SE2251265A1 - Powder for dust core - Google Patents

Powder for dust core

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Publication number
SE2251265A1
SE2251265A1 SE2251265A SE2251265A SE2251265A1 SE 2251265 A1 SE2251265 A1 SE 2251265A1 SE 2251265 A SE2251265 A SE 2251265A SE 2251265 A SE2251265 A SE 2251265A SE 2251265 A1 SE2251265 A1 SE 2251265A1
Authority
SE
Sweden
Prior art keywords
powder
dust core
mass
iron
parts
Prior art date
Application number
SE2251265A
Inventor
Hirofumi Hojo
Mituhiro Sato
Satomi URUSHIBATA
Original Assignee
Kobe Steel Ltd
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Filing date
Publication date
Application filed by Kobe Steel Ltd filed Critical Kobe Steel Ltd
Publication of SE2251265A1 publication Critical patent/SE2251265A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/20Magnets 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
    • H01F1/22Magnets 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
    • H01F1/24Magnets 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

An object of the present invention is to provide a powder for a dust core, the powder containing a lubricant and being capable of increasing transverse strength of the dust core to be obtained. A powder for a dust core according to one aspect of the present invention includes: an iron-based powder; a chemical film formed on a surface of the iron-based powder; a surface treatment layer formed on a surface of the chemical film and containing a silane coupling agent; a resin layer laminated on a surface of the surface treatment layer and containing a silicone resin as a principal component; and a lubricant present on a surface of the resin layer, wherein the chemical film contains phosphorus, and at least one of nickel and cobalt.

Description

DESCRIPTION POWDER FOR DUST CORE [TECHNICAL FIELD] [000 l] The present invention relates to a powder for a dust core.
[BACKGROUND ART] id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2" id="p-2"
[0002] A dust core is used as a magnetic core in an inductor such as a motor, a choke coil, a reactor, and the like. This dust core is required to be superior in terrns of both mechanical characteristics and magnetic characteristics. id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3" id="p-3"
[0003] This dust core is produced by compression molding of a powder for a dust core which includes an iron-based powder. As the mechanical characteristics of the dust core, high transverse strength is required. The transverse strength of the dust core is improved by increasing a density thereof [0004] As the magnetic characteristics of the dust core, low core loss, a high magnetic flux density, and the like are required. Covering the iron-based powder with an electrically insulated layer is effective for reducing the core loss. Furtherrnore, increasing the density of the dust core is effective for increasing the magnetic flux density. id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5" id="p-5"
[0005] Thus, increasing the density of the dust core while coating the iron-based powder with the electrically conductive layer is effective for enhancing the mechanical characteristics and the magnetic characteristics of the dust core. id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6" id="p-6"
[0006] Recently, in order to increase the density of the dust core, applying a lubricant on an inner face of a die has been proposed. However, due to this feature, an applying operation becomes complicated and a longer time period is required for the applying operation, whereby production efficiency declines. id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7" id="p-7"
[0007] From such a perspective, a technique of mixing a lubricant into a powder for a dust core beforehand has been proposed (see Japanese Unexamined Patent Application, Publication No. 2013-149659 and PCT Intemational Publication No. 20l l/77694).
[PRIOR ART DOCUMENTS] [PATENT DOCUMENTS] [0008] Patent Document 1: Japanese Unexamined Patent Application, Publication No. 20 1 3 - 14965 9 Patent Document 2: PCT Intemational Publication No. 2011/77694 [SUMMARY OF THE INVENTION] [PROBLEMS TO BE SOLVED BY THE INVENTION] [0009] Patent Document 1 disclo ses a composite powder which has on a surface of a metal powder, a complex oxide layer consisting mainly of Fe-P and an organic layer containing Si, in this order, the composite powder being obtained by mixing a lubricant with the metal powder. [00 1 0] Patent Document 2 disclo ses a powder for a dust core obtained by: mixing a soft magnetic powder and an inorganic insulatiVe powder with a binder insulatiVe resin to obtain a granulated product, and then mixing a lubricating resin therewith. Patent Document 2 discloses that as an inorganic insulatiVe substance constituting the inorganic insulatiVe powder, at least one of MgO, AlgOg, TiOg, and CaO can be used. Patent Document 2 discloses that a silane coupling agent may be added to enhance adhesiveness between the soft magnetic powder and the inorganic insulative powder. [001 1] However, when, as disclo sed in Patent Document 1 and Patent Document 2, the lubricant is mixed with the powder for a dust core beforehand, a region in which the lubricant was present may become a void after evaporation or therrnal degradation of the lubricant, resulting in reduction of the density of the dust core to be obtained. As a result, sufficiently increasing the transVerse strength of the dust core may fail. [00 12] The present inVention was made in View of the foregoing circumstances, and an object of the present inVention is to provide a powder for a dust core, the powder including a lubricant and being capable of increasing the transVerse strength of the dust core to be obtained.
