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WO2007052772A1 - POUDRE MAGNETIQUE TENDRE DE TYPE Fe-Si A BASE DE FER ENDUITE D'UN FILM DE DEPOT D'OXYDE ET SON PROCEDE DE PRODUCTION - Google Patents

POUDRE MAGNETIQUE TENDRE DE TYPE Fe-Si A BASE DE FER ENDUITE D'UN FILM DE DEPOT D'OXYDE ET SON PROCEDE DE PRODUCTION Download PDF

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Publication number
WO2007052772A1
WO2007052772A1 PCT/JP2006/322028 JP2006322028W WO2007052772A1 WO 2007052772 A1 WO2007052772 A1 WO 2007052772A1 JP 2006322028 W JP2006322028 W JP 2006322028W WO 2007052772 A1 WO2007052772 A1 WO 2007052772A1
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WIPO (PCT)
Prior art keywords
soft magnetic
iron
powder
magnetic powder
based soft
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Application number
PCT/JP2006/322028
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English (en)
Japanese (ja)
Inventor
Muneaki Watanabe
Ryoji Nakayama
Original Assignee
Mitsubishi Materials Pmg Corporation
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Publication date
Priority claimed from JP2005319247A external-priority patent/JP4883755B2/ja
Application filed by Mitsubishi Materials Pmg Corporation filed Critical Mitsubishi Materials Pmg Corporation
Publication of WO2007052772A1 publication Critical patent/WO2007052772A1/fr

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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
    • 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
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • 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 deposited oxide film coated Fe-Si based iron-based soft film in which a deposited acid film having Mg, Si, Fe and O forces is coated on the surface of a Fe-S iron-based soft magnetic powder.
  • the present invention relates to a magnetic powder and a method for producing the same.
  • the composite soft magnetic material prepared by using this deposited acid-coating-coated Fe-Si-based iron-based soft magnetic powder is a variety of electromagnetic circuit components that require low iron loss. For example, it is used as a material for various electromagnetic parts such as motors, actuators, yokes, cores, and rear tuttles.
  • a raw material powder for producing a soft magnetic material having a high specific resistance Si: containing 0.1 to 10% by mass, the balance being Fe and an Fe-Si-based iron group having inevitable impurity power
  • a soft magnetic powder is known, and a soft magnetic powder in which a high-resistance material is coated on the surface of this Fe—Si-based iron-based soft magnetic powder is also known.
  • the soft magnetic powder having a high resistance material formed on the surface is compression-molded, and the obtained green compact is sintered to have a structure in which the high resistance material is interposed between the soft magnetic particles and to have a high specific resistance.
  • a method for producing a magnetic material is also known (see JP-A-5-258934).
  • an Mg-containing ferrite oxide film can be considered. ⁇ Even if a green compact is produced by press-molding a film-coated Fe-Si-based iron-based soft magnetic powder, and the green compact is subjected to high-temperature strain relief firing, a sufficiently high specific resistance cannot be obtained.
  • Mg-containing ferrite is generally unstable with respect to heat, and when heat is applied, the ferrite structure changes, resulting in a decrease in insulation, and soon the composite soft magnetic material obtained has a decrease in insulation. This is partly due. Furthermore, the conventional Fe-Si-based iron-based soft magnetic powder coated with an Mg-containing ferrite oxide film is coated with an Mg-containing ferrite oxide film by a chemical method.
  • Composite soft magnetic material produced by press-molding and firing Fe-Si-based iron-based soft magnetic powder coated with a conventional Mg-containing ferrite acid film with insufficient adhesion of Mg-containing ferrite acid film to the surface
  • the material had a drawback that the Mg-containing ferrite oxide film was peeled off or torn during press forming, so that a sufficient insulating effect could not be exhibited, and therefore a sufficiently high specific resistance could not be obtained.
  • the present inventors have found that a high-resistance material film is formed on the surface of the Fe-Si-based iron-based soft magnetic powder surface that does not break during press-molding. Oxidation that adheres firmly, further reduces the eddy current loss and lowers the coercive force and lowers the hysteresis loss without lowering the surface insulation even if high temperature strain relief firing is performed after press forming Research was carried out to obtain a film-coated Fe-Si-based iron-based soft magnetic powder.
  • the surface of the Fe-Si-based iron-based soft magnetic powder or Fe powder is A high-concentration Si diffusion layer containing high-concentration Si can also be formed in the SU-containing Fe—Si-based iron-based soft magnetic powder or Fe powder.
  • a surface-oxidation high-concentration Fe-Si system having an oxide layer on the high-concentration Si diffusion layer Iron-based soft magnetic raw material powder can be produced.
  • This mixed powder obtained by adding and mixing Mg powder to this high-oxidized Fe-Si based iron-based soft magnetic raw material powder is mixed with temperature: 150 ⁇ : L 100 ° C, pressure: 1 X 10 _12 ⁇ 1 X
  • a deposited oxide film with Mg, Si, Fe and O forces is formed on the surface of the Fe-Si-based iron-based soft magnetic powder.
