JP4723442B2 - Powder cores and iron-based powders for dust cores - Google Patents

Description

  The present invention compacts soft magnetic iron-based powders such as iron powder and iron-based alloy powders (hereinafter collectively referred to as iron-based powders) to produce a dust core for electromagnetic parts. The present invention relates to an iron-based powder for a dust core used in the process.

  For magnetic cores (core materials) of electromagnetic parts (such as motors) used in alternating current, conventionally laminated magnetic steel sheets and electric iron sheets have been used, but in recent years, soft magnetic iron-based powders have been used. Dust-molded powder magnetic cores have come to be used. This dust core is manufactured by pouring soft magnetic iron-based powder into a mold, compacting it, and then strain relief annealing. By compacting the iron-based powder, the degree of freedom in shape increases, and even a three-dimensional magnetic core can be easily manufactured. Therefore, the electromagnetic component can be made smaller or lighter than using a magnetic core in which electromagnetic steel plates, electric iron plates or the like are laminated.

  For example, Patent Documents 1 and 2 are known as techniques for producing such iron-based powders. In these documents, in order to provide raw material iron powder for a magnetic powder compact having magnetic properties equivalent to or better than electrolytic iron powder, in addition to the chemical composition of iron powder, the apparent density and particle thickness of iron powder, It is disclosed that the particle size distribution, the green density, the ferrite particle size and the like are defined.

  By the way, when producing a powder magnetic core from iron-based powder, the ease of flow when iron-based powder is poured into a mold (fluidity) and the filling property when iron-based powder is poured into a mold are good. It is hoped that. This is because the fluidity and fillability greatly affect the production efficiency. However, in Patent Documents 1 and 2, priority is given to improving magnetic characteristics by flattening, and fluidity and filling properties of iron-based powders are not considered, and production efficiency is poor. Further, the anisotropy of the dust core due to the anisotropy of the iron powder shape due to flattening was not taken into consideration.

  Such a powder magnetic core exhibits good electromagnetic conversion characteristics in a high frequency band of, for example, 1 kHz or more. However, in general, a driving condition in which a motor is operating [for example, a driving frequency is several hundred Hz to 1 kHz and a driving magnetic flux is 1 T (Tesla). )]], The electromagnetic conversion characteristics tend to deteriorate. This deterioration of electromagnetic conversion characteristics [that is, energy loss during magnetic conversion (iron loss)] is the sum of hysteresis loss and eddy current loss if the change in magnetic flux in the material is not accompanied by a relaxation phenomenon (such as magnetic resonance). (For example, refer nonpatent literature 1).

  Of these, it is known that the hysteresis loss is affected by the strain introduced during the production of the raw material powder and during the compacting. Therefore, if strain relief annealing is performed after compacting, the introduced strain is released and hysteresis loss can be reduced.

On the other hand, eddy current loss is Joule loss of induced current accompanying electromotive force generated by electromagnetic induction with respect to magnetic field change. This eddy current loss is considered to be proportional to the magnetic field change rate, that is, the square of the frequency, and the eddy current loss increases as the electric resistance of the dust core decreases and as the range through which the eddy current flows increases. This eddy current is roughly classified into an intraparticle eddy current flowing in individual iron-based powder particles and an interparticle eddy current flowing between iron-based powder particles. Therefore, if the electrical insulation of each iron-based powder is complete, no inter-particle eddy current is generated, so that only intra-particle eddy current is generated, and eddy current loss can be reduced.
JP-A-61-223101 JP-A-62-137812 “SEI Technical Review No. 166”, published by Sumitomo Electric Industries, Ltd., March 2005, p. 1-6

  The present invention has been made in view of such circumstances, and the purpose thereof is to improve the production efficiency by improving the fluidity and filling properties of the iron-based powder. Is to provide. Another object of the present invention is to provide an iron-based powder with an insulating film that has high production efficiency and can reduce eddy current loss when compacted into a powder magnetic core. Another object of the present invention is to provide an iron-based powder with an insulating film that has high production efficiency and can reduce iron loss when a dust core is formed by dust molding. Another object of the present invention is to provide a dust core obtained by molding such an iron-based powder with an insulating film.

  The inventors of the present invention have repeatedly studied to increase the production efficiency by improving the fluidity when pouring the iron-based powder into a mold and the filling property when filling the mold with the iron-based powder. As a result, it has been found that the shape and particle size of the iron-based powder may be appropriately controlled. Also, in order to reduce eddy current loss and iron loss when this iron-based powder is compacted into a powder magnetic core, the type of insulating film formed on the surface of the iron-based powder may be specified. The headline and the present invention were completed.

  That is, the iron-based powder for a dust core according to the present invention that has solved the above-mentioned problems is an average aspect ratio of 3 to 10 and passes when sieving using a sieve having an opening of 250 μm. The point is that the content is 95% by mass or more.