[MEANS FOR SOLVING THE PROBLEMS] [00 1 3] A powder for a dust core according to one aspect of the present invention includes: an iron-based powder; a chemical film formed on a surface of the iron-based powder; a surface treatment layer formed on a surface of the chemical film and containing a silane coupling agent; a resin layer laminated on a surface of the surface treatment layer and containing a silicone resin as a principal component; and a lubricant present on a surface of the resin layer, wherein the chemical film contains phosphorus, and at least one of nickel and cobalt. [00 l 4] The powder for a dust core is provided with the chemical film, the surface treatment layer, and the resin layer on the surface side of the iron-based powder in this order, and the lubricant is present on the surface of the resin layer. Since the chemical film contains phosphorus and at least one of nickel and cobalt, and the resin layer is laminated on the surface of the chemical film via the surface treatment layer, the powder for a dust core enables increasing the transverse strength of a dust core to be formed by using the powder for a dust core. [00 l 5] A content of the silane coupling agent with respect to 100 parts by mass of the iron-based powder is preferably greater than or equal to 0.05 parts by mass and less than or equal to 0.30 parts by mass, and a content of the silicone resin with respect to l00 parts by mass of the iron-based powder is preferably greater than or equal to 0.05 parts by mass and less than or equal to 0.30 parts by mass. When the contents of the silane coupling agent and the silicone resin with respect to l00 parts by mass of the iron-based powder thus fall within the above ranges, the transverse strength of the dust core can be further increased. [00 l 6] An amount of addition of the lubricant with respect to l00 parts by mass of the iron-based powder is preferably greater than or equal to 0.20 parts by mass and less than or equal to 0.40 parts by mass. When the amount of addition of the lubricant with respect to l00 parts by mass of the iron-based powder thus falls within the above range, the transverse strength of the dust core can be further increased while sufficiently enhancing slipperiness, with respect to a die, of a molded product to be obtained by compression molding the powder for a dust core. [00 l 7] It is to be noted that the term "principal component" as referred to herein means a component having the highest content in terms of mass, and means, for example, a component having a content of greater than or equal to 50% by mass.
[EFFECTS OF THE INVENTION] [00 l 8] As described above, the powder for a dust core according to the one aspect of the present invention includes the lubricant, and is capable of increasing the transverse strength of the dust core to be obtained.
[DESCRIPTION OF EMBODIMENTS] [00 l 9] Hereinafter, embodiments of the present invention are described in detail. id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20" id="p-20"
[0020] Powder for Dust Core The powder for a dust core includes: an iron-based powder; a chemical film formed on a surface of the iron-based powder; a surface treatment layer forrned on a surface of the chemical film; a resin layer laminated on a surface of the surface treatment layer; and a lubricant present on a surface of the resin layer. The chemical film, the surface treatment layer, and the resin layer are provided on the surface of the iron-based powder in this order. That is to say, with regard to the powder for a dust core, the chemical film is formed directly on the surface of the iron-based powder, the surface treatment layer is formed directly on the surface of the chemical film, and the resin layer is formed directly on the surface of the surface treatment layer. The lubricant is present on an outerrnost surface of the powder for a dust core. [002 l ] Iron-based powder The iron-based powder is a soft magnetic material. The iron-based powder may be exemplified by a pure iron powder, an iron-based alloy powder, an iron-based amorphous powder, and the like. Examples of the iron-based alloy powder include a Fe-Al alloy, a Fe-Si alloy, Sendust, Perrnalloy, and the like. The iron-based powder is produced by, for example, making mo lten iron (or a molten iron alloy) into fine particles by an atomization method, carrying out reduction, and then pulverizing. According to this production method, an average particle diameter of the iron-based powder can be controlled to be about greater than or equal to 20 um and less than or equal to 250 um. The lower limit of the average particle diameter is preferably 50 um. The upper limit of the average particle diameter is preferably l50 um. It is to be noted that the "average particle diameter of the iron-based powder" as referred to means a particle diameter (median diameter) corresponding to a cumulative particle size distribution of 50% in a particle size distribution as evaluated by a sieving method. id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22" id="p-22"
[0022] Chemical film The chemical film is an insulating layer having an electric insulation property. The chemical film contains P (phosphorus), and at least one of Ni (nickel) and Co (cobalt). [0023] The chemical film is a phosphoric acid-based chemical film produced by a chemical treatment by using a treatment liquid in which a compound containing phosphorus (for example, orthophosphoric acid (H3PO4)) is dissolved. The chemical film may contain a Fe (iron) element derived from the iron-based powder. id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24" id="p-24"
