WO2010061525A1 - 軟磁性材料の製造方法、および圧粉磁心の製造方法 - Google Patents

軟磁性材料の製造方法、および圧粉磁心の製造方法 Download PDF

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WO2010061525A1
WO2010061525A1 PCT/JP2009/005635 JP2009005635W WO2010061525A1 WO 2010061525 A1 WO2010061525 A1 WO 2010061525A1 JP 2009005635 W JP2009005635 W JP 2009005635W WO 2010061525 A1 WO2010061525 A1 WO 2010061525A1
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Prior art keywords
soft magnetic
producing
metal particles
magnetic material
silicone
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PCT/JP2009/005635
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English (en)
French (fr)
Japanese (ja)
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草別和嗣
前田徹
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住友電気工業株式会社
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Priority claimed from JP2008301637A external-priority patent/JP4513131B2/ja
Application filed by 住友電気工業株式会社 filed Critical 住友電気工業株式会社
Priority to US12/994,672 priority Critical patent/US8568644B2/en
Priority to EP09828775.8A priority patent/EP2359963B1/en
Priority to CN2009801191376A priority patent/CN102046310B/zh
Publication of WO2010061525A1 publication Critical patent/WO2010061525A1/ja

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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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/108—Mixtures obtained by warm mixing
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic

Definitions

  • the present invention relates to a method for producing a soft magnetic material which is a material for a dust core, and a method for producing a dust core using the soft magnetic material.
  • Hybrid vehicles and the like have a booster circuit in the power supply system to the motor.
  • a reactor is used as one component of this booster circuit.
  • the reactor has a configuration in which a coil is wound around a core.
  • an energy loss called iron loss occurs in the core.
  • the iron loss is generally represented by the sum of hysteresis loss and eddy current loss, and is particularly noticeable when used at high frequencies.
  • a dust core may be used as the core of the reactor.
  • the dust core is formed by pressing a soft magnetic material composed of composite magnetic particles having an insulating coating formed on the surface of the soft magnetic metal particles, and the metal particles are insulated from each other by the insulating coating. The effect of reducing is high.
  • the powder magnetic core is manufactured through pressure molding, there is a possibility that the insulating coating of the composite magnetic particles may be damaged by the pressure during the pressure molding. As a result, the soft magnetic metal particles in the dust core come into contact with each other to increase the eddy current loss, and the high frequency characteristics of the dust core may be deteriorated.
  • Patent Document 1 is formed by forming a multi-layered insulating layer comprising an insulating coating, a heat-resistant protective coating, and a flexible protective coating on the surface of the soft magnetic metal particles. It solves the problems caused by heat treatment.
  • a phosphorus compound, a silicon compound or the like can be used as an insulating coating
  • an organic silicon compound or the like can be used as a heat-resistant protective coating
  • a silicone or the like can be used as a flexible protective coating.
  • a wet coating method is cited as a method for forming an insulating layer.
  • the wet coating method is a method of forming an insulating coating on the surface of a coating target by immersing the coating target in an organic solvent in which an insulating material is dissolved, stirring the mixture, evaporating the organic solvent, and then curing. That is, the formation of the insulating coating requires three steps of stirring, evaporation, and curing, so that the productivity of the soft magnetic material is not good.
  • a silicone film is selected as the insulating layer to be formed on the coating target
  • the condensation polymerization of the silicone is promoted in a heated atmosphere, and the silicone coating is applied to the surface of the coating target.
  • one of the objects of the present invention is to efficiently produce a soft magnetic material having a plurality of insulating layers on the surface of soft magnetic metal particles in order to suppress a decrease in magnetic properties due to pressure molding and heat treatment.
  • the object is to provide a method for producing a soft magnetic material.
  • Another object of the present invention is to provide a method for manufacturing a dust core for manufacturing a dust core having excellent high frequency characteristics.
  • the present inventors paid attention to two insulating layers adjacent to each other in the thickness direction on the surface of the soft magnetic metal particles, and found that the above object can be achieved by limiting the configuration of the two insulating layers. Based on this finding, the present invention is defined below.
