WO2013108643A1 - Corps de poudre magnétique doux comprimé - Google Patents

Corps de poudre magnétique doux comprimé Download PDF

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WO2013108643A1
WO2013108643A1 PCT/JP2013/050033 JP2013050033W WO2013108643A1 WO 2013108643 A1 WO2013108643 A1 WO 2013108643A1 JP 2013050033 W JP2013050033 W JP 2013050033W WO 2013108643 A1 WO2013108643 A1 WO 2013108643A1
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powder
soft magnetic
magnetic material
iron
oxidation
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PCT/JP2013/050033
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English (en)
Japanese (ja)
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和也 西
青野　泰久
憲一 相馬
今川　尊雄
北条　啓文
友綱 上條
大脇　武史
三谷　宏幸
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株式会社日立産機システム
株式会社神戸製鋼所
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Publication of WO2013108643A1 publication Critical patent/WO2013108643A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/33—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F3/00—Cores, Yokes, or armatures
    • H01F3/08—Cores, Yokes, or armatures made from powder

Definitions

  • the present invention relates to a powder soft magnetic material produced by compression molding soft magnetic powder.
  • a powder soft magnetic material produced by compression molding soft magnetic powder represented by iron powder or the like at a high pressure is used for a magnetic core of a motor, a reactor for a power supply circuit, or the like.
  • the advantage of dust cores is that the magnetic properties are isotropic and the fabrication of three-dimensional shaped cores is easy. For this reason, when applied to a motor such as a motor core, the dust core is expected to contribute to downsizing and weight reduction of the motor as compared with a laminated core manufactured by laminating silicon steel plates.
  • a powder soft magnetic material using pure iron as soft magnetic powder is inexpensive and has high ductility of iron powder and high density of magnetic material, and has an advantage of increasing magnetic flux density. Development towards the target has been activated.
  • iron loss In addition to the high magnetic flux density, it is important that the energy loss due to heat generation under the fluctuation of an alternating magnetic field called iron loss is small as the characteristics required for the powder magnetic soft magnetic material.
  • Iron loss is mainly represented by the sum of eddy current loss and hysteresis loss.
  • the cause of the eddy current loss is the heat generated by the eddy current flowing between the particles of iron powder constituting the powder soft magnetic material.
  • the cause of the hysteresis loss is heat generation caused by the movement of the domain wall inside the iron powder.
  • Hysteresis loss is lattice distortion inside iron powder, that is, vacancies that are structural defects that generate distortion, interstitial atoms, dislocations, lattice defects such as dislocations and grain boundaries, and impurities atoms other than Fe and precipitates composed of them. It is strongly influenced by To reduce hysteresis loss, it is necessary to perform heat treatment on the soft magnetic material after compression molding in order to reduce distortion inside iron powder introduced by molding.
  • strain reduction heat treatment Heat treatment of a molded body for the purpose of strain reduction (hereinafter, referred to as “strain reduction heat treatment”) is generally performed in an inert gas atmosphere such as nitrogen gas in many cases.
  • an inert gas atmosphere such as nitrogen gas
  • the insulating film on the powder surface constituting the powder soft magnetic material is partially destroyed to increase the eddy current loss, or the inside of the iron powder
  • the iron loss increases due to the diffusion of oxygen to the metal and the increase in hysteresis loss.
  • the strain reduction heat treatment in the air which does not require atmosphere control can simplify the heat treatment equipment and shorten the treatment time, and is advantageous from the viewpoint of reducing the process cost in manufacturing.
  • the compacted soft magnetic material is subjected to heat treatment in a high temperature atmosphere at 500 ° C. or higher, there is a problem that the iron loss is increased due to the above-mentioned oxidation.
  • Patent Documents 1 and 2 disclose a technology in which iron powder coated with a phosphoric acid inorganic insulating layer on its surface is mixed with an organic lubricant, compacted, and heat-treated in an oxidizing atmosphere.
  • Patent Literatures 1 and 2 describe heat treatment in a steam atmosphere at 300 to 600 ° C. for the purpose of strengthening, and prior to this heat treatment, Patent Literature 1 is performed at 250 to 550 ° C. in the air.
  • heat treatment in an inert gas at 500 ° C. or lower or in the air is carried out for the purpose of removing the lubricant of the compact.
  • the phosphoric acid inorganic insulating layer used here has high adhesion and is excellent in the deformation followability of the powder surface at the time of molding, but has a disadvantage that the oxidation resistance in a high temperature oxidizing atmosphere is low.
  • the iron powder surface is easily oxidized after the heat treatment in an oxidizing atmosphere such as air or water vapor, the insulating layer is destroyed, and the iron loss increases.
  • An object of the present invention is to provide a powder soft magnetic material having excellent magnetic properties without an increase in iron loss.
  • the powder soft magnetic material according to the present invention has the following features.
  • an oxidation-influenced layer which is a layer containing an iron oxide and a layered Si oxide, is formed at the boundary between the iron powders (iron powder interface).
  • FIG. 1 It is a cross-sectional schematic diagram of the powder-powder soft-magnetic body by this embodiment. It is a schematic diagram of the iron powder interface of an oxidation influence layer. It is a schematic diagram which shows the microstructure of the iron powder interface of an unoxidized area
  • the inventors conducted technical studies based on the problems described above, and even after heat treatment in an oxidizing atmosphere such as the air, iron loss of the powder soft magnetic material does not increase, and it has excellent magnetic properties and low process cost.
  • iron loss of the powder soft magnetic material does not increase, and it has excellent magnetic properties and low process cost.