  It is preferable that an insulating film is formed on the surface of the iron-based powder, and the insulating film is, for example, a phosphoric acid-based chemical film. This phosphoric acid-based chemical film preferably contains one or more elements selected from the group consisting of Na, S, Si, W and Co. It is preferable that a silicone resin film is further formed on the surface of the phosphoric acid-based chemical film. The present invention includes a dust core obtained by molding the iron-based powder.

  According to the present invention, since the shape and particle size of the iron-based powder are appropriately controlled, the fluidity of the iron-based powder and the filling property when the iron-based powder is filled in the mold can be improved. , Can increase production efficiency. Further, according to the present invention, since the type of the insulating film formed on the surface of the iron-based powder is specified, the dust core obtained by compacting the iron-based powder with the insulating film has an eddy current loss. And iron loss is reduced.

  In order to improve the fluidity of the iron-based powder and the filling property when the iron-based powder is filled in the mold, the average aspect ratio of the iron-based powder is controlled to 3 to 10 and a sieve having an opening of 250 μm is used. And adjusted so that the passing amount when sieving is 95% by mass or more.

  Regarding the average aspect ratio of the iron-based powder, when the average aspect ratio is less than 3, the shape of the iron-based powder becomes nearly spherical and the flowability is improved, but the apparent aspect when the iron-based powder is filled in the mold is apparent. Since the density is reduced, the filling property is deteriorated. Therefore, production efficiency cannot be increased. The average aspect ratio of the iron-based powder is preferably 3.5 or more, more preferably 4 or more. However, if the average aspect ratio exceeds 10, the degree of flatness of the iron-based powder becomes too large, resulting in poor fluidity, and the apparent density when the iron-based powder is filled in the mold becomes small, so the filling property is low. Deteriorate.

  Also, if the iron-based powder is too flat and the anisotropy increases, the length of the powder is aligned in the direction perpendicular to the compression direction at the time of compacting, so the dust core is in the direction perpendicular to the compression axis. However, the permeability in the compression direction is reduced. Thus, the difference in permeability is caused by the fact that as the anisotropy of the iron-based powder increases, the longitudinal demagnetizing force generated in the iron-based powder decreases, so that the magnetic flux easily flows and the permeability increases. Because it becomes. Therefore, in the dust core formed by compacting iron-based powder, when the powder is thin and flattened like a thin disk, the magnetic permeability in the compression axis direction of the dust core is compressed. Since the magnetic properties of the dust core are smaller than the magnetic permeability in the plane direction, the magnetic core constituting the three-dimensional magnetic circuit [for example, a motor core (for example, rotor, stator, etc.)] Since anisotropy occurs in the magnetic permeability inside the dust core, the physical properties of the entire dust core are difficult to predict and are difficult to put into practical use. On the other hand, since the average aspect ratio of the iron-based powder of the present invention is 10 or less, the iron-based powder can be suitably used for a dust core constituting a three-dimensional magnetic circuit. The average aspect ratio of the iron-based powder is preferably 9 or less, more preferably 8 or less.

  As will be described later, the aspect ratio can be controlled by changing conditions during flattening (for example, flattening time).

  The aspect ratio means the ratio of the major axis to the minor axis (major axis / minor axis) and can be measured, for example, by the following procedure. First, in accordance with “Metal powder sieving analysis test method” (JPMA P02-1992) defined by the Japan Powder Metallurgy Industry Association, sieves with openings of 250 μm, 180 μm, 150 μm, 106 μm, 75 μm, 63 μm, and 45 μm are used. The particle size is less than 45 μm, 45 μm to less than 63 μm, 63 μm to less than 75 μm, 75 μm to less than 106 μm, 106 μm to less than 150 μm, 150 μm to less than 180 μm, 180 μm to less than 250 μm, 250 μm or more. Remove iron-based powder of 250 μm or more. Next, randomly from each powder group having a particle size of less than 45 μm, 45 μm to less than 63 μm, 63 μm to less than 75 μm, 75 μm to less than 106 μm, 106 μm to less than 150 μm, 150 μm to less than 180 μm, 180 μm to less than 250 μm Ten powders are collected, and the aspect ratio (major axis / minor axis) of these 70 powders is observed and measured at 100 to 200 times using a microscope [for example, a scanning electron microscope (SEM)]. The average of the measurement results is taken as the average aspect ratio. The major axis means the equivalent diameter of the circumscribed circle of the powder (maximum length of the powder), and the minor axis means the thickness of the powder in the direction perpendicular to the major axis direction of the powder (maximum length direction of the powder). To do.

