WO2006028100A1 - Mg含有酸化膜被覆軟磁性金属粉末の製造方法およびこの粉末を用いて複合軟磁性材を製造する方法 - Google Patents
Mg含有酸化膜被覆軟磁性金属粉末の製造方法およびこの粉末を用いて複合軟磁性材を製造する方法 Download PDFInfo
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- 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
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- 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
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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
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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
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- 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
- B22F2998/10—Processes characterised by the sequence of their steps
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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the present invention relates to a method for producing a Mg-containing oxide film-coated soft magnetic metal powder and a method for producing a composite soft magnetic material using the Mg-containing oxide film-coated soft magnetic metal powder produced by this method.
- This composite soft magnetic material is used as a material for various electromagnetic circuit components such as magnetic core, electric motor core, generator core, solenoid core, ignition core, rear core core, transformer core, choke coil core or magnetic sensor core.
- the present invention relates to a raw material powder for producing an Mg-containing oxide film-coated soft magnetic metal powder.
- Soft magnetic materials used in various electromagnetic circuit components such as magnetic cores, motor cores, generator cores, solenoid cores, idling cores, rear cores, transformer cores, choke coil cores, or magnetic sensor cores have low iron loss. Therefore, it is generally known that the electric resistance is high and the coercive force is small. Furthermore, since there is a demand for miniaturization and high response of electromagnetic circuits in recent years, higher magnetic flux density is also regarded as important.
- a laminated steel plate is known in which an insulating layer having an MgO force is applied to the surface of a soft magnetic metal plate (see Patent Document 1).
- this laminated steel sheet has good magnetic flux density and electrical resistance, it is difficult to produce electromagnetic parts with complicated shapes.
- composite soft magnetic metal powder is produced by coating the surface of soft magnetic metal powder with MgO insulating coating by wet method such as chemical plating or coating. Possible methods include making powders by press molding and firing, or making soft composites with MgO as an insulating layer by mixing soft magnetic metal powder with Mg ferrite powder, press forming and firing. It is done.
- metal soft magnetic magnetic powder iron powder, insulated iron powder, Fe A1-based iron-based soft magnetic alloy powder, Fe Ni-based iron-based soft magnetic alloy powder, Fe Cr-based iron-based soft magnetic alloy Powder, Fe Si-based iron-based soft magnetic alloy powder, Fe Si-A1-based iron-based soft magnetic alloy powder, Fe-Co-based iron-based soft magnetic alloy powder, Fe Co V-based iron-based soft magnetic alloy powder or Fe-P-based Iron-based soft magnetic alloy powder is generally known.
- Patent Document 1 Japanese Patent Laid-Open No. 63-226011
- a composite magnetic material in which a high resistivity substance is interposed between iron powder particles has been proposed.
- One example is a mixture of iron powder, a compound that generates SiO, and MgCO or MgO powder power.
- a molded body is produced by compression molding, and this molded body is maintained at a temperature of 500 to 1100 ° C. From this, a glass phase mainly composed of SiO and MgO is formed between the iron powder particles, and the iron powder Between particles
- Patent Document 1 Japanese Patent Laid-Open No. 2003-217919
- a method of producing a composite soft magnetic metal powder by wet method such as chemical plating or coating with an MgO insulating film on the soft magnetic metal powder is expensive and difficult to mass-produce.
- the metal powder is expensive, and the composite soft magnetic material produced using this expensive composite soft magnetic metal powder has a drawback that it is expensive.
- the composite soft magnetic metal powder produced by this method is more stable in the MgO insulating film than the soft magnetic metal powder, so that it is difficult for a diffusion reaction to occur between the MgO insulating film and the surface of the soft magnetic metal powder.
- Adhesion between the MgO insulating film formed on the surface and the surface of the soft magnetic metal powder is insufficient, and when the composite soft magnetic metal powder produced by this wet method is press-molded, the MgO insulating film is broken during press forming. Therefore, the composite soft magnetic material produced using the composite soft magnetic metal powder produced by this wet method has a drawback that a sufficiently high resistance cannot be obtained.
- the method of adding an insulating Mg ferrite powder to a soft magnetic metal powder, mixing, pressing, and firing can provide an inexpensive composite soft magnetic material because the manufacturing cost is low.
- MgO is concentrated at the three grain boundaries of the metal soft magnetic grains.
- the resulting composite soft magnetic material has a low specific resistance because it has an intermediate structure and MgO is less likely to be uniformly dispersed at the grain boundaries.
- the composite soft magnetic sintered material obtained by adding the above-mentioned conventional high resistivity substance to iron powder and sintering is particularly specific resistance among density, bending strength, specific resistance and magnetic flux density. Therefore, there has been a demand for a composite soft magnetic sintered material having an even higher specific resistance.
- Oxidized soft magnetic metal powder is used as a raw material powder, and mixed powder obtained by adding and mixing Mg powder to this raw material powder is temperature: 150 to: L 100 ° C, pressure: 1 Soft magnetic metal powder when heated in an inert gas atmosphere or vacuum atmosphere of X 10 1 12 ⁇ 1 X 10 " 1 MPa, and further in an acid atmosphere if necessary, temperature: 50-400 ° C An Mg-containing oxide film-coated soft magnetic metal powder having an oxide insulating film containing Mg on the surface was obtained, and this Mg-containing oxide film-coated soft magnetic metal powder was made of an Mg-containing oxide film coated with a conventional Mg ferrite film.
- this Mg-containing oxide film-coated soft magnetic metal powder is fired at a temperature of 400 to 1300 ° C.
- the composite soft magnetic material obtained in this way has a structure in which the Mg-containing oxide film is uniformly dispersed at the grain boundaries and the Mg-containing oxide film is not concentrated and dispersed at the three-grain boundary points.
- Oxidized soft magnetic metal powder is used as raw material powder, and mixed powder obtained by adding and mixing Mg powder to this raw material powder is temperature: 150 ⁇ : L 100 ° C, pressure: 1 In order to heat in an inert gas atmosphere or a vacuum atmosphere of X 10 1 12 to 1 X 10 " 1 MPa, it is preferable to heat the mixed powder while rolling,
- the above-mentioned soft magnetic metal powders are generally known! / Powdered iron powder, insulated iron powder, Fe—A1-based iron-based soft magnetic alloy powder, Fe—Ni-based iron-based soft powder Magnetic alloy powder, Fe-Cr-based iron-based soft magnetic alloy powder, Fe-Si-based iron-based soft magnetic alloy powder, Fe-Si-A1-based iron-based soft magnetic alloy powder, Fe-Co-based iron-based soft magnetic alloy powder, Research results such as the use of Fe—Co—V-based iron-based soft magnetic alloy powder or Fe—P-based iron-based soft magnetic alloy powder were obtained.
- Soft magnetic powder by maintaining soft magnetic powder in an oxidizing atmosphere at room temperature to 500 ° C. After adding or mixing with the oxide-coated soft magnetic powder with oxides formed on the surface of the metal, the mixture is heated or heated in a vacuum atmosphere at a temperature of 600 to 1200 ° C while mixing. When Mg powder is added and mixed or heated in a vacuum atmosphere with mixing at a temperature of 400-800 ° C, an Mg-Si-containing oxide film is formed on the surface of the soft magnetic powder. Oxide-containing soft magnetic powder is obtained, and the composite soft magnetic sintered material produced using the Mg Si-containing oxide-coated soft magnetic powder produced by this method is composed of a conventional compound that produces Si 2 O and MgCO or MgO. Compression molding and baking a mixture of
- the resulting composite soft magnetic sintered material is superior in density, bending strength, specific resistance and magnetic flux density.
- Mg powder is added and mixed at the same time or heated in a vacuum atmosphere while mixing at a temperature of 400-1200 ° C, Mg-Si-containing oxide film is formed on the surface of soft magnetic powder.
- Si-containing oxide-coated soft magnetic powder was obtained.
- the composite soft magnetic sintered material prepared using the Mg-Si-containing oxide-coated soft magnetic powder was composed of a conventional compound that generates SiO and MgCO. Or compression molding a mixture of MgO powder force and sintering
- the density, bending strength, specific resistance and magnetic flux density are superior to the composite soft magnetic sintered material obtained
- the composite soft magnetic sintered material is made of conventional SiO
- the addition amount of the silicon monoxide powder is in the range of 0.01 to 1% by mass.
- the addition amount of the Mg powder is in the range of 0.05 to 1% by mass.
- the vacuum atmosphere is a vacuum atmosphere having a pressure of 1 ⁇ 10 1 12 to 1 ⁇ 10 _1 MPa. .
- An oxidized soft magnetic metal powder is used as a raw material powder, and mixed powder obtained by adding and mixing Mg powder to this raw material powder is mixed at a temperature of 150 to: L 100 ° C, pressure: 1 X 10 1 12 ⁇ 1 X 10
- the acid-oxidation treatment of the soft magnetic metal powder according to (1) is a heat treatment in an oxidizing atmosphere at a temperature of 50 to 500 ° C.
