JP2006241583A - METHOD FOR PRODUCING SOFT MAGNETIC METAL POWDER COATED WITH Mg-CONTAINING OXIDE FILM, AND METHOD FOR PRODUCING COMPOSITE SOFT MAGNETIC MATERIAL FROM THE POWDER - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a soft magnetic metal powder coated with an Mg-containing oxide film and to provide a method for producing a composite soft magnetic material from the soft magnetic metal powder coated with the Mg-containing oxide film. <P>SOLUTION: The soft magnetic metal powder coated with the Mg-containing oxide film is produced by mixing a soft magnetic metal powder heat-treated at 40 to 500°C in an oxidizing atmosphere with an Mg powder, and then heating or heating and tumbling a mixed powder at 150 to 1,100°C in an inert gas or in a vacuum atmosphere under a pressure of 1×10<SP>-12</SP>to 1×10<SP>-1</SP>MPa. The composite soft magnetic material is produced from the soft magnetic metal powder coated with the Mg-containing oxide film. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

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. The magnetic material is used as a material for various electromagnetic circuit components such as a magnetic core, a motor core, a generator core, a solenoid core, an ignition core, a reactor, a transformer, a choke coil core, or a magnetic sensor core.
Furthermore, 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, ignition cores, reactors, transformers, choke coil cores or magnetic sensor cores are required to have low iron loss. It is generally known that high electrical resistance and low coercive force are required. Furthermore, in recent years, since the miniaturization and high response of the electromagnetic circuit have been demanded, higher magnetic flux density is also regarded as important.
As an example of such a magnetic core material made of a soft magnetic material, a laminated steel plate is known in which an insulating layer made of MgO is applied to the surface of a soft magnetic metal plate and laminated (see Patent Document 1). However, although this laminated steel sheet has good magnetic flux density and electrical resistance, it is difficult to produce electromagnetic parts having complicated shapes. To produce electromagnetic parts with complex shapes, a composite soft magnetic metal powder is prepared by coating the surface of the soft magnetic metal powder with a MgO insulating film by a wet method such as chemical plating or coating. A method of producing a fired composite soft magnetic material having MgO as an insulating layer by mixing a soft magnetic metal powder together with an Mg ferrite powder, press forming, and firing is conceivable.

The metal soft magnetic powder includes iron powder, insulated iron powder, Fe-Al iron-based soft magnetic alloy powder, Fe-Ni iron-based soft magnetic alloy powder, Fe-Cr iron-based soft magnetic alloy. Powder, Fe-Si-based iron-based soft magnetic alloy powder, Fe-Si-Al-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 An Fe-P iron-based soft magnetic alloy powder or the like is generally known.
JP 63-226011 A

The method of producing composite soft magnetic metal powder by wet method such as chemical plating or coating with MgO insulating coating on the soft magnetic metal powder is expensive and difficult to mass produce, so the composite soft magnetic metal powder produced by this method is expensive. Thus, the composite soft magnetic material produced using this expensive composite soft magnetic metal powder has a drawback that it is expensive. In addition, since the composite soft magnetic metal powder produced by this method has a MgO insulating film that is more stable than the soft magnetic metal powder, a diffusion reaction hardly occurs 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. When the composite soft magnetic metal powder produced by this wet method is press-molded, the MgO insulating film is broken during press molding. The composite soft magnetic material produced using the composite soft magnetic metal powder produced by this wet method cannot exhibit a sufficient insulating effect, and has a drawback that a sufficiently high resistance cannot be obtained.
On the other hand, 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. The composite soft magnetic material has a structure in which MgO is concentrated at the three grain boundary points of the metal soft magnetic grains, and MgO is less likely to be uniformly dispersed at the grain boundaries. The specific resistance was low.

Then, as a result of conducting research to solve such a problem, the present inventors,
(A) The oxidized soft magnetic metal powder is used as a raw material powder, and the mixed powder obtained by adding and mixing the Mg powder to this raw material powder is temperature: 150 to 1100 ° C., pressure: 1 × 10 ⁻¹² to 1 × When heated in an inert gas atmosphere or vacuum atmosphere of 10 ⁻¹ MPa and further heated in an oxidizing atmosphere at a temperature of 50 to 400 ° C. as necessary, an oxide insulating film containing Mg is formed on the surface of the soft magnetic metal powder. An Mg-containing oxide film-coated soft magnetic metal powder is obtained, and this Mg-containing oxide film-coated soft magnetic metal powder has much higher adhesion than the conventional Mg-containing oxide film-coated soft magnetic metal powder on which an Mg ferrite film is formed. Even if the green powder is made by pressing the Mg-containing oxide film-coated soft magnetic metal powder, the insulating film is less likely to break and peel off. In the composite soft magnetic material obtained by firing the green compact at a temperature of 400 to 1300 ° C., the Mg-containing oxide film is uniformly dispersed at the grain boundaries, and the Mg-containing oxide film is concentrated at the three grain boundary points. To obtain an organization that does not disperse,
(B) 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 temperature: 150 to 1100 ° C., pressure: 1 × 10 ⁻¹² to 1 × In order to heat in an inert gas atmosphere or a vacuum atmosphere of 10 ⁻¹ MPa, it is preferable to heat while rolling the mixed powder.
(C) As said soft magnetic metal powder, generally known iron powder, insulated iron powder, Fe-Al iron-based soft magnetic alloy powder, Fe-Ni 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-Al-based iron-based soft magnetic alloy powder, Fe-Co-based iron-based soft magnetic alloy powder, Fe-Co-V-based iron Research results have been obtained, such as the use of a base soft magnetic alloy powder or an Fe-P iron-based soft magnetic alloy powder.

