-Fe-O ternary oxide deposition film containing (Mg, Fe)O and a silicone resin present at the interface thereof (and in the form of a plate measuring 60 mm ⁇ 10 mm ⁇ 5 mm). Then, heat treatment was carried out on the precursor under the temperature conditions shown in Table 2 in a steam atmosphere or in air, namely an oxidizing atmosphere, to obtain a target soft-magnetic composite material obtained by compaction and heat treatment.
  • bending strength of the sample nos. 1 to 3, which were not subjected to heat treatment after heat treatment was within the range of 52 to 94 MPa.
  • bending strength was improved in all cases for the sample nos. 4 to 12, 15, and 17 to 26, in which heat treatment was carried out at 400 to 560°C after having heat treated the samples at a temperature of 550 to 650°C in a non-oxidizing atmosphere such as a nitrogen gas atmosphere or hydrogen gas atmosphere.
  • a non-oxidizing atmosphere such as a nitrogen gas atmosphere or hydrogen gas atmosphere.
  • bending strength was 83 and was not improved.
  • specific electrical resistance was extremely low.
  • FIG 2 is an enlarged photograph showing the metal structure of the surface portion (a portion at a depth of 1 mm from the location of the uppermost surface) of the sample no.. 8 of a high-strength soft-magnetic composite material obtained by compacting and heat treatment as claimed in the present invention obtained in the example.
  • Energy dispersive X-ray (EDX) analysis was carried out at positions 111, 112, 113, 114, 115 and 116 in the metal structure shown in FIG. 2 . Those results are shown in FIGS. 3 to 8 .
  • An analysis result for the position 111 of the soft-magnetic particles, is shown in FIG. 3 .
  • An analysis result for the position 112, which corresponds to a peripheral portion of the soft-magnetic particles, is shown in FIG.
  • FIG. 4 An analysis result for the position 113, which corresponds to a portion predicted to be an Mg-containing oxide film located outside the soft-magnetic metal particles, is shown in FIG. 5 .
  • An analysis result for the position 115, which corresponds to the portion predicted to be an Mg-containing oxide film located outside the soft-magnetic metal particles, is shown in FIG. 7 .
  • FIG. 8 An analysis result for the position 116, which corresponds to a peripheral portion of the soft-magnetic metal particles, is shown in FIG. 8 .
  • FIG. 9 is an enlarged photograph of the metal structure of a surface portion (a portion at a depth of 0.5 mm from the location of the uppermost surface) of the sample no.. 8 of the high-strength soft-magnetic composite material obtained by compaction and heat treatment as claimed in the present invention obtained in an example.
  • X-ray diffraction analyses were carried out at positions 1, 2, 3, 4, 5 and 6 in the metal structure shown in FIG. 9 . These results are shown in FIGS. 10 to 15 .
  • positions 1 and 2 correspond to the locations of the boundaries of three Mg-containing oxide-coated soft-magnetic particles in the form of grain boundary triple junctions.
  • the position 3 corresponds to the location of another grain boundary triple junction.
  • the positions 4 and 5 correspond to the boundaries of two Mg-containing oxide-coated soft-magnetic particles.
  • the position 6 corresponds to a location near a boundary of three Mg-containing oxide-coated soft-magnetic particles in the form of a grain boundary triple junction.
  • FIG. 16 is an enlarged photograph of the metal structure of the sample no. 8 of the high-strength soft-magnetic composite material obtained by compaction and heat treatment as claimed in the invention obtained in an example. As shown in FIG. 16 , it was confirmed that there were the Mg-containing oxide films on the outer periphery of the soft-magnetic metal particles at a thickness of about 30 to 50 nm. In addition, it was confirmed that there was the surface side boundary layer of about the same width between the films.
  • the high-strength soft-magnetic composite material obtained by compaction and heat treatment (soft-magnetic material) according to the present invention can be used as an electromagnetic circuit component such as a magnetic core, motor core, generator core, solenoid core, ignition core, reactor core, transformer core, choke coil core or magnetic sensor core, and can be applied to an electromagnetic circuit component capable of demonstrating superior characteristics in any of these applications.
  • electromagnetic circuit components such as a magnetic core, motor core, generator core, solenoid core, ignition core, reactor core, transformer core, choke coil core or magnetic sensor core
  • Examples of electrical equipment in which these electromagnetic circuit components are incorporated include motors, generators, solenoids, injectors, electromagnetic valve actuators, inverters, converters, transformers, relays and magnetic sensor systems, and in addition to enhancing the efficiency and performance of these electrical equipments, the size and weight thereof can be reduced.