[0024] When the chemical film contains Ni, the transverse strength of the dust core to be obtained tends to increase. In the case in which the chemical film contains Ni, the lower limit of a content of Ni with respect to l00 parts by mass of the powder in which the chemical film was formed on the surface of the iron-based powder is preferably 0.001 parts by mass, and more preferably 0.01 parts by mass. On the other hand, the upper limit of the content of Ni with respect to 100 parts by mass of the powder is preferably 0.05 parts by mass, and more preferably 0.03 parts by mass. When the content falls within the above range, uniforrnity of film thickness of the chemical film can be achieved (in other words, generation of a part of the chemical film in which the film thickness is extremely low can be prevented) and an insulation property of the powder for a dust core can be secured, and in addition, achieving higher density of a mo lded product obtained by compression molding the powder for a dust core (hereinafter, may be also merely referred to as "molded product") is facilitated. Furthermore, heat resistance of the powder for a dust core is improved, thereby enabling heat treatment of the powder for a dust core at a high temperature, and the core loss of the dust core to be obtained tends to be reduced. id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25" id="p-25"
[0025] In the case in which the chemical film contains Ni, provided that a content of P contained in the chemical film is defined as Mp [mol] and the content of Ni contained in the chemical film is defined as MNi [mo l], the lower limit of a ratio (MNi/Mp) of the content of Ni to the content of P is preferably 0.1, and more preferably 0.15. On the other hand, the upper limit of the ratio (MNi/Mp) is preferably 0.5, and more preferably 0.4. When the ratio (MNi/Mp) falls within the above range, the uniforrnity of the film thickness of the chemical film is easier to achieve. id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26" id="p-26"
[0026] In the case in which the chemical film contains Co, the lower limit of a content of Co with respect to 100 parts by mass of the powder in which the chemical film was formed on the surface of the iron-based powder is preferably 0.005 parts by mass. On the other hand, the upper limit of the content of Co with respect to 100 parts by mass of the powder is preferably 0.1 parts by mass. When the content falls within the above range, the uniforrnity of the film thickness of the chemical film can be achieved and an insulation property of the powder for a dust core can be secured, and in addition, achieving higher density of the molded product is facilitated. Furthermore, the heat resistance of the powder for a dust core is improved, heat treatment of the powder for a dust core at a high temperature is enabled, and the core loss of the dust core to be obtained tends to be reduced. id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27" id="p-27"
[0027] As other component(s), element(s) of Na (sodium), K (potassium), N (nitrogen), S (sulfur), Cl (chlorine), and/or the like may be contained in the chemical film. These components may be added as needed in order to control a pH of the treatment liquid in which the compound containing phosphorus is dissolved, or to promote a reaction of the treatment liquid. id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28" id="p-28"
[0028] The chemical film preferably contains K as the other component. When the chemical film contains K, inhibition of forrning a semiconductor by bonding between O (oxygen) and Fe in the film during heat treatment at a high temperature is enabled. Thus, a decrease in specific electrical resistance and a decline in the transverse strength owing to the heat treatment can be inhibited. id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29" id="p-29"
[0029] In the case in which the chemical film contains the other component(s), a content of each of these components with respect to 100 parts by mass of the iron-based powder is preferably greater than or equal to 0.00l parts by mass and less than or equal to l.0 parts by mass. It is to be noted that the chemical film may contain component(s) aside from the other component(s) within a range not leading to impairrnent of the effects of the present invention. id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30" id="p-30"
[0030] The lower limit of a film thickness of the chemical film is preferably l nm and more preferably l0 nm. On the other hand, the upper limit of the film thickness of the chemical film is preferably 250 nm and more preferably 50 nm. When the film thickness is less than the lower limit, the insulation property may be insufficient. Conversely, when the film thickness is greater than the upper limit, it may be difficult to achieve sufficiently high density of the molded product to be obtained. [003 l] Surface treatment layer The surface treatment layer is an insulating layer having an electric insulation property. The surface treatment layer contains the silane coupling agent. The silane coupling agent has both a functional group which reacts with and bonds to an organic material such as a silicone resin, and a functional group which reacts with and bonds to an inorganic material. The silane coupling agent is interposed between the chemical film and the resin layer, and increases adhesiveness between the chemical film and the resin layer. The silane coupling agent may be partially arranged in the chemical film. id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32" id="p-32"