The present invention was made based on the results of such research,
(1) An oxidized soft magnetic metal powder is used as a raw material powder, and a mixed powder obtained by adding and mixing Mg powder to this raw material powder is temperature: 150 to 1100 ° C., pressure: 1 × 10 ⁻¹² to 1 A method for producing an Mg-containing oxide film-coated composite soft magnetic powder heated in an inert gas atmosphere or a vacuum atmosphere of × 10 ^-1 MPa,
(2) 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 1100 ° C., pressure: 1 × 10 ⁻¹² to 1 A method for producing a Mg-containing oxide film-coated composite soft magnetic powder that is heated while rolling in an inert gas atmosphere or a vacuum atmosphere of × 10 ^-1 MPa,
(3) The oxidation treatment of the soft magnetic metal powder according to (1) or (2) described above is a method for producing an Mg-containing oxide film-coated composite soft magnetic powder that is heat-treated in an oxidizing atmosphere at a temperature of 50 to 500 ° C.
(4) The soft magnetic metal powder is iron powder, insulated iron powder, Fe-Al iron-based soft magnetic alloy powder, Fe-Ni iron-based soft magnetic alloy powder, Fe-Cr iron-based soft magnetic alloy powder. Fe-Si-based iron-based soft magnetic alloy powder, Fe-Si-Al-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 The method for producing an Mg-containing oxide film-coated soft magnetic metal powder according to (1), (2) or (3), which is a P-based iron-based soft magnetic alloy powder,
(5) The Mg-containing oxide film-coated soft magnetic metal powder produced by the method according to (1), (2), (3) or (4) is further heated in an oxidizing atmosphere at a temperature of 50 to 400 ° C. It is characterized by the method for producing the Mg-containing oxide film-coated soft magnetic metal powder.

The raw material powder used in the manufacturing method of the Mg-containing oxide film-coated soft magnetic metal powder of the present invention is an oxidized soft magnetic metal powder, and the present invention uses the oxidized soft magnetic metal powder as an Mg-containing oxide film. It is used as a raw material powder for producing a coated soft magnetic metal powder. Therefore, the present invention
(6) Mg-containing oxide film-coated raw magnetic powder for producing soft magnetic metal powder obtained by oxidizing soft magnetic metal powder,
(7) The soft magnetic metal powder is iron powder, insulated iron powder, Fe-Al iron-based soft magnetic alloy powder, Fe-Ni iron-based soft magnetic alloy powder, Fe-Cr iron-based soft magnetic alloy powder. Fe-Si-based iron-based soft magnetic alloy powder, Fe-Si-Al-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 The raw material powder for producing an Mg-containing oxide film-coated soft magnetic metal powder according to (6), which is a -P-based iron-based soft magnetic alloy powder.

Using the Mg-containing oxide film-coated soft magnetic metal powder produced by the method described in (1), (2), (3), (4) or (5), the specific resistance and mechanical strength are increased by a usual method. An excellent composite soft magnetic material can be produced. Therefore, the present invention
(8) After press-molding the Mg-containing oxide film-coated soft magnetic metal powder produced by the method described in (1), (2), (3), (4) or (5), the temperature is 400 to 1300 ° C. A method for producing a composite soft magnetic material excellent in specific resistance and mechanical strength to be fired
(9) The Mg-containing oxide film-coated soft magnetic metal powder produced by the method described in (1), (2), (3), (4) or (5) above is added to an organic insulating material, an inorganic insulating material, or an organic material. It is characterized by a method for producing a composite soft magnetic material excellent in specific resistance and mechanical strength, in which a mixed material of an insulating material and an inorganic insulating material is mixed and then compacted and fired at 500 to 1000 ° C.