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9318244B2 (en) 2012-02-17 2016-04-19 Tdk Corporation Soft magnetic powder core
US9805855B2 (en) 2014-01-14 2017-10-31 Hitachi Metals, Ltd. Magnetic core and coil component using same
EP2589450A4 (fr) * 2010-06-30 2017-12-06 Panasonic Intellectual Property Management Co., Ltd. Matériau magnétique composite et processus de production de celui-ci
EP2680281A4 (fr) * 2011-02-22 2017-12-20 Mitsubishi Materials Corporation Matériau composite à aimantation temporaire ayant une faible intensité d'aimantation et une induction magnétique élevée, son procédé de production et composant de circuit électromagnétique
EP3441989A4 (fr) * 2016-03-31 2019-09-25 Mitsubishi Materials Corporation Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique
EP3693101A4 (fr) * 2017-10-04 2021-03-31 Mitsubishi Materials Corporation Poudre magnétique douce revêtue d'un isolant à base de silice et procédé de production associé

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BR112012022585A2 (pt) * 2010-04-01 2019-09-24 Hoeganaes Corp composição de pó metalúrgico, método para produzir um componente magnético compactado, componente metalúrgico de pó compactado e método para produzir uma composição de componente metalúrgico de pó compactado e recozido
JP5240234B2 (ja) * 2010-04-30 2013-07-17 株式会社デンソー 圧粉磁心の製造方法
JP2012049203A (ja) * 2010-08-24 2012-03-08 Toyota Central R&D Labs Inc 圧粉磁心、磁心用粉末およびそれらの製造方法
CN101996723B (zh) * 2010-09-29 2012-07-25 清华大学 一种复合软磁磁粉芯及其制备方法
JP5597512B2 (ja) * 2010-10-14 2014-10-01 株式会社神戸製鋼所 圧粉磁心の製造方法およびこの製造方法によって得られる圧粉磁心
JP5580725B2 (ja) * 2010-12-20 2014-08-27 株式会社神戸製鋼所 圧粉磁心の製造方法、および該製造方法によって得られた圧粉磁心
KR101503104B1 (ko) * 2011-08-01 2015-03-16 삼성전기주식회사 금속 자성 분말, 상기 금속 자성 분말을 포함하는 자성층 재료, 및 자성층 재료를 이용한 자성층을 포함하는 적층형 칩 부품
KR101688299B1 (ko) * 2012-08-10 2016-12-20 가부시키가이샤 무라타 세이사쿠쇼 자성체 조성물 및 코일 부품
JP6075605B2 (ja) * 2012-09-14 2017-02-08 アイシン精機株式会社 軟磁性体及びその製造方法
CN103943321B (zh) * 2013-01-23 2017-04-12 Tdk株式会社 磁芯和线圈型电子部件
CN104282406B (zh) * 2013-07-04 2017-04-12 Tdk株式会社 软磁性体组合物及其制造方法、磁芯、以及线圈型电子部件
JP2015028985A (ja) * 2013-07-30 2015-02-12 Tdk株式会社 軟磁性体組成物およびその製造方法、磁芯、並びに、コイル型電子部品
JP7324130B2 (ja) * 2019-11-27 2023-08-09 Ｄｏｗａエレクトロニクス株式会社 シリコン酸化物被覆軟磁性粉末および製造方法