- An oxide-coated soft magnetic powder in which an iron oxide film is formed on the surface of the soft magnetic powder is produced by heating and holding the soft magnetic powder at room temperature to 500 ° C. in an oxidizing atmosphere.
- the addition amount of the silicon monoxide powder is in the range of 0.01 to 1% by mass, and the addition amount of the Mg powder is in the range of 0.05 to 1% by mass.
- the vacuum atmosphere is a vacuum atmosphere having a pressure of 1 ⁇ 10 — 12 to 1 ⁇ 10 — 1 MPa.
- (6), (7), (8), (9) or (10) The production method of the Mg—Si-containing acid oxide-coated soft magnetic powder described above is characterized.
- the oxide-coated soft magnetic powder forms an iron oxide film on the surface of the soft magnetic powder by maintaining the soft magnetic powder in an oxidizing atmosphere (for example, in the air) at a temperature of room temperature to 500 ° C. Make Can.
- This ferric oxide film has the effect of improving the coverage of SiO and / or Mg.
- the heating temperature during the production of the oxide-coated soft magnetic powder was set to room temperature to 500 ° C. More preferably, the range is from room temperature to 300 ° C. More preferably, the acid atmosphere is a dry acid atmosphere.
- the amount of Mg powder added is limited to 0.05 to 1% by mass. If it is less than 0.05 mass, the Mg film formed on the surface of the oxide-coated soft magnetic powder is insufficient in thickness, so that the amount of Mg contained in the Mg—Si-containing oxide film is insufficient. A Mg-Si oxide film having a thickness cannot be obtained, but this is not preferable. On the other hand, if it exceeds 1% by mass, the formed Mg film becomes too thick and the resulting Mg-Si-containing oxide film is not obtained. This is preferable because the density of the composite soft magnetic material obtained by compacting and firing the clay-coated soft magnetic powder is reduced.
- the method for producing an Mg-Si-containing oxide-coated soft magnetic powder of the present invention conditions for adding and mixing SiO powder, Mg powder, or a mixed powder of SiO powder and Mg powder with the oxide-coated soft magnetic powder
- the vacuum atmosphere of 600-1200 ° C was used because the SiO vapor pressure was low even when heated at less than 600 ° C, so that a sufficiently thick SiO film or Mg-Si-containing oxide film was obtained.
- the soft magnetic powder will sinter and the desired Mg-Si-containing oxide-coated soft magnetic powder will not be obtained. It is because it is not preferable.
- the heating atmosphere at that time is preferably a vacuum atmosphere of pressure: 1 ⁇ 10 _12 to 1 ⁇ 10 _1 MPa, more preferably heating while rolling.
- the soft magnetic powder used when producing the oxide-coated soft magnetic powder is preferably a soft magnetic powder having an average particle diameter of 5 to 50 O / zm. The reason for this is that if the average particle size force is too small, the compressibility of the powder is lowered, and the volume ratio of the soft magnetic powder is lowered. If is more than 500 / zm, the eddy current inside the soft magnetic powder increases and the permeability at high frequencies decreases.
- the oxide-coated soft magnetic powder in which an iron oxide film is formed on the surface of the soft magnetic powder is used as the raw material powder. It is necessary to. Therefore, the present invention
- a raw material powder for producing an Mg—Si-containing oxide-coated soft magnetic powder comprising an oxide-coated soft magnetic powder in which an iron oxide film is formed on the surface of the soft magnetic powder.
- the raw material powder used in the method for producing the Mg-containing oxide film-coated soft magnetic metal powder of the present invention is an oxidized soft magnetic metal powder.
- the present invention uses the oxidized soft magnetic metal powder as Mg It is used as a raw material powder for producing an oxide film-coated soft magnetic metal powder. Therefore, the present invention
- the soft magnetic metal powder includes iron powder, insulated iron powder, Fe-A1 iron-based soft magnetic alloy powder, Fe Ni-based iron-based soft magnetic alloy powder, Fe Cr-based iron-based soft magnetic alloy Powder, Fe Si-based iron-based soft magnetic alloy powder, Fe Si A1-based iron-based soft magnetic alloy powder, Fe Co-based iron-based soft magnetic alloy powder, Fe Co-V-based iron-based soft magnetic alloy powder or Fe P-based iron-based
- the raw material powder for producing an Mg-containing oxide film-coated soft magnetic metal powder according to (6), which is a soft magnetic alloy powder, is characterized.
- Fe-Si-based iron-based soft magnetic powder having a high-concentration Si-diffusion layer containing high-concentration Si was prepared by oxidizing the resulting Fe-Si-based iron-based soft magnetic powder having a high-concentration Si-diffusion layer.
- the Mg-containing oxide film-covered soft magnetic metal powder produced by the method according to the above (1), (5), (7), (8) or (9) It is characterized by a method of producing a composite soft magnetic material with excellent specific resistance and mechanical strength, which is made by mixing a material, or a mixture of organic and inorganic insulating materials, then compacted and fired at 500 to 1000 ° C. It is what you have.
- an oxidation treatment is performed in order to produce a mixed powder by adding and mixing Mg powder to the oxidized soft magnetic metal powder. It is preferable to add 0.05 to 2% by mass of Mg powder to the soft magnetic metal powder prepared to produce a mixed powder. If the amount of Mg powder added to the oxidized soft magnetic metal powder is less than 0.05 mass, the amount of Mg coating formed is insufficient, and therefore a sufficiently thick Mg-containing oxide film is obtained. On the other hand, if added over 2% by mass, the thickness of the Mg coating becomes too thick and the thickness of the Mg-containing oxide film becomes too thick. This is because the composite soft magnetic material obtained by firing the powder is preferable to reduce the magnetic flux density.
- the oxidation treatment of the soft magnetic metal powder has the effect of improving the coverage of Mg, and in an oxidizing atmosphere, temperature: 50 to 500 ° C or distilled water or pure water, temperature: 50 to 100 ° Hold on C By doing. In this case, it is not efficient at less than 50 ° C., but it is not preferable to keep the temperature in an oxidizing atmosphere at over 500 ° C. because firing occurs. More preferably, the oxidizing atmosphere is a dry acid atmosphere.
- FIG. 1 illustrates a burn diagram showing a temperature change with time when the soft magnetic metal powder is oxidized.
- the heat is applied in the oxidizing atmosphere by heating in an oxidizing atmosphere.
- Fig. 1 (b) It can be performed in a pattern in which the temperature is raised to a high temperature and held, and as shown in Fig. 1 (c), the temperature is raised to a high temperature and held, and then the temperature is lowered to a low temperature and held. This may be performed in a pattern that is accompanied by temperature rise and fall, and has virtually no retention, as shown in the pattern shown in Fig. 1 (d).
- the temperature shown in FIGS. 1 (a) to (d) can be set in the same pattern with the upper limit being 100 ° C. and the lower limit being 50 ° C.
- the burn showing the temperature change with time when the soft magnetic metal powder is subjected to the acid treatment is not limited to FIG. 1 50 to 500 ° It can be changed freely within the range of C.
- the reason for setting the heating temperature to 150 to: L 100 ° C is that, if the temperature is less than 150 ° C, the pressure needs to be less than 1 X 10 _ 12 MPa, which is industrially difficult. On the other hand, if the temperature exceeds 1100 ° C, there is a lot of Mg loss, so if the pressure exceeds 1 X 10 _1 MPa, the coating efficiency of the Mg coating will decrease and it will be formed This is preferable because the thickness of the Mg coating becomes uneven.
- a more preferred range of the heating temperature of the mixed powder powder of soft magnetic metal powder and Mg powder is 300 to 900 ° C, is not more preferable atmosphere pressure range is 1 X 10 _10 ⁇ 1 X 10 _2 MPa.
- FIG. 2 shows a Pann diagram showing the temperature change. Usually, it is performed by heating at a constant temperature as shown in Fig. 2 (a), but it can be changed as shown in Fig. 2 (b). As shown in Fig. 1 (d), the temperature can be raised and held at a low temperature. After that, it may be performed in a pattern in which the temperature is lowered and held at a low temperature. Furthermore, the pattern shown in FIG. 1 (a) may be repeated a plurality of times as shown in FIG. 1 (e). Further, as shown in the pattern shown in FIG. 1 (f), the pattern may be held at a high temperature, held at a low temperature in the middle, and held at a high temperature again.
- Pann showing a change in temperature with respect to time when the oxidized soft magnetic metal powder is heated or rolled while being heated. It is not limited to Fig. 2, but within the range of 150 to 1100 ° C! You can change it freely.