  • the powder soft magnetic material according to the present invention uses the composite powder produced as follows as a raw material. First, the surface of a metal powder containing iron powder as a main component is covered with an Fe-P-based composite oxide as an inorganic insulating layer by a phosphorylation treatment. Further, an organic layer containing Si is applied in the form of a solution to the upper layer portion, and dried. A lubricant is mixed with the metal powder to prepare a composite powder as a raw material of the powder soft magnetic material. The composite powder is compacted into a soft magnetic material, and the subsequent strain reduction heat treatment is carried out in an oxidizing atmosphere under appropriate temperature and time conditions. According to the present invention, it is possible to prevent an increase in iron loss of the powder soft magnetic material by suppressing the growth of the oxide film generated on the surface of the iron powder and the influence of oxidation to the inside of the iron powder.
  • the particle size of iron powder constituting the powder soft magnetic material is further controlled, and the proportion of relatively fine iron powder having a particle size of less than 100 ⁇ m is made less than 30% by weight.
  • the volume ratio occupied by the boundary between iron powder (hereinafter referred to as "iron powder interface") inside the magnetic body is reduced to prevent the progress of oxidation inside the magnetic body.
  • the iron powder interface is narrowed to prevent the progress of oxidation inside the magnetic material.
  • the powder soft magnetic material according to the present embodiment comprises an inorganic insulating layer containing phosphoric acid, an organic layer containing Si, and an iron powder (composite iron powder) compounded with a lubricant as raw materials. Do.
  • the composite iron powder is compacted into a soft magnetic material, and the subsequent strain reduction heat treatment is carried out in an oxidizing atmosphere under appropriate temperature and time conditions to obtain the surface area of the powder soft magnetic material (surface And an oxidation affected layer) in the region including the vicinity of the surface.
  • the oxidation-influenced layer in the present embodiment is a region in which an oxide of iron and an oxide of Si are formed at the interface between iron powders (the boundary between iron powders) constituting the powder soft magnetic material. And formed on the surface area of the powder soft magnetic material. Iron oxide and Si oxide in the oxidation affected layer are formed as the iron powder, the insulation coating, the forming aid, and the lubricant are denatured by heating and oxidation reaction.
  • FIG. 1 is a schematic cross-sectional view of the powder soft magnetic material according to the present embodiment, showing a cross-sectional texture.
  • the powder compact soft magnetic body 1 is constituted by the bonding of a large number of iron powders 2, and in FIG. 1 has a ring shape and shows a cross section perpendicular to the circumferential direction.
  • the powder soft magnetic body 1 is composed of a surface area including the surface and the vicinity of the surface, and an inner area which is an inner portion of the powder soft magnetic body 1, the surface area is an oxidation affected layer 3, and the inner area is oxidized.
  • the unoxidized region 4 is not formed.
  • the powder soft magnetic body 1 of the present embodiment is characterized in that the influence of oxidation is limited only to the oxidation affected layer 3 formed in the surface area, and the internal area is made an unoxidized area 4 which is in an unoxidized state. is there.
  • the surface of the iron powder is coated with an inorganic material having a chemical composition close to that of the complex oxide containing Fe and P, or an inorganic layer as the insulating layer.
  • the coating treatment of the insulating layer is performed by phosphate chemical conversion treatment.
  • the surface of the iron powder of the substrate is dissolved by oxidation and reacted with phosphoric acid, whereby a composite oxide layer mainly composed of Fe-P is formed on the surface of the iron powder.
  • the Fe-P complex oxide layer while having very high adhesion to the pure iron of the base material, is more resistant to deformation of iron powder compared with other oxide systems such as SiO 2 and Al 2 O 3 .
  • the ability to follow is very good. For this reason, the Fe—P-based composite oxide layer does not receive any damage that would cause the insulation deterioration such as peeling or breakage even during surface deformation during compacting.
  • the Fe—P-based composite oxide layer has a glass (amorphous) structure up to about 550 ° C., and crystallizes by heating at a high temperature exceeding 550 ° C. However, even after crystallization, the insulating property of the Fe—P-based composite oxide layer is maintained as long as the insulating layer is stably present on the surface of the iron powder and significant damage such as peeling does not occur.
  • the upper layer portion of the Fe—P-based composite oxide layer is covered with an organic layer containing Si in an overlapping manner.
  • the organic layer containing Si can be coated with an organic substance such as a silicone resin in the form of a solution, uniformly coated on the iron powder surface and then dried.
  • an oxidation suppression layer mainly composed of Si is formed on the iron powder interface of the oxidation affected layer. Be done.
  • the oxidation suppressing layer has an effect of reducing the iron loss of the powder soft magnetic material.
  • a lubricant is preferably added to the iron powder coated with the two insulating layers of the Fe—P-based composite oxide layer and the organic layer containing Si of the present embodiment for the purpose of imparting formability.
  • the material of the lubricant is not particularly limited, but conventionally known ones may be used. Specific examples thereof include metal salts such as zinc stearate and lithium stearate, and other waxes.
  • the lubricant is preferably added in the range of 0.05 to 0.8% by mass.
  • the above-described composite iron powder is compacted into a soft magnetic material, and a heat treatment for reducing strain is performed in an oxidizing atmosphere. At this time, the heat treatment is carried out under appropriate temperature and time conditions to form an oxidation-influenced layer on the surface area of the powder soft magnetic material.
  • oxygen (O) passes through and diffuses through the Fe-P-based composite oxide layer, and easily oxidizes with the pure Fe in the base, An oxide mainly composed of Fe such as 3 O 4 is formed.