  The iron-based powder of the present invention has an average aspect ratio of 3 to 10, and has a passage of 99% by mass or more when sieved using a sieve having an opening of 250 μm (60 mesh). That is, sieving is performed using a sieve having an opening of 250 μm (60 mesh), and the powder remaining on the sieve is removed. By removing the powder having a particle diameter of 250 μm or more and increasing the powder having a particle diameter of less than 250 μm, in combination with the aspect ratio, the apparent density when the iron-based powder is filled in the mold can be increased. The filling property into the mold can be improved.

  In the present invention, it is preferable that the amount of passage when sieving using a sieve having an opening of 150 μm (100 mesh) is 80% by mass or more. In addition, you may remove the passage part when sieving using the sieve of opening 45micrometer (325 mesh).

  As described above, the iron-based powder of the present invention can improve the fluidity and filling properties of the iron-based powder by appropriately controlling the shape and particle size of the iron-based powder, thereby increasing the production efficiency. be able to.

  In order to reduce the eddy current loss of the powder magnetic core obtained by compacting such iron-based powder, when the iron-based powder is compacted, an insulator is present at the interface between the iron-based powders. Just do it. In order for the insulator to be present at the interface between the iron-based powders, for example, a powder obtained by compacting a laminate of an insulating film on the surface of the iron-based powder or a mixture of the iron-based powder and the insulating powder is used. What is necessary is just to compact. Preferably, the iron-based powder is formed by laminating an insulating film on the surface.

  The kind of the insulating film or the insulating powder is not particularly limited, and a known one can be used. For example, when the specific resistance of the molded body is measured by a four-terminal method, the specific resistance is about 50 μΩ · m or more. If it becomes what.

  As a material for the insulating film, for example, an inorganic substance such as a phosphoric acid-based chemical film or a chromium-based chemical film or a resin can be used. Examples of the resin include olefin resins such as silicone resin, phenol resin, epoxy resin, phenoxy resin, polyamide resin, polyimide resin, polyphenylene sulfide resin, styrene resin, acrylic resin, styrene / acrylic resin, ester resin, urethane resin, and polyethylene. Carbonate resins, ketone resins, fluororesins such as fluorinated methacrylate and vinylidene fluoride, engineering plastics such as PEEK, or modified products thereof can be used.

Of these insulating films, a phosphoric acid-based chemical film may be formed. The phosphoric acid-based chemical film is a glassy film formed by chemical conversion treatment with orthophosphoric acid (H ₃ PO ₄ ) or the like, and is excellent in electrical insulation.

  The film thickness of the phosphoric acid-based chemical film is preferably about 1 to 250 nm. This is because if the film thickness is thinner than 1 nm, the insulating effect is hardly exhibited. However, when the film thickness exceeds 250 nm, the insulating effect is saturated, and the density of the green compact is hindered. Speaking of the adhesion amount, about 0.01 to 0.8% by mass is a suitable range.

  The phosphoric acid-based chemical film preferably contains one or more elements selected from the group consisting of Na, S, Si, W and Co. When these elements effectively prevent oxygen in the phosphoric acid-based chemical conversion film from forming Fe and semiconductors during strain relief annealing at high temperatures, and effectively suppress a decrease in specific resistance due to strain relief annealing. It is possible.

  Two or more of these elements may be used in combination. The combination is easy and the thermal stability is excellent in the combination of Si and W, Na, S and Co, and the most preferable is the combination of Na, S and Co.

  In order to suppress a decrease in specific resistance even if strain annealing is performed at a high temperature by adding these elements, P is 0.005 to 1 as an amount in 100% by mass of iron powder after forming the phosphoric acid-based chemical conversion film. Mass%, Na 0.002 to 0.6 mass%, S 0.001 to 0.2 mass%, Si 0.001 to 0.2 mass%, W 0.001 to 0.5 mass% , Co is preferably 0.005 to 0.1% by mass.

  Moreover, Mg and B may be contained in the phosphoric acid system chemical film of this invention. At this time, 0.001-0.5 mass% is suitable for both Mg and B as the amount in 100 mass% of the iron powder after forming the phosphoric acid-based chemical conversion film.

  In the present invention, it is recommended that a silicone resin film is further formed on the surface of the phosphoric acid-based chemical film. The silicone resin film has the effect of improving the mechanical stability of the dust core as well as improving the thermal stability of the electrical insulation. That is, at the end of the crosslinking / curing reaction of the silicone resin (when the green compact is molded), a Si—O bond having excellent heat resistance is formed, resulting in an insulating film having excellent thermal stability. Further, since the powders are firmly bonded to each other, the mechanical strength is increased.

