WO2018052108A1 - 磁心およびコイル部品 - Google Patents
磁心およびコイル部品 Download PDFInfo
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- WO2018052108A1 WO2018052108A1 PCT/JP2017/033423 JP2017033423W WO2018052108A1 WO 2018052108 A1 WO2018052108 A1 WO 2018052108A1 JP 2017033423 W JP2017033423 W JP 2017033423W WO 2018052108 A1 WO2018052108 A1 WO 2018052108A1
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- magnetic core
- based alloy
- peak intensity
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- magnetic
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Images
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- C22C—ALLOYS
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- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- 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
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- 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
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- 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
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- 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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- H01F17/04—Fixed inductances of the signal type with magnetic core
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- H01F27/28—Coils; Windings; Conductive connections
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- H01F3/08—Cores, Yokes, or armatures made from powder
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- H01F27/00—Details of transformers or inductances, in general
- H01F27/28—Coils; Windings; Conductive connections
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- H01F27/2828—Construction of conductive connections, of leads
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- H01F27/28—Coils; Windings; Conductive connections
- H01F27/29—Terminals; Tapping arrangements for signal inductances
- H01F27/292—Surface mounted devices
Definitions
- the present invention relates to a magnetic core using Fe-based alloy particles containing Al, and a coil component using the same.
- coil parts such as inductors, transformers, chokes, and motors have been used in a wide variety of applications such as home appliances, industrial equipment, and vehicles.
- a general coil component is often composed of a magnetic core (magnetic core) and a coil wound around the magnetic core.
- ferrite having excellent magnetic properties, flexibility in shape, and cost is widely used.
- magnetic alloy powders such as Fe—Si, Fe—Ni, Fe—Si—Cr, and Fe—Si—Al are used as the metal magnetic powder.
- the magnetic core obtained by consolidating the compact of the magnetic alloy powder has a high saturation magnetic flux density, but has a low electrical resistivity because it is an alloy powder, and the magnetic alloy powder is previously prepared using water glass or a thermosetting resin. Insulation coating is often used.
- the magnetic core used for the coil component is required to have a high initial permeability.
- the initial permeability tends to increase as the density of the magnetic core is increased by increasing the density of the compact to reduce the voids between the particles or increasing the heat treatment temperature.
- molding at a high pressure may cause damage to the mold and may limit the magnetic core shape.
- the heat treatment temperature is raised, the sintering of the metal-based magnetic powder proceeds and insulation may not be obtained.
- the present invention has been made in view of the above problems, and an object thereof is to provide a magnetic core having a high initial permeability and a coil component using the same.
- a first invention is a magnetic core using particles of an Fe-based alloy containing Al, The particles of the Fe-based alloy are bonded through an oxide derived from the Fe-based alloy,
- the magnetic core has a peak intensity ratio (P3 / P2) between 0.015 and 0.050 of the peak intensity P3 of the superlattice peak of the Fe 3 Al ordered structure appearing in the vicinity of ° C and the peak intensity P2.
- the initial permeability ⁇ i is preferably 55 or more.
- the second invention is a coil component including the magnetic core and the coil of the first invention.
- FIG. 2B is a partial cross-sectional view taken along line A-A ′ in FIG. 2A.
- Sample No. produced in the Examples 5-No. It is a figure explaining the X-ray-diffraction spectrum of * 9. It is a figure which shows the relationship between peak intensity ratio (P1 / P2) and initial permeability (mu) i.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- Sample No. produced in the Examples 6 is a SEM image of a cross section of 6 magnetic cores.
- FIG. 1A is a perspective view schematically showing a magnetic core of the present embodiment
- FIG. 1B is a front view thereof.
- the magnetic core 1 includes a cylindrical conductor winding part 5 for winding a coil, and a pair of flange parts 3a and 3b disposed to be opposed to both ends of the conductor winding part 5, respectively.
- the appearance of the magnetic core 1 has a drum shape.
- the cross-sectional shape of the conductive wire winding part 5 is not limited to a circle, and any shape such as a square, a rectangle, and an ellipse can be adopted.
- the collar part may be arrange
- the illustrated shape example shows one form of the magnetic core configuration, and the effects of the present invention are not limited to the illustrated configuration.
- the magnetic core according to the present invention is formed of a heat treatment body of Fe-based alloy particles, and is an aggregate in which a plurality of Fe-based alloy particles containing Al are bonded through an oxide layer containing Fe oxide. It is configured. Furthermore, the magnetic core according to the present invention has Fe 3 Al which is a compound of Fe and Al.
- the Fe oxide is an oxide derived from an Fe-based alloy formed by heat treatment of an Fe-based alloy, and is present at the grain boundary between the particles of the Fe-based alloy or at the surface of the magnetic core, and the insulating layer separating the particles Also works.