  • pure Fe reacts with O to form an oxide, an increase in volume occurs, and the Fe—P-based composite oxide layer and the organic layer containing Si undergo excessive deformation.
  • the adhesion between the two insulating layers and the base material is sharply reduced, and the insulating layer is peeled off and decomposed, whereby the formation of the oxide mainly composed of Fe further progresses.
  • the “Fe-based oxide” in 1) is mainly produced by the oxidation of iron powder.
  • the “Fe—Si complex oxide” in 2) is formed by complex oxidation of Si in the organic layer with the Fe oxide.
  • the “Fe—P—Si complex oxide” in 3) is produced by peeling off the insulating layer on the surface of the iron powder and reacting / aggregating with Fe.
  • the “Fe-based oxide” containing almost no Fe in 4) is generated by oxidizing, aggregating, and rearranging Si contained in the organic layer containing Si by a thermal reaction.
  • FIG. 2 is a schematic view of the iron powder interface of the oxidation affected layer.
  • the iron powder interface 10 is formed of Fe-based oxide 11 (Fe 3 O 4 ) and Fe—Si composite oxide 12, and massive Fe—P—Si composite oxidation. things 13, and an oxide of layered that the Si mainly contains almost no Fe 14 is composed of 3 tissue named (SiO 2).
  • the oxidation reaction of the powder soft magnetic material at the time of heat treatment proceeds by the diffusion of oxygen atoms entering from the surface of the soft magnetic material into the interior of the powder soft magnetic material through the iron powder interface. That is, the iron powder interface is a diffusion path of oxygen at the time of heat treatment.
  • the role of the oxide 14 (for example, SiO 2 ) mainly containing Si, which does not substantially contain Fe in 4) present at the iron powder interface 10 of the oxidation affected layer, is important.
  • the Si-based oxide 14 is reacted and generated simultaneously with the Fe-based oxides 11 and 2) of the 1) Fe-Si composite oxide 12.
  • the structure of the oxide 14 mainly composed of Si becomes a layer having a thickness of several tens of nm, and is arranged so as to divide the iron powder interface 10 longitudinally and laterally.
  • the Fe-based oxide 11 (Fe 3 O 4 etc.) of 1) and the Fe-Si complex oxide 12 of 2) have a thickness of several tens of nm and a gap of the Si-based oxide 14 of mainly Si. It is formed to fill the
  • the layered oxide 14 mainly composed of Si in 4) is very excellent in oxidation resistance as compared with the oxides 1) to 3) containing Fe. It is presumed that this layered oxide mainly composed of Si functions as an oxidation suppressing layer that blocks the diffusion of oxygen during heat treatment by dividing and arranging the iron powder interface 10. It is a major feature of the powder soft magnetic material according to the present embodiment that an oxide mainly composed of Si not containing Fe is present in the oxidation affected layer as an oxidation suppression layer.
  • the microstructure of the lower part of these oxidation-influenced layers has a different appearance from the oxidation-influenced layers.
  • a dense composite oxide layer containing Fe, P and Si is formed as an insulating layer on the surface of the iron powder in the inner region of the powder soft magnetic material.
  • This composite oxide layer has a two-layer structure consisting of a lower layer in contact with the iron powder surface and an upper layer on the upper side thereof, and the compounding ratio of P to Si is different in each layer.
  • P is relatively abundant together with Fe, but the content of Si is small.
  • the upper layer is characterized in that the content of P is small and Si is contained more than in the lower layer.
  • Such a two-layered composite oxide layer consisting of a "Fe-P-based lower layer” rich in Fe and P and a "Si-rich upper layer” rich in Si is initially present on the surface of iron powder.
  • a structure in which the Fe—P-based composite oxide layer and the organic layer containing Si are stacked is changed by heating and formed.
  • the insulating layer having a two-layer structure on the surface of the iron powder preferably has a total thickness of 10 to 200 nm. If the total thickness of the insulating layers is less than 10 nm, the insulation property is unfavorably reduced. If the total thickness of the two layers exceeds 200 nm, the distance between the iron powders increases, which is not preferable because it leads to a decrease in magnetic flux density.
  • the outer interface (the interface which is not in contact with the iron powder) of the two-layered insulating layer is filled with an organic substance mainly containing C and O and containing some Si.
  • the organic substance filling the interface is presumed to be a structure in which chemical components such as metal soap or wax of the organic layer containing Si and the lubricant before heat treatment are changed by heating.
  • the interface microstructure in the inner region of the powder soft magnetic material is the structure found in the oxidation affected layer (ie, an oxide mainly composed of Fe, an Fe-Si composite oxide, an Fe-P-Si composite) It shows a different aspect from the structure of oxide) and a structure containing an oxide mainly containing Si and containing almost no Fe.
  • the oxidation affected layer ie, an oxide mainly composed of Fe, an Fe-Si composite oxide, an Fe-P-Si composite
  • Such an inner region of the powder soft magnetic material is referred to as an "unoxidized region" because oxidation hardly occurs. In the unoxidized region, almost no reaction with oxygen which penetrates and diffuses from the outside through the iron powder interface occurs. This unoxidized region is shown as unoxidized region 4 in FIG.
  • FIG. 3 is a schematic view showing the microstructure of the iron powder interface in the unoxidized region.
  • a lower layer 21 mainly composed of Fe-P is an inorganic insulating covering layer
  • the Si-rich upper layer 22 is an oxide insulating layer, so these two layers are dense insulating layers.