  • the method for producing a soft magnetic material of the present invention is a method for producing a soft magnetic material used for producing a dust core, and includes the following steps.
  • a step of preparing a material powder made of composite magnetic particles in which an insulating coating having hydration water is formed on the surface of soft magnetic metal particles (hereinafter referred to as step A).
  • a step of preparing a resin material containing silicone that cures by hydrolysis / condensation reaction (hereinafter referred to as step B).
  • a step of mixing the material powder and the resin material in a heating atmosphere of 80 to 150 ° C. to form a silicone coating on the surface of the insulating coating hereinafter referred to as step C).
  • a soft magnetic material composed of composite magnetic particles in which a surface of a soft magnetic metal particle is covered with a plurality of insulating layers of an insulating coating and a silicone coating can be manufactured efficiently and in a short time. Can do. This is because the hydration water contained in the insulating coating promotes the formation of the silicone coating. The detailed mechanism will be described in detail later.
  • step D A step of press-molding the soft magnetic material produced by the above-described method for producing a soft magnetic material.
  • step E A heat treatment step for removing strain introduced into the soft magnetic metal particles during pressure molding.
  • a dust core of the present invention since the soft magnetic material of the present invention is pressed and molded and then subjected to high-temperature heat treatment, strain and transition introduced into the metal particles of the soft magnetic material during pressurization Can be sufficiently removed.
  • the reason why the heat treatment temperature after pressurization of the soft magnetic material can be increased is because the soft magnetic material made of composite magnetic particles in which the surface of the soft magnetic metal particles is covered with a plurality of insulating layers is used.
  • a dust core from which distortion and the like have been sufficiently removed is excellent in energy efficiency because iron loss is reduced.
  • the powder magnetic core thus obtained can be suitably used as, for example, a reactor core.
  • the material powder to be prepared is a collection of composite magnetic particles having an insulating coating having hydrated water on the surface of soft magnetic metal particles.
  • the soft magnetic metal particles those containing 50% by mass or more of iron are preferable, and examples thereof include pure iron (Fe).
  • iron alloys such as Fe-Si alloys, Fe-Al alloys, Fe-N alloys, Fe-Ni alloys, Fe-C alloys, Fe-B alloys, Fe-Co alloys, Fe A material selected from the group consisting of -P-based alloys, Fe-Ni-Co-based alloys, and iron Fe-Al-Si can be used.
  • pure iron in which 99% by mass or more is Fe is preferable.
  • the average particle diameter of the soft magnetic metal particles is 1 ⁇ m or more and 70 ⁇ m or less.
  • the average particle size of the soft magnetic metal particles is more preferably 50 ⁇ m or more and 70 ⁇ m or less.
  • the average particle diameter means a particle diameter of particles in which the sum of masses from particles having a small particle diameter reaches 50% of the total mass in the particle diameter histogram, that is, 50% particle diameter.
  • the soft magnetic metal particles may have a shape with an aspect ratio of 1.5 to 1.8.
  • Soft magnetic metal particles having an aspect ratio in the above range can increase the demagnetizing factor when a dust core is used, compared with particles having a small aspect ratio (close to 1.0), and have excellent high frequency characteristics. It can be a magnetic core. Moreover, the strength of the dust core can be improved.
  • the insulating film coated on the surface of the soft magnetic metal particles functions as an insulating layer between the metal particles.
  • an insulating coating By covering the metal particles with an insulating coating, the contact between the metal particles can be suppressed, and the relative magnetic permeability of the molded body can be suppressed.
  • the presence of the insulating coating can suppress the eddy current from flowing between the metal particles and reduce the eddy current loss of the dust core.
  • the insulating coating is not particularly limited as long as it contains hydrated water and has excellent insulating properties.
  • phosphate, titanate, or the like can be suitably used as the insulating coating.
  • the insulating coating made of phosphate is excellent in deformability, even if soft magnetic metal particles are deformed when a soft magnetic material is pressed to produce a powder magnetic core, it will follow the deformation. Can do.