- the oxide of Fe formed from the Fe-based alloy is regulated to 0.015 or less in the peak intensity ratio (P1 / P2). And a compound derived from Fe 3 Al, restricted to 0.015 or 0.050 or less at the peak intensity ratio (P3 / P2).
- the initial permeability can be increased by defining each peak intensity ratio (P1 / P2, P3 / P2).
- the peak intensity ratio (P1 / P2) of the X-ray diffraction is determined by analyzing the magnetic core by the X-ray diffraction method (XRD), and the peak intensity P1 of the Fe oxide (104 plane) and the maximum diffraction intensity in the X-ray diffraction spectrum.
- the Fe 3 Al ordered structure superlattice, the Fe oxide, and the Fe-based alloy of the bcc structure were measured using an X-ray diffractometer, and the JCPDS (Joint Committee) was obtained from the obtained X-ray diffraction chart. on Powder Diffraction Standards) card.
- the superlattice peak of the Fe 3 Al ordered structure is Fe 3 Al from JCPDS card: 00-050-0955, the Fe oxide is from the diffraction peak to Fe 2 O 3 by JCPDS card: 01-079-1741, and the bcc structure
- This Fe-based alloy can be identified as bcc-Fe by JCPDS card: 01-071-4409.
- the diffraction peak angle fluctuates with the data of the JCPDS card due to the solid solution of elements and includes errors, so the case where the diffraction peak angle (2 ⁇ ) is very close to each JCPDS card is defined as “near”. ing. Specifically, the diffraction peak angle (2 ⁇ ) of Fe 3 Al is set to 26.3 ° to 26.9 °, and the diffraction peak angle (2 ⁇ ) of Fe oxide is set to a range of 32.9 ° to 33.5 °. The angle (2 ⁇ ) of the diffraction peak of the Fe-based alloy having the bcc structure was 44.2 ° to 44.8 °.
- the Fe-based alloy contains Al, and may further contain Cr from the viewpoint of corrosion resistance, and Si in anticipation of improvement of magnetic characteristics. Further, it may contain impurities mixed from raw materials and processes.
- the composition of the Fe-based alloy of the present invention is not particularly limited as long as it can constitute a magnetic core that can obtain conditions such as the aforementioned peak intensity ratios (P1 / P2, P3 / P2).
- Al is an element that enhances corrosion resistance and the like, and contributes to oxide formation by heat treatment described later. Further, from the viewpoint of contributing to the reduction of magnetocrystalline anisotropy, the Al content in the Fe-based alloy is set to 13.8 mass% or more and 16 mass% or less. If the Al content is too small, the effect of reducing the magnetocrystalline anisotropy is not sufficient, and the effect of improving the core loss cannot be obtained.
- the stoichiometric composition bal. Fe25at. It is known that Fe 3 Al is generated in the vicinity of% Al (bal.Fe13.8Al in mass%). Therefore, the composition of the Fe-based alloy is preferably in a range including the stoichiometric composition of Fe 3 Al in the binary composition of Fe and Al. On the other hand, if the amount of Al is excessive, the saturation magnetic flux density is lowered and sufficient magnetism may not be obtained. Therefore, Al is preferably 15.5% by mass or less.
- Cr is a selective element and may be included in the Fe-based alloy as an element that enhances the corrosion resistance of the alloy.
- Cr is useful for constituting the Fe-based alloy particles to be bonded through the Fe-based alloy oxide layer in the heat treatment described later.
- the content of Cr in the Fe-based alloy is preferably 0% by mass or more and 7% by mass or less. If the amount of Al or Cr increases too much, the saturation magnetic flux density decreases and the alloy becomes hard. Therefore, the total content of Cr and Al is more preferably 18.5% by mass or less.
- the content of Al is larger than that of Cr so that an oxide layer having a high Al ratio can be easily formed.
- the Fe-based alloy is composed of Al, and if necessary, the remainder other than Cr is mainly composed of Fe.
- other elements can be included as long as advantages such as improvement of formability and magnetic properties are exhibited.
- the nonmagnetic element lowers the saturation magnetic flux density and the like, the content of such other elements is preferably 1.5% by mass or less of the total amount of 100% by mass.
- Si is usually used as a deoxidizer in order to remove oxygen (O) which is an impurity.
- O oxygen
- the added Si is separated as an oxide and removed during the refining process, but a part of it remains and is often included in the alloy up to about 0.5 mass% as an inevitable impurity.
- a raw material with high purity and refining it by vacuum melting, etc. it is not preferable from the viewpoint of cost because the mass productivity is poor.
- the particles become hard.
- the Si amount when the Si amount is included, the initial permeability may be increased and the magnetic core loss may be reduced as compared with the case where Si is not included.
- 1% by mass or less of Si may be included.