[0032] The silane coupling agent is not particularly limited, and a silane coupling agent represented by the general forrnula: X-Si-(OR)n (wherein X represents an alkyl group having a polar group at an end thereof; R represents an alkyl group having more than or equal to l and fewer than or equal to 3 carbon atoms; and n is an integer of greater than or equal to l and less than or equal to 3) can be employed. The polar group in X may be exemplified by a group having an amino group, a ureide group, an epoxy group, a thiol group, a methacryloxy group, or the like, and of these, the group having an amino group is preferred. [0033] The lower limit of a content of the silane coupling agent with respect to l00 parts by mass of the iron-based powder is preferably 0.05 parts by mass, and more preferably 0.10 parts by mass. On the other hand, the upper limit of the content is preferably 0.30 parts by mass, and more preferably 0.20 parts by mass. When the content is less than the lower limit, sufficiently forming the surface treatment layer on the surface of the chemical film may fail, whereby sufficiently increasing the adhesiveness between the chemical film and the resin layer may fail. Conversely, when the content is greater than the upper limit, owing to occurrence of a condensation reaction between particles of the unreacted silane coupling agent, sufficiently increasing the adhesiveness between the chemical film and the resin layer may fail. Furthermore, when the content is greater than the upper limit, the surface treatment layer may become excessively thick, whereby sufficiently increasing the density of the mo lded product may fail. As a result, the transverse strength and/or the magnetic characteristics such as the magnetic flux density of the dust core to be obtained may be insufficient. id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34" id="p-34"
[0034] Resin layer The resin layer is an insulating layer having an electric insulation property. Furthermore, the resin layer concurrently serves as a bonding layer which bonds to the resin layers of other particles of the powder for a dust core at the time of compression mo lding the powder for a dust core (a time of concluding a crosslinking/curing reaction of the silicone resin). id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35" id="p-35"
[0035] The resin layer contains the silicone resin as the principal component. By bonding to the silane coupling agent which constitutes the surface treatment layer, the silicone resin increases the adhesiveness between the resin layer and the chemical film. [003 6] The silicone resin is not particularly limited, and in light of inhibiting stickiness of the powder for a dust core to improve handleability, the silicone resin preferably contains many trifunctional T units (RSiXg, wherein X represents a hydrolyzable group) rather than bifunctional D units (RgSiXg, wherein X represents a hydrolyzable group). However, when the silicone resin contains many tetrafunctional Q units (SiX4, wherein X represents a hydrolyzable group), in conducting a pre-curing treatment, described later, the silicone resin may rigidly bind to the silicone resin contained in the resin layers of other particles of the powder for a dust core. In this light, the lower limit of the T units of the silicone resin is preferably 60 mo l%, and more preferably 80 mo l%. Furthermore, the T units most preferably account for 100%. [003 7] Examples of R in each unit include a methyl group and a phenyl group. As R contained in the silicone resin, the methyl group accounting for greater than or equal to 50 mol% is preferred, and the methyl group accounting for greater than or equal to 70 mol% is more preferred. Moreover, the Silicone resin is most preferably a methyl silicone resin not containing the phenyl group as R. It is to be noted that a ratio between the methyl group and the phenyl group in the silicone resin and functionality thereof may be analyzed by FT-IR and/or the like. id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38" id="p-38"
[0038] The lower limit of a content of the silicone resin in the resin layer is typically 50% by mass, preferably 70% by mass, and more preferably 90% by mass. Furthermore, the content of the silicone resin in the resin layer is mo st preferably l00% by mass. When the content is less than the lower limit, it may be difficult to achieve suff1ciently high density of the mo lded product to be obtained. id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39" id="p-39"
[0039] The lower limit of a content of the silicone resin with respect to l00 parts by mass of the iron-based powder is preferably 0.05 parts by mass, and more preferably 0.10 parts by mass. On the other hand, the upper limit of the content is preferably 0.30 parts by mass, and more preferably 0.20 parts by mass. When the content is less than the lower limit, it may be difficult to sufficiently increase the transverse strength of the dust core to be obtained. Furthermore, when the content is less than the lower limit, heat resistance of the resin layer may be insuff1cient. Conversely, when the content is greater than the upper limit, a decrease in the magnetic flux density may increase. id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40" id="p-40"
[0040] Lubricant In compression mo lding the powder for a dust core to form a molded product, the lubricant reduces frictional resistance between particles of the powder for a dust core, and between the powder for a dust core and a die. The lubricant is, for example, in powdered form. [004 1 ] The lubricant can be exemplified by an organic lubricant and an inorganic lubricant, and can be used either alone of one type or as a mixture of two or more types. [0042] Exemplary organic lubricants include a hydrocarbon-based lubricant, a fatty acid-based lubricant, a higher alcohol-based lubricant, an aliphatic amide-based lubricant, a metallic soap-based lubricant, an ester-based lubricant, and the like. id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43" id="p-43"
[0043] Examples of the hydrocarbon-based lubricant include liquid paraff1n, paraff1n wax, synthetic polyethylene wax, and the like. Examples of the fatty acid-based lubricant include stearic acid. Examples of the higher alcohol-based lubricant include stearyl alcohol.