- mixed powder obtained by adding and mixing Mg powder to soft magnetic metal powder is mixed with temperature: 150 to: L 100 ° C, pressure: 1 X 10 _12 to 1 X If heating is performed while heating or rolling in an inert gas atmosphere or vacuum atmosphere of 10 _1 MPa, and then subjected to an oxidation treatment in which heating is performed at a temperature of 50 to 400 ° C in an oxidizing atmosphere, the softness is reduced. An Mg-containing oxide film is formed on the surface of the magnetic metal powder, and the Mg-containing oxide film-coated soft magnetic metal powder of the present invention can be manufactured. If the heating temperature at this time is less than 50 ° C, it is not efficient. On the other hand, if the heating temperature is kept above 400 ° C in an acid atmosphere, firing is not preferable. More preferably, the acid atmosphere is a dry acid atmosphere.
- FIG. 3 shows an example of a burn diagram showing a temperature change with respect to time when the oxidation treatment is performed.
- heating is performed in an acidic atmosphere as in the pattern shown in Fig. 3 (a) .
- Fig. 3 (b) the temperature is raised to a low temperature and held, and then the temperature is increased. It can be done in a pattern where the temperature is raised and held, or it can be done in a pattern where the temperature is raised and held at a high temperature and then lowered and held as shown in Fig. 3 (c).
- the pattern may be performed in a pattern with virtually no holding, accompanied by temperature rise and fall.
- the burn indicating the temperature change with time during the acid treatment is not limited to that shown in FIG.
- the soft magnetic metal powder as the raw material powder used in the method for producing the Mg-containing oxide film-coated soft magnetic metal powder of the present invention includes conventionally known iron powder, insulation-treated iron powder, Fe-A1 -Based iron-based soft magnetic alloy powder, Fe-Ni-based iron-based soft magnetic alloy powder, Fe-Cr-based iron-based soft magnetic alloy powder, Fe-Si-based iron-based soft magnetic alloy powder, Fe-Si- A1-based iron base Soft magnetic alloy powder, Fe-Co-based iron-based soft magnetic alloy powder, Fe-Co-V-based iron-based soft magnetic alloy powder or Fe-P-based iron-based soft magnetic alloy powder, more specifically, iron powder Is a pure iron powder, and the insulation-treated iron powder was coated on the surface of the iron powder by adding and mixing a phosphate-coated iron powder, or a wet solution such as a silica sol-gel solution (silicate) or an alumina sol-gel solution. And then dried and calcined with acid or aluminum coated iron
- Fe—A1-based iron-based soft magnetic alloy powder contains A1: 0.1-20, the balance being Fe and Al-based iron-based soft magnetic alloy powder (for example, Fe-15% Al palm powder having a composition of A1),
- Fe—Ni-based iron-based soft magnetic alloy powder contains Ni: 35 to 85%, Mo: 5% or less, Cu: 5% or less, Cr: 2% or less, Mn: 0.
- a nickel-based soft magnetic alloy powder (for example, Fe-49% Ni powder) containing one or more of 5% or less, the balance being Fe and inevitable impurities
- Fe-Cr-based iron group Soft magnetic alloy powder contains Cr: 1-20%, and if necessary, contains A1 or 5% or less, Ni: 5% or less, and the balance is Fe and unavoidable impurities Fe—Cr-based iron-based soft magnetic alloy powder,
- Fe-Si-based iron-based soft magnetic alloy powder is Fe-S related iron-based soft magnetic alloy powder containing Si: 0.1 to 10%, the balance being Fe and inevitable impurities, Fe-Si-Al-based iron-based soft magnetic alloy powder contains Si: 0.1 to 10%, A1: 0.1 to 20%, with the balance being Fe and Si-A1 iron Based soft magnetic alloy powder
- Fe—Co—V-based iron-based soft magnetic alloy powder contains Co: 0.1 to 52%, V: 0.1 to 3%, with the balance being Fe and Fe—Co—V-based iron. Based soft magnetic alloy powder
- the Fe-Co-based iron-based soft magnetic alloy powder is a Fe-Co-based iron-based soft magnetic alloy powder containing Co: 0.1 to 52%, with the balance being Fe and inevitable impurities,
- Fe—P-based iron-based soft magnetic alloy powder contains P: 0.5 to 1%, and the balance is Fe—P-based iron-based soft magnetic alloy powder consisting of Fe and inevitable impurities. Is preferable).
- the soft magnetic metal powder is preferably a soft magnetic metal powder having an average particle size in the range of 5 to 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 soft magnetic metal powder is lowered, so the value of the magnetic flux density is lowered. If the diameter is larger than 500 m, the eddy current inside the soft magnetic metal powder increases and the permeability at high frequencies decreases.
- the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention is used. It can be produced by compacting and sintering by the usual method, but the average particle size: 0.05 to 1 m of silicon oxide and aluminum oxide of 0.5 m or less.
- a mixed powder is prepared by mixing and mixing so as to be composed of a Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention, and the remaining powder is compacted by an ordinary method. It can be produced by molding and sintering.
- the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention has an Mg-containing oxide film formed on the surface thereof, and this Mg-containing oxide film is composed of silicon oxide and aluminum oxide.
- a composite oxide is formed by reaction, and a composite soft magnetic material having a high specific resistance is obtained with a composite oxide having a high resistance at the grain boundary of the soft magnetic powder. Since it is sintered through aluminum fluoride, a composite soft magnetic material with excellent mechanical strength can be produced. In this case, the coercive force can be kept small when the acid key is mainly sintered with acid aluminum, so that a composite soft magnetic material with less hysteresis loss can be produced.
- the firing is preferably performed in an inert gas atmosphere or an acidic gas atmosphere at a temperature of 400 to 1300 ° C! /.
- a wet solution such as a sol-gel (silicate) solution of silica or a sol-gel solution of alumina is added to the Mg-containing oxide film-coated iron powder of the present invention and mixed, and then dried.
- the composite soft magnetic material can be produced by firing at a temperature of 400 to 1300 ° C. in an inert gas atmosphere or an oxidizing gas atmosphere.
- the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention is mixed with an organic insulating material, an inorganic insulating material, or a mixed material of an organic insulating material and an inorganic insulating material, to obtain a specific resistance and A composite soft magnetic material having further improved strength can be produced.
- organic insulating materials epoxy resin, fluorine resin, phenol resin, urethane resin, silicone resin, polyester resin, phenoxy resin, urea resin, isocyanate resin, acrylic resin, Polyimide resin, PPS resin, etc. can be used.
- the inorganic insulating material phosphates such as iron phosphate, various glassy insulators, water glass mainly composed of soda silicate, insulating oxides, and the like can be used.
- one or more of boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide is added to B 2 O 3 to the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention.
- a composite soft magnetic material can be produced by blending 3 to 1% by mass and then compacting and then compacting the resulting compacted body at a temperature of 500 to 1000 ° C.
- the composite soft magnetic material produced in this way is composed of one or more of boron oxide, vanadium oxide, bismuth oxide, antimony oxide and molybdenum oxide.
- the Mg-containing oxide film formed by the method of the present invention is formed on the surface of the soft magnetic metal powder, and includes the Mg-containing oxide film and boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide. A film reacts with one or more of these.
- this composite soft magnetic material is made of a boron oxide sol solution or powder, an acid-vanadium sol solution or powder, an acid-bismuth sol solution or powder, an acid-antimony sol solution or
- One or more of the sol solution or powder of powder and acid-molybdenum is 0.05 to 1% by mass in terms of BO, VO, BiO, SbO, and MoO, and the balance is the above-mentioned
- Inventive Mg-containing oxide film-coated iron powder is formulated and mixed, and the resulting mixed oxide is compacted, molded, and sintered at a temperature of 500-1000 ° C. You can get it by doing this.
- the composite soft magnetic material produced using the Mg-containing oxide film-coated soft magnetic metal powder of the present invention has high density, high strength, high specific resistance, and high magnetic flux density.
- the fact that it has the characteristics of high frequency and low iron loss with its magnetic flux density can also be used as a material for various electromagnetic circuit components that make use of this characteristic.
- the Mg—Si-containing oxide coating produced by the method of the present invention is used.
- the coated soft magnetic powder can be produced by compression molding by a conventional method and then firing in an inert gas atmosphere or an oxidizing gas atmosphere at a temperature of 400 to 1300 ° C.
- organic insulating material an inorganic insulating material, or a mixed material of an organic insulating material and an inorganic insulating material with the Mg-Si-containing oxide-coated soft magnetic powder produced by the method of the present invention.
- a composite soft magnetic material with further improved strength can be produced.
- organic insulating materials epoxy resin, fluorine resin, phenol resin, urethane resin, silicone resin, polyester resin, phenoxy resin, urea resin, isocyanate resin, acrylic resin, Polyimide resin, PPS resin, etc. can be used.