As a silicone resin, since the powder is sticky when the curing is slow and the handling property after film formation is poor, the trifunctionality is less than the bifunctional D unit (R ₂ SiX ₂ : X is a hydrolyzable group). T unit: one (RSiX ₃ X is as defined above) with many are preferred. However, if a large amount of tetrafunctional Q units (SiX ₄ : X is the same as above) is contained, the powders are strongly bound during pre-curing, and the subsequent molding process cannot be performed. It is not preferable. Accordingly, a silicone resin having a T unit of 60 mol% or more is preferable, a silicone resin having 80 mol% or more is more preferable, and a silicone resin having all T units is most preferable.

  As the silicone resin, a methylphenyl silicone resin in which R is a methyl group or a phenyl group is generally used, and heat resistance is higher when there are more phenyl groups.

  However, when one or more elements selected from the group consisting of Na, S, Si, W, and Co are contained in the phosphoric acid-based chemical film, and the strain relief annealing is performed at a high temperature, the presence of the phenyl group is It ’s not very effective. The reason is considered that the bulkiness of the phenyl group disturbs the dense glass network structure, and conversely reduces the thermal stability and the compound formation inhibiting effect with iron. Therefore, when strain relief annealing is performed at a high temperature, it is preferable to use a methylphenyl silicone resin having a methyl group of 50 mol% or more (for example, KR255, KR311, etc., manufactured by Shin-Etsu Chemical Co., Ltd.), and 70 mol% or more (for example, Shinetsu) KR300 manufactured by Chemical Industry Co., Ltd.) is more preferable, and methylsilicone resin having no phenyl group (for example, KR251, KR400, KR220L, KR242A, KR240, KR500, KC89 manufactured by Shin-Etsu Chemical Co., Ltd.) is most preferable. In addition, about the ratio and functionality of the methyl group of a silicone resin, and a phenyl group, it can analyze by FT-IR etc.

  The thickness of the silicone resin film is preferably 1 to 200 nm. A more preferable thickness is 1 to 100 nm. The total thickness of the phosphoric acid-based chemical film and the silicone resin film is preferably 250 nm or less. If it exceeds 250 nm, the decrease in magnetic flux density may become large. In order to reduce the iron loss, it is desirable to form the phosphoric acid-based chemical film thicker than the silicone resin film.

  The adhesion amount of the silicone resin film is adjusted to be 0.05 to 0.3% by mass when the total of the iron-based powder on which the phosphoric acid-based chemical conversion film is formed and the silicone resin film is 100% by mass. It is preferable to do. When it is less than 0.05% by mass, the insulation is inferior and the electrical resistance is lowered. On the other hand, if it is added more than 0.3% by mass, it is difficult to achieve a high density of the molded body.

  In the above, the description has been made centering on the case of compacting the laminate of the insulating film on the surface of the iron-based powder, but the present invention is not limited to this, for example, on the surface of the iron-based powder, A powder obtained by mixing a powder coated with an inorganic material such as a phosphoric acid-based chemical film or a chromium-based chemical film and an insulating powder made of the above resin may be compacted. The blending amount of the resin is preferably about 0.05 to 0.5% by mass with respect to the entire mixed powder.

  The iron-based powder for dust core of the present invention may further contain a lubricant. The action of this lubricant can reduce the frictional resistance between powders when compacting iron-based powders, or between iron-based powders and the inner wall of the mold, and prevent mold galling and heat generation during molding. Can do.

  In order to effectively exhibit such an effect, it is preferable that the lubricant is contained in an amount of 0.2% by mass or more in the total amount of the powder. However, if the amount of lubricant increases, it is against the densification of the green compact, so it is preferable to keep it at 0.8% by mass or less. In the case of compacting, if the lubricant is applied to the inner wall surface of the mold and then molded (mold lubrication molding), the amount of lubricant may be less than 0.2% by mass.

  As the lubricant, conventionally known ones may be used. Specifically, metal stearate powder such as zinc stearate, lithium stearate, calcium stearate, and paraffin, wax, natural or synthetic resin derivatives. Etc.

  The powder-based iron core powder of the present invention is of course used for the production of a powder magnetic core, but the powder magnetic core obtained by molding the powder-based iron core of the present invention is included in the present invention. The This powder magnetic core is mainly used as a core of a rotor, a stator or the like of a motor used mainly in alternating current.

  The iron-based powder of the present invention satisfies the above requirements for the average aspect ratio and the particle size distribution, and its production method is not particularly limited.For example, the raw iron-based powder is subjected to flattening and then reduced, After pulverizing this, it can be manufactured by sieving using a sieve having an opening of 250 μm.

  The raw iron-based powder is a ferromagnetic metal powder. Specific examples include pure iron powder, iron-based alloy powder (Fe-Al alloy, Fe-Si alloy, Sendust, Permalloy, etc.), and amorphous powder. Can be mentioned. Such raw material iron-based powder can be produced, for example, by an atomizing method.

  The raw iron-based powder may be preliminarily classified by sieving using a sieve having an opening of 250 μm to remove the powder remaining on the sieve.