  • an organic layer 23 mainly composed of C and O and containing Si is present between the insulating layers, and fills the iron powder interface 10. As a result, the insulation between the iron powder is maintained in the unoxidized region, and the eddy current loss is reduced.
  • the insulating layer on the surface of the iron powder is broken, and the eddy current loss increases. If the effect of oxidation during atmospheric heat treatment affects the entire compacted soft magnetic material, the unoxidized tissue disappears. As a result, the iron loss of the powder soft magnetic material increases, leading to the deterioration of the magnetic properties. Therefore, it is not preferable that the whole of the powder soft magnetic material is affected by oxidation.
  • the formation of the oxidation affected layer is limited to the surface region of the powder soft magnetic material only, and the internal region of the powder soft magnetic material is not oxidized It is important to keep the condition.
  • diffusion of oxygen to the inner region of the powder soft magnetic material can be achieved by forming an oxidation suppression layer of an oxide mainly composed of Si in the iron powder interface of the oxidation affected layer. It is possible to suppress the internal region into an unoxidized state (to be an unoxidized region).
  • the iron powder as the raw material of the powder soft magnetic material has a content of elements other than Fe such as Mn, Cr, Si, P and S. Iron powder as low as possible is preferred.
  • water atomization or gas atomization treatment Since the iron powder after atomization treatment contains many gas impurities such as O, C, N, etc., it is necessary to carry out a heat treatment in a reducing atmosphere containing hydrogen at 800 to 1000 ° C. to purify the iron powder. .
  • the size (particle size) of the iron powder constituting the powder soft magnetic material affects the magnetic properties after the strain reduction heat treatment.
  • the proportion of fine iron powder having a particle size of less than 100 ⁇ m is large, the volume proportion of the iron powder interface increases in the inside of the powder soft magnetic material.
  • the iron powder interface serves as a diffusion path of oxygen to the inside of the powder soft magnetic material at the time of strain reduction heat treatment. For this reason, in the case of a powder soft magnetic material having the same density, when the volume ratio of the interface portion is high, the oxidation-affected layer easily grows to the inside, and the core loss increases.
  • the proportion in the range of 100 to 400 ⁇ m is 70% or more by weight, and the proportion of the fine iron powder below 100 ⁇ m is less than 30% by weight. If it is such a ratio, the growth to the inside of the oxidation influence layer at the time of distortion reduction heat processing will be suppressed, and an iron loss will fall.
  • the average particle size of the entire iron powder is preferably 120 to 250 ⁇ m from the viewpoint of core loss reduction. An excessively large particle size of the iron powder is not preferable because it leads to an increase in eddy current loss.
  • the proportion of coarse iron powder having a particle size of more than 400 ⁇ m is preferably less than 30% by weight.
  • the composite powder as a raw material of the powder soft magnetic material obtained by the above method is subjected to excessive plastic deformation under high pressure by die molding, It is magnetic.
  • the molding pressure is usually 800 MPa or more, and it is preferable to increase the density so that the ratio of metal Fe to the powder soft magnetic material is 94% or more in volume ratio.
  • the density of the powder soft magnetic material When the density of the powder soft magnetic material is low, the distance between the iron powders constituting the magnetic body, that is, the width of the iron powder interface is increased.
  • oxygen is contained in the gaps of the oxidation-inhibited layer of the oxidation-affected layer (an oxide distributed in a thin layer containing mostly Fe and containing Si). It diffuses inside the compacted soft magnetic material. As a result, the core loss increases as the proportion of the unoxidized area inside the dusted soft magnetic material decreases. Therefore, making the density of the powder soft magnetic material sufficiently high to narrow the width of the iron powder interface is effective in reducing iron loss.
  • the density of the powder soft magnetic material is preferably at least 7.45 g / cm 3 or more, preferably 7.50 g / cm 3 or more.
  • the ratio of metal Fe to the powder soft magnetic material is more preferably 94.0% or more, preferably 95.0% or more in volume ratio.
  • the proportion of the iron powder itself is less than 94.0% by volume, it is not preferable because it causes an increase in iron loss of the powder soft magnetic material after heat treatment. It is difficult in terms of molding process to increase the density of powder soft magnetic material to over 7.75 g / cm 3 , and there is also the possibility of an increase in eddy current loss due to breakage of the insulating layer, so the density is 7.75 g It is preferable to set it as / cm ⁇ 3 > or less.
  • the occupancy rate of the iron powder itself is preferably 98.5% or less.
  • the “thickness” of the powder soft magnetic material is defined. At any point on the surface of the powder soft magnetic material, a straight line is drawn in the direction perpendicular to the surface toward the inside of the powder soft magnetic material. In this straight line, the length of a line segment from the surface to the other surface on the opposite side of the powder soft magnetic material (the back side of the powder soft magnetic material) is the powder softness at any given location. It is defined as the thickness of the magnetic body. When explaining using FIG. 1, the thickness of the powder soft magnetic material is D. When the surface of the powder soft magnetic material is a curved surface, a straight line is drawn in the direction perpendicular to the contact surface on the surface to define the thickness. That is, the thickness at any place of the powder soft magnetic material is the length of the powder soft magnetic material at that place in the direction perpendicular to the surface of the place.
  • the length of the oxidation affected layer in the above-mentioned line segment is referred to as "thickness".