- phosphates such as iron phosphate, various glassy insulators, water glass mainly composed of soda silicate, insulating oxides, and the like can be used.
- one or more of boron oxide, vanadium oxide, bismuth oxide, antimony oxide and molybdenum oxide is added to the Mg-Si-containing oxide-coated soft magnetic powder produced by the method of the present invention.
- the composite soft magnetic material produced in this way is one or more of boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide in terms of BO, VO, BiO, SbO, and MoO.
- Mg—Si-containing oxide-coated soft magnetic powder produced by the method of the present invention 0.05 to 1% by mass, with the balance being composed of the Mg—Si-containing oxide-coated soft magnetic powder produced by the method of the present invention.
- an Mg-Si-containing oxide film formed on the surface of the Mg-Si-containing oxide-coated soft magnetic powder produced by the method of the present invention, and boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide A film reacting with one or more of them is formed.
- the composite soft magnetic material includes a sol solution or a powder of boron oxide, a sol solution or a powder of vanadium oxide, a sol solution or a powder of acid bismuth oxide, a sol solution or a powder of acid oxyantimony, and One or two or more of the sol-molybdenum oxymolybdenum sol solution or powder is converted into BO, VO, BiO, SbO, MoO in an amount of 0.05 to 1% by mass, and the balance is the above-mentioned
- the Mg-Si-containing oxide-coated soft magnetic powder of the invention is blended and mixed so that the resulting mixed oxide is compacted, molded, and temperature: 500 to 1000 ° It can be obtained by sintering with C.
- a wet solution such as a sol-gel (silicate) solution of silica or a sol-gel solution of alumina is added to the Mg-Si-containing oxide-coated soft magnetic powder of the present invention, followed by drying and drying.
- the composite soft magnetic material can be produced by firing at 500 to 1000 ° C. in an inert gas atmosphere or an oxidizing gas atmosphere.
- the composite soft magnetic material produced using the Mg-Si-containing oxide-coated soft magnetic powder of the present invention has high density, high strength, high specific resistance, and high magnetic flux density.
- the fact that it has the characteristics of high magnetic flux density and high frequency and low iron loss can also be used as a material for various electromagnetic circuit components that make use of this characteristic.
- FIG. 1 is a burn diagram showing a change in temperature with respect to time when a soft magnetic metal powder is oxidized.
- FIG. 2 is a burn diagram showing a change in temperature with respect to time when an oxidized soft magnetic metal powder is heated or heated while rolling.
- FIG. 3 A Pann diagram showing temperature change with time during the treatment with acid after heating or rolling.
- soft magnetic powder A As the soft magnetic metal powder, all have a mean particle size: 70 m, pure iron powder (hereinafter, this pure iron powder is referred to as soft magnetic powder A),
- soft magnetic powder B Fe atomized Fe—Al-based iron-based soft magnetic alloy powder (hereinafter, this Fe—A1-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder B),
- soft magnetic powder C atomized Fe-M-based iron-based soft magnetic alloy powder (hereinafter, this Fe-Ni-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder C),
- soft magnetic powder D Fe atomized Fe—Cr-based iron-based soft magnetic alloy powder (hereinafter, this Fe—Cr-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder D),
- soft magnetic powder E atomized Fe-Si-based iron-based soft magnetic alloy powder (hereinafter, this atomized Fe-Si-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder E),
- Fe-Si-A1-based iron-based soft magnetic alloy Fe atomized Fe-Si-A1-based iron-based soft magnetic alloy powder (hereinafter referred to as Fe-Si-A1-based iron-based soft magnetic alloy)
- the powder is soft magnetic powder F)
- Fe Co-V-based iron-based soft magnetic alloy powder containing Co: 30% V: 2% and remaining balance of Fe and inevitable impurities (hereinafter referred to as this Fe-Co-V-based iron-based soft magnetic alloy)
- the powder is called soft magnetic powder G)
- Fe P-based iron-based soft magnetic alloy powder containing 0.6%, the balance being Fe and inevitable impurities (hereinafter, this Fe-P-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder.
- H commercially available phosphate-coated iron powder (hereinafter, this phosphate-coated iron powder is called soft magnetic powder I),
- Fe Co-based iron-based soft magnetic alloy powder containing 30% Co with the balance being Fe and inevitable impurities (hereinafter, this Fe-Co-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder 3 ⁇ 4 [ ) Was prepared.
- Mg powder was blended so as to have the blending ratio shown in Table 1.
- Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling while maintaining the pressure and temperature shown in Table 1 in argon gas or in a vacuum atmosphere.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold and press-molded to obtain a plate-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter. : Ring-shaped green compact with dimensions of 35mm, inner diameter: 25mm, height: 5mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 1 for 30 minutes. Then, composite soft magnetic materials comprising plate-like and ring-like fired bodies were produced, and the present invention methods 1 to 7 and comparative methods 1 to 3 were carried out.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention methods 1 to 7 and comparative methods 1 to 3 were measured, and the results are shown in Table 1.
- Mg ferrite powder was blended with the soft magnetic powder A prepared in the examples so as to have a blending ratio shown in Table 1, and the blended powder was stirred while rolling in the atmosphere to mix the mixed powder.
- the obtained mixed powder is 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 outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 1 in a nitrogen atmosphere. It consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 1 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material obtained by the conventional method 1 and having a plate-like fired body strength were measured, and the results are shown in Table 1. Further, the composite soft magnetic material having a ring-like fired body strength is also obtained. The material was lined and the magnetic flux density was measured with a BH tracer. The results are shown in Table 1.
- Mg powder is blended so as to have the same blending ratio as in Example 1 shown in Table 2, and this blended powder is placed in Table 2 in argon gas or vacuum atmosphere. After rolling while maintaining the indicated pressure and temperature, the Mg-containing oxide film-coated soft magnetic metal powder was prepared by performing the oxidation treatment under the conditions shown in Table 2.
- soft magnetic powder B Fe—A1-based iron-based soft magnetic alloy powder
- Mg powder was blended so as to have the blending ratio shown in Table 3
- the mixed powder was rolled while maintaining the pressure and temperature shown in Table 3 in an argon gas or a vacuum atmosphere to produce a Mg-containing oxide-coated soft magnetic metal powder.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was placed in a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter.
- Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 3 for 30 minutes.
- composite soft magnetic materials comprising plate-like and ring-like fired bodies were produced, and the present invention methods 8 to 14 and comparative methods 4 to 6 were performed.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention method 8-14 and comparative method 4-6 were measured, and the results are shown in Table 3.
- the composite soft magnetic material, which also has a ring-like fired body strength, was lined, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 3.
- Mg ferrite powder was blended so as to have a blending ratio shown in Table 3, and the blended powder was stirred while rolling in the atmosphere to obtain a mixed powder.
- the obtained mixed powder is put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 3 in a nitrogen atmosphere. It consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 2 was performed.
- Mg ⁇ is a characteristic of Mg 1 composite soft magnetic material
- Mg powder is mixed with the raw material powder B (FeAl-based iron-based soft magnetic alloy powder) so as to have the same mixing ratio as in Example 2 shown in Table 4, and this mixed powder is mixed with argon gas.
- rolling was performed while maintaining the pressure and temperature shown in Table 4 in a vacuum atmosphere, and then oxidation treatment under the conditions shown in Table 4 was performed to produce a Mg-containing oxide film-coated soft magnetic metal powder.
- Table 4 shows the results of carrying out the present invention method 8 'to 14', comparative method 4 '6' and conventional method 2 '.
- Mg powder was blended so as to have the blending ratio shown in Table 5 Then, this mixed powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 5 to produce a Mg-containing oxide film-coated soft magnetic metal powder.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter. : Ring-shaped green compact with dimensions of 35mm, inner diameter: 25mm, height: 5mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 5 for 30 minutes. Then, composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the present invention methods 15 to 21 and comparative methods 7 to 9 were carried out.
- the relative density, specific resistance and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained in the present invention method 15 to 21 and comparative methods 7 to 9 were measured, and the results are shown in Table 5, A composite soft magnetic material having a ring-like fired body strength was scored, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 5.
- the Mg ferrite powder was blended with the soft magnetic powder C prepared in the examples so as to have the blending ratio shown in Table 5, and the blended powder was stirred while rolling in the atmosphere to obtain a mixed powder.
- the obtained mixed powder is put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is formed, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 5 for 30 minutes, and consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 3 was performed.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material obtained by the conventional method 3 and having the sintered body strength were measured and the results are shown in Table 5.
- the composite soft magnetic material with a ring-like fired body strength was subjected to leaping, and the magnetic flux density was measured with a BH trainer. The results are shown in Table 5.
