WO2010026984A1 - 圧粉磁心用粉末、圧粉磁心、及びこれらの製造方法 - Google Patents
圧粉磁心用粉末、圧粉磁心、及びこれらの製造方法 Download PDFInfo
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- WO2010026984A1 WO2010026984A1 PCT/JP2009/065326 JP2009065326W WO2010026984A1 WO 2010026984 A1 WO2010026984 A1 WO 2010026984A1 JP 2009065326 W JP2009065326 W JP 2009065326W WO 2010026984 A1 WO2010026984 A1 WO 2010026984A1
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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
- H01F1/26—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 by macromolecular organic substances
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- 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
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- 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
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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
- H01F1/33—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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F2003/026—Mold wall lubrication or article surface lubrication
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2998—Coated including synthetic resin or polymer
Definitions
- the present invention relates to a powder for a powder magnetic core in which at least an insulating layer is coated on the surface of a magnetic powder composed of magnetic particles, a method for producing the powder, a powder magnetic core produced from the powder for a powder magnetic core, and a method for producing the same. .
- a magnetic core used for an electric motor or the like is manufactured by compacting a powder for a powder magnetic core.
- an insulating layer is coated on the particle surface of the magnetic powder in order to ensure electrical insulation between the magnetic powders after pressure molding.
- a powder for a powder magnetic core a powder for a powder magnetic core in which a polymer resin having an excellent insulating property such as a silicone resin is applied to the surface of the magnetic powder and a resin insulating layer is coated as an insulating layer
- a powder for a powder magnetic core in which an oxide such as silica (SiO 2 ) is deposited on the surface by chemical vapor deposition (CVD) and the oxide insulating layer is coated as the insulating layer can be mentioned.
- an oxide insulating layer and a silicone resin insulating layer are sequentially formed as an insulating layer from the particle surface of the magnetic powder in the thickness direction. Powders for powder magnetic cores have been proposed (see, for example, Patent Document 1 and Patent Document 2). JP 2006-233295 A JP 2008-88505 A
- the oxide insulating layer 93A includes iron particles 92A and silicone resin as magnetic particles.
- the familiarity with the insulating layer 93B is improved. Thereby, the high specific resistance of the powder magnetic core after annealing can be maintained.
- the present state is that the joint portion (grain boundary) between the silicone resin insulating layers 93B and 93B is the weakest portion, and the strength of the dust core has not been increased.
- the silicone resin insulating layer 93B of the powder for powder magnetic core when forming the silicone resin insulating layer 93B of the powder for powder magnetic core, a silicone resin containing an organic solvent is applied to the particle surface of the powder, and the organic solvent is applied at a temperature of 100 to 200 ° C. after the application. Volatilize and dry the powder particles.
- a dust core when a dust core is formed from such a powder for a powder magnetic core, there are few Si—O—Si bond bonds especially between the silicone resin insulating layers 93B and 93B. The bond is weak and the strength of the dust core cannot be obtained sufficiently.
- the present invention has been made in view of the above-described problems, and an object of the present invention is to provide a pressure which can improve the mechanical strength of the dust core without deteriorating the magnetic properties of the dust core. It is providing the powder for powder magnetic cores, its manufacturing method, a powder magnetic core, and its manufacturing method.
- a powder for a powder magnetic core is a powder for a powder magnetic core including a powder for a powder magnetic core in which an insulating layer is coated on a particle surface of the magnetic powder.
- the surface layer portion of the insulating layer is provided with a polymer resin insulating layer containing vinylsilane and hydrosilane.
- the polymer resin insulating layer contains vinylsilane Si—CH ⁇ CH 2 and hydrosilane Si—H, so that at the production stage of the dust core, adjacent powder particles for the dust core can be obtained.
- a hydrosilylation reaction (addition reaction) between vinylsilane and hydrosilane can be developed.
- the polymer resin insulation layer of the powder magnetic core powder of the powder magnetic core powder according to the present invention has a composition in particular, as long as it contains vinylsilane and hydrosilane in an insulating polymer resin.
- the polymer resin is not limited, and examples thereof include a polymer resin such as a polyimide resin, a polyamide resin, an aramid resin, or a silicone resin.
- a more preferable polymer resin insulating layer is a silicone resin, which is a so-called addition-curing type silicone resin.
- the powder for a powder magnetic core referred to in the present invention refers to an aggregate of magnetic particles having a particle surface coated with an insulating layer.
- the insulating layer as used in the field of this invention means the layer for ensuring the electrical insulation between the magnetic powder (particles) after shaping
- the surface layer part said to this invention means the layer formed in the outer side among the insulating layers coat
- the powder for a powder magnetic core according to the present invention further includes an oxide insulating layer as the insulating layer between the magnetic powder and the polymer resin insulating layer.
- the conformability (adhesion) between the magnetic powder and the polymer resin insulation layer can be further improved by forming the oxide insulation layer.
- the oxide insulating layer of the powder for a powder magnetic core according to the present invention is not particularly limited as long as it is a layer that improves the conformability between the magnetic particles and the polymer resin insulating layer, and is silica, alumina, or zirconia. Insulating layers containing oxides such as ceramic materials, insulating layers containing oxides obtained by oxidizing the surface of magnetic powder and inorganic salts such as phosphates, etc. An oxide layer is preferred.
- a more preferable oxide insulating layer is an insulating layer containing a phosphate or an Al—Si-based oxide.
- the oxide insulating layer of the powder for a powder magnetic core according to the present invention has a two-layer structure, and a phosphate is provided from the surface of the magnetic particles toward the polymer resin insulating layer. More preferably, an insulating layer including an insulating layer and an insulating layer including an Al—Si-based oxide are sequentially provided. According to the present invention, by forming the insulating layer containing phosphate on the surface of the magnetic powder, the adhesion between the insulating layer containing phosphate and the magnetic powder is improved, and the Al—Si-based oxide is formed. Adhesion between these layers can be improved by sequentially laminating the insulating layer and the polymer resin insulating layer. As a result, the conformability of the polymer resin insulating layer to the magnetic particles is further improved.
- the oxide insulating layer of the powder for a powder magnetic core according to the present invention more preferably contains vinyl silane.
- the vinyl silane and the hydrosilane are also present between the oxide insulating layer and the polymer resin insulating layer (interface) at the production stage of the dust core.
- a hydrosilylation reaction can be further developed.
- Si—C—C—Si bonds can be obtained not only between the adjacent polymer resin insulation layers of the powder for powder magnetic cores but also between the oxide insulation layer and the polymer resin insulation layer. . This mechanical bond between the layers can further stabilize the mechanical strength of the dust core.