  • the thickness of the oxidation-influenced layer is not defined where the above-mentioned line segment passes only the surface area, but is defined as where the above-mentioned line segment passes through the inner area and the two surface areas sandwiching the inner area. Do. The two surface areas are located on opposite sides of the soft magnetic powder body. As described with reference to FIG. 1, the thickness of the oxidation affected layer is d1 and d2, and d3 is not the thickness of the oxidation affected layer.
  • the thickness (length of the above-mentioned line segment) of the powder soft magnetic material may differ depending on the measurement site.
  • the thickness of the oxidation-influenced layer may be different from the thickness at an arbitrary position and the thickness at a position on the opposite side of the dusted soft magnetic material (the back side of the dusted soft magnetic material) with respect to this position. If it demonstrates using FIG. 1, d1 and d2 do not need to be equal. That is, the thickness of the oxidation affected layer may not be uniform.
  • the thickness of the oxidation-influenced layer is preferably in the following ratio with respect to the thickness of the powder soft magnetic material in the case of a simple ring-shaped powder soft magnetic material having a circular or rectangular cross section, etc. .
  • the thickness of the oxidation-influenced layer is the thickness (d1 in FIG. 1) at any location of the powder soft magnetic material and the opposite side of the powder soft magnetic material with respect to this location (the back side of the powder soft magnetic material
  • the total of the thickness (d2 in FIG. 1) and the thickness of the portion at 1) is 1/16 or more and 1 ⁇ 2 or less of the thickness (D in FIG. 1) of the powder soft magnetic material It is optimal from the magnetic properties of the soft magnetic material.
  • this arbitrary place the place where d1 in FIG. 1 is defined
  • place on the opposite side of the powder soft magnetic material with respect to this place place where d2 in FIG. 1 is defined
  • the total thickness of the oxidation-affected layer at a point opposite to any part of the powder soft magnetic material is less than 1/16 of the thickness of the powder soft magnetic material, it is estimated that the heat treatment time is short It is not preferable because strain reduction is insufficient to cause an increase in iron loss.
  • this total exceeds 1 ⁇ 2 of the thickness of the powder soft magnetic material, the ratio of the volume of the unoxidized region in the powder soft magnetic material decreases. In this case, the core loss of the powder soft magnetic material is increased to deteriorate the magnetic properties, which is not preferable.
  • the cross section may not have a simple ring shape such as a circle or a rectangle, but may have a three-dimensional complex shape having a projection such as a claw.
  • the difference in the shape causes a difference in thickness in the powder soft magnetic material.
  • the proportion of the oxidation-influenced layer relatively increases to exceed 1/2 at portions where the thickness of the powder soft magnetic material is small.
  • the total thickness of the oxidation affected layer is the thickness of the powder soft magnetic material at a location where the thickness of the powder soft magnetic material is averaged. It is preferable that it is 1/16 or more and 1/2 or less.
  • the thickness of the oxidation affected layer of the powder soft magnetic material it is also possible to evaluate by observing the microstructure of the cross section of the powder soft magnetic material.
  • SEM scanning electron microscope
  • EDS energy dispersive X-ray spectroscopy
  • the width from the surface of the powder soft magnetic material is measured at a plurality of points in the region where the oxide containing Fe is present at the iron powder interface. It becomes possible to evaluate the thickness of the oxidation affected layer directly.
  • the strain reduction heat treatment of the powder soft magnetic material is preferably carried out mainly in an air atmosphere from the viewpoint of reduction of the process cost.
  • a steam atmosphere or an oxidation atmosphere in which a pure oxygen gas of 20% or less (preferably 0.5 to 20%) by volume ratio is added to an inert gas such as nitrogen, argon or helium, The same effect is obtained.
  • the maximum holding temperature of the heat treatment is preferably in the range of 500 ° C. or more and less than 650 ° C.
  • the holding temperature is less than 500 ° C., the strain reduction of the iron powder constituting the powder soft magnetic material becomes insufficient, and the iron loss increases, which is not preferable.
  • the holding temperature is 650 ° C. or more, it is not preferable because the iron powder is excessively oxidized and the ratio of the unoxidized region inside the green compact is decreased to increase iron loss.
  • the holding time at the maximum temperature should be at least 5 minutes in the above temperature range. If the holding time is less than 5 minutes, the strain reduction of the iron powder becomes insufficient, and the iron loss of the powder soft magnetic material increases, which is not preferable. If the retention is excessive for a long time, the oxidation of iron powder is promoted and the iron loss is increased.
  • the optimum holding time depends on the heat treatment temperature.
  • the maximum heat treatment time is preferably 2 hours. If it exceeds 2 hours, the iron powder is excessively oxidized, and the proportion of the unoxidized region inside the green compact decreases, which is not preferable because iron loss increases.
  • the heat treatment temperature is preferably 1 hour at maximum. When it exceeds 1 hour, it is not preferable because the iron powder is excessively oxidized and iron loss increases.
  • the maximum heat treatment time is preferably 30 minutes. If it exceeds 30 minutes, it is not preferable because the iron powder is excessively oxidized to increase iron loss.
  • the heat-treated body After the end of the holding, it is preferable to take out the heat-treated body from the heating furnace to room temperature and air-cool as soon as possible. When it is placed in a heating furnace and cooled, it is not preferable because oxidation of iron powder becomes excessive and iron loss increases.
  • the pure iron ingot material was pulverized by water atomizing treatment after being dissolved in air.
  • the atomized iron powder was purified by repeating the hydrogen reduction heat treatment at 950 ° C. for 2 hours twice.
  • the oxygen concentration contained as an impurity after purification was 500 mass ppm or less.