Examples of the aliphatic amide-based lubricant include fatty acid amides such as stearamide, oleamide, and erucamide; alkylene fatty acid amides such as methylene bis-stearamide and ethylene bis-stearamide; and the like. Examples of the metallic soap-based lubricant include zinc stearate, calcium stearate, lithium stearate, and the like. Examples of the ester-based lubricant include monoglyceride stearate. id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44" id="p-44"
[0044] As the inorganic lubricant, for example, an inorganic compound having a density of greater than or equal to 4.0 g/ cm3 can be used. Examples of the inorganic compound include mo lybdenum disulfide (MoSg), zinc oxide (ZnO), and the like. id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45" id="p-45"
[0045] The lower limit of an amount of addition of the lubricant with respect to l00 parts by mass of the iron-based powder is preferably 0.20 parts by mass, and more preferably 0.25 parts by mass. On the other hand, the upper limit of the amount of addition is preferably 0.40 parts by mass, and more preferably 0.35 parts by mass. When the amount of addition is less than the lower limit, sufficiently improVing the lubricity of the powder for a dust core with respect to the die or the like may fail. Conversely, when the amount of addition is greater than the upper limit, voids due to the lubricant may be formed in the dust core produced by using the powder for a dust core. As a result, it may be difficult to achieve sufficiently high density of the dust core. id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46" id="p-46"
[0046] Method for Producing Powder for Dust Core The method for producing the powder for a dust core includes: a step (chemical film-forming step) of forrning the chemical film on the surface of the iron-based powder; a step (surface treatment layer-forrning step) of forrning the surface treatment layer on the surface of the chemical film; a step (resin layer-laminating step) of laminating the resin layer on the surface of the surface treatment layer; and a step (lubricant-mixing step) of mixing a powder after the resin layer laminating-step with the lubricant. id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47" id="p-47"
[0047] Chemical film-forming step In the chemical film-forming step, for example, a solution (treatment liquid) obtained by dissolving in an aqueous solvent, a compound which contains P and a compound which contains Ni or Co is mixed with the iron-based powder, and then drying is performed. [0048] Examples of the compound containing P include orthophosphoric acid (H3PO4), (NH2OH)2-H2PO4, and the like. Examples of the compound containing Ni include nickel nitrate (Ni(NO3)2), nickel sulfate, nickel chloride, nickel carbonate, and the like. Examples of the compound containing Co include Co3(PO4)z, COs(PO4)z'8H2O, and the like. Furthermore, as a compound containing both P and Ni, nickel pyrophosphate (NigPgOv) or the like can be used. id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49" id="p-49"
[0049] To control pH and/or promote a reaction, the treatment liquid may contain additiVe(s) such as: an alkaline salt of Na and/or K; ammonia and an ammonium salt; a sulfate; a nitrate; a phosphate; and/or the like. Examples of the sulfate include (NH2OH)2- H2SO4 and the like. Examples of the phosphate include KH2PO4, NaH2PO4, (NH2OH)2- H2PO4, and the like. Of these, KH2PO4 and NaH2PO4 contribute to controlling the pH of the treatment solution, and (NH2OH)2-H2SO4 and (NH2OH)2-H2PO4 contribute to promoting a reaction of the treatment liquid. In the case of the treatment liquid containing the above additiVe(s), element(s) of Na, K, S, and/or the like are contained in the chemical film to be obtained. In the case in which the chemical film contains K, the powder for a dust core enables more easily preventing a decrease in specific electrical resistance and a decline in the transverse strength due to the heat treatment. [005 0] Water, and/or hydrophilic organic so lvents of alcohols, ketones, and the like, as well as mixtures thereof, can be used as the aqueous solvent. A well-known surfactant may be contained in the aqueous solvent. [005 1] The chemical film-forming step, for example, includes: adding the treatment liquid to the iron-based powder, mixing a resultant liquid with a well-known mixer, ball mill, kneader, V-type mixing machine, pelletizer, or the like, and then drying in an ambient air at greater than or equal to 150 °C and less than or equal to 250° C under a reduced pressure or in a Vacuum. Consequently, the chemical conVersion film is formed on the surface of the iron-based powder. In the chemical film-forming step, a particle diameter may be controlled by passing the powder after the drying through a sieVe having a mesh opening size of about greater than or equal to 200 um and less than or equal to 600 um. id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52" id="p-52"
[0052] Surface treatment layer-forrning step In the surface treatment layer-forming step, a solution in which the silane coupling agent is dissolved in a solvent is added on the surface of the chemical film formed in the chemical film-forming step, and then dried. id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53" id="p-53"
[0053] The so lvent in which the silane coupling agent is to be dissolved is not particularly limited, and for example, water, and/or hydrophilic organic so lvents of alcohols, ketones, and the like, as well as mixtures thereof, can be used. id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54" id="p-54"
