WO2010061525A1

WO2010061525A1 - Method for producing soft magnetic material and method for producing dust core

Info

Publication number: WO2010061525A1
Application number: PCT/JP2009/005635
Authority: WO
Inventors: 草別和嗣; 前田徹
Original assignee: 住友電気工業株式会社
Priority date: 2008-11-26
Filing date: 2009-10-26
Publication date: 2010-06-03
Also published as: EP2359963B1; CN102046310A; EP2359963A4; KR20110089237A; EP2359963A1; CN102046310B

Abstract

Disclosed is a method for efficiently producing a soft magnetic material which comprises a plurality of insulating layers on the surface of a soft magnetic metal particle. Specifically, a soft magnetic material serving as a material for a dust core is produced by: a step of preparing a material powder which is composed of composite magnetic particles, each obtained by forming an insulating coating film having hydrated water on the surface of a soft magnetic metal particle; a step of preparing a resin material containing a silicone which is cured by a hydrolysis-polycondensation reaction; and a step of forming a silicone coating film on the surface of the insulating coating film by mixing the material powder and the resin material in a heating atmosphere of 80-150˚C.

Description

Method for producing soft magnetic material and method for producing dust core

The present invention relates to a method for producing a soft magnetic material which is a material for a dust core, and a method for producing a dust core using the soft magnetic material.

Hybrid vehicles and the like have a booster circuit in the power supply system to the motor. A reactor is used as one component of this booster circuit. The reactor has a configuration in which a coil is wound around a core. When such a reactor is used in an alternating magnetic field, an energy loss called iron loss occurs in the core. The iron loss is generally represented by the sum of hysteresis loss and eddy current loss, and is particularly noticeable when used at high frequencies.

In order to reduce the iron loss, a dust core may be used as the core of the reactor. The dust core is formed by pressing a soft magnetic material composed of composite magnetic particles having an insulating coating formed on the surface of the soft magnetic metal particles, and the metal particles are insulated from each other by the insulating coating. The effect of reducing is high.

However, since the powder magnetic core is manufactured through pressure molding, there is a possibility that the insulating coating of the composite magnetic particles may be damaged by the pressure during the pressure molding. As a result, the soft magnetic metal particles in the dust core come into contact with each other to increase the eddy current loss, and the high frequency characteristics of the dust core may be deteriorated.

In addition, since distortion and transition introduced into the soft magnetic metal particles after the pressure forming cause a increase in hysteresis loss, heat treatment must be performed after the pressure forming, but the insulating coating may be deteriorated. It is difficult to perform heat treatment at high temperature. If the heat treatment temperature is not sufficient, the strain introduced into the metal particles cannot be removed sufficiently, resulting in an increase in hysteresis loss and the high frequency characteristics of the dust core may be degraded.

Therefore, for example, the technique described in Patent Document 1 is formed by forming a multi-layered insulating layer comprising an insulating coating, a heat-resistant protective coating, and a flexible protective coating on the surface of the soft magnetic metal particles. It solves the problems caused by heat treatment. According to the technique of this document, a phosphorus compound, a silicon compound or the like can be used as an insulating coating, an organic silicon compound or the like can be used as a heat-resistant protective coating, and a silicone or the like can be used as a flexible protective coating.

JP 2006-202956 A

However, there is a problem that the process of forming a plurality of insulating layers on the surface of the soft magnetic metal particles is complicated and the productivity of the soft magnetic material is poor.

When forming a plurality of insulating layers, it is fundamental to form the insulating layers sequentially on the surface of the soft magnetic metal particles. For example, in the technique described in Patent Document 1, a wet coating method is cited as a method for forming an insulating layer. The wet coating method is a method of forming an insulating coating on the surface of a coating target by immersing the coating target in an organic solvent in which an insulating material is dissolved, stirring the mixture, evaporating the organic solvent, and then curing. That is, the formation of the insulating coating requires three steps of stirring, evaporation, and curing, so that the productivity of the soft magnetic material is not good.