- the powder magnetic core manufactured by the conventional manufacturing method can be used.
- the strength of the dust core can be increased and the magnetic properties can be improved.
- it is suitable for use as a dust core, but when trying to increase the strength of the dust core, the magnetic characteristics may be deteriorated.
- the iron-based magnetic powder has an annealing temperature of 600 ° C. or higher, and it has been found that the volume reduction described above becomes significant when heated in such a temperature range. As a result, the powder core formed thereby increased eddy current loss, and new knowledge was obtained that the magnetic properties of the powder magnetic core may deteriorate.
- the invention of the powder for powder magnetic core shown below is based on this new knowledge, and the powder for powder magnetic core according to the present invention is based on the powder for powder magnetic core described above, and the polymer resin insulation layer. It is more preferable to further contain a silicon oxide precursor that becomes silicon oxide when heated.
- the silicon oxide phase is uniformly dispersed in the polymer resin insulating layer in the powder magnetic core during annealing, and the volume of the polymer resin insulating layer is Reduction can be suppressed.
- the insulation between the magnetic particles of a dust core can be maintained, the fall of an eddy current loss can be suppressed, and a higher magnetic characteristic can be hold
- the silicon oxide precursor only needs to form a silicon oxide phase in the polymer resin insulating layer at least under a temperature condition in which a hydrosilylation reaction occurs, and the phase is crystallized.
- the phase may be any one of a solid phase, an amorphized phase, and a phase in which these phases are combined. That is, the type of the silicon oxide precursor is not particularly limited as long as a siloxane structure represented by — (Si—O) n— (n is 2 or more) can be formed during heating.
- examples of such silicon oxide precursors include methyl-based straight silicone resins, and the side chain functional groups are not particularly limited as long as they are silicone resins and silicone oils having a siloxane bond as the main chain.
- silicone resin having a high Si and O content More preferably, it further includes a methyl group or an ethyl group in the side chain of the silicone resin.
- silicon oxide precursors include polymethylsiloxane, polyethyl silicate, octamethylcyclotetrasiloxane, hexamethyldisiloxane, octamethyltrisiloxane, hexamethylcyclotrisiloxane, decamethylcyclopentasiloxane, orthosilicate. It may be tetraethyl acid, or a combination thereof.
- the ratio of the polymer resin in the dust core powder (the ratio of the polymer resin insulating layer in one particle) is 0.6% by mass or less. More preferably.
- the strength of the dust core (crushing ring strength) can be increased.
- the ratio of the polymer resin insulation layer referred to in the present invention is the ratio of the polymer resin to the entire powder for the powder magnetic core, and 0.6 mass% or less means each particle of the powder.
- a polymer resin of 0.6% by mass or less is coated as an insulating layer.
- the silicone resin constituting the silicone resin insulating layer includes, as a side chain, a methyl group and a vinyl group for causing a hydrosilylation reaction with the hydrosilane, and the silicone resin. More preferably, the vinyl group contains 2 to 10% of all side chains and the methyl group contains 38 to 77% of all side chains.
- the vinyl group of the side chain of the silicone resin that is, the vinyl group of vinylsilane that undergoes a hydrosilylation reaction with the Si—H hydrosilane is contained in 2 to 10% of the total side chain. That is, the silicone resin contains Si—H hydrosilane in a proportion equal to or greater than that of the vinyl group.
- strength of the powder magnetic core after annealing can be raised reliably. That is, when the vinyl group is less than 2%, sufficient strength cannot be obtained, and when it exceeds 10%, the methyl group shown below cannot be contained sufficiently.
- the vortex loss can be reduced by containing 38 to 77% of methyl groups in the side chain of the silicone resin in all side chains.
- the magnetic powder as used in the present invention refers to an aggregate (powder) of magnetic particles having magnetic permeability, and is preferably a soft magnetic metal powder, and examples thereof include iron, cobalt, and nickel. . More preferable materials are iron-based materials such as iron (pure iron), iron-silicon alloys, iron-nitrogen alloys, iron-nickel alloys, iron-carbon alloys, iron-boron alloys, iron. -Cobalt alloys, iron-phosphorus alloys, iron-nickel-cobalt alloys, iron-aluminum-silicon alloys, and the like.
- the magnetic powder can include water atomized powder, gas atomized powder, pulverized powder, etc. When considering the suppression of the breakdown of the insulating layer during pressure molding, select a powder with less unevenness on the surface of the powder. More preferably.
- the method for producing a powder for a powder magnetic core according to the present invention is a method for producing a powder for a powder magnetic core in which the surface of a magnetic powder comprising magnetic particles is coated with an insulating layer, and vinyl silane is formed on the surface layer of the insulating layer. And an insulating layer of a polymer resin containing hydrosilane, and more preferably, the polymer resin insulating layer further contains a silicon oxide precursor that is heated to become silicon oxide. Further, the polymer resin is added to the magnetic powder so that the polymer resin is 0.6% by mass or less with respect to the powder for powder magnetic core, and the added polymer resin More preferably, the polymer resin insulation layer is coated.
- the polymer resin is a silicone resin
- the silicone resin includes, as a side chain, a methyl group and a vinyl group for reacting the hydrosilane with a hydrosilylation reaction, and the silicone resin.
- the resin contains 2 to 10% of the vinyl group in all side chains and 38 to 77% of the methyl group in all side chains.
- the coated polymer resin insulating layer in a heating temperature range of 100 to 160 ° C. and a heating time range of 10 to 45 minutes.
- this heating temperature is less than 100 ° C., or when the heating time is less than 10 minutes, the powder fluidity presumed to be derived from the unreacted functional group is deteriorated.
- this heating temperature exceeds 160 ° C.
- the method for manufacturing a powder for a powder magnetic core according to the present invention includes oxidizing the particle surface so as to form an oxide insulating layer as the insulating layer between the magnetic particles and the polymer resin insulating layer.
- the oxide insulating layer in this case is more preferably an insulating layer containing a phosphate or an Al—Si-based oxide.
- the oxide insulating layer has a two-layer structure, and includes an insulating layer containing a phosphate from the surface of the magnetic particles toward the polymer resin insulating layer, and an Al—Si-based layer. It is more preferable to sequentially form an insulating layer containing an oxide.
- the oxide insulating layer may further contain vinyl silane.
- the present invention also discloses a method for suitably producing a dust core from the dust core powder or the dust core powder obtained by the production method.
- the method for producing a dust core according to the present invention includes a step of pressurizing the dust core powder to form a dust core, and heating the dust core to hydrosilylate the vinyl silane and the hydrosilane. And a step of reacting.
- a Si—C—C—Si bond can be obtained by heating the molded powder magnetic core to cause a hydrosilylation reaction between the insulating layers.