[0054] Resin layer-laminating step In the resin layer-laminating step, a solution in which the Silicone resin is dissolved in a solvent is added on the surface of the surface treatment layer formed in the surface treatment layer-forming step, and then dried. id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55" id="p-55"
[0055] As the solvent in which the silicone resin is to be dissolved, for example, alcohols, and petroleum-based organic so lvents such as toluene and xylene can be used. [0056] In the resin layer-laminating step, heating is preferably performed at a temperature allowing for volatilization of the so lvent dissolved in the silicone resin, also being a temperature lower than the curing temperature of the silicone resin, to suff1ciently volatilize the solvent. The drying temperature in the resin layer-laminating step differs in accordance with a type of the solvent, and is preferably, for example, greater than or equal to 60 °C and less than or equal to 80 °C. In the resin layer-laminating step, the powder after the drying is preferably passed through a sieve having a mesh opening size of about greater than or equal to 300 um and less than or equal to 600 um in order to eliminate aggregated clumps. [005 7] In the resin layer-laminating step, after the drying, it is preferred that the powder having the resin layer laminated thereon is heated, and a treatment is performed to terrninate a step of softening the silicone resin in a powder state (hereinafter, the treatment to terrninate the step of softening the silicone resin in the powder form may be also referred to as the "pre-curing treatment"). A procedure of performing the pre-curing treatment may be exemplif1ed by a method in which the powder after the drying is heated for a short time period at a temperature approximate to the curing temperature of the silicone resin. A heating temperature in the pre-curing treatment may be, for example, greater than or equal to l00 °C and less than or equal to 200 °C. A heating time period in the pre-curing treatment may be, for example, greater than or equal to 5 min and less than or equal to l00 min. Furthermore, as a procedure for performing the pre-curing treatment, a method in which a curing agent is used may be adopted. id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58" id="p-58"
[0058] Since the particles of the powder after the pre-curing treatment have not been completely adhered and hardened together, the powder can be easily crushed. After pre-curing the silicone resin, a powder being superior in flowability can be obtained by crushing. This powder can be charged like sand into the die at a time of performing the compression molding by warm molding at, for example, about greater than or equal to l00 °C and less than or equal to 250 °C. Accordingly, charging the powder for a dust core into the die can be easily and certainly performed. Furthermore, by performing this pre-curing treatment, adhesiveness between the particles of the powder for a dust core can be increased ll during mo lding, thereby enabling promoting an increase in the density of the mo lded product to be obtained. It is to be noted that the powder after the pre-curing treatment is preferably passed through a sieve having a mesh opening size of about greater than or equal to 300 um and less than or equal to 600 um to make the particle diameter uniform. [005 9] Method for Producing Dust Core With regard to the powder for a dust core, after performing the compression mo lding, the dust core is formed by performing a heat treatment. That is to say, the method for producing a dust core includes: a step (compression molding step) of compression molding the powder for a dust core; and a step (heat treatment step) of subj ecting to the heat treatment, the mo lded product after the compression mo lding. [0060] Compression mo lding step The compression molding step may, for example, be performed by a well-known method using a die. Contact pressure in the compression mo lding step is preferably greater than or equal to 490 MPa and less than or equal to 1,960 MPa, and more preferably greater than or equal to 790 MPa and less than or equal to 1,180 MPa. In particular, in the compression mo lding step, when the compression molding is performed with a contact pressure of greater than or equal to 980 MPa, producing the dust core having a high density is facilitated. The compression molding step may be performed by either of room temperature molding or Warm mo lding, and carrying out Warm molding is preferred in light of obtaining the dust core having high density. [006 1 ] Heat treatment step In the heat treatment step, the molded product obtained in the compression mo lding step is annealed. By this heat treatment step, the lubricant contained in the molded product is volatilized or therrnally degraded. Since the powder for a dust core includes, on the surface of the iron-based powder, the chemical film, the surface treatment layer, and the resin layer in this order, even in the case of the lubricant being volatilized or therrnally degraded, sufficiently great transverse strength of the dust core to be obtained can be achieved. id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62" id="p-62"