  The flat working may be performed so that the average aspect ratio of the iron-based powder becomes 3 to 10 using, for example, plastic working such as ball mill (for example, vibration ball mill) or attritor rolling.

  The conditions for flattening vary depending on the composition of the iron-based powder and the equipment used, so it cannot be uniformly defined, but the amount of iron-based powder input, the type of ball, the size of the ball, the amount of ball input, The aspect ratio of the iron-based powder can be adjusted by controlling the frequency (number of rotations), flat processing time, amplitude, and the like.

  The flattened powder is reduced by heating in a reducing atmosphere. The reducing conditions are not particularly limited, and heating may be performed at about 800 to 1100 ° C. in a reducing atmosphere (for example, a hydrogen gas atmosphere or a hydrogen gas-containing atmosphere).

  After the reduction, it is crushed and sieved using a sieve having a mesh size of 250 μm in accordance with “Metal powder sieve analysis test method” (JPMA P02-1992) prescribed by the Japan Powder Metallurgy Industry Association. If the remaining powder is removed, the iron-based powder of the present invention can be obtained.

  Next, a method for laminating an insulating film on the iron-based powder of the present invention will be described. In the following, a case where a phosphoric acid-based chemical film and a silicone resin film are laminated on the surface of the iron-based powder in this order as the insulating film will be described.

A solution obtained by dissolving orthophosphoric acid (H ₃ PO ₄ : P source) or the like in an aqueous solvent in order to laminate a phosphoric acid-based chemical conversion film as an insulating film on the surface of the iron-based powder obtained by classification. (Treatment solution) may be mixed with the iron-based powder and dried.

  Further, when the phosphoric acid-based chemical film contains one or more elements selected from the group consisting of Na, S, Si, W and Co, a compound containing the element to be included in the film is included. It can be formed by mixing a solution (treatment liquid) obtained by dissolution with the iron-based powder and drying.

These compounds include Na ₂ HPO ₄ (P and Na sources), Na ₃ [PO ₄ · 12WO ₃ ] · nH ₂ O (P, Na and W sources), Na ₄ [SiW ₁₂ O ₄₀ ] · nH ₂ O. (Na, Si and W sources), Na ₂ WO ₄ .2H ₂ O (Na and W sources), H ₂ SO ₄ (S source), H ₃ PW ₁₂ O ₄₀ .nH ₂ O (P and W sources), SiO ₂ · 12WO ₃ · 26H ₂ O (Si and W sources), MgO (Mg sources), H ₃ BO ₃ (B sources), Co ₃ (PO ₄ ) ₂ (P and Co sources), Co ₃ (PO _{4 2} · 8H ₂ O (P and Co sources) can be used.

  As said aqueous solvent, water, hydrophilic organic solvents, such as alcohol and a ketone, and these mixtures can be used, You may add a well-known surfactant in a solvent as needed.

  In laminating the phosphoric acid-based chemical film, a treatment liquid having a solid content of about 0.1 to 10% by mass is prepared, and about 1 to 10 parts by mass is added to 100 parts by mass of the iron-based powder. Phosphoric acid-based chemical film by mixing with a mixer (eg, mixer, ball mill, kneader, V-type mixer, granulator, etc.) and drying at 150-250 ° C. in the air, under reduced pressure or under vacuum. An iron-based powder in which is formed is obtained.

  When a silicone resin film is further formed on the surface of the phosphoric acid-based chemical film, the silicone resin is dissolved in alcohols, petroleum-based organic solvents such as toluene and xylene, and this solution is mixed with the phosphoric acid-based chemical film. It can form by mixing the iron base iron powder which formed the film | membrane, and volatilizing an organic solvent.

  The film forming conditions are not particularly limited, but the resin solution prepared so that the solid content is about 2 to 10% by mass is 0.5% with respect to 100 parts by mass of the iron-based powder on which the phosphoric acid-based chemical film is formed. About 10 to 10 parts by mass may be added, mixed and dried. If the amount is less than 0.5 parts by mass, mixing takes time, but if it exceeds 10 parts by mass, drying may take time or the film may become non-uniform. The resin solution may be appropriately heated.

  The same mixer as described above can be used. However, when forming a silicone resin film, the organic solvent may be volatilized by heat drying. At the time of drying by heating, for example, it may be heated by an oven or the like, but the mixing container may be heated by warm water or the like. After drying, it is preferable to pass through a sieve having an opening of about 300 μm.

  It is recommended to pre-cure the silicone resin film after drying. By pre-curing the silicone resin and then pulverizing it, a powder having excellent fluidity can be obtained, and it can be put into the mold as sand like sand during compacting. If it is not pre-cured, for example, powders may adhere to each other during warm molding, and it may be difficult to charge the mold in a short time. Pre-curing is very significant for improving handling in actual operation. It has also been found that the specific resistance of the resulting dust core is greatly improved by pre-curing. Although this reason is not clear, it is thought that it may be because the adhesiveness with the iron powder at the time of curing increases.