- the mechanical strength of the dust core can be improved. That is, the chemical bond can be obtained between adjacent polymer resin insulating layers.
- the oxide insulating layer contains vinylsilane or hydrosilane, the chemical bond can be obtained also between the oxide insulating layer and the polymer resin insulating layer.
- the silicon oxide precursor forms a silicon oxide phase uniformly dispersed in the polymer resin insulation layer during annealing. And it can suppress that a polymer resin insulating layer shrink
- the hydrosilylation reaction can be expressed by using a catalyst, applying heat, or combining these. More preferably, the heating in the method of manufacturing the dust core is performed under a temperature condition of 300 ° C. to 1000 ° C.
- a hydrosilylation reaction between vinylsilane and hydrosilane can be suitably expressed without using a catalyst.
- the dust core can be annealed in this temperature range, the strain introduced into the dust core can be removed in accordance with the reaction.
- the polymer resin insulation layer contains a silicon oxide precursor
- silicon oxide is generated in the polymer resin insulation layer in the dust core, and volume reduction of the polymer resin insulation layer can be suppressed.
- the heating temperature when the heating temperature is lower than 300 ° C., it is difficult to develop the hydrosilylation reaction without using a catalyst. Furthermore, when a silicon oxide precursor is included, this precursor is not included in this temperature range. It is difficult to become silicon oxide from the body. On the other hand, when the heating temperature is higher than 1000 ° C., the Si—C—C—Si bond bonded by hydrosilylation is broken, and the mechanical strength of the dust core is lowered. It is difficult to ensure the insulation.
- the method for producing a dust core it is more preferable to perform heating for causing hydrosilylation and annealing the dust core in an oxygen-free atmosphere.
- the oxidation of the dust core can be suppressed by annealing in an oxygen-free atmosphere.
- the oxygen-free atmosphere include an inert gas atmosphere such as nitrogen gas, argon gas, and helium gas, or a vacuum, and can suppress oxidation of the dust core due to oxygen gas. If so, the atmosphere is not particularly limited.
- a dust core suitably produced from the powder for dust core is also disclosed.
- the dust core according to the present invention is a dust core including an insulating layer-coated particle in which an insulating layer is coated on a magnetic particle, and the dust core is composed of the insulating layer-coated particles among the insulating layers.
- the insulating layer forming the grain boundary is composed of a polymer resin insulating layer, and has an Si—C—C—Si bond between the polymer resin insulating layers of the adjacent insulating layer covering grains. .
- the present invention while having an Si—C—C—Si bond between the polymer resin insulating layers of the adjacent insulating layer-coated grains, the same or more magnetic characteristics as in the prior art are secured. The strength of the powder magnetic core can be ensured.
- the magnetic particles constituting the powder magnetic core referred to in the present invention correspond to the form after pressure forming of the magnetic particles constituting the powder for powder magnetic core, and have the same composition as the magnetic particles described above. It is what has.
- the insulating layer-coated grains constituting the dust core correspond to the form after pressure forming of the particles constituting the dust core powder (magnetic particles having an insulating layer formed on the particle surface). is there.
- an oxide insulating layer is further formed between the magnetic particles and the polymer resin insulating layer, and the oxide insulating layer is a phosphate or an Al—Si-based oxide. More preferably, the insulating layer contains. Furthermore, as another aspect, the oxide insulating layer has a two-layer structure, and an insulating layer containing phosphate and an Al—Si-based oxide from the magnetic particles toward the polymer resin insulating layer Are sequentially formed. As shown in the powder for powder magnetic core, these oxide insulating layers can improve the conformability between the magnetic particles and the polymer resin insulating layer.
- the dust core according to the present invention more preferably has a Si—C—C—Si bond between the oxide insulating layer and the polymer resin layer. According to the present invention, the mechanical strength of the dust core can be further stabilized by the chemical bond between the layers.
- the dust core according to the present invention preferably further includes silicon oxide in the polymer resin insulating layer, and the silicon oxide is represented by — (Si—O) n— (n is 2 or more). More preferably, it is included as a phase having the siloxane structure shown. According to the present invention, by including such silicon oxide in the polymer resin insulating layer, it is possible to reduce the iron loss and improve the magnetic characteristics of the dust core.
- the magnetic powder core which is ensured in mechanical strength and excellent in insulation and magnetic properties, is used for a stator and a rotor constituting a driving motor for a hybrid vehicle and an electric vehicle, and for a reactor constituting a power converter.
- a stator and a rotor constituting a driving motor for a hybrid vehicle and an electric vehicle
- a reactor constituting a power converter.
- the mechanical strength can be improved by the hydrosilylation reaction between vinylsilane and hydrosilane without deteriorating the magnetic properties of the dust core.
- FIG. 6B is a diagram for explaining a case where the polymer resin contains a silicon oxide precursor.
- FIG. 1 The figure for demonstrating the vortex loss-crushing strength of Example 1 and Comparative Example 1.
- 2 Magnetic powder
- 2A Magnetic particles
- 3A Insulating layer
- 4 Vinylsilane
- 10 Insulating layer coated particles
- 10A Insulating layer coated particles
- 31, 31A Insulating layer containing phosphate (oxide insulation) Layer
- 32, 32A insulating layer (oxide insulating layer) containing Al—Si-based oxide
- 33, 33 ′, 33A, 33B polymer resin insulating layer
- 100 dust core
- FIG. 1 is a schematic view showing a powder for a powder magnetic core according to this embodiment.
- the powder for a powder magnetic core according to this embodiment is an aggregate of particles 10 coated with an insulating layer 3, and the insulating layer 3 covers the particle surfaces 21 of the iron-based magnetic particles 2.
- the insulating layer 3 has a polymer resin insulating layer 33 described later on the surface layer portion (outer layer) of the powder 10 for dust core.
- the magnetic particles 2 are particles made of pure iron manufactured by gas atomization (particles made of gas atomized powder), and are soft magnetic metal particles having an average particle diameter of 450 ⁇ m or less.
- the insulating layer 3 is a multilayered layer composed of oxide insulating layers 31 and 32 and a polymer resin insulating layer 33.
- the oxide insulating layers 31 and 32 are layers formed between the magnetic particles 2 and the polymer resin insulating layer 33, and include an insulating layer 31 containing phosphate and an Al—Si-based oxide containing vinylsilane 4. It is a two-layer structure provided with the insulating layer 32 containing.