In the manufacturing method of the Mg-containing oxide film-coated soft magnetic metal powder of the present invention, Mg powder is added to the oxidized soft magnetic metal powder and mixed to produce a mixed powder. It is preferable to prepare a mixed powder by adding 0.05 to 2 mass% of the 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 cannot be obtained. On the other hand, if added over 2 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 magnetic flux density of the obtained composite soft magnetic material is lowered, which is not preferable.
The oxidation treatment of the soft magnetic metal powder has the effect of improving the coverage of Mg, and is performed by maintaining the temperature: 50 to 500 ° C. or distilled water or pure water at a temperature of 50 to 100 ° C. in an oxidizing atmosphere. . In this case, it is not efficient when the temperature is less than 50 ° C., and on the other hand, if the temperature exceeds 500 ° C. in an oxidizing atmosphere, firing is not preferable. More preferably, the oxidizing atmosphere is a dry oxidizing atmosphere.
FIG. 1 illustrates a Pann diagram showing a temperature change with time when the soft magnetic metal powder is oxidized. Usually, the oxidation treatment is performed by heating in an oxidizing atmosphere as shown in the pattern shown in FIG. 1 (a). However, the temperature is raised to a low temperature and maintained as shown in FIG. It may be performed in a pattern in which the temperature is raised and held, or may be carried out in a pattern in which the temperature is raised and held at a high temperature and then lowered and held as shown in FIG. As in the pattern shown in FIG. 1 (d), it may be performed in a pattern that is accompanied by a temperature rise and a temperature fall and has substantially no holding. Moreover, in distilled water or pure water, it can carry out by the same pattern by setting the temperature of Fig.1 (a)-(d) to the upper limit of 100 degreeC and the minimum of 50 degreeC. In the manufacturing method of the Mg-containing oxide film-coated soft magnetic metal powder of the present invention, the panning showing the temperature change with respect to time when the soft magnetic metal powder is oxidized is not limited to FIG. It can be freely changed within.

Inert gas atmosphere or vacuum of mixed powder obtained by adding and mixing Mg powder to oxidized soft magnetic metal powder, temperature: 150 to 1100 ° C., pressure: 1 × 10 ⁻¹² to 1 × 10 ⁻¹ MPa Heat in an atmosphere while heating or rolling. Here, the heating atmosphere is an inert gas atmosphere having a pressure of 1 × 10 ⁻¹² to 1 × 10 ⁻¹ MPa or a vacuum atmosphere, and an inert gas atmosphere having a pressure of 1 × 10 ⁻¹² to 1 × 10 ⁻¹ MPa. This is because it includes an atmosphere that can be said to be a high vacuum.
The reason why the heating temperature is set to 150 to 1100 ° C. is that if the temperature is lower than 150 ° C., the pressure needs to be lower than 1 × 10 ⁻¹² MPa, which is industrially difficult and not effective. When the temperature exceeds 1100 ° C., it is not preferable because there is a lot of Mg loss. When the pressure exceeds 1 × 10 ⁻¹ MPa, the coating efficiency of the Mg coating decreases, and the thickness of the formed Mg coating is not uniform. This is because it is not preferable. A more preferable range of the heating temperature of the mixed powder of the soft magnetic metal powder and the Mg powder is 300 to 900 ° C., and a more preferable range of the atmospheric pressure is 1 × 10 ⁻¹⁰ to 1 × 10 ⁻² MPa.
FIG. 2 illustrates a Pann diagram showing a temperature change with time when the oxidized soft magnetic metal powder is heated or rolled while being heated. Usually, it is performed by heating at a constant temperature as in the pattern of FIG. 2 (a), but it may be changed as shown in FIG. 2 (b), and the pattern of FIG. In this pattern, the temperature may be raised to a low temperature and held, and then raised to a high temperature and held. Alternatively, as shown in FIG. It may be performed in a pattern in which the temperature is lowered and held. Furthermore, the pattern shown in FIG. 1A may be repeated a plurality of times like the pattern shown in FIG. Further, as shown in the pattern shown in FIG. 1 (f), the pattern may be held at a high temperature and then held at a low temperature and then held at a high temperature again.
In the manufacturing method of the Mg-containing oxide film-coated soft magnetic metal powder of the present invention, the Pann showing the temperature change with respect to time when heating the oxidized soft magnetic metal powder while heating or rolling is limited to FIG. Instead, it can be freely changed within a range of 150 to 1100 ° C.

  When a mixed powder of soft magnetic metal powder and Mg powder oxidized under such conditions is heated while rolling, an oxide film containing Mg is formed on the surface of the soft magnetic metal powder, and the Mg-containing oxide film-coated soft magnetic metal powder May be formed, but oxidation of Mg may be insufficient. In order to avoid such a situation, the Mg-containing oxide film-coated soft magnetic metal powder obtained by rolling is more preferably heat-treated in an oxidizing atmosphere at a temperature of 50 to 400 ° C., and the temperature is 50 It is not preferable because the sintering starts when heated above 400 ° C. Therefore, the temperature was set to 50 to 400 ° C.