  • the phosphate coating has high adhesion to iron-based soft magnetic metal particles and is difficult to fall off from the metal particle surface.
  • a metal phosphate compound such as iron phosphate, manganese phosphate, zinc phosphate, or calcium phosphate can be used.
  • the insulating coating containing hydrated water may be formed in advance using a material containing hydrated water.
  • the thickness of the insulating coating is preferably 10 nm or more and 1 ⁇ m or less.
  • the thickness of the insulating coating is preferably 10 nm or more and 1 ⁇ m or less.
  • the thickness of the insulating coating can be examined as follows. First, the film composition obtained by composition analysis (TEM-EDX: transmission electron microscope energy dispersive X-ray spectroscopy), and the amount obtained from inductively coupled plasma mass (ICP-MS) The equivalent thickness is derived. Then, the film is directly observed with a TEM photograph, and it is confirmed that the order of the equivalent thickness derived earlier is an appropriate value. This definition can also be applied to the thickness of the silicone film described later.
  • TEM-EDX transmission electron microscope energy dispersive X-ray spectroscopy
  • ICP-MS inductively coupled plasma mass
  • the resin material to be prepared is not particularly limited as long as it is a silicone that is cured by a hydrolysis / condensation polymerization reaction.
  • a compound represented by Si m (OR) n (m and n are natural numbers) can be used.
  • OR is a hydrolyzable group, and examples thereof include an alkoxy group, an acetoxy group, a halogen group, an isocyanate group, and a hydroxyl group.
  • an alkoxy oligomer having a molecular end blocked with an alkoxysilyl group ⁇ Si—OR
  • alkoxy group examples include methoxy, ethoxy, propoxy, isopropoxy, butoxy, sec-butoxy and tert-butoxy.
  • the hydrolysis group is preferably methoxy.
  • the silicone coating formed by hydrolysis / condensation polymerization of the resin material is excellent in deformability, so that it does not easily crack or crack when the soft magnetic material is pressed, and hardly peels from the surface of the insulating coating. Moreover, since the silicone film is excellent in heat resistance, excellent insulation can be maintained even when the heat treatment temperature after press-molding the soft magnetic material is high.
  • ⁇ Process C Mixing of material powder and resin material ⁇ The mixing of the material powder and the resin material is performed in a heated atmosphere of 80 to 150 ° C. By mixing, the resin material is coated on the surface of the composite magnetic particle. At this time, due to the heating atmosphere, the hydrated water contained in the insulating coating of the composite magnetic particles is released, and the hydrolysis of the resin material is promoted. The removal of hydrated water starts at about 80 ° C., and the higher the temperature, the higher the rate of removal, and the hydrolysis and condensation polymerization reaction of the resin material is promoted. Therefore, the heating atmosphere is preferably 100 to 150 ° C. When the temperature is increased, organic substances generated during hydrolysis / condensation polymerization, for example, methanol can be easily removed if the hydrolysis group is methoxy.
  • heat treatment is performed after mixing the raw materials, and hydrolysis / condensation polymerization of the resin material is caused to proceed by water molecules contained in the heated atmosphere. Since there is an insulating film that is a source of water molecules directly under the material, hydrolysis / condensation polymerization of the insulating material proceeds in a very short time.
  • the heat treatment conditions after mixing were conventionally 150 ° C. ⁇ 60 minutes or more (recommended conditions by the resin manufacturer), 80-150 ° C. ⁇ 10-30 It can be about minutes.
  • the generation source of water molecules is present in the vicinity of the resin material, the resin material coated on the surface of the insulating coating is surely made into a silicone coating even when mixing in large batches of the order of several tens of kg. be able to.
  • the ratio of blending the material powder and the resin material can be appropriately selected so as to satisfy the characteristics required for the powder magnetic core to be produced.
  • the ratio of the resin material during mixing that is, the ratio of the resin material to the total of the material powder and the resin material is 0.5-2. It is preferable to set it as 5 mass%. If the proportion of the resin material is in the range of 0.5 to 2.5% by mass, the entire surface of the composite magnetic particle can be covered with a silicone coating, so that the insulation between the soft magnetic metal particles is improved. be able to.