  Specifically, pre-curing is performed at 100 to 200 ° C. for 5 to 100 minutes. 10-30 minutes is more preferable at 130-170 degreeC. Even after preliminary curing, as described above, it is preferable to pass through a sieve having an opening of about 300 μm.

  Next, in producing a dust core, a powder in which an insulating film is formed on the surface of the iron-based powder (for example, an iron-based powder in which the phosphoric acid-based chemical film is formed, or the surface of the phosphoric acid-based chemical film) Further, an iron-based powder having a silicone resin film formed thereon may be formed and then subjected to strain relief annealing.

  The compacting method is not particularly limited, and a known method can be adopted. The suitable conditions for compacting are 490 to 1960 MPa (more preferably 790 to 1180 MPa) in terms of surface pressure. The molding temperature can be either room temperature molding or warm molding (100 to 250 ° C.). It is preferable to perform warm molding by mold lubrication molding because a high-strength powder magnetic core can be obtained.

  After molding, strain relief annealing is performed to reduce the hysteresis loss of the dust core. The conditions for strain relief annealing are not particularly limited, and known conditions can be applied.

  In particular, when the phosphoric acid-based chemical conversion film contains one or more elements selected from the group consisting of Na, S, Si, W, and Co, the temperature for strain relief annealing may be made higher than before. This can further reduce the hysteresis loss of the dust core. The temperature of strain relief annealing at this time is preferably 400 ° C. or higher, and if there is no deterioration in specific resistance, it is desirable to perform strain relief annealing at a higher temperature.

  The atmosphere for performing strain relief annealing is not particularly limited as long as it does not contain oxygen, but is preferably an inert gas atmosphere such as nitrogen. The time for performing strain relief annealing is not particularly limited, but is preferably 20 minutes or more, more preferably 30 minutes or more, and further preferably 1 hour or more.

  In the above description, the case where the iron-based powder according to the present invention is formed by laminating an insulating film is described. However, the present invention is not limited to this, and phosphoric acid is formed on the surface of the iron-based powder. A powder obtained by mixing a powder coated with an inorganic material such as a chemical conversion coating or a chromium conversion coating and an insulating powder made of the above resin may be compacted.

  Hereinafter, the present invention will be described in more detail with reference to examples. However, the following examples are not intended to limit the present invention, and may be implemented with appropriate modifications within a range that can meet the purpose described above and below. These are all possible and are within the scope of the present invention.

Reference example 1
50 kg of atomized powder “Atomel 300NH” manufactured by Kobe Steel was put into a vibrating ball mill, and the powder was flattened.

  The vibration type ball mill uses the “MB-50 type” made by Chuo Kakoh, and 400 kg of 5/8 inch carbon steel balls are put into it, the frequency is 1200 cpm (times / min), and the amplitude is 8 mm. processed. At this time, the processing time was changed as shown in Table 1 below.

  After flattening, reduction was performed at 970 ° C. for 2 hours in a hydrogen gas atmosphere. After reduction, the pulverized powder is sieved using a sieve having an opening of 250 μm in accordance with “Metal Powder Sieve Analysis Test Method” (JPMA P02-1992) prescribed by the Japan Powder Metallurgy Industry Association. The powder remaining on the top was removed to obtain an iron-based powder.

  About this iron-based powder, using a sieve having an opening of 250 μm, 180 μm, 150 μm, 106 μm, 75 μm, 63 μm, and 45 μm, the particle size is less than 45 μm, 45 μm or more and less than 63 μm, 63 μm or more and less than 75 μm, 75 μm or more and less than 106 μm, 106 μm These were classified into 8 types of less than 150 μm, 150 μm or more and less than 180 μm, 180 μm or more and less than 250 μm, or 250 μm or more. As a result, the amount of passage when sieving using a sieve with an opening of 250 μm (60 mesh) is as shown in Table 1 below, and the passage when sieving using a sieve with an opening of 150 μm (100 mesh) The content was 80% by mass or more.

  Ten powders were randomly collected from each classified powder (excluding powders having a particle size of 250 μm or more), and the shapes of these 70 powders were measured using a scanning electron microscope (SEM). The aspect ratio (major axis / minor axis) was measured by observation at ˜200 times. The average aspect ratio was calculated by averaging the measurement results, and the results are shown in Table 1 below. Further, FIG. 1 shows the relationship between the flat processing time and the average aspect ratio.

  On the other hand, the apparent density, fluidity, and fillability of the iron-based powder were evaluated by the following procedure.