  • the Mg contained in the deposited oxide film that also has Mg, Si, Fe, and O forces has a Mg concentration gradient that increases with increasing Mg content closer to the outermost surface, and O is closer to the outermost surface.
  • the O concentration increases as the O content increases, while Fe has a concentration gradient where the Fe content decreases as it is closer to the outermost surface, and Si is closer to the outermost surface of the deposited oxide film. It has a Si concentration gradient in which the Si content increases closer to the outermost surface.
  • the Mg, Si, Fe, and O-force deposited acid film contains MgO solid crystalline wustite (MgO dissolved in wustite (FeO) in the substrate.
  • MgO solid crystalline wustite
  • FeO wustite
  • part of Fe and Si is contained as metal Fe or Fe-Si alloy.
  • the deposited oxide film having Mg, Si, Fe, and O force has toughness because it contains metallic Fe, and easily follows the deformation of the powder during compacting.
  • the deposited oxide film with Mg, Si, Fe and O forces has toughness because it has a fine crystal structure with a crystal grain size of 200 nm or less, and follows the deformation of the powder during compacting. Easy
  • the deposited acid film covering Fe-Si based iron-based soft magnetic powder in which the deposited acid film including Mg, Si, Fe and O force is formed on this surface is a conventional Fe-Si based iron base.
  • Mg-containing ferrite oxide film coating with Mg-containing ferrite-acid film on the surface of soft magnetic powder Compared with Fe-Si-based iron-based soft magnetic powder, the oxide film for Fe-Si-based iron-based soft magnetic powder Since the adhesion is remarkably excellent, the oxide film, which is an insulating film, is broken during press molding, and Fe—S related iron-based soft magnetic powder is less likely to come into contact with each other.
  • the Mg, Si, Fe and The deposited oxide film made of O is chemically more stable than Mg-containing fried acid film, so that the insulation property of the oxide film is reduced even if high temperature strain relief firing is performed after press molding. High resistance can be maintained without reducing the eddy current loss. Force can be kept low hysteresis losses can be reduced, thus, the composite soft magnetic material to have a low iron loss can be obtained.
  • the present invention has been made based on the above research results, and has the following aspects.
  • a first aspect of the present invention is a deposited acid-coating-coated Fe—S-related iron-based soft magnetic powder, wherein the deposited acid also has Mg, Si, Fe, and O forces on the surface of the Fe—S-related iron-based soft magnetic powder.
  • the film is formed This is a deposited oxide film-coated Fe—Si-based iron-based soft magnetic powder.
  • a second aspect of the present invention is the deposited oxide film-coated Fe Si-based iron-based soft magnetic powder according to the first aspect, wherein the Fe Si-based iron-based soft magnetic powder is Si: 0.1 to 10% by mass.
  • the deposited acid film-coated Fe—Si based iron-based soft magnetic powder according to the first or second aspect, wherein the deposited acid solution also has the Mg, Si, Fe and O forces.
  • the Mg and O contents increase toward the surface, the Fe content decreases toward the surface, and Si is near the outermost surface of the deposited oxide film!
  • a fourth aspect of the present invention is the deposited acid-coating-coated Fe—Si-based iron-based soft magnetic powder according to any one of the first aspect, the second aspect, or the third aspect, wherein the Mg, Si,
  • the deposited oxide film that also has Fe and O forces contains a crystalline MgO solid solution wustite-type phase, which contains metal Fe or Fe-Si alloy, and is deposited oxide film Fe-Si This is an iron-based soft magnetic powder.
  • the deposited acid film-coated Fe S-coated iron-based soft magnetic powder according to any one of the first aspect, the second aspect, the third aspect, or the fourth aspect,
  • the deposited oxide film with Mg, Si, Fe and O forces is a deposited Si oxide-based Fe-based soft magnetic powder with a fine crystal structure with an average crystal grain size of 200 nm or less.
  • a deposited oxide film-coated Fe Si-based iron-based soft magnetic powder in which a deposited oxide film having Mg, Si, Fe and O forces is formed on the surface of the Fe-Si-based iron-based soft magnetic powder of the present invention.
  • Si powder is added to Fe Si-based iron-based soft magnetic powder, mixed, and then heated in a non-oxidizing atmosphere, whereby the Fe Si-based iron-based soft magnetic powder is coated on the surface of the Fe Si-based iron-based soft magnetic powder.
  • An Fe Si-based iron-based soft magnetic powder having a high-concentration Si diffusion layer that also contains high-concentration Si in the soft magnetic powder is prepared.
  • the surface-oxidized Fe Si-based iron-based soft powder having an oxide layer on the high-concentration Si diffusion layer is obtained.
  • Magnetic raw material powder is prepared.