- the insulating layer 31 containing phosphate is coated on the surface 21 of the magnetic particle 2, and the insulating layer 32 containing Al—Si-based oxide further covers the insulating layer 31 containing phosphate. Yes. That is, the oxide insulating layer sequentially forms the insulating layer 31 containing phosphate and the insulating layer 32 containing Al—Si-based oxide from the particle surface of the magnetic particle 2 toward the polymer resin insulating layer 33. It will be.
- the insulating layer 31 containing phosphate and the insulating layer 32 containing Al—Si-based oxide function as a base layer, and the insulating layer 31 is made of phosphorous such as PO, SrPO, SrBPO, and the like. It is desirable to include an acid salt, more preferably SrBPO.
- the insulating layer 32 is preferably made of Al—Si alkoxide.
- the polymer resin insulating layer 33 is an insulating layer of a silicone resin containing vinylsilane 4 and hydrosilane, and is coated on the surface of the insulating layer 32 containing an Al—Si-based oxide.
- Such a powder for a powder magnetic core is manufactured as follows. First, a magnetic powder made of pure iron manufactured by gas atomization is prepared. Then, phosphate treatment is performed on the magnetic powder made of the magnetic particles 2.
- This phosphate treatment is a generally known treatment.
- a treatment solution is prepared by dissolving strontium carbonate and boric acid in ion exchange water with phosphoric acid as a main ingredient.
- the magnetic powder is immersed in the treatment liquid, the treatment liquid is stirred, and then dried in a nitrogen atmosphere, whereby the insulating layer 31 containing an oxide whose surface is oxidized and a phosphate is formed. Obtainable.
- Such an insulating layer 31 is a film in which a part of the magnetic particles 2 is a film, and has good compatibility with the insulating layer 32 described later.
- Si alkoxide such as aminopropyltriethoxysilane (preferably Si alkoxide further containing vinyltrimethoxysilane) and Al alkoxide (eg aluminum isobutoxide) are mixed in a dehydrated organic solvent (eg tetravidrofuran).
- a dehydrated organic solvent eg tetravidrofuran.
- a silicone resin-containing solution obtained by dissolving an addition-curable silicone resin containing vinylsilane and hydrosilane in an organic solvent such as alcohol is prepared, and impregnated with a powder composed of the magnetic particles 2 on which the insulating layer 32 is formed.
- the organic solvent is removed by drying.
- a polymer resin insulating layer 33 containing a silicone resin is further formed on the surface of the insulating layer 32.
- the temperature for drying the dehydrated organic solvent and the organic solvent is at least 100 ° C. to 160 ° C. By drying at such a temperature, it will be described later. Suppresses the occurrence of hydrosilylation reaction between vinylsilane and hydrosilane.
- the silicone resin may contain a curing catalyst. However, since the hydrosilylation reaction may occur at a lower temperature during drying, this curing catalyst is not included in this embodiment.
- FIG. 2 is a view for explaining a dust core and a method for manufacturing the same according to the present embodiment.
- A is added to the end of the reference numerals corresponding to the components of the insulating layer-coated particles 10 shown in FIG.
- the magnetic particles 2A constituting the dust core 100 shown in FIG. 2 correspond to the form after the pressure molding of the magnetic particles 2 constituting the dust core powder, and the magnetic particles 2 of FIG. It has an equivalent composition.
- the insulating layer-coated particles 10A constituting the dust core 100 correspond to the form after the pressure forming of the insulating layer-coated particles 10 constituting the dust core powder of FIG.
- a higher fatty acid-based lubricant is applied to the inner surface of the mold, and the powder for the magnetic powder core described above is filled into the mold and pressure-molded.
- the mold may be heated to perform a mold lubrication warm molding method.
- the applied pressure is preferably 500 to 2000 MPa.
- a dust core including the insulating layer coated grains 10A in which the insulating layer 3A is coated on the surfaces of the magnetic grains 2A is formed.
- the insulating layer 3A forms a polymer resin insulating layer 33A on the surface layer portion of the insulating layer-coated grain 10A.
- the insulating layer that forms the grain boundaries of the insulating layer-coated grains 10 ⁇ / b> A and 10 ⁇ / b> A among the insulating layer 3 is composed of the polymer resin insulating layer 33 ⁇ / b> A.
- Layers 32A are formed sequentially.
- a hydrosilylation reaction between vinylsilane and hydrosilane is caused to occur. Specifically, by heating the dust core after molding under a temperature condition within a temperature range of 300 ° C. to 1000 ° C., more preferably in a nitrogen atmosphere or in a vacuum (under an oxygen-free atmosphere), Between the insulating layer 32A containing the Al—Si-based oxide of the powder 10 for dust core and the polymer resin insulating layer 33A, and between the polymer resin insulating layers 33A, 33A of the powders for dust core adjacent to each other. The vinyl silane and hydrosilane are subjected to a hydrosilylation reaction, and the dust core 100 is annealed. As described above, in this embodiment, the hydrosilylation reaction can be developed simultaneously with the annealing of the dust core, and the Si—C—C—Si bond can be obtained.
- the hydrosilylation reaction causes a gap between the insulating layer 32A of the insulating layer-covered grain 10A and the polymer resin insulating layer 33A (that is, the grain boundary of the insulating layer-covered grain).
- Si—C—C—Si bonds are formed between the adjacent polymer resin insulation layers 33A and 33A of the powder for powder magnetic core, and the powder magnetic core applied at the time of molding is annealed. The distortion of the magnetic particles 2A can be removed.
- an insulating layer 31A containing phosphate is formed on the surface of the magnetic particles 2A, and the adhesion between the insulating layer 31A containing phosphate and the magnetic particles 2A is improved. Further, by sequentially laminating the insulating layer 32A containing an Al—Si-based oxide and the polymer resin insulating layer 33A, the adhesion between these layers can be improved. As a result, the conformability of the polymer resin insulating layer 33A with respect to the magnetic particles 2A is further improved.
- the polymer resin insulating layer 33 containing vinylsilane and hydrosilane has a Si—C—C—Si bond formed by subjecting the dust core to a hydrosilylation reaction during annealing after molding. Since it can produce
- this phenomenon becomes remarkable when annealing is performed at 600 ° C. or higher in order to remove the distortion of the magnetic particles 2A during molding.
- the molded dust core has an increased eddy current loss, which may deteriorate the magnetic properties of the dust core.
- a polymer resin insulation layer 33 ′ in which the amount of silicon oxide precursor (methyl straight silicone resin) is increased is formed on the polymer resin insulation layer 33 described above.
- This type of silicon oxide precursor becomes a silicon oxide phase when heated at 300 ° C. or higher.
- a resin methyl straight silicone in which a silicon oxide precursor or a methyl group is increased to an addition-curing type silicone resin at the stage of forming the polymer resin insulation layer 32 described above.