  The apparent density of the iron-based powder was measured in accordance with “Apparent Density Test Method for Metallic Powder” (JPMA P06-1992) defined by the Japan Powder Metallurgy Industry Association. The measurement results and the results evaluated on the basis of the following criteria are shown in Table 1 below. Further, FIG. 2 shows the relationship between the apparent density of the iron-based powder and the average aspect ratio.

[Standard]
◎: apparent density of 3.20g / cm ³ or more ○: apparent density of 3.15g / cm ³ or more and less than 3.20g / cm ³ △: an apparent density of 2.90g / cm ³ or more, 3. 15 g / cm ³ less ×: apparent density less than 2.90 g / cm ³

  The fluidity of the iron-based powder was measured according to “Metal powder fluidity test method” (JPMA P07-1992) prescribed by the Japan Powder Metallurgy Industry Association, and the fluidity of the powder was evaluated. The measurement results and the evaluation results based on the following criteria are shown in Table 1 below. FIG. 3 shows the relationship between the fluidity of the iron-based powder and the average aspect ratio.

[Standard]
◎ (pass): fluidity is 19.0 seconds / 50 g or less ○ (pass): fluidity exceeds 19.0 seconds / 50 g, 22.0 seconds / 50 g or less Δ (failure): fluidity is 22. 0 sec / 50 g and 25.0 sec / 50 g or less x (failed): fluidity exceeds 25.0 sec / 50 g

  The fillability of the iron-based powder was judged by adopting the one with the lower evaluation by comparing the apparent density and the fluidity results. The evaluation results are shown in Table 1 below.

  From Table 1, it can be considered as follows. No. No. 1 is an example in which flat processing is not performed, and the flowability is good because the shape of the iron-based powder is almost spherical, but the apparent density is low, so that the filling property when filling the mold is poor. In contrast, no. In Nos. 2 to 4, since the shape and particle size of the iron-based powder are appropriately controlled, the apparent density is large, the fluidity is improved, and the filling property is improved. On the other hand, no. Nos. 5 to 12 have either poor apparent density or fluidity and poor filling properties.

As apparent from FIG. 2, when the average aspect ratio of the iron-based powder is controlled to 3 to 10, the apparent density becomes 3.2 g / cm ³ or more. As is apparent from FIG. 3, the fluidity can be reduced to 22 seconds / 50 g or less by controlling the average aspect ratio of the iron-based powder to 3 to 10.

Reference example 2
The surface of the iron-based powder (Nos. 1 to 4 in Table 1) shown in Table 1 of Reference Example 1 was subjected to insulation treatment, and this was compacted to obtain a dust core.

  Insulation treatment is performed according to the following procedure: (1) only a silicone resin film is formed, (2) only a phosphoric acid-based chemical film is formed, and (3) a silicone resin film is formed on the surface of the phosphoric acid-based chemical film. did.

[Insulation treatment conditions]
The phosphoric acid-based chemical conversion film comprises 1000 parts of water, 70 parts of H ₃ PO ₄ , 270 parts of sodium phosphate [Na ₃ PO ₄ ], and hydroxylamine sulfate [(NH ₂ OH) ₂ H ₂ SO ₄ ]. A mixture of 70 parts is used as a stock solution, and 50 parts of a treatment liquid diluted 20 times is added to 1000 parts of the powder and mixed for 5 to 60 minutes using a V-type mixer. It dried for 30 minutes and passed through a sieve with an opening of 300 μm. The film thickness of the phosphoric acid-based chemical film was about 50 nm.

  The silicone resin film is prepared by dissolving “KR220L” (100 mol% methyl group, 100 mol% T unit) manufactured by Shin-Etsu Chemical Co., Ltd. in toluene to produce a resin solution having a solid content concentration of 2% by mass. On the other hand, the mixture was added and mixed so that the resin solid content was 0.1%, followed by heating and drying (75 ° C., 30 minutes). That is, the adhesion amount of the silicone resin film is 0.1 mass% in the case of (1) above when the iron-based powder on which the silicone resin film is formed is 100 mass%, and in the case of (3) above, When the total of the iron-based powder on which the acid-based chemical conversion film was formed and the silicone resin film was 100% by mass, it was 0.1% by mass.

  The iron-based powder on which the insulating film was formed was classified by the same method as above using a sieve having an opening of 250 μm, and the powder remaining on the sieve was removed to adjust the particle size. The powder after particle size adjustment was pre-cured (in air, 150 ° C., 30 minutes), and then compacted using this.