  • This surface-oxidized Fe Si-based iron-based soft magnetic raw material powder is mixed with Mg powder to produce a mixed powder.
  • the resulting mixed powder is heated in an inert gas atmosphere or vacuum atmosphere of temperature: 150 ⁇ : LI 00 ° C, pressure: 1 x 10 1 12 ⁇ 1 x 10_1 MPa Fe-Si
  • An iron-based soft magnetic powder can be obtained.
  • the Fe—Si-based iron-based soft magnetic powder has a high-concentration Si diffusion layer on the surface of the Fe-Si-based iron-based soft magnetic powder, and the SU-containing Fe-Si-based soft magnetic powder also includes a high concentration Si.
  • An iron-based soft magnetic powder can be obtained by adding Si powder to Fe powder, mixing, heating in a non-oxidizing atmosphere, and diffusing and infiltrating Si into the Fe powder.
  • the present invention further has the following aspects.
  • the sixth aspect of the present invention is a method for producing a deposited oxide film-coated Fe—Si-based iron-based soft magnetic powder, and after adding and mixing Si powder into an Fe—Si-based iron-based soft magnetic powder or Fe powder, By heating in a non-oxidizing atmosphere, the Fe-Si-based iron-based soft magnetic powder or Fe powder has a high concentration of Si on the surface of the Fe-Si-based iron-based soft magnetic powder or Fe powder.
  • the Fe-Si-based iron-based soft magnetic powder having a high-concentration Si diffusion layer containing high-concentration Si was prepared, and the obtained Fe-Si-based iron-based soft magnetic powder having a high-concentration Si diffusion layer was oxidized to obtain a high concentration.
  • a surface oxidized Fe-Si-based iron-based soft magnetic raw material powder having an oxide layer on the Si diffusion layer was prepared, and a surface acid Fe-Si system having an acid layer on the high-concentration Si diffusion layer.
  • the deposited oxide film-coated Fe—Si-based iron-based soft magnetic powder according to any one of the first aspect, the second aspect, the third aspect, the fourth aspect, or the fifth aspect.
  • a surface-oxidized Fe-Si-based iron-based soft magnetic raw material powder for manufacturing wherein the composition of Si contained in the entire Fe-Si-based iron-based soft magnetic powder on the surface of the Fe-Si-based iron-based soft magnetic powder
  • the term "deposited oxide film" t ⁇ ⁇ refers to an oxide film in which atoms constituting the film, which are normally sputtered by vacuum evaporation, are deposited on a substrate, for example.
  • the deposited oxide film with Mg, Si, Fe and O force formed on the surface of the Fe-Si based iron-based soft magnetic powder of the present invention is F The film formed on the surface of the Fe-Si iron-based soft magnetic powder with the reaction of Si and Mg on the surface of the e-Si-based iron-based soft magnetic powder.
  • the film thickness of the deposited oxide film with Mg, Si, Fe, and O force formed on the surface of this Fe-Si-based iron-based soft magnetic powder is a composite obtained by compacting and firing.
  • it is preferably in the range of 5 nm to 500 nm. If the film thickness is less than 5 nm, the specific resistance of the powdered composite soft magnetic material is insufficient and the eddy current loss increases. The magnetic flux density is decreased, which is preferable!
  • a more preferable film thickness is 5 ⁇ ! Within the range of ⁇ 200nm.
  • the deposited oxide film coated with the deposited acid film coating Fe-S related iron-based soft magnetic powder according to any one of the first to fifth aspects is formed with Mg, Si, Fe and O force.
  • the finer the crystal grains, the more preferable the crystal grain size is preferably a fine crystal structure of 200 nm or less. By having such a fine crystal structure, it is possible for the microcrystalline deposited oxide film to follow the deformation of the powder during compacting and prevent the coating from being broken. Contact bonding between soft magnetic powders can be prevented, and even if high temperature strain relief firing is performed, the oxide is stable and insulation deterioration can be prevented, resulting in high resistance and low eddy current loss. It is not preferable because the magnetic flux density of the composite soft magnetic material formed by compacting with a crystal grain size larger than 200 ⁇ m is lowered.
  • the Fe-Si-based iron-based soft magnetic powder used for producing the deposited oxide film-coated Fe-Si-based iron-based soft magnetic powder according to any one of the first to fifth embodiments has an average particle size of 5 to Preference is given to using powders in the range of 500 m. The reason is that if the average particle size is less than 5 m, the compressibility of the powder is lowered, and the volume ratio of the powder is lowered, so the value of the magnetic flux density is lowered. If it is too large, the eddy current inside the powder increases and the permeability at high frequencies decreases.
  • the resistivity and strength of the deposited oxide film-coated Fe-Si based iron-based soft magnetic powder of the present invention described above are mixed with an organic insulating material, an inorganic insulating material, or a mixed material of an organic insulating material and an inorganic insulating material. Further improved composite soft magnetic materials can be produced.