Also, for example, when a silicone film is selected as the insulating layer to be formed on the coating target, after the coating target and silicone are mixed with a mixer, the condensation polymerization of the silicone is promoted in a heated atmosphere, and the silicone coating is applied to the surface of the coating target. There is also a method of forming. In this case, there are two steps of material mixing and heat treatment. However, considering the formation of a plurality of insulating layers on the surface of the soft magnetic metal particles, it can be said that there are still many production processes.

Therefore, one of the objects of the present invention is to efficiently produce a soft magnetic material having a plurality of insulating layers on the surface of soft magnetic metal particles in order to suppress a decrease in magnetic properties due to pressure molding and heat treatment. The object is to provide a method for producing a soft magnetic material.

Another object of the present invention is to provide a method for manufacturing a dust core for manufacturing a dust core having excellent high frequency characteristics.

The present inventors paid attention to two insulating layers adjacent to each other in the thickness direction on the surface of the soft magnetic metal particles, and found that the above object can be achieved by limiting the configuration of the two insulating layers. Based on this finding, the present invention is defined below.

The method for producing a soft magnetic material of the present invention is a method for producing a soft magnetic material used for producing a dust core, and includes the following steps.
A step of preparing a material powder made of composite magnetic particles in which an insulating coating having hydration water is formed on the surface of soft magnetic metal particles (hereinafter referred to as step A).
A step of preparing a resin material containing silicone that cures by hydrolysis / condensation reaction (hereinafter referred to as step B).
A step of mixing the material powder and the resin material in a heating atmosphere of 80 to 150 ° C. to form a silicone coating on the surface of the insulating coating (hereinafter referred to as step C).

According to the method for producing a soft magnetic material of the present invention, a soft magnetic material composed of composite magnetic particles in which a surface of a soft magnetic metal particle is covered with a plurality of insulating layers of an insulating coating and a silicone coating can be manufactured efficiently and in a short time. Can do. This is because the hydration water contained in the insulating coating promotes the formation of the silicone coating. The detailed mechanism will be described in detail later.

Moreover, the manufacturing method of this invention powder magnetic core is equipped with the following processes.
A step of press-molding the soft magnetic material produced by the above-described method for producing a soft magnetic material (hereinafter referred to as step D).
A heat treatment step (hereinafter referred to as step E) for removing strain introduced into the soft magnetic metal particles during pressure molding.

According to the method for manufacturing a dust core of the present invention, since the soft magnetic material of the present invention is pressed and molded and then subjected to high-temperature heat treatment, strain and transition introduced into the metal particles of the soft magnetic material during pressurization Can be sufficiently removed. The reason why the heat treatment temperature after pressurization of the soft magnetic material can be increased is because the soft magnetic material made of composite magnetic particles in which the surface of the soft magnetic metal particles is covered with a plurality of insulating layers is used. A dust core from which distortion and the like have been sufficiently removed is excellent in energy efficiency because iron loss is reduced. The powder magnetic core thus obtained can be suitably used as, for example, a reactor core.

Hereinafter, the constituent elements of each step included in the method for producing a soft magnetic material and the method for producing a dust core of the present invention will be described in detail.

≪Process A: Preparation of material powder≫
The material powder to be prepared is a collection of composite magnetic particles having an insulating coating having hydrated water on the surface of soft magnetic metal particles.

As the soft magnetic metal particles, those containing 50% by mass or more of iron are preferable, and examples thereof include pure iron (Fe). In addition, iron alloys such as Fe-Si alloys, Fe-Al alloys, Fe-N alloys, Fe-Ni alloys, Fe-C alloys, Fe-B alloys, Fe-Co alloys, Fe A material selected from the group consisting of -P-based alloys, Fe-Ni-Co-based alloys, and iron Fe-Al-Si can be used. In particular, from the viewpoint of magnetic permeability and magnetic flux density, pure iron in which 99% by mass or more is Fe is preferable.