In compacting, after applying a pre-cured powder after applying zinc stearate dispersed in alcohol to the mold surface, the surface pressure is 10 ton / cm ² (980 MPa) at room temperature (25 ° C.). Press to form with. The size of the molded body for measuring specific resistance is 31.75 mm × 12.7 mm × thickness of about 5 mm. The density of this molded body is shown in Table 2 below. The shape of the molded body for measuring iron loss was a ring shape having an outer diameter of 45 mm, an inner diameter of 33 mm, and a thickness of about 5 mm, with the primary winding having 400 turns and the secondary winding having 25 turns. The density of this compact is shown in Table 2 below.

  After the dust molding, strain relief annealing was performed at 450 ° C. for 30 minutes in a nitrogen atmosphere to obtain a dust core. The heating rate was about 50 ° C./min, and the furnace was cooled after strain relief annealing.

  The specific resistance of the obtained powder magnetic core was measured by a four-terminal method using a digital multimeter “VOAC-7510” manufactured by Iwasaki Tsushinki Co., Ltd., whose surface was polished with No. 400. The measurement results were evaluated according to the following criteria. The evaluation results are shown in Table 2.

[Standard]
◎: Specific resistance is 100 μΩ · m or more ○: Specific resistance is 50 μΩ · m or more and less than 100 μΩ · m Δ: Specific resistance is 35 μΩ · m or more and less than 50 μΩ · m ×: Specific resistance is less than 35 μΩ · m

  Moreover, the iron loss of the obtained molded body was measured at a frequency of 200 Hz and an excitation magnetic flux density of 1.5 T using an automatic magnetic test apparatus “Y-1807” manufactured by Yokogawa Electric Corporation. The measurement results were evaluated according to the following criteria, and the evaluation results are also shown in Table 2.

[Standard]
◎: Iron loss is 40 W / kg or less ○: Iron loss is more than 40 W / kg, less than 50 W / kg Δ: Iron loss is 50 W / kg or more, less than 60 W / kg ×: Iron loss is 60 W / kg or more

Example 3
The relationship between the composition of the phosphoric acid-based chemical conversion film and the specific resistance was investigated. The surface of the iron-based powder (No. 2) shown in Table 1 of Reference Example 1 was subjected to insulation treatment in the same procedure as in Reference Example 2, and this was compacted to obtain a dust core. In addition, when forming a phosphoric acid type | system | group chemical film, the composition of the phosphoric acid type | system | group chemical film was changed using the stock solution of the composition shown below.

No. Stock solution used in 31 (reference example): 1000 parts of water, 193 parts of H ₃ PO ₄ Stock solution used in No. 32 (reference example): 1000 parts of water, 193 parts of H ₃ PO ₄ , 31 parts of MgO, 30 parts of H ₃ BO ₃ Stock solution used in No. 33 (reference example): 1000 parts of water, 193 parts of H ₃ PO ₄ , 31 parts of MgO, 30 parts of H ₃ BO ₃ , 143 parts of H ₃ PW ₁₂ O ₄₀ .nH ₂ O No . Stock solution used in No. 34: 1000 parts of water, 193 parts of H ₃ PO ₄ , 31 parts of MgO, 30 parts of H ₃ BO ₃ , 143 parts of SiO ₂ · 12WO ₃ · 26H ₂ O 1000 parts of a stock solution ... water used in 35, 270 parts of Na ₂ HPO _4, 70 parts of _{H 3 PO 4, (NH 2} OH) 2 H 2 SO 4 and 70 parts of No. Stock solution used in 36: 1000 parts of water, 70 parts of H ₃ PO ₄ , 270 parts of Na ₃ PO ₄ , 70 parts of (NH ₂ OH) ₂ H ₂ SO ₄ , Co ₃ (PO ₄ ) ₂ · 8H 100 parts of ₂ O

  The specific resistance and iron loss of the obtained dust core were measured under the same conditions as in Reference Example 2 and evaluated in the same manner. The evaluation results are shown in Table 3.

FIG. 1 is a graph showing the relationship between flat processing time and average aspect ratio. FIG. 2 is a graph showing the relationship between the apparent density and the average aspect ratio of the iron-based powder. FIG. 3 is a graph showing the relationship between the fluidity of the iron-based powder and the average aspect ratio.

Claims (4)

Rights are average aspect ratio from 3 to 10, a iron-based powder for dust core passage content is 95 mass% or more when and was sieved using a mesh opening 250μm sieve,
The iron-based powder has an insulating film made of a phosphoric acid-based chemical film on the surface, and
The phosphoric acid-based chemical conversion film contains two or more elements selected from the group consisting of Na, S, Si, W and Co, and has an iron base with an insulating film for a dust core. Powder. The iron-based powder according to claim 1, wherein the phosphoric acid-based chemical conversion film further contains Mg and B. The iron-based powder according to claim 1 or 2 , wherein a silicone resin film is further formed on the surface of the phosphoric acid-based chemical film. A dust core obtained by molding the iron-based powder with an insulating film according to any one of claims 1 to 3 .

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