  • organic insulating materials epoxy resin, fluorine resin, phenol resin, urethane resin, silicone resin, polyester resin, phenoxy resin, urea resin, isocyanate resin, Krill resin, polyimide resin, PPS resin, etc. can be used.
  • phosphates such as iron phosphate, various glassy insulators, water glass mainly composed of sodium silicate, insulating oxides, and the like can be used.
  • the deposited oxide film-coated Fe—Si-based iron-based soft magnetic powder of the present invention is compacted, and the resulting compacted compact is sintered at a temperature of 500 to 1000 ° C. to obtain a composite soft magnetic material. Can be produced.
  • the composite soft magnetic material produced using the deposited acid-coating-coated Fe—Si-based iron-based soft magnetic powder of the present invention has high density, high strength, high specific resistance and high magnetic flux density.
  • the electromagnetic circuit component include a magnetic core, an electric motor core, a generator core, a solenoid core, an idling core, a rear tuttle, a transformer, a choke coil core, and a magnetic sensor core.
  • an electric device incorporating an electromagnetic circuit component made of a composite soft magnetic material having high resistance using the oxide film-coated Fe—Si-based iron-based soft magnetic powder of the present invention includes an electric motor, a generator, a solenoid, There are injectors, electromagnetically driven valves, inverters, converters, transformers, relays, magnetic sensor systems, etc., which can improve the efficiency and performance of electric equipment and make it compact and lightweight.
  • a composite soft magnetic material When a composite soft magnetic material is produced using the deposited oxide film-coated Fe-Si-based iron-based soft magnetic powder of the present invention, it has a high specific resistance, so it has a low eddy current loss and further has a coercive force. Since it is low, a composite soft magnetic material having a low hysteresis loss can be stably produced at low cost, and it has excellent effects in the electrical and electronic industries.
  • FIG. 1 is a graph showing the results of measuring the concentration distribution of Mg, 0, Si and Fe in the depth direction of a deposited oxide film using an Auger electron spectrometer.
  • Fe-Si based iron-based soft magnetic powder consisting of raw material powder with average particle size: 75 ⁇ m, Si: 1% by mass, remaining Fe and inevitable impurities, and average particle size: 1 ⁇ m or less Pure Si Powder was prepared. Furthermore, Mg powder having an average particle diameter of 50 ⁇ m was prepared.
  • the mixed powder is mixed to produce high-concentration Si on the surface of the Fe Si-based iron-based soft magnetic powder by heat-treating it in a hydrogen atmosphere at a temperature of 950 ° C for 1 hour.
  • Mg powder 99.8 mass%: 0.2 mass. % Mixed to make a mixed powder, and the resulting mixed powder is held for 1 hour while rolling under conditions of temperature: 650 ° C and pressure: 2.7 X 10 _4 MPa
  • a deposited oxide film with Mg, Si, Fe and O forces is formed on the surface of the Fe Si-based iron-based soft magnetic powder.
  • Invented oxide film coating powder) 1) was prepared.
  • the deposited oxide film formed on the deposited oxide film-coated powder 1 of the present invention is a deposited oxide film composed of Mg, Si, Fe and O, and the deposited oxide film is submerged in the substrate. It was confirmed by analyzing with X-ray photoelectron spectrometer that the metal Fe and Fe Si alloy were contained, and analyzing the binding energy. Furthermore, the structure of the deposited oxide film in the deposited oxide film coating powder 1 of the present invention was observed with an electron microscope, the thickness of the deposited oxide film and the maximum crystal grain size were measured, and the results are shown in Table 1. . Further, it was confirmed by electron diffraction pattern that Mg and O contained in the deposited oxide film having Mg, Si, Fe and O forces were contained as crystalline MgO solid solution wustite type phase.
  • the concentration distribution of Mg, 0, Si, and Fe in the depth direction of the deposited oxide film consisting of Mg, Si, Fe, and O force was measured using an Auger electron spectrometer, and the results are shown in Table 1.
  • the concentration distribution of Mg, 0, Si and Fe in the depth direction of the deposited oxide film consisting of Mg, Si, Fe and O of the deposited oxide film coated powder 1 of the present invention was measured using an Auger electron spectrometer.
  • Figure 1 shows the measurement diagram at the time. In FIG. 1, the horizontal axis of Etching Time 0 is the outermost surface. Therefore, in FIG.
  • the thus obtained deposited oxide film-coated powder 1 of the present invention was put into a mold and press-molded to obtain a plate-shaped green compact having dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness, and the outside.
  • a ring-shaped green compact with a diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm, and firing the resulting green compact in a nitrogen atmosphere at a temperature of 500 ° C for 30 minutes
  • the composite soft magnetic material having a plate-like and ring-like fired body strength was prepared, the specific resistance of the composite soft magnetic material made of this plate-like fired body was measured, and the results are shown in Table 1.