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, insulated iron powder, Fe-Al based iron-based soft powder. 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-Al-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, more specifically,
Iron powder is pure iron powder,
Insulated iron powder is composed of phosphate coated iron powder, or a wet solution such as silica sol-gel solution (silicate) or alumina sol-gel solution. Or aluminum oxide coated iron powder,
The Fe—Al-based iron-based soft magnetic alloy powder contains Al: 0.1-20, and the balance is Fe—Al-based iron-based soft magnetic alloy powder composed of Fe and inevitable impurities (for example, Fe-15% Al). Alpalm powder having a composition),
Fe-Ni-based iron-based soft magnetic alloy powder contains 35% to 85% of Ni: Mo: 5% or less, Cu: 5% or less, Cr: 2% or less, Mn: 0.5% or less as required A nickel-based soft magnetic alloy powder (for example, Fe-49% Ni powder) containing one or more of the above, the balance being Fe and inevitable impurities,
Fe-Cr-based iron-based soft magnetic alloy powder contains Cr: 1 to 20%, optionally contains one or two of Al: 5% or less and Ni: 5% or less, with the balance being Fe-Cr iron-based soft magnetic alloy powder composed of Fe and inevitable impurities,
The Fe—Si-based iron-based soft magnetic alloy powder is a Fe—Si-based iron-based soft magnetic alloy powder containing Si: 0.1 to 10%, the balance being Fe and inevitable impurities,
The Fe—Si—Al-based iron-based soft magnetic alloy powder contains Si: 0.1 to 10%, Al: 0.1 to 20%, and the balance is Fe—Si—Al-based iron composed of Fe and inevitable impurities. Base soft magnetic alloy powder,
The Fe—Co—V iron-based soft magnetic alloy powder contains Co: 0.1 to 52%, V: 0.1 to 3%, and the balance is Fe—Co—V iron containing Fe and inevitable impurities. Base soft magnetic alloy powder,
The Fe—Co-based iron-based soft magnetic alloy powder is an Fe—Co-based iron-based soft magnetic alloy powder containing Co: 0.1 to 52%, the balance being Fe and inevitable impurities,
The 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 unavoidable impurities (above,% indicates mass%). Preferably).

  And as for these soft magnetic metal powder, it is preferable to use the soft magnetic metal powder which exists in the range of average particle diameter: 5-500 micrometers. The reason is that if the average particle size is less than 5 μm, 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 it is larger than 500 μm, the eddy current inside the soft magnetic metal powder increases and the magnetic permeability at high frequency decreases.

In order to produce a composite soft magnetic material using the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention, the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention is used in the usual manner. Can be produced by compacting and sintering with an average particle size: 0.05 to 1% by mass of one or two of silicon oxide and aluminum oxide having a particle size of 0.5 μm or less, and the balance By mixing and mixing so as to consist of the Mg-containing oxide film-coated soft magnetic metal powder prepared by the method of the present invention, a mixed powder is prepared, and this mixed powder is compacted and sintered by a conventional method. Can be produced.
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 its surface, and this Mg-containing oxide film reacts with silicon oxide or aluminum oxide to form a composite oxide. A composite soft magnetic material having a high specific resistance in which a composite oxide having a high resistance is interposed at the grain boundary of the soft magnetic powder, and is sintered through silicon oxide or aluminum oxide. An excellent composite soft magnetic material can be produced. In this case, the coercive force can be kept small from being sintered mainly with silicon oxide or aluminum oxide, and thus a composite soft magnetic material with little hysteresis loss can be produced. It is preferably performed at a temperature of 400 to 1300 ° C. in an active gas atmosphere or an oxidizing gas atmosphere.
In addition, a wet solution such as a silica sol-gel (silicate) solution or an alumina sol-gel solution is added to the Mg-containing oxide film-coated iron powder of the present invention, and the mixture is dried, and the dried mixture is compression-molded and then inert gas. A composite soft magnetic material can be produced by firing at a temperature of 400 to 1300 ° C. in an atmosphere or an oxidizing gas atmosphere.

Further, specific resistance and strength are further improved by mixing organic insulating material, inorganic insulating material, or mixed material of organic insulating material and inorganic insulating material into Mg-containing oxide film-coated soft magnetic metal powder prepared by the method of the present invention. The composite soft magnetic material can be produced. In this case, as the organic insulating material, epoxy resin, fluorine resin, phenol resin, urethane resin, silicone resin, polyester resin, phenoxy resin, urea resin, isocyanate resin, acrylic resin, polyimide resin, PPS resin, or the like can be used. As the inorganic insulating material, phosphates such as iron phosphate, various glassy insulators, water glass mainly composed of sodium silicate, insulating oxides, and the like can be used.
In addition, one or more of boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide is added to B ₂ O ₃ , V in the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention. ₂ O ₅ , Bi ₂ O ₃ , Sb ₂ O ₃ , 0.05 to 1% by mass in terms of MoO ₃ are mixed and mixed, and then compacted, and the resulting compact is obtained at a temperature of 500 to 1000 ° C. A composite soft magnetic material can be produced by sintering with. 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, B ₂ O ₃ , V ₂ O ₅ , Bi ₂ O _3. , Sb ₂ O ₃ , MoO _{3 in} terms of 0.05 to 1% by mass, with the balance being composed of Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention. In this case, the Mg-containing oxide film formed on the surface of the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention and one of boron oxide, vanadium oxide, bismuth oxide, antimony oxide, and molybdenum oxide. A film in which the seeds or two or more kinds are reacted is formed.
Further, this composite soft magnetic material is composed of a boron oxide sol solution or powder, a vanadium oxide sol solution or powder, a bismuth oxide sol solution or powder, an antimony oxide sol solution or powder, and a molybdenum oxide sol solution or powder. 1 to 2 or more of B ₂ O ₃ , V ₂ O ₅ , Bi ₂ O ₃ , Sb ₂ O ₃ , MoO _{3 in} terms of 0.05 to 1% by mass, and the balance being the Mg-containing oxide film of the present invention It mix | blends so that it may become a composition which consists of a covering iron powder, it mixes, the obtained mixed oxide is compacted and shape | molded, Then, it can obtain by sintering at temperature: 500-1000 degreeC.