[0062] The lower limit of a heat treatment temperature in the heat treatment step is preferably 500 °C, and more preferably 550 °C. On the other hand, the upper limit of the heat treatment temperature in the heat treatment step is preferably 700 °C, and more preferably 650 °C. When the heat treatment temperature is less than the lower limit, sufficiently decreasing hysteresis lo ss of the dust core to be obtained may fail. Conversely, when the heat treatment temperature is greater than the upper limit, the insulating layers (the chemical film, the surface treatment layer, and the resin layer) covering the surface of the 12 iron-based powder may deteriorate. [0063] An atmosphere at the time of the heat treatment in the heat treatment step is not particularly limited, and an atmosphere of an inert gas of nitrogen or the like is preferred. A heat treatment time period in the heat treatment step may be set within a range in which the specific electrical resistance of the dust core to be obtained does not decrease. The lower limit of the heat treatment time period is, for example, preferably 20 min, more preferably 30 min, and still more preferably 60 min. id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64" id="p-64"
[0064] Dust Core The dust core is obtained by cooling to normal temperature after the heat treatment step. The lower limit of the transverse strength of the dust core is preferably 46 MPa, more preferably 50 MPa, and still more preferably 60 MPa. With regard to the powder for a dust core, due to the chemical film, the surface treatment layer, and the resin layer being provided on the surface of the iron-based powder in this order, the transverse strength of the dust core to be obtained can be increased to greater than or equal to the lower limit. It is to be noted that the upper limit of the transverse strength is not particularly limited since it is more preferable as it becomes higher, and the upper limit may be, for example, l00 MPa. It is to be noted that the "transverse strength" as referred to herein means a Value in accordance with JIS-Z25 1 1: 2006. id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65" id="p-65"
[0065] Advantages Since the chemical film contains phosphorus and at least one of nickel and cobalt, and the resin layer is laminated on the surface of the chemical film Via the surface treatment layer, the powder for a dust core enables increasing the transverse strength of the dust core to be formed by using the powder for a dust core. id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66" id="p-66"
[0066] Other Embodiments The above-described embodiment is not to be construed as limiting the configuration of the present inVention. Therefore, constituent elements of each part of the above-described embodiment may be omitted, replaced, or added based on the description in the present specification and common technical knowledge, and such omission, replacement, and addition should be construed as falling within the scope of the present inVention. EXAMPLES [0067] Hereinafter, the present disclosure is further specifically described by way of Examples, but the present disclo sure is not limited to the following Examples. id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68" id="p-68"
[0068] 13 Examples No. 1 to No. 7 Production of powder for dust core As the iron-based powder, an iron-based powder being a pure iron powder obtained by a water atomization method was used, including as inevitable impurities, C S 0.01% by mass, Si S 0.03% by mass, P S 0.02% by mass, and S S 0.01% by mass, wherein a particle size distribution involved particle diameters of less than 150 um accounting for 16% by mass, particle diameters of greater than or equal to 150 um and less than 180 um accounting for 41% by mass, particle diameters of greater than or equal to 180 um and less than 250 um accounting for 42% by mass, and particle diameters of greater than or equal to 250 um accounting for 1% by mass. The chemical film containing P and Ni, the surface treatment layer containing the silane coupling agent, and the resin layer containing the silicone resin as the principal component were provided on the surface of the iron-based powder in this order, and then the lubricant was mixed with the powder after the laminating of the resin layer. Specifically, 10 parts by mass in total of nickel pyrophosphate and nickel nitrate were added to 100 mL of a base preparation being a phosphoric acid solution obtained by mixing 50 parts by mass of water, 35 parts by mass of KH2PO4, 10 parts by mass of H3PO4, and 10 parts by mass of (NH2OH)2-H2PO4, and further, 50 parts by mass of the treatment liquid diluted such that a difference between the phosphorus content after film formation and the phosphorus content before film formation was 0.04% were mixed with 1,000 parts by mass of the iron-based powder; the mixture was dried at 200 °C for 30 min in an ambient air, and then passed through a sieve having a mesh opening size of 600 um (chemical film-forming step). [0069] Next, a solution in which "Z-6011," a silane coupling agent manufactured by Dow Toray Co., Ltd., was dissolved in water was mixed with the powder after the chemical f1lm-forming step such that a proportion of the silane coupling agent with respect to 100 parts by mass of the iron-based powder was as shown in Table 1, and the mixture was subjected to drying at 125 °C for 30 min (surface treatment layer-forming step). Subsequently, a solution in which "SR2400," a silicone resin manufactured by Dow Toray Co., Ltd., was dissolved in toluene was mixed with the powder after the surface treatment layer-forming step such that the content of the silicone resin with respect to 100 parts by mass of the iron-based powder was as shown in Table 1, and the mixture was subjected to drying at 75 °C for 30 min (resin layer-laminating step). Furthermore, the lubricant was mixed with the powder after the resin layer-laminating step. Stearamide and zinc oxide were used as the lubricant, and the stearamide and zinc oxide were added in the proportions shown in Table 1 with respect to 100 parts by mass of the iron-based powder (lubricant-mixing step). id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70" id="p-70"