- Mg powder was blended so as to have the same blending ratio as Example 3 shown in Table 6, and this blended powder was mixed with argon. After rolling while maintaining the pressure and temperature shown in Table 6 in a gas or vacuum atmosphere, the Mg-containing oxide film-coated soft magnetic metal powder was produced by performing the oxidation treatment under the conditions shown in Table 6.
- Table 6 shows the results of carrying out the inventive methods 15 ′ to 21 ′, the comparative methods 7 ′ to 9 ′ and the conventional method 3 ′.
- the composite soft property magnetic material also has M thermal rolling conditions.
- the composite soft magnetic materials produced by the present method 15 21 and the present method 15 '21' are the composite soft magnetic materials produced by the conventional method 3 and the conventional method 3 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all excellent. However, it can be seen that the composite soft magnetic materials produced by Comparative Method 79 and Comparative Method 7'9 'are not preferred because of their poor relative density and magnetic flux density characteristics.
- Replacement paper (Rule 26) (Gold powder) is mixed with Mg powder so that the blending ratio shown in Table 7 is achieved, and this blended powder rolls while maintaining the pressure and temperature shown in Table 7 in argon gas or vacuum atmosphere. Thus, an Mg-containing oxide film-coated soft magnetic metal powder was produced.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold, press-molded, and pressed into a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm and an outer diameter.
- Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 7 for 30 minutes.
- composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the present invention methods 22 to 28 and comparative methods 10 to 12 were carried out.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention method 22-28 and comparative method 10-12 were measured, and the results are shown in Table 7.
- a composite soft magnetic material having a ring-like fired body strength was scored and the magnetic flux density was measured with a BH tracer. Table 7 shows the results.
- Mg ferrite powder was blended with the soft magnetic powder D prepared in the examples so as to have a blending ratio shown in Table 7, and the blended powder was stirred while rolling in the atmosphere to mix the mixed powder.
- the obtained mixed powder is 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 outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is formed, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 7 for 30 minutes, and consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 4 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material having a plate-like fired body strength obtained by the conventional method 4 were measured, and the results are shown in Table 7. Further, the composite soft magnetic material having a ring-like fired body strength is also shown. The material was lined and the magnetic flux density was measured with a BH tracer. The results are shown in Table 7.
- the condition is M or M gg
- Mg powder was blended so as to have the same blending ratio as Example 4 shown in Table 8, and this blended powder was mixed with argon gas or After rolling while maintaining the pressure and temperature shown in Table 8 in a vacuum atmosphere, an Mg-containing oxide film-coated soft magnetic metal powder was produced by performing oxidation treatment under the conditions shown in Table 8.
- the composite soft magnetic materials produced by the present invention method 22-28 and the present invention method 22'-35 ' are the composite soft magnetic materials produced by the conventional method 4 and the conventional method 4'. It can be seen that the bending strength, magnetic flux density, and specific resistance are all superior to the magnetic material. However, it can be seen that the composite soft magnetic materials produced by the comparative methods 10 to 12 and the comparative methods 10 ′ to 15 ′ are not preferable because of their poor relative density and magnetic flux density characteristics.
- Mg powder was blended to a blending ratio shown in Table 9 with respect to soft magnetic powder E (FeSi-based iron-based soft magnetic alloy powder) oxidized under the conditions shown in Table 9, and this Mix powder
- An Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling while maintaining the pressure and temperature shown in Table 9 in a Lugon gas or vacuum atmosphere.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was placed in a mold and press-molded to obtain a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm and an outer diameter.
- Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 9 for 30 minutes.
- composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the present invention methods 29 to 35 and comparative methods 13 to 15 were carried out.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained in the present invention method 29-35 and comparative method 13-15 were measured, and the results are shown in Table 9.
- a composite soft magnetic material having a ring-like fired body strength was subjected to squiggling, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 9.
- the Mg ferrite powder was blended with the soft magnetic powder E prepared in the examples so as to have the blending ratio shown in Table 9, and the blended powder was stirred while rolling in the atmosphere to obtain a mixed powder.
- the obtained mixed powder is put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 9 in a nitrogen atmosphere. It consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 5 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material obtained by the conventional method 5 and having a plate-like fired body strength were measured, and the results are shown in Table 9. Further, the composite soft magnetic material having a ring-like fired body strength is also obtained. The wire was lined and the magnetic flux density was measured with a BH tracer. The results are shown in Table 9.
- Mg powder is blended so that the blending ratio is the same as in Example 5 shown in Table 10, and this blended powder is mixed with argon gas. Or After rolling while maintaining the pressure and temperature shown in Table 10 in a vacuum atmosphere, an Mg-containing oxide film-coated soft magnetic metal powder was produced by oxidation treatment under the conditions shown in Table 10.
- the composite soft magnetic materials produced by the inventive method 29-35 and the inventive method 36'-49 ' are the composite soft magnetic materials produced by the conventional method 5 and the conventional method 5'. It can be seen that the bending strength, magnetic flux density, and specific resistance are all superior to the magnetic material. However, it can be seen that the composite soft magnetic materials produced by the comparative methods 13 to 15 and the comparative methods 16 ′ to 21 ′ are not preferable because the properties of the relative density and the magnetic flux density are inferior.
- Mg powder should have the mixing ratio shown in Table 11 And blend this powder with argon gas or vacuum atmosphere at the pressure and temperature shown in Table 11. By rolling while holding, an Mg-containing oxide film-coated soft magnetic metal powder was produced.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold and press-molded to form a plate-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter. : Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 11 for 30 minutes. Then, composite soft magnetic materials comprising plate-like and ring-like fired bodies were produced, and the present invention methods 36 to 42 and comparative methods 16 to 18 were carried out.
- the Mg ferrite powder was blended with the soft magnetic powder F prepared in the examples so as to have the blending ratio shown in Table 11, and the blended powder was stirred while rolling in the atmosphere to obtain a mixed powder.
- the obtained mixed powder is put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 11 in a nitrogen atmosphere, and consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 6 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material obtained by the conventional method 6 and having a plate-like fired body strength were measured, and the results are shown in Table 11. Further, the composite soft magnetic material having a ring-like fired body strength is further obtained. The magnetic material was scored and the magnetic flux density was measured with a BH tracer. The results are shown in Table 11.
- the Mg powder was blended in the same blending ratio as in Example 6 shown in Table 12, and this blended powder was mixed with argon. Gas Alternatively, rolling was performed in a vacuum atmosphere while maintaining the pressure and temperature shown in Table 12, and then the oxidation treatment under the conditions shown in Table 12 was performed to produce a Mg-containing oxide-coated soft magnetic metal powder.
- the composite soft magnetic materials produced by the present invention method 36 to 42 and the present invention method 50 'to 5 6' are composite materials produced by the conventional method 6 and the conventional method 6 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all superior to those of soft magnetic materials. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 16 to 18 and Comparative Methods 22 ′ to 24 ′ are not preferable because of their poor relative density and magnetic flux density characteristics.
- Mg powder should have a mixing ratio shown in Table 13
- the Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling the compounded powder in argon gas or in a vacuum atmosphere while maintaining the pressure and temperature shown in Table 13.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was placed in a mold, press-molded, and pressed into a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm and an outer diameter.
- Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 13 for 30 minutes.
- composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the present invention methods 43 to 49 and comparative methods 19 to 21 were carried out.
- Mg ferrite powder was blended with the soft magnetic powder G prepared in the examples so as to have the blending ratio shown in Table 13, and the blended powder was stirred while rolling in the atmosphere, and the mixed powder was mixed.
- the obtained mixed powder is 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 outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the resulting green compact is fired for 30 minutes at a temperature shown in Table 13 in a nitrogen atmosphere, and consists of a plate-shaped and ring-shaped fired body.
- a soft magnetic material was prepared and the conventional method 7 was performed.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material obtained by the conventional method 7 and having the sintered body strength were measured and the results are shown in Table 1.
- Fig. 3 the composite soft magnetic material with ring-shaped fired body strength was lined, and the magnetic flux density was measured with a BH tray. The results are shown in Table 13.
- the Mg powder was blended so as to have the same blending ratio as in Example 7 shown in Table 14, and this blending was performed.
- the powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 14, and then subjected to an oxidation treatment under the conditions shown in Table 14 to obtain an Mg-containing oxide film-coated soft magnetic metal powder. Produced.
- the composite soft magnetic materials produced by the present invention method 43 to 49 and the present invention method 57 'to 70' are composite materials produced by the conventional method 7 and the conventional method 7 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all superior to soft magnetic materials. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 19 to 21 and Comparative Methods 25 ′ to 30 ′ are not preferable because of their poor relative density and magnetic flux density characteristics.
- Soft magnetic powder H Fe— iron-based iron-based soft magnetic compound subjected to oxidation treatment under the conditions shown in Table 15 (Gold powder) is mixed with Mg powder so that the blending ratio shown in Table 15 is achieved, and this blended powder is rolled while maintaining the pressure and temperature shown in Table 15 in argon gas or vacuum atmosphere. Thus, an Mg-containing oxide film-coated soft magnetic metal powder was produced.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was placed in a mold and press-molded to obtain a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm and an outer diameter.