  • the thickness of the silicone coating film formed can be made thicker than before, the heat treatment temperature after pressure molding can be increased during the production of the dust core described later.
  • the ratio of the preferable resin material is larger than the ratio of the resin material (about 0.25% by mass) in the conventional soft magnetic material manufacturing method in which mixing and heat treatment are separately performed.
  • the resin material can be blended at this ratio because it promotes the hydrolysis / condensation polymerization reaction of the resin material by blending in a heated atmosphere, and the organic substance generated during this reaction, for example, methanol if the hydrolyzable group is methoxy. This is because it can be easily removed.
  • the thickness of the silicone coating is preferably 10 nm to 0.2 ⁇ m. If it is the silicone film of the thickness of this range, the insulation between soft-magnetic metal particles can be ensured, without a magnetic flux density falling too much.
  • a catalyst may be added as a means for promoting the formation of a silicone film in the mixing step.
  • organic acids such as formic acid, maleic acid, fumaric acid and acetic acid
  • inorganic acids such as hydrochloric acid, phosphoric acid, nitric acid, boric acid and sulfuric acid can be used. If the amount of the catalyst added is too large, gelation of the resin material is caused, so an appropriate amount may be selected.
  • the soft magnetic material produced as described above since the surface of the soft magnetic metal particles is covered with the insulating coating and the silicone coating, even if the soft magnetic material is pressed and molded in the subsequent step D, The soft magnetic metal particles hardly come into direct contact with each other.
  • the silicone film is formed on the outermost surface of the composite magnetic particle, even if a high-temperature heat treatment is performed in the subsequent step E, the insulating film can be prevented from being thermally decomposed, and the soft magnetic metal particles can be contacted with each other. Can be effectively prevented.
  • the soft magnetic material of the present invention is superior in magnetic characteristics when a powder magnetic core is used even if the blending ratio of the resin material is the same. This is presumably because the mixing of the material powder and the resin material and the formation of the silicone film by heat treatment are performed at the same time, so that a silicone film having a relatively uniform thickness is formed.
  • the pressure molding step can be typically performed by injecting the soft magnetic material obtained in step C into a predetermined-shaped molding die, and pressing and hardening the material.
  • the pressure at this time can be selected as appropriate.
  • it is preferably about 900 to 1300 MPa (preferably 960 to 1280 MPa).
  • the heat treatment is performed in order to remove the distortion or transition introduced into the soft magnetic metal particles in the step D.
  • the high heat treatment temperature means that the distortion and transition introduced into the soft magnetic metal particles can be sufficiently removed, so that the hysteresis loss of the dust core can be effectively reduced.
  • a soft magnetic material having an insulating coating and a silicone coating on the surface of soft magnetic metal particles can be produced with high productivity.
  • the surface of the soft magnetic metal particles is covered with an insulating coating and a silicone coating, so that the coating is damaged both during pressure molding and during heat treatment after pressure molding. It is difficult to reduce the insulation.
  • a dust core from which distortion and the like are sufficiently removed can be manufactured.
  • the powder magnetic core from which distortion and the like are removed has little energy loss when used at a high frequency, and thus can exhibit excellent characteristics as a core of a reactor, for example. Further, when this dust core is used as, for example, a core of a reactor, the direct current superimposition characteristics are excellent, so that the core can be made gapless.
  • a dust core (prototype material 1, prototype material 2) was produced by the method for producing a dust core of the present invention including the following steps (A) to (E), and the physical properties thereof were measured. Moreover, the dust core (comparative material) was produced with the manufacturing method of the conventional dust core, and the physical characteristic was measured. The physical properties of the prototype material 1, the prototype material 2 and the comparative material were compared.
  • B A step of preparing a resin material containing silicone that is cured by hydrolysis / condensation polymerization reaction in the presence of water.
  • C A step of mixing a powder material and a resin material in a heated atmosphere at 80 to 150 ° C. to form a silicone coating on the surface of the insulating coating.