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. This composite soft magnetic material has high magnetic flux density. Since it has the characteristics of high-frequency and low iron loss, it can be used as a material for various electromagnetic circuit components utilizing this characteristic.

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 has the characteristics of high magnetic flux density and high frequency and low iron loss. It can be used as a material for circuit components. Examples of the electromagnetic circuit component include a magnetic core, a motor core, a generator core, a solenoid core, an ignition core, a reactor, a transformer, 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. Can be made smaller and lighter.
As described above, when a composite soft magnetic material is produced using the Mg-containing oxide film-coated soft magnetic metal powder produced by the method of the present invention, a composite soft magnetic material having excellent specific resistance and mechanical strength can be produced at low cost. It can be obtained and has excellent effects in the electrical and electronic industries.

As the soft magnetic metal powder, all have an average particle size: 70 μm,
Pure iron powder (hereinafter, this pure iron powder is referred to as soft magnetic powder A),
Atomized Fe—Al-based iron-based soft magnetic alloy powder consisting of Al: 10% by mass, balance: Fe (hereinafter, this Fe—Al-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder B),
Atomized Fe—Ni-based iron-based soft magnetic alloy powder consisting of Ni: 49% by mass, balance: Fe (hereinafter, this Fe—Ni-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder C),
Atomized Fe—Cr-based iron-based soft magnetic alloy powder composed of Cr: 10% by mass, balance: Fe (hereinafter, this Fe—Cr-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder D),
Atomized Fe-Si-based iron-based soft magnetic alloy powder composed of Si: 3% by mass, balance: Fe (hereinafter, this atomized Fe-Si-based iron-based soft magnetic alloy powder is referred to as soft magnetic powder E),
Atomized Fe-Si-Al-based iron-based soft magnetic alloy powder containing Si: 3% by mass, Al: 3% and the balance: Fe (hereinafter, this Fe-Si-Al-based iron-based soft magnetic alloy powder is softened) Called magnetic powder F),
Fe: Co-V-based iron-based soft magnetic alloy powder containing Co: 30%, V: 2%, the balance being Fe and inevitable impurities (hereinafter referred to as this Fe-Co-V-based iron-based soft magnetic alloy powder) Soft magnetic powder G),
P: Fe-P-based iron-based soft magnetic alloy powder containing 0.6% and 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),
As insulation-treated iron powder, commercially available phosphate-coated iron powder (hereinafter, this phosphate-coated iron powder is referred to as soft magnetic powder I),
Co: Fe-Co-based iron-based soft magnetic alloy powder containing 30% and 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 J) was prepared. .
Further, Mg powder having an average particle size of 30 μm and Mg ferrite powder having an average particle size of 3 μm were prepared.

Example 1
With respect to soft magnetic powder A (pure iron powder) subjected to oxidation treatment under the conditions shown in Table 1, Mg powder is blended so as to have a blending ratio shown in Table 1, and this blended powder is mixed with argon gas or vacuum. The Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling while maintaining the pressure and temperature shown in Table 1 in the 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: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 1 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was 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 in the present invention methods 1 to 7 and comparative methods 1 to 3 were measured, and the results are shown in Table 1. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 1.

Conventional Example 1
An Mg ferrite powder was blended with the soft magnetic powder A prepared in the example so as to have a blending ratio shown in Table 1, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 1 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 1 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 1 were measured, and the results are shown in Table 1. Further, the composite soft magnetic material made of the ring-like fired body The material was wound, the magnetic flux density was measured with a BH tracer, and the results are shown in Table 1.

  From the results shown in Table 1, the composite soft magnetic materials produced by the inventive methods 1 to 7 are superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 1. I understand that. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 1 to 3 are not preferable because the properties of relative density and magnetic flux density are inferior.

Example 2
With respect to the soft magnetic powder B (Fe—Al-based iron-based soft magnetic alloy powder) subjected to the oxidation treatment under the conditions shown in Table 2, the Mg powder is blended so as to have the blending ratio shown in Table 2, The blended powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 2 to prepare 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 2 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material composed of a sintered product was produced, and the present invention methods 8 to 14 and comparative methods 4 to 6 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 methods 8 to 14 and comparative methods 4 to 6 were measured, and the results are shown in Table 2. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 2.