- Ring-shaped green compact with dimensions of 35 mm, inner diameter: 25 mm, height: 5 mm is formed, and the resulting green compact is fired in a nitrogen atmosphere at the temperature shown in Table 15 for 30 minutes.
- composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the present invention methods 50 to 56 and comparative methods 22 to 24 were carried out.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention method 50 to 56 and comparative method 22 to 24 were measured, and the results are shown in Table 15.
- a composite soft magnetic material with a ring-like fired body strength was scored and the magnetic flux density was measured with a BH tracer. Table 15 shows the results.
- the Mg ferrite powder was blended with the soft magnetic powder H prepared in the examples so that the blending ratio shown in Table 15 was achieved, and the blended powder was stirred while rolling in the atmosphere to mix the mixed powder.
- the obtained mixed powder is 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 outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the resulting green compact is fired for 30 minutes at a temperature shown in Table 15 in a nitrogen atmosphere, and consists of a plate-shaped and ring-shaped fired body.
- a soft magnetic material was produced and the conventional method 8 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material obtained by the conventional method 8 and having a plate-like fired body strength were measured, and the results are shown in Table 15. Further, the composite soft magnetic material having a ring-like fired body strength is further obtained.
- the magnetic material was scored and the magnetic flux density was measured with a BH tracer. The results are shown in Table 15.
- the Mg powder is blended so as to have the same blending ratio as in Example 8 shown in Table 16, and this blended powder is mixed with argon gas or After rolling while maintaining the pressure and temperature shown in Table 16 in a vacuum atmosphere, an Mg-containing oxide film-coated soft magnetic metal powder was prepared by performing oxidation treatment under the conditions shown in Table 16.
- the composite soft magnetic materials produced by the present invention method 50 to 56 and the present invention method 71 'to 8 4' are composite materials produced by the conventional method 8 and the conventional method 8 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all superior to soft magnetic materials. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 22 to 24 and Comparative Methods 31 'to 36' are not preferable because of their poor relative density and magnetic flux density characteristics.
- Mg powder was added to the soft magnetic powder I (phosphate-coated iron powder) subjected to the oxidation treatment under the conditions shown in Table 17 so that the mixing ratio shown in Table 17 was obtained.
- Combined powder with Argo The Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling while maintaining the pressure and temperature shown in Table 17 in a nitrogen gas or vacuum atmosphere.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold and press-molded to form a plate-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter. : 35mm, Inner diameter: 25mm, Height: Ring-shaped green compact with dimensions of 5mm, and the resulting green compact is fired in nitrogen atmosphere for 30 minutes at the temperature shown in Table 17 Then, composite soft magnetic materials composed of plate-like and ring-like fired bodies were produced, and the inventive methods 57 to 63 and the comparative methods 25 to 27 were carried out.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention method 57-63 and comparative method 25-27 were measured, and the results are shown in Table 17,
- a composite soft magnetic material with a ring-like fired body strength was scored and the magnetic flux density was measured with a BH tracer. The results are shown in Table 17.
- Mg ferrite powder was blended with the soft magnetic powder I prepared in the examples so as to have a blending ratio shown in Table 17, and the blended powder was stirred while rolling in the atmosphere to obtain a mixed powder.
- the obtained mixed powder is put into a mold and press-molded to obtain a plate-like green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter: 35 mm, inner diameter: 25 mm, height: 5
- a ring-shaped green compact with dimensions of mm is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 17 in a nitrogen atmosphere, and consists of a plate-shaped and ring-shaped fired body.
- a composite soft magnetic material was prepared and the conventional method 9 was performed.
- the relative density, specific resistance, and bending resistance of the composite soft magnetic material obtained by the conventional method 9 and having a plate-like fired body strength were measured, and the results are shown in Table 17.
- the magnetic material was lined and the magnetic flux density was measured with a BH tracer. The results are shown in Table 17.
- Mg powder is blended in the same blending ratio as in Example 9 shown in Table 18, and this blended powder is mixed with argon gas or vacuum atmosphere. After rolling while maintaining the pressure and temperature shown in Table 18, the Mg-containing oxide film-coated soft magnetic metal powder was prepared by performing the oxidation treatment shown in Table 18.
- Table 18 shows the results of carrying out the present method 85 'to 91', comparative method 37 'to 39' and conventional method 9 '.
- the composite soft magnetic materials produced by the inventive method 57 to 63 and the inventive method 85 'to 9 1' are composite materials produced by the conventional method 9 and the conventional method 9 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all superior to soft magnetic materials. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 25 to 27 and Comparative Methods 37 'to 39' are not preferable because of their poor relative density and magnetic flux density characteristics.
- Mg powder Fe-Co based iron-based soft magnetic alloy powder
- oxidation treatment under the conditions shown in Table 19
- Mg powder was blended so as to have the blending ratio shown in Table 19
- this blended powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 19 to produce a Mg-containing oxide film-coated soft magnetic metal powder.
- the obtained Mg-containing oxide film-coated soft magnetic metal powder was put into a mold and press-molded to form a plate-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and outer diameter. : 35mm, inside A ring-shaped green compact with a diameter of 25 mm and a height of 5 mm was molded, and the obtained green compact was baked for 30 minutes at a temperature shown in Table 19 in a nitrogen atmosphere. A composite soft magnetic material composed of a ring-shaped fired body was produced, and the present method 64 to 70 and the comparative method 28 to 30 were carried out.
- the relative density, specific resistance, and bending strength of the composite soft magnetic material comprising the plate-like fired bodies obtained by the present invention method 64-70 and comparative method 28-30 were measured, and the results are shown in Table 19.
- the composite soft magnetic material with ring-shaped fired body strength was subjected to leaping, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 19.
- the powder Fe—Co-based iron-based soft magnetic alloy powder
- Mg powder so that the mixing ratio is the same as in Example 10 shown in Table 20, and this mixed powder is mixed with argon gas or After rolling while maintaining the pressure and temperature shown in Table 20 in a vacuum atmosphere, an Mg-containing oxide film-coated soft magnetic metal powder was produced by performing an oxidation treatment under the conditions shown in Table 20.
- Table 20 shows the results of carrying out the present method 92 'to 98', comparative method 40 'to 42' and conventional method 10 '.
- the composite soft magnetic materials produced by the present invention method 64 to 70 and the present invention method 92 'to 9 8' are composite materials produced by the conventional method 10 and the conventional method 10 '. It can be seen that the bending strength, magnetic flux density and specific resistance are all superior to the soft magnetic material. However, it can be seen that the composite soft magnetic materials produced by the comparative methods 28 to 30 and the comparative methods 40 'to 42' are not preferable because the properties of relative density and magnetic flux density are inferior.
- the soft magnetic raw material powder pure iron powder having an average particle diameter of 70 / z m
- A1 10% by mass, balance: atomized Fe—Al-based iron-based soft magnetic alloy powder made of Fe, [0168] Ni: 49% by mass, balance: atomized Fe-Ni-based iron-based soft magnetic alloy Powder, [0169] Cr: 10% by mass, balance: atomized Fe—Cr-based iron-based soft magnetic alloy powder, [0170] Si: 3% by mass, balance: atomized Fe-Si-based iron-based soft Magnetic alloy powder,
- Fe-Co-V-based iron-based soft magnetic alloy powders containing Co: 30%, V: 2%, the balance being Fe and inevitable impurities were prepared.
- oxide-coated soft magnetic powders having an iron oxide film on the surface were prepared and prepared as raw powders.
- SiO powder having an average particle size: 10 m and Mg powder having an average particle size: 50 ⁇ m were prepared.
- An oxide film containing Mg and Si on the surface of the soft magnetic powder by preparing the powder and holding the resulting mixed powder at a temperature of 650 ° C and a pressure of 2.7 X 10 _4 MPa for 1 hour An Mg-Si-containing oxide-coated soft magnetic powder was formed.
- Each of these Mg-Si-containing oxide-coated soft magnetic powders is placed in a mold and press-molded to obtain a plurality of plate-like green compacts having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and the outside.
- a ring-shaped green compact with dimensions of 35 mm in diameter, 25 mm in inner diameter and 5 mm in height is molded, and the resulting green compact is fired in a nitrogen atmosphere at a temperature of 600 ° C for 30 minutes.
- the composite soft magnetic material composed of the plate-like and ring-shaped fired bodies was manufactured, the specific resistance of the composite soft magnetic material comprised of the plate-like fired bodies was measured, and the results are shown in Table 21, and the ring A composite soft magnetic material made of a sinter-like fired body is wire-lined to produce magnetic flux density, coercive force, and magnetic flux density of 1.5T, iron loss and magnetic flux density at a frequency of 50Hz, and iron loss at a frequency of 1.0T and a frequency of 400Hz. Table 21 shows the measurement results.