  • D A step of pressure-molding a soft magnetic material comprising a silicone film formed on the surface of an insulating film of soft magnetic metal particles.
  • E A heat treatment step for removing strain introduced into the soft magnetic metal particles during pressure molding.
  • An iron powder having a purity of 99.8% or more (average particle diameter of 50 ⁇ m, aspect ratio of 1.51) produced by a water atomization method was prepared as soft magnetic metal particles. Then, a phosphate chemical conversion treatment was performed on the surface of the metal particles to form an insulating coating made of iron phosphate containing hydration water in advance, thereby producing composite magnetic particles.
  • the insulating coating substantially covered the entire surface of the soft magnetic metal particles, and the average thickness was 50 nm. Moreover, it was 7.78 in mass% when the hydration water contained in an insulating film was measured by thermal desorption gas analysis.
  • the aggregate of the composite magnetic particles is a material powder for producing a soft magnetic material.
  • ⁇ Process B As a resin material containing silicone that is cured by hydrolysis / condensation polymerization reaction, TSR116 manufactured by GE Toshiba Silicone Co., Ltd. and XC96-B0446 manufactured by the same company were prepared. These are alkoxy resin type silicone oligomers whose molecular ends are blocked with alkoxysilyl groups ( ⁇ Si—R), and the hydrolyzable group (—R) is methoxy. In addition, the order of the process A and the process B is not ask
  • Step C The material powder prepared in step A and the resin material (TSR116, XC96-B0446) prepared in step B were put into a mixer and mixed in a heated atmosphere at 150 ° C. for 10 minutes to obtain a soft magnetic material. Of the materials charged in the mixer, the proportion of TSR116 was 0.75% by mass, and the proportion of XC96-B0446 was 0.5% by mass. The rotation speed of the mixer is 300 rpm. Met.
  • a soft magnetic material in which the surface of the composite magnetic particle was coated with a silicone film was obtained.
  • the average thickness of the silicone film formed on the surface of the composite magnetic particle was 200 nm.
  • the soft magnetic material obtained in step C was poured into a mold having a predetermined shape and subjected to pressure molding by applying a pressure of 960 MPa to obtain a rod-shaped test piece and a ring-shaped test piece.
  • the size of each test piece is as follows. Bar-shaped test piece: For evaluation of DC superposition characteristics Length 55mm, width 10mm, thickness 7.5mm Ring-shaped test piece: for evaluation of magnetic properties, outer diameter 34 mm, inner diameter 20 mm, thickness 5 mm
  • the prototype 2 is different from the prototype 1 in the following points.
  • the ratio of the resin material in Step C is 0.25% by mass (the ratio of TSR116 and XC96-B0446 is the same as that of Prototype material 1).
  • the average thickness of the silicone film was 100 nm.
  • the comparative material is different from the prototype material 1 in the points listed below.
  • the ratio of the resin material in Step C is 0.25% by mass (the ratio of TSR116 to XC96-B0446 is the same as that of the prototype material). In this case, the average thickness of the silicone film was 100 nm. 2.
  • a silicone film was formed by heat treatment at 150 ° C. for 60 minutes. That is, although the amount of resin material to be cured is small, the total production time of the soft magnetic material is 60 minutes longer than the prototype material. This difference in manufacturing time is expected to become more prominent as more soft magnetic material is manufactured.
  • a bar-shaped test piece and a ring-shaped test piece were prepared in the same manner as the prototype materials 1 and 2, and the DC superposition characteristics and the magnetic characteristics were measured in the same manner as the prototype materials 1 and 2.
  • Winding was applied to the ring-shaped test piece to prepare a measuring member for measuring the magnetic properties of the test piece.
  • a measuring member for measuring the magnetic properties of the test piece.
  • an excitation magnetic flux density Bm: 1 kG ( 0.1 T)
  • an excitation magnetic flux density Bm: 2 kG ( 0. 2T)
  • the frequency curve of iron loss was fitted by the following three formulas by the least square method, and the hysteresis loss coefficient Kh (mWs / kg) and the eddy current loss coefficient Ke (mWs 2 / kg) were calculated.