Conventional example 2
Mg ferrite powder was blended with the soft magnetic powder B prepared in the examples so as to have a blending ratio shown in Table 2, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 2 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 2 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 2 were measured, and the results are shown in Table 2. Further, the composite soft magnetic material made of the ring-like fired body The material was wound, the magnetic flux density was measured with a BH tracer, and the results are shown in Table 2.

  From the results shown in Table 2, the composite soft magnetic material produced by the inventive methods 8 to 14 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 2. I understand that. However, it can be seen that the composite soft magnetic material produced by Comparative Methods 4 to 6 is not preferable because the characteristics of relative density and magnetic flux density are inferior.

Example 3
With respect to soft magnetic powder C (Fe—Ni-based iron-based soft magnetic alloy powder) subjected to oxidation treatment under the conditions shown in Table 3, Mg powder was blended so as to have a blending ratio shown in Table 3, The mixed powder was rolled in an argon gas or a vacuum atmosphere while maintaining the pressure and temperature shown in Table 3 to prepare 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was formed, and the obtained green compact was baked for 30 minutes at a temperature shown in Table 3 in a nitrogen atmosphere. A composite soft magnetic material made of a sintered product was 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 by the present invention methods 15 to 21 and comparative methods 7 to 9 were measured, and the results are shown in Table 3. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 3.

Conventional example 3
An Mg ferrite powder was blended with the soft magnetic powder C prepared in the examples so as to have a blending ratio shown in Table 3, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 3 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A 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 made of the plate-like fired body obtained by the conventional method 3 were measured, and the results are shown in Table 3. Furthermore, the composite soft magnetic material made of the ring-like fired body The material was wound and the magnetic flux density was measured with a BH tracer. The results are shown in Table 3.

  From the results shown in Table 3, the composite soft magnetic material produced by the inventive methods 15 to 21 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 3. I understand that. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 7 to 9 are not preferable because the properties of relative density and magnetic flux density are inferior.

Example 4
With respect to the soft magnetic powder D (Fe—Cr-based iron-based soft magnetic alloy powder) subjected to the oxidation treatment under the conditions shown in Table 4, the Mg powder was blended so as to have the blending ratio shown in Table 4, The blended powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 4 to prepare 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was formed, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 4 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was 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 strength of the composite soft magnetic material comprising the plate-like fired bodies obtained in the present invention methods 22 to 28 and comparative methods 10 to 12 were measured, and the results are shown in Table 4. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 4.

Conventional example 4
An Mg ferrite powder was blended with the soft magnetic powder D prepared in the example so as to have a blending ratio shown in Table 4, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 4 for 30 minutes to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 4 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 4 were measured, and the results are shown in Table 4. Further, the composite soft magnetic material made of the ring-like fired body The material was wound and the magnetic flux density was measured with a BH tracer. The results are shown in Table 4.

  From the results shown in Table 4, the composite soft magnetic material produced by the inventive methods 22 to 28 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 4. I understand that. However, it can be seen that the composite soft magnetic material produced by Comparative Methods 10 to 12 is not preferable because the characteristics of relative density and magnetic flux density are inferior.

Example 5
With respect to the soft magnetic powder E (Fe—Si-based iron-based soft magnetic alloy powder) oxidized under the conditions shown in Table 5, Mg powder was blended so as to have the blending ratio shown in Table 5, and this blended 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was formed, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 5 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was 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 by the present invention methods 29 to 35 and comparative methods 13 to 15 were measured, and the results are shown in Table 5. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 5.

Conventional Example 5
An Mg ferrite powder was blended with the soft magnetic powder E prepared in the examples so as to have a blending ratio shown in Table 5, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 5 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 5 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 5 were measured, and the results are shown in Table 5. Further, the composite soft magnetic material made of the ring-like fired body The material was wound, the magnetic flux density was measured with a BH tracer, and the results are shown in Table 5.

  From the results shown in Table 5, the composite soft magnetic material produced by the inventive methods 29-35 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 5. I understand that. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 13 to 15 are not preferable because the properties of relative density and magnetic flux density are inferior.

Example 6
With respect to soft magnetic powder F (Fe—Si—Al-based iron-based soft magnetic alloy powder) subjected to the oxidation treatment under the conditions shown in Table 6, Mg powder was blended so as to have the blending ratio shown in Table 6. Then, this blended powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 6 to prepare 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 6 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was produced, and the present invention methods 36 to 42 and comparative methods 16 to 18 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 36 to 42 and comparative methods 16 to 18 were measured, and the results are shown in Table 6. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 6.

Conventional Example 6
Mg ferrite powder was blended with the soft magnetic powder F prepared in the examples so as to have a blending ratio shown in Table 6, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 6 for 30 minutes to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 6 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 6 were measured, and the results are shown in Table 6. Further, the composite soft magnetic material made of the ring-like fired body The material was wound and the magnetic flux density was measured with a BH tracer. The results are shown in Table 6.