  • the composite soft magnetic material consisting of plate-like and ring-like sintered bodies was prepared, the specific resistance of the composite soft magnetic material also having the plate-like sintered body force was measured, and the results are shown in Table 1. It was shown to.
  • a composite soft magnetic material having a ring-like sintered body strength is subjected to a winding, and the magnetic flux density, the coercive force, and the magnetic flux density 1.5 T, the iron loss and magnetic flux density 1.0 T at a frequency of 50 Hz, the frequency Magnetic properties such as iron loss at 400 Hz were measured, and the results are shown in Table 1.
  • the deposited oxide film-coated powder 1 of the present invention produced in Example 1 uses the Mg-containing ferrite oxide-coated Fe—Si-based iron-based soft magnetic powder produced in Conventional Example 1. Compared to the prepared composite soft magnetic material, the density is not much different, but the composite soft magnetic material prepared using the deposited oxide film coated powder 1 of the present invention prepared in Example 1 was prepared in Conventional Example 1.
  • Conventionally deposited oxide coating powder Mg-containing ferrite oxide coating Fe-Si-based iron base Compared to composite soft magnetic materials made using soft magnetic powder, the magnetic flux density is high, the coercive force is small, and the specific resistance is remarkably high. It has a characteristic that it has characteristics such as a small loss.
  • an Fe—Si-based iron-based soft magnetic powder having a particle size shown in Table 2 and containing Si: 1% by mass and composed of the remaining Fe and inevitable impurities was prepared. Furthermore, pure Si powder having an average particle size of 1 ⁇ m or less and Mg powder having an average particle size of 50 ⁇ m were prepared.
  • a high-concentration Si diffusion layer is formed on the surface of the Fe--S soft iron-based soft magnetic powder by heat-treating the resulting mixed powder in a hydrogen atmosphere at a temperature of 950 ° C for 1 hour.
  • a surface oxidized Fe—Si-based iron-based soft magnetic raw material powder having an oxide layer on a high-concentration Si diffusion layer was prepared by maintaining the temperature at 220 ° C. in the atmosphere. .
  • the prepared mixed powder is treated for 1 hour while rolling under the conditions of temperature: 650 ° C and pressure: 2.7 X 10 _4 MPa, hereinafter referred to as “Mg coating treatment”)
  • the Fe-Si-based iron-based soft magnetic powder is formed by depositing a deposited acid-containing film made of Mg, Si, Fe and O on the surface of the Fe-Si-based iron-based soft magnetic powder
  • the deposited oxide film formed on the deposited oxide film-coated Fe-Si-based iron-based soft magnetic powder obtained by the present invention method 1-3 is a deposited oxide film having Mg, Si, Fe and O forces. It was confirmed by analyzing with X-ray photoelectron spectrometer and binding energy that this deposited oxide film contains metal Fe and Fe-Si alloy in the substrate. . Furthermore, the structure of the deposited acid film in the acid film-coated Fe-S iron-based soft magnetic powder was examined with an electron microscope. It is observed from the electron diffraction pattern that Mg and O contained in the deposited acid film containing Mg, Si, Fe and O force are included as crystalline MgO solid solution wustite phase. confirmed.
  • Mg, 0, Si and Fe in the depth direction of the deposited oxide film with Mg, Si, Fe and O force was measured using an Auger electron spectrometer, it was found to be included in the deposited oxide film.
  • Mg and O content increases and Mg and O content increases on the surface, Fe decreases on the surface and Si content is closer to the outermost surface of the deposited oxide film. It has become a component that it has a Si concentration gradient with increasing amounts.
  • the deposited acid film coating Fe-Si based iron-based soft magnetic powder obtained by the method of the present invention 1 to 3 was added to and mixed with a silicone resin at a mixing ratio of 2% by mass.
  • a resin-coated composite powder in which the surface of a Si-based iron-based soft magnetic powder is coated with a silicone resin, and this resin-coated composite powder is placed in a mold heated to 120 ° C and press-molded to create a vertical Obtained by molding a plate-shaped green compact with dimensions of 55 mm, width: 1 Omm, thickness: 5 mm and ring-shaped green compact with dimensions of outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm
  • the green compact is fired in a vacuum at a temperature of 700 ° C for 30 minutes to produce a composite soft magnetic material consisting of a plate-like and ring-like fired body.
  • the specific resistance of the magnetic material was measured, and the results are shown in Table 2. Further, the composite soft magnetic material having a ring-like fired body strength was subjected to a winding line to obtain a magnetic flux density. , Coercive force, and magnetic flux density 0. 1T, the iron loss at a frequency 20kHz were measured. The results are shown in Table 2.
  • an Fe-Si-based iron-based soft magnetic powder having a particle size shown in Table 2 and containing Si: 1% by mass and comprising the remaining Fe and inevitable impurities is prepared.