[0070] 14 Production of dust core samples The powder after the lubricant-mixing step (powder for a dust core) was compression mo lded into a molded product. Specifically, the powder for a dust core at norrnal temperature was placed in a die heated to 80 °C, and pressure molded at a contact pressure of 800 MPa (8.16 ton/cmz) into a molded product having a cuboid shape of 18 mm >< 32 mm >< 12.5 mm. Subsequently, this molded product was subjected to stress relief annealing in a nitrogen atmosphere with a rate of temperature rise of 10 °C/min, an end-point temperature of 600 °C, and a retention time period of 30 min (heat treatment step). The molded product after the heat treatment step was fumace-cooled to norrnal temperature to give samples ofNo. 1 to No. 7. [007 1 ] No. 8 Production of powder for dust core As the iron-based powder, the same powder of those in No. 1 to No. 7 was used, and the chemical film containing P and Ni, and the resin layer containing the silicone resin as the principal component were provided on the surface of this iron-based powder in this order. Subsequently, the lubricant was mixed with the powder after laminating the resin layer. In No. 8, the powder for a dust core was produced in a similar manner to those of No. 1 to No. 7, except that the surface treatment layer containing the silane coupling agent was not provided, and the contents of the silicone resin and the lubricant with respect to l00 parts by mass of the iron-based powder were as shown in Table 1. [0072] Production of dust core sample The powder following the lubricant-mixing step (powder for a dust core) was compression mo lded into a molded product in an operation similar to those of No. 1 to No. 7 (compression molding step). Subsequently, the mo lded product was subj ected to stress relief annealing under conditions similar to those of No. l to No. 7 (heat treatment step). The mo lded product after the heat treatment step was fumace-cooled to norrnal temperature to give the sample of No. 8. [0073] Density A density (g/cm3) of each of the samples of No. 1 to No. 8 was deterrnined. The density was deterrnined by measuring the mass and size of each sample, and then performing a calculation. The calculation results are shown in Table l. [0074] Transverse Strength The transverse strength [MPa] of each of the samples of No. 1 to No. 8 was deterrnined in accordance with J IS Z-251 l: 2006. The measurement results are shown in Table 1. id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75" id="p-75"
[0075] Table 1 Powder for dust core Dust core content with respect to 100 parts by mass of iron-based powder transverse (Pafïs bY mass) density _ strength cgupling lubflCant [g/cm3] silicone resin [MPa] agfiflï stearamide zinc oxide No. 1 0.05 0.10 0.25 0.05 7.50 46 No. 2 0.10 0.10 0.25 0.05 7.50 63 No. 3 0.15 0.10 0.25 0.05 7.51 58 No. 4 0.20 0.10 0.25 0.05 7.45 56 No. 5 0.20 0.10 0.30 0.05 7.50 63 No. 6 0.10 0.15 0.25 0.05 7.52 65 No. 7 0.10 0.20 0.25 0.05 7.47 65 No. 8 - 0.10 0.25 0.05 7.52 45 id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76" id="p-76"
[0076] Evaluation Results As shown in Table 1, No. 1 to No. 7, in which the chemical film containing P and Ni, the surface treatment layer containing the silane coupling agent, and the resin layer containing the silicone resin as the principal component were provided on the surface of the iron-based powder in this order, had higher transverse strength than No. 8, which did not include the surface treatment layer containing the silane coupling agent. In particular, No. 2 to No. 7, in which the content of the silane coupling agent with respect to 100 parts by mass of the iron-based powder was greater than or equal to 0.10 parts by mass, had dramatically higher transverse strength than did No. 8. [INDUSTRIAL APPLICABILITY] [0077] As described above, the powder for a dust core according to the one aspect of the present invention is suitable for increasing the transverse strength of the dust core to be obtained. 17

Claims (3)

1. A powder for a dust core, the powder comprising: an iron-based powder; a chemical film formed on a surface of the iron-based powder; a surface treatment layer forrned on a surface of the chemical film and comprising a silane coupling agent; a resin layer laminated on a surface of the surface treatment layer and comprising a silicone resin as a principal component; and a lubricant present on a surface of the resin layer, wherein the chemical film comprises phosphorus, and at least one of nickel and cobalt.
2. The powder for a dust core according to claim 1, wherein a content of the silane coupling agent with respect to 100 parts by mass of the iron-based powder is greater than or equal to 0.05 parts by mass and less than or equal to 0.30 parts by mass, and a content of the silicone resin with respect to 100 parts by mass of the iron-based powder is greater than or equal to 0.05 parts by mass and less than or equal to 0.30 parts by mass.
3. The powder for a dust core according to claim 1 or 2, wherein an amount of addition of the lubricant with respect to 100 parts by mass of the iron-based powder is greater than or equal to 0.20 parts by mass and less than or equal to 0.40 parts by mass. 18
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