- Example 12 [0175] The oxide-coated soft magnetic powder, which was the raw material powder prepared earlier, was replaced with SiO powder and Mg powder, respectively.
- Oxide-coated soft magnetic powder: SiO powder: Mg powder 99.7 mass%: 0.1 mass%: 0. Simultaneously add and mix at a ratio of 2% by mass to prepare a mixed powder.
- the obtained mixed powder is softened by holding it at a temperature of 650 ° C and a pressure of 2.7 X 10 _4 MPa for 3 hours.
- An Mg-Si-containing oxide-coated soft magnetic powder in which an oxide film containing Mg and Si was formed on the surface of the magnetic powder was prepared.
- Each of these Mg-Si-containing oxide-coated soft magnetic powders is placed in a mold and press-molded to obtain a plurality of plate-like green compacts having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and the outside.
- a ring-shaped green compact with dimensions of 35 mm in diameter, 25 mm in inner diameter and 5 mm in height is molded, and the resulting green compact is fired in a nitrogen atmosphere at a temperature of 600 ° C for 30 minutes.
- the composite soft magnetic material composed of the plate-like and ring-shaped fired bodies was manufactured, the specific resistance of the composite soft magnetic material comprised of the plate-like fired bodies was measured, and the results are shown in Table 21, and the ring A composite soft magnetic material made of a sinter-like fired body is wire-lined to produce magnetic flux density, coercive force, and magnetic flux density of 1.5T, iron loss and magnetic flux density at a frequency of 50Hz, and iron loss at a frequency of 1.0T and a frequency of 400Hz.
- Table 22 shows the measurement results.
- An oxide film containing Mg and Si is formed on the surface of the soft magnetic powder by holding the obtained mixed powder at a temperature of 650 ° C and a pressure of 2.7 X 10 _4 MPa for 3 hours.
- Mg-Si-containing oxide-coated soft magnetic powder was prepared.
- Each of these Mg—Si-containing oxide-coated soft magnetic powders is placed in a mold and press-molded to form a plurality of plate-like green compacts having dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness, and the outside. Obtained by molding a ring-shaped green compact with a diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm The green compact was fired in a nitrogen atmosphere at a temperature of 600 ° C for 30 minutes to produce a composite soft magnetic material consisting of a plate-shaped and ring-shaped fired body. The specific resistance of the composite soft magnetic material is measured and the results are shown in Table 21.
- the composite soft magnetic material made of a ring-shaped fired body is subjected to a wire to create a magnetic flux density, a coercive force, and a magnetic flux density of 1.5 T.
- Iron loss and magnetic flux density at a frequency of 50 Hz 1.
- Magnetic properties such as iron loss at OT and a frequency of 400 Hz were measured, and the results are shown in Table 23.
- the conventional mixed powder is prepared by mixing so that the ratio is as follows. The obtained conventional mixed powder is put into a mold and press-molded to form a plate having dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness.
- Green compact and outer diameter 35mm, inner diameter: 25mm, height: Ring-shaped compact with dimensions of 5mm, molded, and the resulting compact is held in nitrogen atmosphere at a temperature of 600 ° C for 30 minutes
- the composite soft magnetic sintered material composed of plate-shaped and ring-shaped sintered bodies was produced by sintering under the conditions described above, the specific resistance of the composite soft magnetic material also having a plate-shaped sintered body force was measured, and the results were displayed.
- a composite soft magnetic material made of a ring-shaped sintered body is subjected to a winding line, and the magnetic flux density, coercive force, and magnetic flux density 1. Magnetic characteristics such as iron loss and magnetic flux density at 5T, frequency 50Hz and iron loss at 1.0T, frequency 400Hz were measured, and the results are shown in Tables 21-23.
- Iron loss is the iron loss at a magnetic flux density of 1.5T and a frequency of 50Hz.
- Iron loss is the iron loss at magnetic flux density 1.OT, frequency 400Hz.
- the composite soft magnetic material using the Mg—Si-containing oxide-coated soft magnetic powder prepared in Examples 1 to 3 is the same as the Mg— Compared to the composite soft magnetic material using Si-containing oxide-coated soft magnetic powder, the density is not much different, but the Mg-Si-containing oxide-coated soft magnetic powder prepared in Examples 1 to 3 was used. Compared to the composite soft magnetic material using the Mg-Si-containing oxide-coated soft magnetic powder prepared in Conventional Example 1, the composite soft magnetic material has a higher magnetic flux density, a smaller coercive force, and a higher specific resistance. For this reason, the iron loss is remarkably small, and in particular, the iron loss decreases as the frequency increases.
- Example 14 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 pure particle with average particle size: 1 ⁇ m or less Si powder was prepared. Furthermore, Mg powder having an average particle diameter of 50 ⁇ m was prepared.
- a mixed powder is prepared by mixing, and the resulting mixed powder is heat-treated 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 is formed by forming a layer and then holding it in the atmosphere at a temperature of 250 ° C. did.
- 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. 1) was prepared.
- the thus obtained deposited acid film coating powder 1 of the present invention is placed in a mold and press-molded to form a plate-shaped powder having dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness.
- Body and outer diameter 35 mm, inner diameter: 25 mm, height: 5 mm
- the ring-shaped green compact with the dimensions of 5 mm was molded.
- the resulting green compact was held in a nitrogen atmosphere at a temperature of 500 ° C for 30 minutes.
- the composite soft magnetic material composed of plate and ring-shaped fired bodies was produced by firing under the conditions, and the specific resistance of the composite soft magnetic material composed of this plate-like fired body was measured. The results are shown in Table 24.
- a composite soft magnetic material made of a ring-shaped fired body is subjected to a wire, and the magnetic flux density, coercive force, and magnetic flux density 1.5T, and the iron loss and magnetic flux density at a frequency of 50Hz are 1.0T and the frequency is 400Hz.
- the magnetic properties such as iron loss were measured, and the results are shown in Table 1.
- the specific resistance of the composite soft magnetic material having a plate-like sintered body force is measured and the result is obtained.
- the iron loss and magnetic flux density are shown in Table 24 when the composite soft magnetic material with a ring-shaped sintered body strength is further lined, and the magnetic flux density, coercive force, and magnetic flux density are 1.5 T and the frequency is 50 Hz. 1.
- OT magnetic characteristics such as iron loss at a frequency of 400 Hz were measured, and the results are shown in Table 24.
- Example 14 100 30 7,6 1.57 90 23 20 1200
- Iron loss * indicates the iron loss when the magnetic flux density is 1.5 T and the frequency is 50 ⁇ ⁇ .
- Iron loss ** indicates the iron loss when the magnetic flux density is 1.0 ⁇ and the frequency is 4 0 0 ⁇ .
- the deposited oxide film coating powder 1 of the present invention produced in Example 14 is the same as the Mg-containing ferrite oxide-coated Fe—Si-based iron-based soft magnetic powder produced in Conventional Example 12. Compared to the composite soft magnetic material prepared using the material, the density is not much different, but the composite soft magnetic material prepared using the deposited oxide film coating powder 1 of the present invention prepared in Example 14 is Compared with the composite soft magnetic material produced using the conventional Fe-Si based iron-based soft magnetic powder of the Mg-containing ferrite oxide film coated powder of the conventional deposited acid-coated film coated powder, The high coercive force is small and the specific resistance is remarkably high. Therefore, the iron loss is remarkably small. In particular, the higher the frequency, the smaller the iron loss.
- an Fe—Si-based iron-based soft magnetic powder having a particle size shown in Table 25 and containing 1% by mass of Si and comprising 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 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
- the deposited oxide film coated Fe-Si-based iron-based soft magnetic powder obtained by the method of the present invention 71-73 was mixed with a silicone resin added at a mixing ratio of 2% by mass, and the deposited oxide film coated.
- a resin-coated composite powder in which the surface of the Fe-S-based iron-based soft magnetic powder is coated with silicone resin is prepared, and the resin-coated composite powder is placed in a mold heated to 120 ° C and press-molded.
- Molded plate-shaped green compact with dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm and ring-shaped green compact with dimensions of outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm
- the resulting green compact is fired in vacuum at a temperature of 700 ° C for 30 minutes to produce a composite soft magnetic material with plate-like and ring-like fired body strength.
- the specific resistance of the soft 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.
- Table 25 shows the results of the measurement of iron loss when the temperature, coercive force, magnetic flux density is 0.1 T, and frequency is 20 Hz.
- an Fe-Si-based iron-based soft magnetic powder having the particle size shown in Table 25 and containing 1% by mass of Si 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 comprising a ring-shaped fired body was prepared, the specific resistance of the composite soft magnetic material comprising the plate-like fired body was measured, and the results are shown in Table 25.