  From the results shown in Table 6, the composite soft magnetic material produced by the inventive methods 36 to 42 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 6. I understand that. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 16 to 18 are not preferable because the properties of relative density and magnetic flux density are inferior.

Example 7
For the soft magnetic powder G (Fe-Co-V iron-based soft magnetic alloy powder) subjected to the oxidation treatment under the conditions shown in Table 7, the Mg powder is blended so as to have the blending ratio shown in Table 7. Then, this blended powder was rolled in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 7 to prepare 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-shaped green compact having dimensions of length: 55 mm, width: 10 mm, thickness: 5 mm, and outer diameter: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was formed, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 7 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was produced, and the present invention methods 43 to 49 and comparative methods 19 to 21 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 methods 43 to 49 and comparative methods 19 to 21 were measured, and the results are shown in Table 7. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 7.

Conventional Example 7
Mg ferrite powder was blended with the soft magnetic powder G 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 prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 7 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A 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 made of the plate-like fired body obtained by the conventional method 7 were measured, and the results are shown in Table 7. Further, the composite soft magnetic material made of the ring-like fired body The material was wound and the magnetic flux density was measured with a BH tracer. The results are shown in Table 7.

  From the results shown in Table 7, the composite soft magnetic materials produced by the inventive methods 43 to 49 are superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic materials produced by the conventional method 7. I understand that. However, it can be seen that the composite soft magnetic material produced by Comparative Methods 19 to 21 is not preferable because the characteristics of relative density and magnetic flux density are inferior.

Example 8
With respect to soft magnetic powder H (Fe—P-based iron-based soft magnetic alloy powder) subjected to oxidation treatment under the conditions shown in Table 8, Mg powder was blended so as to have the blending ratio shown in Table 8, An Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling the blended powder in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 8.

  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: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 8 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was produced, and the present invention methods 50 to 56 and comparative methods 35 to 39 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 50 to 56 and comparative methods 35 to 39 were measured, and the results are shown in Table 8, A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 8.

Conventional Example 8
An Mg ferrite powder was blended with the soft magnetic powder H prepared in the examples so as to have a blending ratio shown in Table 8, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired for 30 minutes at a temperature shown in Table 8 in a nitrogen atmosphere to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 8 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 8 were measured, and the results are shown in Table 8. Further, the composite soft magnetic material made of the ring-like fired body was used. The material was wound, the magnetic flux density was measured with a BH tracer, and the results are shown in Table 8.

  From the results shown in Table 8, the composite soft magnetic material produced by the inventive method 50-56 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 8. I understand that. However, it can be seen that the composite soft magnetic materials produced by Comparative Methods 22 to 24 are not preferable because the properties of relative density and magnetic flux density are inferior.

Example 9
With respect to soft magnetic powder I (phosphate coated iron powder) subjected to the oxidation treatment shown in Table 9, Mg powder was blended so as to have the blending ratio shown in Table 9, and this blended powder was mixed with argon. 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 gas or 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: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 9 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was produced, and the present invention methods 57 to 63 and 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 in the present invention methods 57 to 63 and comparative methods 25 to 27 were measured, and the results are shown in Table 9. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 9.

Conventional Example 9
An 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 9, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 9 for 30 minutes to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 9 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 9 were measured, and the results are shown in Table 9. Further, the composite soft magnetic material made of the ring-like fired body The material was wound and the magnetic flux density was measured with a BH tracer. The results are shown in Table 9.

  From the results shown in Table 9, the composite soft magnetic material produced by the inventive method 57 to 63 is superior in both bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 9. I understand that. However, it can be seen that the composite soft magnetic material produced by the comparative methods 25 to 27 is not preferable because the characteristics of relative density and magnetic flux density are inferior.

Example 10
For the soft magnetic powder J (Fe—Co based iron-based soft magnetic alloy powder) subjected to the oxidation treatment under the conditions shown in Table 10, the Mg powder was blended so as to have the blending ratio shown in Table 10, An Mg-containing oxide film-coated soft magnetic metal powder was produced by rolling the blended powder in an argon gas or vacuum atmosphere while maintaining the pressure and temperature shown in Table 10.

  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: 35 mm, inner diameter. A ring-shaped green compact having a size of 25 mm and a height of 5 mm was formed, and the obtained green compact was fired in a nitrogen atmosphere at a temperature shown in Table 10 for 30 minutes to obtain a plate and a ring. A composite soft magnetic material made of a sintered product was produced, and the present invention methods 64-70 and comparative methods 28-30 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 10. A composite soft magnetic material made of a ring-shaped fired body was wound, and the magnetic flux density was measured with a BH tracer. The results are shown in Table 10.