  • the iron powder after purification was sieved to a particle size of 100 to 300 ⁇ m by a mesh, and then the Fe—P-based composite oxide layer was coated on the iron powder surface as an insulating layer by a phosphorylation treatment.
  • the thickness of the Fe—P based composite oxide layer was in the range of 20 to 50 nm.
  • Example material 1 A silicone resin solution was applied to iron powder coated with Fe—P based composite oxide and dried to prepare iron powder (Example material 1).
  • iron powder of Example Material 1 0.4% by mass of a zinc stearate based lubricant was added, and mixed by a V mixer to obtain a soft magnetic composite powder.
  • an iron powder (comparative material 1) coated with only the Fe-P based composite oxide layer was prepared, and 0.4 mass% of zinc stearate based lubricant was added to the iron powder of comparative material 1
  • a mixed powder was also prepared.
  • the above soft magnetic composite powder was pressed at a molding pressure of 1200 MPa to form a ring-shaped powder soft magnetic material having an outer diameter of 50 mm, an inner diameter of 40 mm, and a thickness of 5 mm.
  • the density of the ring-shaped powdery soft magnetic material measured by the Archimedes method was 7.50 to 7.54 g / cm 3 .
  • the compacted soft magnetic material after molding was subjected to strain reduction heat treatment in a box-shaped air heat treatment furnace.
  • the holding temperature of the heat treatment was 550 ° C., the temperature was raised from room temperature to 550 ° C. at a heating rate of 5 ° C./min, and after holding for 30 minutes, it was taken out of the furnace and air cooled.
  • the surface of the soft magnetic powder after heat treatment had a black color overall due to the influence of oxidation.
  • Example Wound 1 was 37 W / kg, and Comparative Wound 1 was 53 W / kg. From the above results, it was found that Example Material 1 had a core loss of 16 W / kg lower than that of Comparative Material 1 and exhibited excellent magnetic properties.
  • the microstructure of the cross section of the powder soft magnetic material was observed using a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the ring-shaped test piece of the example material 1 after magnetic property evaluation was used for TEM observation.
  • Thin film test pieces were collected from two points of the oxidation affected layer 3 in the surface area of the powder soft magnetic body 1 and the unoxidized area 4 in the inner area shown in FIG. 1 using the FIB (focused ion beam) method.
  • a TEM apparatus FE-TEM having an electron emission type of electron emission type and capable of reducing the diameter of a probe of an electron beam to 1 nm level was used.
  • FIG. 4 is a TEM image (bright field image) at the iron powder interface of the oxidation affected layer of the example material 1.
  • FIG. 4 shows two different iron powders and an interface 10 between these iron powders.
  • the width of the iron powder interface 10 is about 200 to 500 nm.
  • a white network 31 exists inside the iron powder interface 10, and the gray tissue 32 is filling the gaps.
  • the white network 31 inside the iron powder interface 1 has a width of 5 to 100 nm.
  • EDS compositional analysis by EDS that only Si and O were detected from the white network 31 and Fe was not present. From this result, it is presumed that the white network 31 present inside the iron powder interface 10 is an Si oxide having an amorphous structure, probably SiO 2 .
  • the gray structure 32 was Fe 3 O 4 , an oxide mainly composed of Fe, and Fe 2 SiO 4 of a composite oxide containing Fe and Si. Since the probe diameter of the electron beam is several nm, the gray structure 32 filling the gaps of the network structure 31 is Fe 3 O 4 and Fe 2 SiO 4 composed of nano-sized fine crystal grains. I understand.
  • a massive oxide having a diameter of several tens to several hundreds of nm containing Fe and P was present at the iron powder interface 10. It is inferred that this massive oxide is formed as the Fe—P based complex oxide coated on the surface of iron powder is detached and aggregated by oxidation.
  • FIG. 5 is a TEM image in the iron powder interface of the unoxidized area
  • the white part is the iron powder interface 10
  • the dark part is the iron powder.
  • the structure of the unoxidized region is different from the structure of the oxidation affected layer shown in FIG. 2 and FIG.
  • a surface layer having a thickness of less than 100 nm was present on the surface of the iron powder, and Fe, P, Si and O were detected from this surface layer by EDS analysis.
  • a relatively large amount of P was detected on the iron powder side (lower layer) of this surface layer, and a small amount of Si was detected.
  • P was small and Si was detected more than in the lower layer.
  • this distinction between lower and upper layers can not be seen due to the resolution of the picture.
  • an oxide-based insulating layer containing Fe, P, Si and O is present on the surface of the iron powder in the unoxidized region, and this insulating layer consists of two layers of different chemical compositions It has been found that it is composed of a layer and a Si-rich upper layer).
  • the two layers are the lower layer 21 mainly composed of Fe-P and the upper layer 22 of Si-rich described with reference to FIG.
  • the white portion is the organic layer 23 mainly composed of C, O, and Si described with reference to FIG.
  • the two insulating layers on the surface of the iron powder in the unoxidized region shown in FIG. 5 do not exist at the iron powder interface 10 of the oxidation affected layer of FIG. From the comparison of the structure of each region in FIGS. 4 and 5 by TEM observation, in the surface region of the ring-shaped test piece of the example material 1 subjected to the strain reduction heat treatment in the atmosphere, the iron powder is oxidized and the insulating coating layer is broken. It was found that an oxidation affected layer was formed. At the iron powder interface of the oxidation affected layer, oxides such as Fe 3 O 4 , Fe 2 SiO 4 and SiO 2 were formed. On the other hand, it was found that oxidation did not reach the inner region of the ring-shaped test piece, and an insulating layer having a two-layer structure different in chemical composition was present on the surface of the iron powder.