- the soft magnetic material 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 Hz were measured. The results are shown in Table 25.
- the composite soft magnetic material produced by the inventive method 71-73 has a higher magnetic flux density, a smaller coercive force, and a significantly higher specific resistance.
- the iron loss is remarkably small. In particular, the iron loss decreases as the frequency increases.
- an Fe—Si-based iron-based soft magnetic powder having the particle size shown in Table 26 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 acid film-coated Fe-S-coated iron-based soft magnetic powder obtained by the method of the present invention 74-76 was mixed with a silicone resin at a compounding ratio of 2% by mass and mixed to form a deposited acid film-coated Fe film.
- 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 length: 55mm, width: 10mm, thickness: 5mm and outer diameter: 35mm, inner diameter :
- a ring-shaped green compact with dimensions of 25 mm and height: 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-shaped fired body was prepared, the specific resistance of the composite soft magnetic material made of this plate-like fired body strength was measured, and the results are shown in Table 3. Further, the composite soft magnetic material having a ring-like fired body strength was also obtained.
- Coiled magnetic material was used to measure the magnetic flux density, coercive force, and iron loss at a magnetic flux density of 0.1 T and a frequency of 20 Hz. Table 26 shows the results.
- an Fe-Si-based iron-based soft magnetic powder having a particle size shown in Table 26 and containing 1% by mass of Si 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 comprising a ring-shaped fired body was prepared, the specific resistance of the composite soft magnetic material comprising the plate-like fired body was measured, and the results are shown in Table 25.
- Table 26 shows the magnetic flux density, coercive force, and iron loss when the magnetic flux density is 0.1 T and the frequency is 20 Hz.
- the iron loss * indicates the iron loss when the magnetic flux density is 0.1 T and the frequency is 20 kH ⁇ .
- the composite soft magnetic material produced by the present invention method 74 to 76 has a higher magnetic flux density, a smaller coercive force and a significantly higher specific resistance than the composite soft magnetic material produced by the conventional method 12. For this reason, the iron loss is remarkably small, and in particular, the iron loss decreases as the frequency increases.
- Fe powder having the particle size shown in Table 27 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.
- Deposited oxide film coating Fe-Si based iron-based soft magnetic powder obtained by the method of the present invention 77-79 is added and mixed with a silicone resin at a blending ratio of 2% by mass to deposit acid film coating.
- a resin-coated composite powder in which the surface of the Fe--S iron-based soft magnetic powder was coated with silicone resin 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, outer diameter: 35 mm, Ring-shaped green compact with inner diameter: 25mm, height: 5mm and ring-shaped green compact with outer diameter: 50mm, inner diameter: 25mm, height: 25mm, and obtained green compact was fired in a vacuum at a temperature of 700 ° C for 30 minutes to produce a composite soft magnetic material composed of plate and ring-shaped fired bodies. The specific resistance of the material was measured and the results are shown in Table 27.
- the composite soft magnetic material which has a small-diameter ring-shaped fired body strength, was lined, and the magnetic flux density, coercive force, and magnetic flux density 0.1 T, frequency 20 Hz. The iron loss at that time was measured, and the results are shown in Table 27.
- the small-diameter ring-shaped green compact was measured for inductance at 20kHz when 20A DC was superimposed, and the AC permeability was determined. Table 28 shows the results.
- a wire tuft was applied to the large-diameter ring-shaped powder fired body to produce a rear tuttle in which the inductance was almost constant.
- This rear tuttle was connected to a general switching power supply with an active filter, and the efficiency (%) of the output power relative to the input power of 1000 W and 1500 W was measured. The results are shown in Table 28.
- the composite soft magnetic material having a small-diameter ring-shaped fired body strength is lined, and the magnetic flux density, coercive force, magnetic flux density 0.1 T, frequency The iron loss at 20 Hz was measured, and the results are shown in Table 27.
- the small-diameter ring-shaped green compacts were measured for inductance at 20kHz when DC was superimposed, and the AC permeability was determined. Table 28 shows the results.
- a wire tuft was applied to the large-diameter ring-shaped powder fired body to produce a rear tuttle in which the inductance was almost constant.
- This rear tuttle was connected to a general switching power supply with an active filter, and the efficiency (%) of the output power relative to the input power of 1000 W and 1500 W was measured. The results are shown in Table 28.
- Iron loss * indicates the iron loss when the magnetic flux density is 0.1 T and the frequency is 20 kHz.
- the composite soft magnetic material produced by the inventive method 77-79 is the composite soft magnetic material produced by the conventional method 13. Compared to, the coercive force is small, the specific resistance is remarkably high, so the iron loss is remarkably small. Speak.
- the composite soft magnetic material having high resistance using the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention is characterized by high magnetic flux density and high frequency and low iron loss. It can be used as a material for various vigorous electromagnetic circuit components.
- the electromagnetic circuit component include a magnetic core, an electric motor core, a generator core, a solenoid core, an idling core, a reactor core, a transformer core, a choke coil core, and a magnetic sensor core.
- Electric devices incorporating these electromagnetic circuit components include motors, generators, solenoids, injectors, electromagnetically driven valves, inverters, converters, transformers, relays, magnetic sensor systems, etc. Performance and small and light weight can be achieved.
- Mg-Si-containing oxide-coated soft magnetic powder can be easily produced at low cost.
- a composite soft magnetic material having high specific resistance and excellent mechanical strength can be obtained at low cost by using magnetic powder, and this composite soft magnetic material has characteristics of high magnetic flux density and high frequency and low iron loss. Therefore, it can be used as a material for various electromagnetic circuit components that make use of this feature.
- the various electromagnetic circuit components include a magnetic core, a motor core, a generator core, a solenoid core, an idler core, a rear core, a transformer core, a choke coil core, or a magnetic sensor core, and these electromagnetic circuit components are incorporated.
- Electric equipment includes motors, generators, solenoids, injectors, electromagnetically driven valves, inverters, converters, transformers, relays, magnetic sensor systems, etc., which improve the efficiency, performance, size, and size of electric equipment. be able to.
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Abstract
Description
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CA002578861A CA2578861A1 (en) | 2004-09-06 | 2005-09-06 | Method for producing soft magnetic metal powder coated with mg-containing oxide film and method for producing composite soft magnetic material using said powder |
EP05782230A EP1808242B1 (en) | 2004-09-06 | 2005-09-06 | METHOD FOR PRODUCING SOFT MAGNETIC METAL POWDER COATED WITH Mg-CONTAINING OXIDIZED FILM AND METHOD FOR PRODUCING COMPOSITE SOFT MAGNETIC MATERIAL USING SAID POWDER |
US11/574,655 US20080003126A1 (en) | 2004-09-06 | 2005-09-06 | Method for Producing Soft Magnetic Metal Powder Coated With Mg-Containing Oxide Film and Method for Producing Composite Soft Magnetic Material Using Said Powder |
US13/227,359 US8409371B2 (en) | 2004-09-06 | 2011-09-07 | Method for producing soft magnetic metal powder coated with Mg-containing oxide film |
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JP2005057195A JP4863628B2 (ja) | 2004-09-06 | 2005-03-02 | Mg含有酸化膜被覆軟磁性金属粉末の製造方法およびこの粉末を用いて複合軟磁性材を製造する方法 |
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JP2005156561A JP4863648B2 (ja) | 2004-09-06 | 2005-05-30 | Mg含有酸化膜被覆軟磁性金属粉末の製造方法およびこの粉末を用いて複合軟磁性材を製造する方法 |
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US13/227,359 Division US8409371B2 (en) | 2004-09-06 | 2011-09-07 | Method for producing soft magnetic metal powder coated with Mg-containing oxide film |
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US20080036566A1 (en) | 2006-08-09 | 2008-02-14 | Andrzej Klesyk | Electronic Component And Methods Relating To Same |
JP5227756B2 (ja) * | 2008-01-31 | 2013-07-03 | 本田技研工業株式会社 | 軟磁性材料の製造方法 |
JP4513131B2 (ja) * | 2008-05-23 | 2010-07-28 | 住友電気工業株式会社 | 軟磁性材料の製造方法、および圧粉磁心の製造方法 |
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- 2005-09-06 EP EP05782230A patent/EP1808242B1/en not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
CN101927344A (zh) | 2010-12-29 |
CA2578861A1 (en) | 2006-03-16 |
US20120070567A1 (en) | 2012-03-22 |
EP1808242B1 (en) | 2012-12-26 |
EP1808242A1 (en) | 2007-07-18 |
US8409371B2 (en) | 2013-04-02 |
EP1808242A4 (en) | 2009-07-01 |
KR20070049670A (ko) | 2007-05-11 |
US20080003126A1 (en) | 2008-01-03 |
CN101927344B (zh) | 2013-01-30 |
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