The average particle diameter of the soft magnetic metal particles is 1 μm or more and 70 μm or less. By setting the average particle size of soft magnetic metal particles to 1 μm or more, the increase in coercive force and hysteresis loss of dust cores made from soft magnetic materials is suppressed without sacrificing the fluidity of soft magnetic materials. it can. Conversely, by setting the average particle size of the soft magnetic metal particles to 70 μm or less, eddy current loss that occurs in a high frequency region of 1 kHz or more can be effectively reduced. The average particle size of the soft magnetic metal particles is more preferably 50 μm or more and 70 μm or less. When the lower limit of the average particle diameter is 50 μm or more, an effect of reducing eddy current loss can be obtained, and the soft magnetic material can be easily handled, and a molded body having a higher density can be obtained. The average particle diameter means a particle diameter of particles in which the sum of masses from particles having a small particle diameter reaches 50% of the total mass in the particle diameter histogram, that is, 50% particle diameter.

Also, the soft magnetic metal particles may have a shape with an aspect ratio of 1.5 to 1.8. Soft magnetic metal particles having an aspect ratio in the above range can increase the demagnetizing factor when a dust core is used, compared with particles having a small aspect ratio (close to 1.0), and have excellent high frequency characteristics. It can be a magnetic core. Moreover, the strength of the dust core can be improved.

The insulating film coated on the surface of the soft magnetic metal particles functions as an insulating layer between the metal particles. By covering the metal particles with an insulating coating, the contact between the metal particles can be suppressed, and the relative magnetic permeability of the molded body can be suppressed. In addition, the presence of the insulating coating can suppress the eddy current from flowing between the metal particles and reduce the eddy current loss of the dust core.

The insulating coating is not particularly limited as long as it contains hydrated water and has excellent insulating properties. For example, phosphate, titanate, or the like can be suitably used as the insulating coating. In particular, since the insulating coating made of phosphate is excellent in deformability, even if soft magnetic metal particles are deformed when a soft magnetic material is pressed to produce a powder magnetic core, it will follow the deformation. Can do. Further, the phosphate coating has high adhesion to iron-based soft magnetic metal particles and is difficult to fall off from the metal particle surface. As the phosphate, a metal phosphate compound such as iron phosphate, manganese phosphate, zinc phosphate, or calcium phosphate can be used. The insulating coating containing hydrated water may be formed in advance using a material containing hydrated water.

The thickness of the insulating coating is preferably 10 nm or more and 1 μm or less. By setting the thickness of the insulating coating to 10 nm or more, it is possible to effectively suppress contact between metal particles and energy loss due to eddy current. Further, by setting the thickness of the insulating coating to 1 μm or less, the ratio of the insulating coating to the composite magnetic particles does not become too large. For this reason, it can prevent that the magnetic flux density of this composite magnetic particle falls remarkably.

The thickness of the insulating coating can be examined as follows. First, the film composition obtained by composition analysis (TEM-EDX: transmission electron microscope energy dispersive X-ray spectroscopy), and the amount obtained from inductively coupled plasma mass (ICP-MS) The equivalent thickness is derived. Then, the film is directly observed with a TEM photograph, and it is confirmed that the order of the equivalent thickness derived earlier is an appropriate value. This definition can also be applied to the thickness of the silicone film described later.

≪Process B: Preparation of resin material≫
The resin material to be prepared is not particularly limited as long as it is a silicone that is cured by a hydrolysis / condensation polymerization reaction. Typically, a compound represented by Si _m (OR) _n (m and n are natural numbers) can be used. OR is a hydrolyzable group, and examples thereof include an alkoxy group, an acetoxy group, a halogen group, an isocyanate group, and a hydroxyl group. In particular, as the resin material, an alkoxy oligomer having a molecular end blocked with an alkoxysilyl group (≡Si—OR) can be suitably used. Examples of the alkoxy group include methoxy, ethoxy, propoxy, isopropoxy, butoxy, sec-butoxy and tert-butoxy. In particular, considering the time for removing the reaction product after hydrolysis, the hydrolysis group is preferably methoxy. These resin materials may be used alone or in combination.