- Resin a resin (methyl straight silicone) in which a silicon oxide precursor or a methyl group is increased to an addition-curing type silicone resin at the stage of forming the polymer resin insulation layer 32 described above.
- Resin is added, these are dissolved in an organic solvent such as alcohol, impregnated with the magnetic powder 2 on which the insulating layer 32 is formed, and then the organic solvent is dried and removed. Further, since the drying temperature is less than 300 ° C. (preferably 100 ° C. to 160 ° C.), at this point, it does not become Si—C—C—Si, but Si—C ⁇ C and Si—H, It will be included in the polymer resin insulation layer 33 '.
- the magnetic powder obtained is subjected to pressure molding and annealing to produce a powder magnetic core.
- the hydrosilylation reaction as shown above is expressed to form Si—C—C—Si bonds, and a silicon oxide phase is formed.
- the silicon oxide phase may be any of a crystallized phase, an amorphized phase, and a combination of these phases.
- Such a — (Si—O) n— Due to the phase having a siloxane structure represented by n is 2 or more), the volume of the produced polymer resin insulating layer 33B of the dust core can be suppressed. In this way, while maintaining the mechanical strength of the powder magnetic core, it is possible to suppress a decrease in insulation between the magnetic particles 2A and 2A and to suppress a decrease in eddy current loss (iron loss) of the powder magnetic core.
- Example 1 ⁇ Preparation of powder for dust core> A gas atomized powder (iron powder) made of pure iron particles having a particle diameter of 150 ⁇ m to 212 ⁇ m was prepared and subjected to a base treatment containing phosphate. Specifically, a coating solution was prepared by dissolving 0.57 g of strontium carbonate, 0.15 g of boric acid, and 1.1 g of phosphoric acid in 100 ml of ion-exchanged water. 100 g of the above iron powder was put into a 500 ml beaker, 20 ml of this coating solution was added, and lightly stirred. Thereafter, this sample was dried at 120 ° C. for 1 hour in an inert oven in a nitrogen atmosphere to form an insulating layer containing phosphate.
- iron powder made of pure iron particles having a particle diameter of 150 ⁇ m to 212 ⁇ m was prepared and subjected to a base treatment containing phosphate.
- a coating solution was prepared by dissolving 0.57 g
- a silicone resin containing vinylsilane and hydrosilane (X-40-2667A (manufactured by Shin-Etsu Chemical Co., Ltd.)) was dissolved in 50 ml of isopropyl alcohol.
- the above-described iron powder is added to this solution, and the solvent is evaporated in the range of 30 to 120 minutes while stirring the solution and powder and heating with an external heater, and the solution is heated to 100 ° C to 200 ° C. Drying was performed in the range.
- the powder for powder magnetic cores in which the silicone resin insulating layer containing vinylsilane and hydrosilane was formed on the surface of the magnetic particles was manufactured.
- the silicone resin insulation layer was coated with a silicone resin insulation layer by adding a silicone resin to the magnetic powder so that the amount of the powder was 0.4% by mass with respect to the powder magnetic core powder.
- a ring-shaped powder magnetic core with an outer diameter of 39 mm, an inner diameter of 30 mm, and a thickness of 5 mm is produced by a mold lubrication warm molding method with a mold temperature of 130 ° C. and a molding pressure of 1600 MPa did. Then, after the molding, heat treatment was performed in a nitrogen atmosphere in the range of 300 ° C. to 1000 ° C. for 1 hour under the conditions shown in FIG.
- Example 1 In the same manner as in Example 1, powder for powder magnetic core was produced. The difference from Example 1 is that the phosphoric acid treatment was not performed, and that a silicone resin insulating layer was formed using a silicone resin (KR242A (manufactured by Shin-Etsu Chemical Co., Ltd.)) containing no vinylsilane and hydrosilane. . And like Example 1, the dust core was created on the conditions shown in FIG.
- Example 1 the improvement of the crushing strength in Example 1 is considered to be caused by the generation of Si—C—C—Si bonds between the silicone resin insulating layers by the hydrosilylation reaction between vinylsilane and hydrosilane.
- the temperature exceeds 1000 ° C., it is presumed that the Si—C—C—Si bond bonded by hydrosilylation is broken and the strength of the crushing strength of Example 1 is reduced.
- Example 1 As shown in FIG. 6, the crushing strength of Example 1 is improved in Example 1 and Comparative Example 1, while the equivalent vortex loss is achieved. As shown in FIG. Higher magnetic flux density than Example 1 but higher strength. From this, it is considered that Example 1 has high mechanical strength while having the same magnetic characteristics as Comparative Example 1.
- Example 2 A powder for a powder magnetic core was produced in the same manner as in Example 1. The difference from Example 1 is that the manufacturing method of the silicone resin insulating layer containing vinylsilane and hydrosilane is different. Specifically, as a material for the silicone resin insulating layer, 0.32 g (80 mass%) of a silicone resin containing vinylsilane and hydrosilane (X-40-2667A (manufactured by Shin-Etsu Chemical Co., Ltd.): hereinafter referred to as XA), methyl-based straight Silicone resin insulation using a solution containing 0.08 g (20% by mass) of a resin (KR242A (manufactured by Shin-Etsu Chemical Co., Ltd.): hereinafter referred to as KR) rich in silicone resin (silicon oxide precursor) in 50 ml of isopropyl alcohol.
- XA methyl-based straight Silicone resin insulation using a solution containing 0.08 g (20% by mass) of a resin
- the drying process is the same as that in the first embodiment. Further, in the same manner, a solution in which the amount of XA is 0.24 g (60% by mass), the amount of KR is 0.16 g (40% by mass), the amount of XA is 0.16 g (40% by mass), KR A mixture of 0.24 g (60% by mass) and a solution of XA: 0.08 g (20% by mass) and KR: 0.32 g (80% by mass)
- the silicone resin insulating layer was coated by the same method as described above.
- the powder magnetic core was manufactured for every annealing temperature shown in FIG. 8 on the conditions similar to Example 1 from the obtained powder for powder magnetic cores.
- the silicone resin is added to the magnetic powder so that the total amount of these silicone resins is 0.4 mass% with respect to the powder for powder magnetic core, and the silicone resin insulating layer is covered.
- Example 3 In the same manner as in Example 2, a powder for a powder magnetic core was produced under the conditions shown in FIG. 8, and a powder magnetic core was produced from the powder for a powder magnetic core.
- the conditions different from those of Example 2 were that, when the powder for powder magnetic core was produced, a Si—Al-based insulating layer was further coated on the phosphate insulating layer, and on that layer, The silicone resin insulating layer is coated under the following conditions.