Family Cites Families (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63158810A (ja) 1986-12-23 1988-07-01 Toshiba Corp 圧粉磁心
JPH05258934A (ja) 1992-03-11 1993-10-08 Kenichi Suzuki 磁性材料及びその製造方法
JPH0974011A (ja) * 1995-09-07 1997-03-18 Tdk Corp 圧粉コアおよびその製造方法
JP2000232014A (ja) * 1999-02-12 2000-08-22 Matsushita Electric Ind Co Ltd 複合磁性材料の製造方法
JP2004297036A (ja) 2002-12-04 2004-10-21 Mitsubishi Materials Corp Ｚｎを含むスピネルフェライト膜被覆鉄軟磁性粉末の製造方法およびその方法で作製した複合焼結軟磁性材
JP2004253787A (ja) 2003-01-30 2004-09-09 Mitsubishi Materials Corp 高強度、高磁束密度および高抵抗を有する複合軟磁性焼結材およびその製造方法
JP4265358B2 (ja) * 2003-10-03 2009-05-20 パナソニック株式会社 複合焼結磁性材の製造方法
JP2005133168A (ja) * 2003-10-31 2005-05-26 Mitsubishi Materials Corp 磁気特性に優れ、高強度および低鉄損を有する複合軟磁性材の製造方法
JP4534523B2 (ja) * 2004-02-25 2010-09-01 パナソニック株式会社 複合焼結磁性材料の製造方法
JP2006185981A (ja) * 2004-12-27 2006-07-13 Mitsubishi Materials Pmg Corp 高強度を有する圧粉磁心材の製造方法
JP2006332525A (ja) * 2005-05-30 2006-12-07 Mitsubishi Materials Pmg Corp 高強度、高磁束密度および高抵抗を有する鉄損の少ない高強度複合軟磁性材およびその製造方法
JP2006332524A (ja) * 2005-05-30 2006-12-07 Mitsubishi Materials Pmg Corp 高強度、高磁束密度および高抵抗を有する鉄損の少ない高強度複合軟磁性材およびその製造方法
JP4134111B2 (ja) * 2005-07-01 2008-08-13 三菱製鋼株式会社 絶縁軟磁性金属粉末成形体の製造方法
WO2007052772A1 (fr) * 2005-11-02 2007-05-10 Mitsubishi Materials Pmg Corporation POUDRE MAGNETIQUE TENDRE DE TYPE Fe-Si A BASE DE FER ENDUITE D'UN FILM DE DEPOT D'OXYDE ET SON PROCEDE DE PRODUCTION
JP2007162103A (ja) * 2005-12-15 2007-06-28 Hitachi Metals Ltd 混合磁性粉末とその製造方法、およびそれを用いてなるシート素材とその製造方法
JP4782058B2 (ja) * 2007-03-28 2011-09-28 株式会社ダイヤメット 高強度軟磁性複合圧密焼成材の製造方法および高強度軟磁性複合圧密焼成材

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2009060895A1 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2589450A4 (fr) * 2010-06-30 2017-12-06 Panasonic Intellectual Property Management Co., Ltd. Matériau magnétique composite et processus de production de celui-ci
EP2680281A4 (fr) * 2011-02-22 2017-12-20 Mitsubishi Materials Corporation Matériau composite à aimantation temporaire ayant une faible intensité d'aimantation et une induction magnétique élevée, son procédé de production et composant de circuit électromagnétique
US9318244B2 (en) 2012-02-17 2016-04-19 Tdk Corporation Soft magnetic powder core
US9805855B2 (en) 2014-01-14 2017-10-31 Hitachi Metals, Ltd. Magnetic core and coil component using same
EP3441989A4 (fr) * 2016-03-31 2019-09-25 Mitsubishi Materials Corporation Noyau de poussière recouvert d'un isolant à base de silicium, procédé de fabrication associé et composant de circuit électromagnétique
US11183321B2 (en) 2016-03-31 2021-11-23 Diamet Corporation Powder magnetic core with silica-based insulating film, method of producing the same, and electromagnetic circuit component
EP3693101A4 (fr) * 2017-10-04 2021-03-31 Mitsubishi Materials Corporation Poudre magnétique douce revêtue d'un isolant à base de silice et procédé de production associé

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CN101849268B (zh) 2012-10-10

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