The silicone coating formed by hydrolysis / condensation polymerization of the resin material is excellent in deformability, so that it does not easily crack or crack when the soft magnetic material is pressed, and hardly peels from the surface of the insulating coating. Moreover, since the silicone film is excellent in heat resistance, excellent insulation can be maintained even when the heat treatment temperature after press-molding the soft magnetic material is high.

≪Process C: Mixing of material powder and resin material≫
The mixing of the material powder and the resin material is performed in a heated atmosphere of 80 to 150 ° C. By mixing, the resin material is coated on the surface of the composite magnetic particle. At this time, due to the heating atmosphere, the hydrated water contained in the insulating coating of the composite magnetic particles is released, and the hydrolysis of the resin material is promoted. The removal of hydrated water starts at about 80 ° C., and the higher the temperature, the higher the rate of removal, and the hydrolysis and condensation polymerization reaction of the resin material is promoted. Therefore, the heating atmosphere is preferably 100 to 150 ° C. When the temperature is increased, organic substances generated during hydrolysis / condensation polymerization, for example, methanol can be easily removed if the hydrolysis group is methoxy.

Conventionally, heat treatment is performed after mixing the raw materials, and hydrolysis / condensation polymerization of the resin material is caused to proceed by water molecules contained in the heated atmosphere. Since there is an insulating film that is a source of water molecules directly under the material, hydrolysis / condensation polymerization of the insulating material proceeds in a very short time. For example, in the case of XC96-B0446 manufactured by GE Toshiba Silicone, the heat treatment conditions after mixing were conventionally 150 ° C. × 60 minutes or more (recommended conditions by the resin manufacturer), 80-150 ° C. × 10-30 It can be about minutes. Moreover, since the generation source of water molecules is present in the vicinity of the resin material, the resin material coated on the surface of the insulating coating is surely made into a silicone coating even when mixing in large batches of the order of several tens of kg. be able to.

The ratio of blending the material powder and the resin material can be appropriately selected so as to satisfy the characteristics required for the powder magnetic core to be produced. In particular, if the purpose is to improve the DC superposition characteristics, the ratio of the resin material during mixing, that is, the ratio of the resin material to the total of the material powder and the resin material is 0.5-2. It is preferable to set it as 5 mass%. If the proportion of the resin material is in the range of 0.5 to 2.5% by mass, the entire surface of the composite magnetic particle can be covered with a silicone coating, so that the insulation between the soft magnetic metal particles is improved. be able to. Moreover, since the thickness of the silicone coating film formed can be made thicker than before, the heat treatment temperature after pressure molding can be increased during the production of the dust core described later.

The ratio of the preferable resin material is larger than the ratio of the resin material (about 0.25% by mass) in the conventional soft magnetic material manufacturing method in which mixing and heat treatment are separately performed. The resin material can be blended at this ratio because it promotes the hydrolysis / condensation polymerization reaction of the resin material by blending in a heated atmosphere, and the organic substance generated during this reaction, for example, methanol if the hydrolyzable group is methoxy. This is because it can be easily removed.

The thickness of the silicone coating is preferably 10 nm to 0.2 μm. If it is the silicone film of the thickness of this range, the insulation between soft-magnetic metal particles can be ensured, without a magnetic flux density falling too much.

In addition, a catalyst may be added as a means for promoting the formation of a silicone film in the mixing step. As the catalyst, organic acids such as formic acid, maleic acid, fumaric acid and acetic acid, and inorganic acids such as hydrochloric acid, phosphoric acid, nitric acid, boric acid and sulfuric acid can be used. If the amount of the catalyst added is too large, gelation of the resin material is caused, so an appropriate amount may be selected.