Conventional Example 10
An Mg ferrite powder was blended with the soft magnetic powder J prepared in the example so as to have a blending ratio shown in Table 10, and the blended powder was stirred while rolling in the atmosphere to prepare a mixed powder. The obtained mixed powder is 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, outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm. A ring-shaped green compact having the following dimensions is molded, and the obtained green compact is fired in a nitrogen atmosphere at a temperature shown in Table 10 for 30 minutes to obtain a composite soft material composed of a plate-shaped and ring-shaped fired body. A magnetic material was prepared and the conventional method 10 was performed. The relative density, specific resistance, and bending strength of the composite soft magnetic material made of the plate-like fired body obtained by the conventional method 10 were measured, and the results are shown in Table 10. Further, the composite soft magnetic material made of the ring-like fired body was used. The material was wound, the magnetic flux density was measured with a BH tracer, and the results are shown in Table 10.

  From the results shown in Table 10, the composite soft magnetic material produced by the method of the present invention 64-70 is superior in bending strength, magnetic flux density and specific resistance compared to the composite soft magnetic material produced by the conventional method 10. I understand that. However, it can be seen that the composite soft magnetic material produced by the comparative methods 28 to 30 is not preferable because the characteristics of relative density and magnetic flux density are inferior.

It is a Pann figure which shows the temperature change with respect to time at the time of oxidizing a soft magnetic metal powder. It is a Pann figure which shows the temperature change with respect to time at the time of heating, heating or rolling the oxidized soft magnetic metal powder.

Claims (13)

An oxidized soft magnetic metal powder is used as a raw material powder, and a mixed powder obtained by adding and mixing Mg powder to the raw material powder is mixed at a temperature of 150 to 1100 ° C. and a pressure of 1 × 10 ⁻¹² to 1 × 10 ^{−. A} method for producing a Mg-containing oxide film-coated soft magnetic metal powder, characterized by heating in an inert gas atmosphere or a vacuum atmosphere of ¹ MPa. An oxidized soft magnetic metal powder is used as a raw material powder, and a mixed powder obtained by adding and mixing Mg powder to the raw material powder is mixed at a temperature of 150 to 1100 ° C. and a pressure of 1 × 10 ⁻¹² to 1 × 10 ^{−. A} method for producing an Mg-containing oxide film-coated soft magnetic metal powder, which is heated while rolling in an inert gas atmosphere or a vacuum atmosphere of ¹ MPa. The oxidation treatment of the soft magnetic metal powder according to claim 1 or 2, wherein the soft magnetic metal powder is heat-treated in an oxidizing atmosphere at a temperature of 50 to 500 ° C. Production method. The soft magnetic metal powder includes iron powder, insulated iron powder, Fe—Al iron-based soft magnetic alloy powder, Fe—Ni iron-based soft magnetic alloy powder, Fe—Cr iron-based soft magnetic alloy powder, Fe— Si-based iron-based soft magnetic alloy powder, Fe-Si-Al-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 4. The method for producing a Mg-containing oxide film-coated soft magnetic metal powder according to claim 1, 2, or 3, wherein the powder is an iron-based soft magnetic alloy powder. An Mg-containing oxide film coating characterized by further heating the Mg-containing oxide film-coated soft magnetic metal powder produced by the method according to claim 1, in an oxidizing atmosphere at a temperature of 50 to 400 ° C. Method for producing soft magnetic metal powder. A raw material powder for producing an Mg-containing oxide film-coated soft magnetic metal powder, characterized by oxidizing a soft magnetic metal powder. The soft magnetic metal powder includes iron powder, insulated iron powder, Fe—Al iron-based soft magnetic alloy powder, Fe—Ni iron-based soft magnetic alloy powder, Fe—Cr iron-based soft magnetic alloy powder, Fe— Si-based iron-based soft magnetic alloy powder, Fe-Si-Al-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 The raw material powder for producing an Mg-containing oxide film-coated soft magnetic metal powder according to claim 6, which is an iron-based soft magnetic alloy powder. A specific resistance and mechanical property, characterized in that the Mg-containing oxide film-coated soft magnetic metal powder produced by the method according to claim 1, 2 is calcined at a temperature of 400 to 1300 ° C. after press molding. A method for producing a composite soft magnetic material having excellent strength. An organic insulating material, an inorganic insulating material, or a mixed material of an organic insulating material and an inorganic insulating material is mixed with the Mg-containing oxide film-coated soft magnetic metal powder produced by the method according to claim 1, 2, 3, 4, or 5. A method for producing a composite soft magnetic material excellent in specific resistance and mechanical strength, which is then compacted and fired at 500 to 1000 ° C. A composite soft magnetic material excellent in specific resistance and mechanical strength produced by the method according to claim 8. An electromagnetic circuit component comprising the composite soft magnetic material according to claim 10. The electromagnetic circuit component according to claim 11, wherein the electromagnetic circuit component is a magnetic core, a motor core, a generator core, a solenoid core, an ignition core, a reactor, a transformer, a choke coil core, or a magnetic sensor core. An electric device incorporating the electromagnetic circuit component according to claim 11.

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