  • Si-based iron-based soft magnetic powder is coated with silicone resin at a mixing ratio of 2% by mass without Mg coating, and mixed to coat the surface of Fe-Si-based iron-based soft magnetic powder with silicone resin.
  • a coated composite powder was prepared. This resin-coated composite powder is placed in a mold heated to 120 ° C and pressed to form a plate-shaped green compact with dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness and an outer diameter of 35 mm.
  • a ring-shaped green compact with an inner diameter of 25 mm and a height of 5 mm was molded, and the resulting green compact was fired in vacuum at a temperature of 700 ° C for 30 minutes.
  • a composite soft magnetic material made of a ring-like fired body was produced, and a composite soft magnetic material made of this plate-like fired body was produced.
  • the specific resistance of the magnetic material was measured, and the results are shown in Table 2.
  • the composite soft magnetic material having a ring-shaped sintered body strength was subjected to a line, and the magnetic flux density, coercive force, magnetic flux density 0.1 T, frequency The iron loss at 20 kHz was measured and the results are shown in Table 2.
  • the composite soft magnetic material produced by the present invention methods 1 to 3 is different from the composite soft magnetic material produced by the conventional method 1.
  • the magnetic flux density is high, the coercive force is small, and the specific resistance is remarkably high. Therefore, the iron loss is remarkably small.
  • an Fe—Si-based iron-based soft magnetic powder having a particle size shown in Table 3 and containing Si: 3% by mass, and composed of the remaining Fe and inevitable impurities was prepared. Furthermore, pure Si powder having an average particle size of 1 m or less and Mg powder having an average particle size of 50 ⁇ m were prepared.
  • a mixed powder is then prepared, and the resulting mixed powder is heat-treated in a hydrogen atmosphere at a temperature of 950 ° C for 1 hour to maintain a high-concentration Si diffusion layer on the surface of the Fe-Si-based iron-based soft magnetic powder.
  • the surface oxidized Fe—Si-based iron-based soft magnetic raw material powder having an oxide layer on the high-concentration Si diffusion layer was produced by maintaining the temperature in the atmosphere at a temperature of 220 ° C.
  • the deposited oxide film formed on the Fe-Si based iron-based soft magnetic powder obtained by the method 4-6 of the present invention is a deposited oxide film with Mg, Si, Fe and O forces. It was confirmed by analyzing with X-ray photoelectron spectrometer that the metal oxide and Fe-Si alloy were contained in the substrate and analyzing the binding energy. Furthermore, the structure of the deposited acid film in the Fe-S coated iron-based soft magnetic powder is observed with an electron microscope, and the Mg, Si, Fe and O forces are also included in the deposited acid film. It was confirmed by electron diffraction pattern that Mg and O were included as crystalline MgO solid solution wustite phase.
  • Mg, 0, Si and Fe in the depth direction of the deposited oxide film with Mg, Si, Fe and O force was measured using an Auger electron spectrometer, it was found to be included in the deposited oxide film.
  • Mg and O content increases with increasing force of Mg and O
  • Fe decreases with force toward the surface
  • Si is closer to the outermost surface near the outermost surface of the deposited oxide film. It has been found that it has a Si concentration gradient with increasing Si content.
  • Deposited oxide film coated Fe-Si based iron-based soft magnetic powder obtained by the method 4 to 6 of the present invention was added to and mixed with a silicone resin at a mixing ratio of 2% by mass.
  • a resin-coated composite powder in which the surface of an Fe—Si-based iron-based soft magnetic powder was coated with a silicone resin was prepared. This resin-coated composite powder is placed in a mold heated to 120 ° C and pressed to form a plate compact having dimensions of 55mm in length, 10mm in width, 5mm in thickness, and outer diameter: 35mm, inner diameter.
  • a ring-shaped green compact with dimensions of 25 mm and height: 5 mm is molded, and the resulting green compact is fired in vacuum at a temperature of 700 ° C for 30 minutes.
  • a composite soft magnetic material made of a green fired body was prepared, the specific resistance of the composite soft magnetic material made of this plate fired body strength was measured, and the results are shown in Table 3.
  • the wire was lined, and the magnetic flux density, coercive force, and iron loss at a magnetic flux density of 0.1 T and a frequency of 20 kHz were measured. The results are shown in Table 3.
  • an Fe-Si-based iron-based soft magnetic powder having the particle size shown in Table 3 and containing Si: 1% by mass and comprising the remaining Fe and inevitable impurities is prepared.
  • Si-based iron-based soft magnetic powder is coated with silicone resin at a mixing ratio of 2% by mass without Mg coating, and mixed to coat the surface of Fe-Si-based iron-based soft magnetic powder with silicone resin.
  • a coated composite powder was prepared. This resin-coated composite powder is placed in a mold heated to 120 ° C and pressed to form a plate-shaped green compact with dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness and an outer diameter of 35 mm.
  • a ring-shaped green compact with an inner diameter of 25 mm and a height of 5 mm was molded, and the resulting green compact was fired in vacuum at a temperature of 700 ° C for 30 minutes.