- the proportion of XA is 60% by mass
- the proportion of KR is 40% by mass
- 50 ml of isopropyl alcohol is used as a solvent.
- a silicone resin was added to the magnetic powder to coat the silicone resin insulation layer. Further, as a heat treatment, this powder for powder magnetic core was subjected to a heat treatment at 130 ° C. for 20 minutes.
- Example 2 In the same manner as in Example 3, in the same manner as in Example 2, under the conditions shown in FIG. 8, a powder magnetic core powder was produced, and a powder magnetic core was produced from this powder magnetic core powder.
- the difference from Example 3 is that the powder for powder magnetic core was manufactured by setting the ratio of XR to 100%.
- Example 2 As in Example 1, the crushing strength, magnetic flux density, and eddy loss were evaluated with an AC BH analyzer. The results are shown in FIGS. 9 to 14 also show the results of Example 1 and Comparative Example 1 described above.
- FIG. 9 is a graph showing the relationship between the vortex loss and the crushing strength at the annealing temperature of 600 ° C. in Examples 1 and 2 and Comparative Example 1.
- FIG. 10 is a graph showing the relationship between the XA ratio [mass%] at an annealing temperature of 600 ° C., the crushing strength, eddy current loss (eddy loss), and magnetic flux density.
- FIG. 11 is a diagram showing the relationship between the annealing temperature and the crushing strength of Examples 1 and 2 and Comparative Example 1.
- FIG. 12 is a diagram showing the relationship between the annealing temperature and eddy loss in Examples 1 and 2 and Comparative Example 1.
- FIG. 13 is a graph showing the relationship between the vortex loss and the crushing strength in Examples 1 to 3 (annealing temperature 600 ° C.) and Comparative Example 2, and FIG. 14 shows Examples 1 to 3 (annealing temperature 600 ° C.).
- FIG. 5 is a diagram showing the relationship between magnetic flux density and crushing strength in Comparative Example 2.
- the content of Si—C ⁇ C that is, the content of vinyl groups
- the content of Si—CH 3 that is, the content of methyl groups
- This content rate is a ratio of the number of vinyl groups and methyl groups in the side chain in all side chains of the mixed silicone resin. It has also been confirmed that this silicone resin contains Si—H at the same rate or higher than the vinyl group. The results are also shown in Table 1 below.
- Example 2 results 2 and discussion 2 As shown in FIG. 9, the crushing strength of Example 2 was higher than that of Example 1 and Comparative Example 1, and the vortex loss of Example 2 was lower than the others. From this result, the powder magnetic core of Example 2 suppressed the decrease in the volume of the silicone resin insulating layer by forming the silicon oxide phase by adding KR while maintaining the strength improvement by the hydrosilylation reaction during annealing. (Decrease in insulation properties is suppressed), and eddy current loss (iron loss) is considered to be smaller than in Example 1.
- the crushing strength is It can be said that the increase in eddy loss is suppressed without decreasing the magnetic flux density. That is, from FIG. 10 and Table 1, it is preferable that the vinyl group contains 2 to 10% of all side chains and the methyl group contains 38 to 77% of all side chains. ) Is hydrosilylated with hydrosilane to contribute to the crushing strength, and further, by containing — (Si—O) n— or CH 3 in the range shown in Table 1, volume reduction is suppressed, and vortex loss It is thought that it contributes to the reduction of.
- Example 2 As shown in FIG. 11, the crushing strength of Example 2 was higher than that of Example 1 and Comparative Example 1 regardless of the annealing temperature. This is presumed that since the polymer resin insulation layer contains KR, which is a silicon oxide precursor, volume reduction of the silicone resin insulation layer is suppressed, resulting in a dense resin insulation layer, resulting in improved strength.
- KR which is a silicon oxide precursor
- Example 3 since the wettability and familiarity of the silicone resin insulating layer were improved by further providing the Si—Al insulating layer, It is considered that the insulation was ensured even with a smaller resin addition amount. Further, for the same reason as that described in Example 2 above, it is considered that Example 3 has an increased crushing strength.
- Example 4 A dust core was produced in the same manner as in Example 3. The difference from Example 3 is that the ratio of the silicone resin to the entire powder was added at a ratio as shown in FIG. 15 (the resin addition ratio was changed), and the ratio of XA was 40% by mass with respect to the entire silicone resin. This is the point. Further, the powder magnetic core powder after the silicone resin insulating layer is coated is also heat-treated at 160 ° C. for 45 minutes. For the obtained dust core, the crushing strength was measured in the same manner as in Example 1. The result is shown in FIG.
- Example 5 A dust core was produced in the same manner as in Example 4. The difference from Example 4 is that the ratio of the silicone resin to the whole powder is 0.4% by mass, and this powder magnetic core is used as a heat treatment of the powder for the powder magnetic core after coating the silicone resin insulating layer. The heat treatment temperature was changed with respect to the powder for use. With respect to the obtained dust core, the magnetic flux density and vortex loss were measured in the same manner as in Example 1. The result is shown in FIG.
- Example 6 A dust core was produced in the same manner as in Example 4. The difference from Example 4 is that the ratio of the silicone resin to the whole powder is 0.4% by mass, and this powder magnetic core is used as a heat treatment of the powder for the powder magnetic core after coating the silicone resin insulating layer. The heat treatment time is changed with respect to the powder for use. With respect to the obtained dust core, the magnetic flux density and vortex loss were measured in the same manner as in Example 1. The result is shown in FIG.
- the ratio of the silicone resin insulation layer (silicone resin ratio) in one particle of the powder for the powder magnetic core, that is, the addition ratio of the silicone resin to the magnetic powder is 0.6% by mass or less. More preferably. It is considered that the strength of the dust core (compression ring strength) can be increased by forming the silicone resin insulating layer so as to have this ratio.
- the coated polymer resin insulating layer it is more preferable to heat-treat the coated polymer resin insulating layer at a heating temperature of 100 to 160 ° C. and a heating time of 10 to 45 minutes. .
- this heating temperature is less than 100 ° C., or when the heating time is less than 10 minutes, the powder fluidity presumed to be derived from the unreacted functional group is deteriorated.
- the powder fluidity is deteriorated.
- the powder does not flow out of the funnel due to the deterioration of the powder fluidity. This deterioration of the fluidity of the powder becomes a serious problem during mass production of dust cores.
- this heating temperature exceeds 160 ° C. or when the heating time exceeds 45 minutes, a large amount of silicon oxide is generated before forming the dust core, and as a result, the dust core is annealed. The amount of silicon oxide produced between particles at the time decreases. Thus, it is assumed that the effect of improving the strength of the dust core cannot be sufficiently obtained.