In the case of the soft magnetic material produced as described above, since the surface of the soft magnetic metal particles is covered with the insulating coating and the silicone coating, even if the soft magnetic material is pressed and molded in the subsequent step D, The soft magnetic metal particles hardly come into direct contact with each other. In addition, since the silicone film is formed on the outermost surface of the composite magnetic particle, even if a high-temperature heat treatment is performed in the subsequent step E, the insulating film can be prevented from being thermally decomposed, and the soft magnetic metal particles can be contacted with each other. Can be effectively prevented.

In addition, comparing the conventional soft magnetic material obtained by mixing and heat treatment after mixing the material powder and the resin material, and the soft magnetic material of the present invention obtained by performing the mixing and heat treatment simultaneously, The present inventors have clarified that the soft magnetic material of the present invention is superior in magnetic characteristics when a powder magnetic core is used even if the blending ratio of the resin material is the same. This is presumably because the mixing of the material powder and the resin material and the formation of the silicone film by heat treatment are performed at the same time, so that a silicone film having a relatively uniform thickness is formed.

≪Process D: Pressure molding≫
The pressure molding step can be typically performed by injecting the soft magnetic material obtained in step C into a predetermined-shaped molding die, and pressing and hardening the material. The pressure at this time can be selected as appropriate. For example, in the case of producing a powder magnetic core that becomes a core of a reactor, it is preferably about 900 to 1300 MPa (preferably 960 to 1280 MPa).

≪Process E: Heat treatment≫
The heat treatment is performed in order to remove the distortion or transition introduced into the soft magnetic metal particles in the step D. The higher the heat treatment temperature, the more the strain can be removed. Therefore, the heat treatment temperature is preferably 400 ° C. or higher, particularly 550 ° C. or higher, and more preferably 650 ° C. or higher. From the viewpoint of removing distortion of the metal particles, the upper limit of the heat treatment is about 800 ° C. With such a heat treatment temperature, not only strain can be removed, but also lattice defects such as transition introduced into the metal particles during pressurization can be removed. The reason why the heat treatment temperature can be increased is that the soft magnetic material of the present invention has a silicone film having a relatively high heat resistance. The high heat treatment temperature means that the distortion and transition introduced into the soft magnetic metal particles can be sufficiently removed, so that the hysteresis loss of the dust core can be effectively reduced.

According to the method for producing a soft magnetic material of the present invention, a soft magnetic material having an insulating coating and a silicone coating on the surface of soft magnetic metal particles can be produced with high productivity. In the manufactured soft magnetic material, the surface of the soft magnetic metal particles is covered with an insulating coating and a silicone coating, so that the coating is damaged both during pressure molding and during heat treatment after pressure molding. It is difficult to reduce the insulation.

Further, according to the method for manufacturing a dust core of the present invention, since the heat treatment is performed at a high temperature after the pressure molding, a dust core from which distortion and the like are sufficiently removed can be manufactured. The powder magnetic core from which distortion and the like are removed has little energy loss when used at a high frequency, and thus can exhibit excellent characteristics as a core of a reactor, for example. Further, when this dust core is used as, for example, a core of a reactor, the direct current superimposition characteristics are excellent, so that the core can be made gapless.

It is explanatory drawing of the test method of a DC superimposition characteristic. It is a graph which shows the test result of a direct current | flow superimposition characteristic, Comprising: A horizontal axis | shaft is direct current | flow superimposition electric current (A), and a vertical axis | shaft is an inductance (microH). It is a graph which shows a direct current | flow superimposition characteristic, Comprising: A horizontal axis is an applied magnetic field (Oa), and a vertical axis | shaft is a differential magnetic permeability.

A dust core (prototype material 1, prototype material 2) was produced by the method for producing a dust core of the present invention including the following steps (A) to (E), and the physical properties thereof were measured. Moreover, the dust core (comparative material) was produced with the manufacturing method of the conventional dust core, and the physical characteristic was measured. The physical properties of the prototype material 1, the prototype material 2 and the comparative material were compared.