  • a composite soft magnetic material made of a ring-like fired body was prepared, and the specific resistance of this composite soft magnetic material made of a plate-like fired body was measured. The results are shown in Table 2.
  • a composite soft magnetic material made of a ring-shaped fired body was wire-lined, and the magnetic flux density, coercive force, and iron loss at a magnetic flux density of 0.1 T and a frequency of 20 kHz were measured. The results are shown in Table 3. It was.
  • the composite soft magnetic material produced by the present invention methods 4 to 6 has a lower magnetic flux density, a smaller coercive force, and a significantly higher specific resistance. Therefore, it can be seen that the iron loss is remarkably small, and that the iron loss decreases as the frequency increases.
  • Example 4 Fe powder having the particle size shown in Table 4 was prepared as a raw material powder. Further, pure Si powder having an average particle size of 1 ⁇ m or less and Mg powder having an average particle size of 50 ⁇ m were prepared.
  • the deposited oxide film formed on the Fe-Si based iron-based soft magnetic powder obtained by the method of the present invention 7-9 is a deposited oxide film with Mg, Si, Fe and O forces. It was confirmed by analyzing with X-ray photoelectron spectrometer that the metal oxide and Fe-Si alloy were contained in the substrate and analyzing the binding energy. Furthermore, the structure of the deposited acid film in the Fe-S coated iron-based soft magnetic powder is observed with an electron microscope, and the Mg, Si, Fe and O forces are also included in the deposited acid film. It was confirmed by electron diffraction pattern that Mg and O were included as crystalline MgO solid solution wustite phase.
  • Mg, 0, Si and Fe in the depth direction of the deposited oxide film with Mg, Si, Fe and O force was measured using an Auger electron spectrometer, it was found to be included in the deposited oxide film.
  • Mg and O content increases and Mg and O content increases on the surface, Fe decreases on the surface and Si content is closer to the outermost surface of the deposited oxide film. It has become a component that it has a Si concentration gradient with increasing amounts.
  • Deposited oxide film coating Fe-Si based iron-based soft magnetic powders obtained by the present invention methods 7 to 9 were added to and mixed with a silicone resin at a blending ratio of 2% by mass.
  • a resin-coated composite powder in which the surface of an Fe—Si-based iron-based soft magnetic powder was coated with a silicone resin was prepared.
  • This resin-coated composite powder is placed in a mold heated to 120 ° C, press-molded, and length: 55mm, width: Plate-shaped green compact with dimensions of 10 mm, thickness: 5 mm, outer diameter: 35 mm, inner diameter: 25 mm, height: molded into a ring-shaped green compact with dimensions of 5 mm, and the resulting green compact is vacuumed Medium, temperature: 700 ° C, baked for 30 minutes to produce a composite soft magnetic material consisting of plate-like and ring-like fired bodies, and the specific resistance of the composite soft magnetic material due to the strength of this plate-like fired body The results are shown in Table 4.
  • the composite soft magnetic material which has a small-diameter ring-shaped fired body strength, is further lined, and the magnetic flux density, coercive force, magnetic flux density is 0.1 T, and the frequency is 20 kHz.
  • the loss was measured and the results are shown in Table 4.
  • the composite soft magnetic material produced by the inventive methods 7 to 9 has a smaller coercive force with a higher magnetic flux density and a much higher specific resistance. For this reason, the iron loss is remarkably small, and it has a characteristic that it has special characteristics (such as the iron loss decreases as the frequency increases).
  • Example 5 Ring-shaped compact having outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm and outer diameter: 50 mm, inner diameter: using the deposited oxide film coating powder 1 of the present invention prepared in Example 1
  • This small-diameter ring is formed by molding a ring-shaped green compact with dimensions of 25 mm and height: 25 mm, and firing the resulting green compact under vacuum at a temperature of 700 ° C for 30 minutes. A green compact and a large outer diameter ring-shaped green compact were produced.
  • the ring-shaped green compact with a height of 25 mm is molded, and the resulting green compact is fired under vacuum at a temperature of 700 ° C for 30 minutes.
  • a powder fired body and a large outer diameter ring-shaped powder fired body were produced.
  • the deposited oxide film-coated powder 1 of the present invention has superior characteristics as a raw material powder for producing reattoria compared to the conventional deposited oxide film-coated powder 1.
  • a composite soft magnetic material is formed.