  • the initial permeability ⁇ i (H / m) was measured using the measurement member.
  • the initial permeability was measured (evaluated using a DC / AC-BH tracer (Metron Giken Co., Ltd.)).
  • the electrical resistance ( ⁇ ) was measured by a four-terminal method using a ring-shaped test piece.
  • a direct current superposition test machine in which a core M composed of a rod-shaped test piece and a spacer S were assembled and a coil C was formed around the core M was produced.
  • the number of coil turns in the test machine was 54
  • the magnetic path length was 220 mm
  • the magnetic path cross-sectional area was 75 mm 2 .
  • the gap length interposed in the core M can be changed by the total thickness of the spacers S.
  • the gap length was changed to 0 mm, 0.6 mm, 1.2 mm, 2.0 mm, 2.8 mm, or 4.0 mm for each testing machine using the core M made of a prototype material.
  • Inductance L ( ⁇ H) was measured when the DC superposition current for a test machine having a power source was changed from 0 A to 40.0 A. Further, for the testing machine using the core M made of the comparative material, the inductance L ( ⁇ H) was measured when the gap length was 2.0 mm and the DC superimposed current was changed from 0 A to 40.0 A.
  • FIG. 2 shows a graph showing inductance values (prototype material 1 and comparative material) with respect to the DC superimposed current measured using the test machine.
  • the inductance L when the applied current is 0 A
  • the differential permeability ( ⁇ B / ⁇ H) of each sample was measured.
  • the differential permeability was calculated based on a measured value obtained by measuring a DC magnetization characteristic in an applied magnetic field 100 Oe using a measurement member in which a winding was wound around a ring-shaped test piece prepared for each sample.
  • FIG. 3 shows the relationship between the applied magnetic field and the differential permeability for the prototype material 1, the prototype material 2, and the comparative material.
  • the smaller the difference between the maximum value and the minimum value of the differential permeability the better the DC superposition characteristics.
  • the method for producing the soft magnetic material of the present invention is the conventional method in that the direct current superposition characteristics of the soft magnetic material are improved. It became clear that it was superior to the method. Moreover, it became clear that the prototype material 1 in which the ratio of the resin material in the process C is 1.25% by mass is superior in direct current superposition characteristics as compared with the prototype material 2 in which the ratio is 0.25% by mass.
  • the embodiment of the present invention is not limited to the above-described embodiment, and can be appropriately changed without departing from the gist of the present invention.
  • the soft magnetic material produced by the method for producing a soft magnetic material of the present invention can be suitably used for producing a dust core having excellent high frequency characteristics and direct current superposition characteristics.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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PCT/JP2009/005635 2008-05-23 2009-10-26 軟磁性材料の製造方法、および圧粉磁心の製造方法 WO2010061525A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US12/994,672 US8568644B2 (en) 2008-05-23 2009-10-26 Method for producing soft magnetic material and method for producing dust core
EP09828775.8A EP2359963B1 (en) 2008-11-26 2009-10-26 Method for producing soft magnetic material and method for producing dust core
CN2009801191376A CN102046310B (zh) 2008-11-26 2009-10-26 制造软磁性材料的方法以及制造压粉铁心的方法

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JP2012248619A (ja) * 2011-05-26 2012-12-13 Sumitomo Electric Ind Ltd 圧粉成形体の成形方法

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JP6243298B2 (ja) * 2014-06-13 2017-12-06 株式会社豊田中央研究所 圧粉磁心およびリアクトル
JP6443269B2 (ja) * 2015-09-01 2018-12-26 株式会社村田製作所 磁心及びその製造方法
JP6378156B2 (ja) * 2015-10-14 2018-08-22 トヨタ自動車株式会社 圧粉磁心、圧粉磁心用粉末、および圧粉磁心の製造方法
CN113692078A (zh) * 2021-07-08 2021-11-23 华南理工大学 一种磁性复合材料的固化系统及方法

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