<Production of Prototype Material 1>
(A) A step of preparing a material powder made of composite magnetic particles in which an insulating coating having hydration water is formed on the surface of soft magnetic metal particles.
(B) A step of preparing a resin material containing silicone that is cured by hydrolysis / condensation polymerization reaction in the presence of water.
(C) A step of mixing a powder material and a resin material in a heated atmosphere at 80 to 150 ° C. to form a silicone coating on the surface of the insulating coating.
(D) A step of pressure-molding a soft magnetic material comprising a silicone film formed on the surface of an insulating film of soft magnetic metal particles.
(E) A heat treatment step for removing strain introduced into the soft magnetic metal particles during pressure molding.

≪Process A≫
An iron powder having a purity of 99.8% or more (average particle diameter of 50 μm, aspect ratio of 1.51) produced by a water atomization method was prepared as soft magnetic metal particles. Then, a phosphate chemical conversion treatment was performed on the surface of the metal particles to form an insulating coating made of iron phosphate containing hydration water in advance, thereby producing composite magnetic particles. The insulating coating substantially covered the entire surface of the soft magnetic metal particles, and the average thickness was 50 nm. Moreover, it was 7.78 in mass% when the hydration water contained in an insulating film was measured by thermal desorption gas analysis. The aggregate of the composite magnetic particles is a material powder for producing a soft magnetic material.

≪Process B≫
As a resin material containing silicone that is cured by hydrolysis / condensation polymerization reaction, TSR116 manufactured by GE Toshiba Silicone Co., Ltd. and XC96-B0446 manufactured by the same company were prepared. These are alkoxy resin type silicone oligomers whose molecular ends are blocked with alkoxysilyl groups (≡Si—R), and the hydrolyzable group (—R) is methoxy. In addition, the order of the process A and the process B is not ask | required.

≪Process C≫
The material powder prepared in step A and the resin material (TSR116, XC96-B0446) prepared in step B were put into a mixer and mixed in a heated atmosphere at 150 ° C. for 10 minutes to obtain a soft magnetic material. Of the materials charged in the mixer, the proportion of TSR116 was 0.75% by mass, and the proportion of XC96-B0446 was 0.5% by mass. The rotation speed of the mixer is 300 rpm. Met.

In this step C, a soft magnetic material in which the surface of the composite magnetic particle was coated with a silicone film was obtained. The average thickness of the silicone film formed on the surface of the composite magnetic particle was 200 nm.

≪Process D≫
The soft magnetic material obtained in step C was poured into a mold having a predetermined shape and subjected to pressure molding by applying a pressure of 960 MPa to obtain a rod-shaped test piece and a ring-shaped test piece. The size of each test piece is as follows.
Bar-shaped test piece: For evaluation of DC superposition characteristics Length 55mm, width 10mm, thickness 7.5mm
Ring-shaped test piece: for evaluation of magnetic properties, outer diameter 34 mm, inner diameter 20 mm, thickness 5 mm

≪Process E≫
The rod-shaped test piece and the ring-shaped test piece obtained in Step D were heat-treated at 600 ° C. for 1 hour in a nitrogen atmosphere. The specimen after the heat treatment is a so-called dust core.

<Production of Prototype Material 2>
The prototype 2 is different from the prototype 1 in the following points. The ratio of the resin material in Step C is 0.25% by mass (the ratio of TSR116 and XC96-B0446 is the same as that of Prototype material 1). In this case, the average thickness of the silicone film was 100 nm.

For this prototype material 2, similarly to the prototype material 1, rod-shaped test pieces and ring-shaped test pieces were prepared, and the DC superposition characteristics and magnetic characteristics were measured in the same manner as the prototype material 1.