  • Example 2 In the same manner as in Example 2, TEM observation of the cross-sectional portion was performed on the ring-shaped test piece of the comparative material 1 after the magnetic property evaluation. As in the second embodiment, the observation position was set to two parts, the surface area and the inner area of the powder soft magnetic material. As a result of observation of the surface area of the comparative material 1, it was found that most of the iron powder interface was filled with an oxide mainly composed of Fe. At the iron powder interface, in addition to this, massive oxides of several tens to several hundreds nm in diameter containing Fe and P were present. It is inferred that this massive oxide is formed as the Fe—P based complex oxide coated on the surface of iron powder is detached and aggregated by oxidation. At the iron powder interface in the surface region of Comparative Example 1, the network-like oxidized layer containing Si, which was seen in Example material 1, did not exist.
  • Example 2 the structure of the iron powder interface in the inner region is almost the same structure as that of the surface region, and the iron powder interface is filled with Fe-based oxide, and Fe, P It has been found that massive oxides of several tens to several hundreds of nm in diameter are present.
  • the inner region of Example material 1 was in the unoxidized state, and the insulating layer having a two-layer structure was present on the surface of the iron powder.
  • the iron powder was oxidized similarly to the surface region, and the insulating layer on the surface of the iron powder was detached and aggregated.
  • Example material 1 From the TEM observation results of Examples 2 and 3, in Example material 1, the SiO 2 layer distributed in the form of a mesh at the iron powder interface of the oxidation affected layer functions as an oxidation suppression layer, It was found that the iron loss is reduced by suppressing the progress of the oxidation to the inside and stably holding the insulating layer on the surface of the iron powder. On the other hand, it is considered that in Comparative Material 1, the network-like SiO 2 layer was not present at the iron powder interface, and the oxidation preventing effect as in Example Material 1 did not work. As a result, in the comparative material 1, the internal area of the powder soft magnetic material is affected by the oxidation, and it is presumed that the core loss is increased by the falling off and aggregation of the insulating layer on the surface of the iron powder.
  • the iron powder subjected to the water atomizing treatment and the hydrogen reduction heat treatment under the same conditions as in Example 1 was sieved using meshes having different openings to prepare a plurality of iron powder samples having different particle sizes.
  • the insulation coating of Fe-P based complex oxide layer and Si resin is carried out in the same manner as in Example 1 and 0.4% of zinc stearate based lubricant is added.
  • a plurality of composite powders with different particle sizes were produced.
  • press molding, heat treatment in air, winding, and magnetic property evaluation were performed under the same conditions as in Example 1 to compare the properties of the respective powder soft magnetic materials.
  • Table 1 shows the average particle diameter and particle size of the powder soft magnetic material obtained by forming and heat treating five types of iron powder (example materials 1, 2, 3 and comparative materials 2 and 3) having different particle sizes.
  • the ratio of iron powder having a diameter of less than 100 ⁇ m, the evaluation result of iron loss (iron loss value), and the thickness of the oxidation affected layer are shown.
  • the average particle diameter of the iron powder decreases in the order of the example materials 1, 2, 3 and the comparative materials 2, 3.
  • the proportion (weight%) containing fine iron powder having a particle size of less than 100 ⁇ m is compared, the proportion of iron powder having a particle size of less than 100 ⁇ m tends to increase as the average particle size decreases.
  • the iron powder having a particle size of less than 100 ⁇ m is 20% or less.
  • iron powder having a particle size of less than 100 ⁇ m is about half in Comparative Material 2 and iron powder having a particle size of less than 100 ⁇ m occupies 80% or more in Comparative Material 3.
  • the core loss value after heat treatment in vacuum is almost the same as that of heat treatment in the atmosphere (the reduction of 1 to 2 W / kg by vacuum heat treatment).
  • the comparative materials 2 and 3 it was found that the core loss after the heat treatment in vacuum was significantly reduced (a reduction of 12 to 15 W / kg) than the heat treatment in air.
  • the iron loss value of the powder soft magnetic material tends to increase reflecting the increase in the coercive force as the iron powder particle size becomes finer.
  • the iron loss value after heat treatment in vacuum in Table 1 is presumed to reflect the tendency of iron powder particle size. Further, it can be seen from Table 1 that, in the case of heat treatment in the atmosphere, the increase in iron loss accompanying the miniaturization of iron powder tends to be further promoted.
  • the powder soft magnetic material after five types of heat treatments shown in Table 1 was cut, resin embedding and polishing were performed on the cross section, and the thickness of the oxidation affected layer was measured by SEM observation and EDS analysis.
  • the thickness of the oxidation affected layer was as thin as less than 1 mm.
  • Comparative Material 2 the thickness of the oxidation affected layer increased to 1.6 mm.
  • Comparative Material 3 it was found that the influence of oxidation was applied to almost the entire cross section. From the above results, as the iron powder constituting the powder soft magnetic material becomes finer, the effect of oxidation at the time of heat treatment in the atmosphere proceeds to the inside of the powder soft magnetic material, and the iron loss increases was shown to promote.
  • Example materials 4 to 6 After preparing five sets of the same iron powder as Example material 1, changing the pressure to 1400MPa, 1300MPa, 1000MPa, 700MPa and 600MPa respectively, heat treatment in the atmosphere at 550 ° C, five types of powder soft Magnetic materials were produced (Example materials 4 to 6, comparative materials 4 and 5). Then, the iron loss of the example materials 4 to 6 and the comparative materials 4 and 5 was evaluated.