  • a composite soft magnetic material having low eddy current loss due to its high specific resistance and low hysteresis loss due to its low coercive force can be produced stably at low cost. It has excellent effects on the electronics industry.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne une poudre magnétique tendre de type Fe-Si, à base de fer, enduite d’un film de dépôt d'oxyde qui comprend des particules magnétiques tendres de type Fe-Si, à base de fer et, formé à la surface de chaque particule, un film de dépôt d'oxyde comprenant Mg, Si, Fe et O. Dans le film de dépôt d'oxyde comprenant Mg, Si, Fe et O les teneurs en magnésium et en oxygène augmentent en se rapprochant de la surface et la teneur en fer diminue en se rapprochant de la surface. Le film de dépôt d'oxyde présente un gradient de concentration en silicium, la teneur en silicium d’une couche autour de la surface extérieure augmentant en se rapprochant de la surface extérieure. La poudre magnétique enduite contient du fer métallique dans la base et présente une structure cristalline fine ayant un diamètre moyen de grain cristallin de 200 nm ou inférieur.
PCT/JP2006/322028 2005-11-02 2006-11-02 POUDRE MAGNETIQUE TENDRE DE TYPE Fe-Si A BASE DE FER ENDUITE D'UN FILM DE DEPOT D'OXYDE ET SON PROCEDE DE PRODUCTION WO2007052772A1 (fr)

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JP2005319247A JP4883755B2 (ja) 2005-05-31 2005-11-02 酸化膜被覆Ｆｅ−Ｓｉ系鉄基軟磁性粉末、その製造方法、複合軟磁性材、リアクトル用コア、リアクトル、電磁気回路部品および電気機器
JP2005-319247 2005-11-02

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009060895A1 (fr) * 2007-11-07 2009-05-14 Mitsubishi Materials Pmg Corporation Matériau composite magnétique doux à haute résistance obtenu par compaction/combustion et son procédé de fabrication
JP2012129217A (ja) * 2010-11-24 2012-07-05 Daido Steel Co Ltd 圧粉磁心のための加圧成形用粉体及び圧粉磁心の製造方法
US20200143967A1 (en) * 2018-11-01 2020-05-07 Panasonic Corporation Dust core and method of manufacturing the same

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09143692A (ja) * 1995-11-29 1997-06-03 Ishikawajima Harima Heavy Ind Co Ltd 高蒸気圧金属の気相メッキ装置及び方法
JPH1187123A (ja) * 1997-09-08 1999-03-30 Mitsubishi Materials Corp 高周波用軟磁性粉末
JP2003306704A (ja) * 2002-04-17 2003-10-31 Mitsubishi Materials Corp 高密度および高透磁性を有するＦｅ−Ｓｉ系複合軟磁性焼結合金およびその製造方法
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
JP2005146315A (ja) * 2003-11-12 2005-06-09 Toyota Central Res & Dev Lab Inc 磁心用粉末、圧粉磁心およびそれらの製造方法
WO2006028100A1 (fr) * 2004-09-06 2006-03-16 Mitsubishi Materials Pmg Corporation PROCÉDÉ DE FABRICATION DE POUDRE DE MÉTAL MAGNÉTIQUE SOUPLE REVÊTUE D’UN FILM OXYDÉ CONTENANT DU Mg ET PROCEDE DE FABRICATION DE MATÉRIAU MAGNETIQUE SOUPLE COMPOSITE UTILISANT LADITE POUDRE

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09143692A (ja) * 1995-11-29 1997-06-03 Ishikawajima Harima Heavy Ind Co Ltd 高蒸気圧金属の気相メッキ装置及び方法
JPH1187123A (ja) * 1997-09-08 1999-03-30 Mitsubishi Materials Corp 高周波用軟磁性粉末
JP2003306704A (ja) * 2002-04-17 2003-10-31 Mitsubishi Materials Corp 高密度および高透磁性を有するＦｅ−Ｓｉ系複合軟磁性焼結合金およびその製造方法
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
JP2005146315A (ja) * 2003-11-12 2005-06-09 Toyota Central Res & Dev Lab Inc 磁心用粉末、圧粉磁心およびそれらの製造方法
WO2006028100A1 (fr) * 2004-09-06 2006-03-16 Mitsubishi Materials Pmg Corporation PROCÉDÉ DE FABRICATION DE POUDRE DE MÉTAL MAGNÉTIQUE SOUPLE REVÊTUE D’UN FILM OXYDÉ CONTENANT DU Mg ET PROCEDE DE FABRICATION DE MATÉRIAU MAGNETIQUE SOUPLE COMPOSITE UTILISANT LADITE POUDRE

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009060895A1 (fr) * 2007-11-07 2009-05-14 Mitsubishi Materials Pmg Corporation Matériau composite magnétique doux à haute résistance obtenu par compaction/combustion et son procédé de fabrication
JP2009117651A (ja) * 2007-11-07 2009-05-28 Mitsubishi Materials Pmg Corp 高強度軟磁性複合圧密焼成材およびその製造方法
JP2012129217A (ja) * 2010-11-24 2012-07-05 Daido Steel Co Ltd 圧粉磁心のための加圧成形用粉体及び圧粉磁心の製造方法
US20200143967A1 (en) * 2018-11-01 2020-05-07 Panasonic Corporation Dust core and method of manufacturing the same

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