<Production of comparative material>
The comparative material is different from the prototype material 1 in the points listed below.
1. The ratio of the resin material in Step C is 0.25% by mass (the ratio of TSR116 to XC96-B0446 is the same as that of the prototype material). In this case, the average thickness of the silicone film was 100 nm.
2. After the material powder and the resin material were mixed for 10 minutes, a silicone film was formed by heat treatment at 150 ° C. for 60 minutes. That is, although the amount of resin material to be cured is small, the total production time of the soft magnetic material is 60 minutes longer than the prototype material. This difference in manufacturing time is expected to become more prominent as more soft magnetic material is manufactured.

For this comparative material, a bar-shaped test piece and a ring-shaped test piece were prepared in the same manner as the prototype materials 1 and 2, and the DC superposition characteristics and the magnetic characteristics were measured in the same manner as the prototype materials 1 and 2.

<Evaluation>
About the prototype materials 1 and 2 produced as mentioned above, and the comparative material, the characteristic value enumerated below was measured. The characteristic values are listed in Table 1 and Table 2 below.

≪Magnetic characteristics≫
A magnetic field of 100 Oe (≈7958 A / m) was applied to the rod-shaped test piece, and the magnetic flux density B100 at that time was measured.

Winding was applied to the ring-shaped test piece to prepare a measuring member for measuring the magnetic properties of the test piece. For this measurement member, using an AC-BH curve tracer, an excitation magnetic flux density Bm: 1 kG (= 0.1 T), an iron loss W1 / 10k at a measurement frequency: 10 kHz, and an excitation magnetic flux density Bm: 2 kG (= 0. 2T), Measurement frequency: Iron loss W2 / 10k (W / kg) at 10 kHz was measured. Further, the frequency curve of iron loss was fitted by the following three formulas by the least square method, and the hysteresis loss coefficient Kh (mWs / kg) and the eddy current loss coefficient Ke (mWs ² / kg) were calculated.
(Iron loss) = (Hysteresis loss) + (Eddy current loss)
(Hysteresis loss) = (Hysteresis loss coefficient) x (Frequency)
(Eddy current loss) = (Eddy current loss coefficient) × (Frequency) ²

Also, the initial permeability μi (H / m) was measured using the measurement member. The initial permeability was measured (evaluated using a DC / AC-BH tracer (Metron Giken Co., Ltd.)).

≪Density≫
The underwater density (g / cm ³ ) of the rod-shaped test piece and the ring-shaped test piece was measured. Both test pieces were confirmed to have the same density.

≪Electric resistance≫
The electrical resistance (Ω) was measured by a four-terminal method using a ring-shaped test piece.

≪DC superposition characteristics≫
As shown in FIG. 1, a direct current superposition test machine in which a core M composed of a rod-shaped test piece and a spacer S were assembled and a coil C was formed around the core M was produced. The number of coil turns in the test machine was 54, the magnetic path length was 220 mm, and the magnetic path cross-sectional area was 75 mm ² . In this testing machine, the gap length interposed in the core M can be changed by the total thickness of the spacers S. In this test, the gap length was changed to 0 mm, 0.6 mm, 1.2 mm, 2.0 mm, 2.8 mm, or 4.0 mm for each testing machine using the core M made of a prototype material. Inductance L (μH) was measured when the DC superposition current for a test machine having a power source was changed from 0 A to 40.0 A. Further, for the testing machine using the core M made of the comparative material, the inductance L (μH) was measured when the gap length was 2.0 mm and the DC superimposed current was changed from 0 A to 40.0 A.

FIG. 2 shows a graph showing inductance values (prototype material 1 and comparative material) with respect to the DC superimposed current measured using the test machine. Here, with respect to the inductance L when the applied current is 0 A, the larger the amount of decrease in the inductance L when the DC superimposed current is larger, the worse the DC superimposed characteristic is.

Furthermore, in order to more clearly evaluate the difference in DC superposition characteristics of each sample, the differential permeability (ΔB / ΔH) of each sample was measured. The differential permeability was calculated based on a measured value obtained by measuring a DC magnetization characteristic in an applied magnetic field 100 Oe using a measurement member in which a winding was wound around a ring-shaped test piece prepared for each sample. FIG. 3 shows the relationship between the applied magnetic field and the differential permeability for the prototype material 1, the prototype material 2, and the comparative material. Here, the smaller the difference between the maximum value and the minimum value of the differential permeability, the better the DC superposition characteristics.