  • Table 2 shows the evaluation results of molding pressure, density and iron loss (iron loss value) for six types of powder soft magnetic materials (example materials 1, 4 to 6 and comparative materials 4 and 5) having different molding pressures. And the thickness of the oxidation affected layer.
  • the density of the powder soft magnetic material is 7.62 g / cm 3 (example material 4), 7.59 g / cm 3 (example material 5), 7.54 g / cm 3 (example examples) as the molding pressure decreases.
  • Material 1) decreases to 7.47 g / cm 3 (example material 6), 7.39 g / cm 3 (comparative material 4), and 7.33 g / cm 3 (comparative material 5).
  • the core loss value is 35 W / kg (example materials 4 and 5), 37 W / kg (example material 1), 41 W / kg (example material 6), 46 W / kg (comparative material 4) as the molding pressure decreases. ), 51 W / kg (comparative material 5) was found to increase.
  • Example 4 the cross section of the powder soft magnetic material was observed by SEM observation and EDS analysis to determine the thickness of the oxidation affected layer. As a result, it was found that the thickness of the oxidation affected layer increased as the density of the powder soft magnetic material decreased. Since the comparative materials 4 and 5 have lower density than the example materials 1 and 4 to 6, the distance between the iron powder interfaces is wide, and as a result, the oxidation through the iron powder interface at the time of heat treatment is promoted. It is thought that the loss increased.
  • Example material 1 Nine sets of iron powder identical to Example material 1 were prepared, and a powder soft magnetic material molded at the same molding pressure (1200 MPa) was subjected to heat treatment in air at different temperatures and times respectively to evaluate core loss. .
  • Table 3 shows the evaluation results of the heat treatment temperature, the holding time, and the iron loss for 10 types of powder soft magnetic materials (example materials 1, 7 to 10, and comparative materials 6 to 10) having different heat treatment temperatures and holding times The core loss value) and the thickness of the oxidation affected layer are shown.
  • the heat treatment temperature is 500 ° C.
  • the holding time is 30 minutes and 120 minutes, respectively.
  • the heat treatment temperature of the example materials 1 and 7 is 550 degreeC, and holding time is respectively 30 minutes and 60 minutes.
  • the example material 10 has a heat treatment temperature of 600 ° C. and a holding time of 30 minutes.
  • the comparative material 10 has a heat treatment temperature of 450 ° C. and a holding time of 30 minutes.
  • the comparative material 7 has a heat treatment temperature of 500 ° C. and a holding time of 180 minutes.
  • the comparative material 6 has a heat treatment temperature of 550 ° C. and a holding time of 120 minutes.
  • the comparative material 8 has a heat treatment temperature of 600 ° C. and a holding time of 60 minutes.
  • the comparative material 9 has a heat treatment temperature of 650 ° C. and a holding time of 30 minutes.
  • the powder soft magnetic materials of Examples 1 and 7 to 10 were heat-treated at the heat treatment temperature and the holding time described above in “6) Best mode of heat treatment process”.
  • the dusted soft magnetic bodies of Comparative Materials 6 to 10 were heat-treated outside the range of the heat-treatment temperature and the holding time.
  • the core loss value is relatively small at 35 to 40 W / kg.
  • the core loss value was a large value exceeding 40 W / kg.
  • the core loss of the comparative material 9 held for 30 minutes at a heat treatment temperature of 650 ° C. also had a large value of 52 W / kg.
  • the thickness of the oxidation affected layer is 0.6 mm or less.
  • the thickness of the oxidation affected layer is 1 mm or more, and the influence of oxidation is greater than that of Example materials 1 and 7 to 10 to the inside of the powder soft magnetic material. It is estimated that the iron loss has been increased by promoting it.
  • the powder soft magnetic material of the comparative material 10 was subjected to a heat treatment for 30 minutes at a temperature lower than the temperature range of the example materials 1 and 7 to 10 at 450 ° C.
  • the powder soft magnetic material of the comparative material 10 had a very small thickness of 0.1 mm for the oxidation affected layer, but the core loss was a relatively large value of 48 W / kg. Although the effect of oxidation is small, the powder soft magnetic material of the comparative material 10 is presumed to have failed to sufficiently reduce iron loss since the heat treatment temperature is low and the reduction in strain in the iron powder is not sufficient.
  • the powder soft magnetic material according to the present invention can be used for electromagnetic components in general, and for example, can be used for a rotor core and a stator core of a motor, an electromagnetic valve, a reactor, and the like.
  • SYMBOLS 1 Powdered-powder soft-magnetic body, 2 ... Iron powder, 3 ... Oxidation affected layer, 4 ... Unoxidized area

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Abstract

La présente invention porte sur un corps de poudre magnétique doux comprimé qui ne soufre pas d'augmentation en perte de fer et qui présente d'excellentes caractéristiques magnétiques. La présente invention porte également un corps de poudre magnétique doux comprimé produit par application de revêtements isolants aux surfaces de particules de poudre métallique qui comprennent des particules de poudre de fer en tant que composant principal et puis moulage par compression des particules de poudre métallique résultantes, une couche affectée par oxydation qui contient des oxydes de fer (11, 12, 13) et de l'oxyde de Si en forme de couche (14) étant présente dans chaque interface de particule de fer (10) qui est la limite entre des particules de poudre de fer, ladite couche affectée par oxydation étant formée par traitement thermique conduit dans une atmosphère oxydante après le moulage par compression.
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