- the oxide insulating layer has a two-layer structure, but only the insulating layer containing phosphate can be used as long as the compatibility between the magnetic powder and the polymer resin insulating layer can be secured.
- it may be a multi-layer structure, and all of them may contain vinyl silane and hydrosilane.
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Abstract
Description
<圧粉磁心用粉末の作製>
粒径が150μm~212μmの純鉄粒子からなるガスアトマイズ粉末(鉄粉)を準備して、リン酸塩を含む下地処理を施した。具体的には、イオン交換水100mlに、炭酸ストロンチウム0.57g、ホウ酸0.15g、リン酸1.1gを溶解してコーティング液を調製した。500mlビーカーに上記鉄粉を100g入れ、このコーティング液20mlを加えて、軽く攪拌した。その後、この試料を、窒素雰囲気中のイナートオーブンで120℃、1時間の乾燥処理を行い、リン酸塩を含む絶縁層を形成した。
圧粉磁心用粉末を金型に投入し、金型温度130℃、成形圧力1600MPaの金型潤滑温間成形法で、外径39mm、内径30mm、厚さ5mmのリング形状の圧粉磁心を作製した。そして、成形後、窒素雰囲気下で、図4に示す条件で300℃~1000℃の範囲で1時間の熱処理を行なった。
実施例1と同じようにして、圧粉磁心用粉末を作製した。実施例1と相違する点は、リン酸処理を行わなかった点と、ビニルシランとヒドロシランを含まないシリコーン樹脂(KR242A(信越化学工業製))を用いて、シリコーン樹脂絶縁層を形成した点である。そして、実施例1と同様に、図4に示す条件で圧粉磁心を作成した。
<リング試験片の評価>
オートグラフを用いて製作した実施例1及び比較例1のリング試験片の圧環強度を評価した。また、リング試験片にコイルを巻き、直流磁気磁束計で磁束密度を評価し、交流BHアナライザーで渦損を評価した。この結果を、図4~7に示す。なお、図4~7に示す、実施例1及び比較例1の磁束密度、圧環強度、渦損は、比較例1の圧粉磁心の熱処理温度(焼鈍温度)を600℃における磁束密度、圧環強度、渦損を基準(1.0)として正規化した値である。なお、これ以降に示す実施例及び比較例の値も同様の正規化を行った値を示している。
図5に示すように、実施例1の場合には、リング試験片の圧環強度を向上させるためには、300℃以上、1000℃以下の熱処理が好ましいと考えられる。実施例1の場合は、300℃~800℃、より好ましくは300℃~400℃の熱処理温度(加熱温度)において、圧環強度が特に向上した。
実施例1と同じように圧粉磁心用粉末を製作した。実施例1と相違する点は、ビニルシランとヒドロシランを含むシリコーン樹脂絶縁層の製造方法が異なる。具体的には、シリコーン樹脂絶縁層の材料として、ビニルシランとヒドロシランを含むシリコーン樹脂(X-40-2667A(信越化学工業製):以下XAという)0.32g(80質量%)と、メチル系ストレートシリコーン樹脂(酸化珪素前駆体)を多く含む樹脂(KR242A(信越化学工業製):以下KRという)0.08g(20質量%)とを、イソプロピルアルコール50mlに溶解した溶液を用いて、シリコーン樹脂絶縁層を被覆した点である。なお、乾燥処理などは、実施例1と同様である。さらに、同様にして、XAの量:0.24g(60質量%)、KRの混合量:0.16g(40質量%)とした溶液、XAの量:0.16g(40質量%)、KRの混合量:0.24g(60質量%)とした溶液、及び、XAの量:0.08g(20質量%)、KRの混合量:0.32g(80質量%)とした溶液を用いて、上に示す方法と同様の方法で、シリコーン樹脂絶縁層を被覆した。このようにして、得られた圧粉磁心用粉末から、実施例1と同様の条件で、図8に示す焼鈍温度ごとに圧粉磁心を製造した。なお、これらのシリコーン樹脂の総量は、圧粉磁心用粉末に対して、0.4質量%となるように、磁性粉末にシリコーン樹脂を添加して、シリコーン樹脂絶縁層の被覆を行っている。
実施例2と同様にして、図8に示す条件で、圧粉磁心用粉末を製造し、この圧粉磁心用粉末から圧粉磁心を製造した。なお、実施例2と相違する条件は、圧粉磁心用粉末を製造する際に、リン酸塩の絶縁層の上に、Si-Al系の絶縁層をさらに被覆し、その層の上に、以下に示す条件でシリコーン樹脂絶縁層の被覆を行った点である。
実施例3と同じようにして、実施例2と同様にして、図8に示す条件で、圧粉磁心用粉末を製造し、この圧粉磁心用粉末から圧粉磁心を製造した。実施例3と相違する点は、XRの割合を100%にして、圧粉磁心用粉末を製造した点である。
実施例1と同じように、圧環強度、交流BHアナライザーで磁束密度、渦損を評価した。この結果を図9~14に示す。なお、図9~14に、上述した実施例1及び比較例1の結果も合わせて記載した。
図9に示すように、実施例2の圧環強度は、実施例1及び比較例1よりも高く、実施例2の渦損は、他のものよりも低くかった。この結果から、実施例2の圧粉磁心は、焼鈍時のヒドロシリル化反応による強度向上を維持しつつ、KRを加えることにより、酸化珪素の相の形成により、シリコーン樹脂絶縁層の体積減少が抑制され(絶縁性の低下が抑制され)、渦電流損失(鉄損)が実施例1よりも小さくなったと考えられる。
実施例3と同様にして、圧粉磁心を製造した。実施例3と相違する点は、粉末全体に対するシリコーン樹脂の割合を図15に示すよう割合で添加した(樹脂添加率を変更した)点、シリコーン樹脂全体に対して、XAの割合を40質量%とした点である。さらに、シリコーン樹脂絶縁層の被覆を行ったのちの圧粉磁心用粉末の熱処理として、この圧粉磁心用粉末に対して160℃、45分の熱処理を行った点も相違する。得られた圧粉磁心に対して、実施例1と同じようにして、圧環強度を測定した。この結果を図15に示す。