≪Evaluation results≫
From the results of Tables 1 and 2, since the prototype materials 1 and 2 and the comparative material ensure insulation between the composite magnetic particles, the hysteresis loss coefficient Kh and the eddy current loss coefficient Ke are both small, and the iron loss can be kept low. ing. Since the prototype material 2 has an insulating film made of iron phosphate and a silicone film having the same film thickness as that of the comparative material, it has almost the same characteristics as the comparative material. On the other hand, since the prototype material 1 has a thicker silicone film than the comparative material, B100 and μi are lower than the comparative material, and numerical values such as iron loss are high. The numerical values of these prototype materials 1 and 2 and the comparative material are markedly superior to those obtained only by forming a phosphate coating on the surface of the soft magnetic metal particles (data not shown). That is, it can be said that the dust core produced using a soft magnetic material having a phosphate coating and a silicone coating on the surface of the soft magnetic metal particles is excellent in high frequency characteristics.

Next, when the result of FIG. 2 is seen, if the prototype material 1 is used, compared with the comparative material, there is less decrease in inductance when the applied current is changed from 0 A to 40.0 A, and the DC superposition characteristics. It turns out that it is excellent in. This is presumed to be because the silicone film in the prototype 1 is formed relatively uniformly thicker than the comparative material, so that the electrical resistance of the prototype is higher and the magnetic permeability is lower than that of the comparative material. Therefore, when producing the core for reactors using the powder magnetic core provided with the structure like the prototype 1, it is possible to omit the gap for adjusting the inductance.

Furthermore, when the result of FIG. 3 is seen, although the trial material 2 and the comparison material have the same addition amount of the resin material, the direct current superimposition characteristic of the inductance is more stable in the trial material 2 than in the comparison material. You can see that Since the only difference between the prototype material 2 and the comparative material is the method for forming the silicone film, the method for producing the soft magnetic material of the present invention is the conventional method in that the direct current superposition characteristics of the soft magnetic material are improved. It became clear that it was superior to the method. Moreover, it became clear that the prototype material 1 in which the ratio of the resin material in the process C is 1.25% by mass is superior in direct current superposition characteristics as compared with the prototype material 2 in which the ratio is 0.25% by mass.

The embodiment of the present invention is not limited to the above-described embodiment, and can be appropriately changed without departing from the gist of the present invention.

The soft magnetic material produced by the method for producing a soft magnetic material of the present invention can be suitably used for producing a dust core having excellent high frequency characteristics and direct current superposition characteristics.

M Core C Coil S Spacer

Claims

A method for producing a soft magnetic material used for producing a dust core,
Preparing a material powder composed of composite magnetic particles in which an insulating film having hydration water is formed on the surface of soft magnetic metal particles;
A step of preparing a resin material containing silicone that is cured by hydrolysis and condensation polymerization;
And a step of mixing the material powder and the resin material in a heated atmosphere at 80 to 150 ° C. to form a silicone film on the surface of the insulating film.
2. The method for producing a soft magnetic material according to claim 1, wherein a ratio of the resin material in the mixing step is 0.5 to 2.5 mass%.
The method for producing a soft magnetic material according to claim 1, wherein an average particle diameter of the soft magnetic metal particles is 1 µm or more and 70 µm or less.
2. The method for producing a soft magnetic material according to claim 1, wherein the soft magnetic metal particles have an aspect ratio of 1.5 to 1.8.
The method for manufacturing a soft magnetic material according to claim 1, wherein the insulating coating is a phosphate coating.
A step of pressure-molding the soft magnetic material produced by the method of producing a soft magnetic material according to claim 1;
And a heat treatment step for removing strain introduced into the soft magnetic metal particles during the pressure forming.