実施例4と同様にして、圧粉磁心を製造した。実施例4と相違する点は、粉末全体に対するシリコーン樹脂の割合を0.4質量%にした点、シリコーン樹脂絶縁層の被覆を行ったのちの圧粉磁心用粉末の熱処理として、この圧粉磁心用粉末に対して熱処理温度を変化させた点である。得られた圧粉磁心に対して、実施例1と同じようにして、磁束密度と渦損を測定した。この結果を図16に示す。
実施例4と同様にして、圧粉磁心を製造した。実施例4と相違する点は、粉末全体に対するシリコーン樹脂の割合を0.4質量%にした点、シリコーン樹脂絶縁層の被覆を行ったのちの圧粉磁心用粉末の熱処理として、この圧粉磁心用粉末に対して熱処理時間を変化させた点である。得られた圧粉磁心に対して、実施例1と同じようにして、磁束密度と渦損を測定した。この結果を図17に示す。
図15に示すように、圧粉磁心用粉末の一粒子におけるシリコーン樹脂絶縁層の割合(シリコーン樹脂の割合)、すなわち、磁性粉末に対しするシリコーン樹脂を添加率は、0.6質量%以下であることがより好ましい。この割合となるように、シリコーン樹脂絶縁層を形成することにより、圧粉磁心の強度(圧環強度)を高めることができると考えられる。
Claims (22)
- 磁性粒子からなる磁性粉末の粒子表面に絶縁層が被覆された圧粉磁心用粉末であって、
前記絶縁層は、該絶縁層の表層部に、ビニルシランとヒドロシランを含む高分子樹脂の絶縁層を備えることを特徴とする圧粉磁心用粉末。 - 前記磁性粒子と前記高分子樹脂絶縁層との間に、前記絶縁層として、酸化物絶縁層をさらに備えることを特徴とする請求項1に記載の圧粉磁心用粉末。
- 前記酸化物絶縁層は、リン酸塩又はAl-Si系酸化物を含む絶縁層であることを特徴とする請求項2に記載の圧粉磁心用粉末。
- 前記酸化物絶縁層は、二層構造であり、前記磁性粒子の表面から前記高分子樹脂絶縁層に向かって、リン酸塩を含む絶縁層、及びAl-Si系酸化物を含む絶縁層を順次備えることを特徴とする請求項2に記載の圧粉磁心用粉末。
- 前記酸化物絶縁層は、ビニルシランを含むことを特徴とする請求項2~4のいずれかに記載の圧粉磁心用粉末。
- 前記高分子樹脂絶縁層は、シリコーン樹脂絶縁層であることを特徴とする請求項1~5のいずれかに記載の圧粉磁心用粉末。
- 前記高分子樹脂絶縁層には、加熱して酸化珪素となる酸化珪素前駆体をさらに含むことを特徴とする請求項6に記載の圧粉磁心用粉末。
- 前記圧粉磁心用粉末の前記高分子樹脂の割合は、0.6質量%以下であることを特徴とする請求項6または7に記載の圧粉磁心用粉末。
- 前記シリコーン樹脂絶縁層を構成するシリコーン樹脂は、側鎖として、メチル基と、前記ヒドロシランとヒドロシリル化反応をさせるためのビニル基とを含み、
前記シリコーン樹脂は、前記ビニル基を、全側鎖中、2~10%含有し、前記メチル基を、全側鎖中、38~77%含有することを特徴とする請求項6~8のいずれかに記載の圧粉磁心用粉末。 - 磁性粒子からなる磁性粉末の粒子表面に絶縁層を被覆した圧粉磁心用粉末の製造方法であって、
該絶縁層の表層部に、ビニルシランとヒドロシランを含む高分子樹脂の絶縁層を被覆することを特徴とする圧粉磁心用粉末の製造方法。 - 前記高分子樹脂絶縁層に、加熱して酸化珪素となる酸化珪素前駆体をさらに含有することを特徴とする請求項10に記載の圧粉磁心用粉末の製造方法。
- 前記圧粉磁心用粉末に対して、前記高分子樹脂が0.6質量%以下となるように、前記磁性粉末に前記高分子樹脂を添加して、前記高分子樹脂絶縁層の被覆を行うことを特徴とする請求項10または11に記載の圧粉磁心用粉末。
- 前記高分子樹脂は、シリコーン樹脂であり、該シリコーン樹脂は、側鎖として、メチル基と、前記ヒドロシランとヒドロシリル化反応と反応させるためのビニル基と、を含み、
前記シリコーン樹脂は、前記ビニル基を、全側鎖中、2~10%含有し、前記メチル基を、全側鎖中、38~77%含有することを特徴とする請求項10~12のいずれかに記載の圧粉磁心用粉末の製造方法。 - 前記被覆された高分子樹脂絶縁層に対して、加熱温度100~160℃の範囲で、かつ、加熱時間10~45分の範囲で、熱処理を行うことを特徴とする請求項10~13のいずれかに記載の圧粉磁心の製造方法。
- 請求項1~9のいずれかに記載の圧粉磁心用粉末、または、請求項10~14のいずれかに記載の製造方法により製造された圧粉磁心用粉末から圧粉磁心を製造する方法であって、
前記圧粉磁心用粉末を加圧して圧粉磁心に成形する工程と、
該圧粉磁心を加熱することにより、前記ビニルシランと前記ヒドロシランとをヒドロシリル化反応させる工程と、を少なくとも含むことを特徴とする圧粉磁心の製造方法。 - 前記加熱を、300℃~1000℃の温度条件で行なうことを特徴とする請求項15に記載の圧粉磁心の製造方法。
- 磁性粒に絶縁層が被覆された絶縁層被覆粒を含む圧粉磁心であって、
該圧粉磁心は、前記絶縁層のうち、前記絶縁層被覆粒同士の粒界を形成する絶縁層が、高分子樹脂絶縁層からなり、隣接する前記絶縁層被覆粒の高分子樹脂絶縁層同士の間において、Si-C-C-Si結合を有することを特徴とする圧粉磁心。 - 前記絶縁層は、前記磁性粒と前記高分子樹脂絶縁層との間に、酸化物絶縁層をさらに備えることを特徴とする請求項17に記載の圧粉磁心。
- 前記酸化物絶縁層は、リン酸塩又はAl-Si系酸化物を含む絶縁層であることを特徴とする請求項18に記載の圧粉磁心。
- 前記酸化物絶縁層は、二層構造であり、前記磁性粒から前記高分子樹脂絶縁層に向かって、リン酸塩を含む絶縁層、及びAl-Si系酸化物を含む絶縁層を順次備えることを特徴とする請求項18に記載の圧粉磁心。
- 前記酸化物絶縁層と前記高分子樹脂層との間に、Si-C-C-Si結合を有することを特徴とする請求項18~20のいずれかに記載の圧粉磁心。
- 前記高分子樹脂絶縁層に、酸化珪素をさらに含むことを特徴とする請求項17~21のいずれかに記載の圧粉磁心。
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JP2017112218A (ja) * | 2015-12-16 | 2017-06-22 | 株式会社村田製作所 | 電子部品 |
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