- the range of this Si amount is a range including not only the case where it exists as an inevitable impurity (typically 0.5% by mass or less) but also the case where a small amount of Si is added.
- the Fe-based alloy as inevitable impurities, for example, Mn ⁇ 1 mass%, C ⁇ 0.05 mass%, Ni ⁇ 0.5 mass%, N ⁇ 0.1 mass%, P ⁇ 0.02 mass% , S ⁇ 0.02 mass%. Further, the smaller the amount of O contained in the Fe-based alloy, the better, and it is preferably 0.5% by mass or less. Any composition amount is a value when the total amount of Fe, Al, Cr and Si is 100 mass%.
- the average particle diameter of the Fe-based alloy particles (here, the median diameter d50 in the cumulative particle size distribution is used) is not particularly limited, but by reducing the average particle diameter, the strength of the magnetic core and the high-frequency characteristics are improved. Therefore, for example, in applications requiring high-frequency characteristics, Fe-based alloy particles having an average particle diameter of 20 ⁇ m or less can be suitably used.
- the median diameter d50 is more preferably 18 ⁇ m or less, and still more preferably 16 ⁇ m or less.
- the median diameter d50 is preferably 5 ⁇ m or more.
- alloy particles that are at least under 32 ⁇ m (that is, passed through a sieve having an opening of 32 ⁇ m).
- the method of manufacturing a magnetic core according to the present embodiment includes a step of forming an Fe-based alloy particle powder to obtain a formed body (formed body forming step), and a step of heat-treating the formed body to form the oxide layer (heat treatment). Process).
- the form of particles of the Fe-based alloy is not particularly limited, but it is preferable to use granular powder represented by atomized powder as a raw material powder from the viewpoint of fluidity and the like.
- Atomization methods such as gas atomization and water atomization are suitable for producing powders of alloys that have high malleability and ductility and are difficult to grind.
- the atomization method is also suitable for obtaining a substantially spherical soft magnetic alloy powder.
- Binder is added to Fe-based alloy powder to bind the particles when pressing Fe-based alloy particles in the molded body formation process and to give the molded body the strength to withstand handling after molding. It is preferable to do.
- the kind of binder is not specifically limited, For example, various organic binders, such as polyethylene, polyvinyl alcohol, an acrylic resin, can be used.
- the organic binder is thermally decomposed by heat treatment after molding. Therefore, an inorganic binder such as a silicone resin that solidifies and remains even after heat treatment or binds powders as Si oxides may be used in combination.
- the amount of the binder added may be an amount that can be sufficiently distributed between the particles of the Fe-based alloy or can ensure a sufficient compact strength. On the other hand, if the amount is too large, the density and strength are lowered. From this viewpoint, the amount of binder added is preferably 0.5 to 3.0 parts by weight with respect to 100 parts by weight of an Fe-based alloy having an average particle diameter of 10 ⁇ m, for example.
- the oxide layer formed in the heat treatment step functions to bind the particles of the Fe-based alloy, so the use of the inorganic binder is omitted. It is preferable to simplify the process.
- the mixing method of the Fe-based alloy particles and the binder is not particularly limited, and conventionally known mixing methods and mixers can be used.
- the mixed powder is an agglomerated powder having a wide particle size distribution due to its binding action.
- a granulated powder having a desired secondary particle size suitable for molding can be obtained.
- a lubricant such as stearic acid or stearate.
- the amount of the lubricant added is preferably 0.1 to 2.0 parts by weight with respect to 100 parts by weight of the Fe-based alloy particles.
- the lubricant can be applied to the mold.
- the obtained mixed powder is pressure-molded to obtain a molded body.
- the mixed powder obtained by the above procedure is preferably granulated as described above and subjected to a pressure forming step.
- the granulated mixed powder is pressure-molded into a predetermined shape such as a toroidal shape or a rectangular parallelepiped shape using a molding die.
- the pressure molding may be room temperature molding or warm molding performed by heating to such an extent that the binder does not disappear.
- the molding pressure during pressure molding is preferably 1.0 GPa or less. By molding at a low pressure, it is possible to realize a magnetic core having high magnetic properties and high strength while suppressing breakage of the mold.
- molding method of mixed powder are not limited to said pressure molding.
- the molded body is subjected to heat treatment (high temperature oxidation) to obtain a heat treated body.
- heat treatment high temperature oxidation
- This oxide layer is grown by reacting Fe-based alloy particles with oxygen (O) by heat treatment, and is formed by an oxidation reaction exceeding the natural oxidation of the Fe-based alloy.
- the oxide layer covers the surface of the Fe-based alloy particles and further fills the voids between the particles.
- heat treatment can be performed in an atmosphere in which oxygen exists, such as in the air or in a mixed gas of oxygen and an inert gas.
- the heat treatment can be performed in an atmosphere in which water vapor exists, such as in a mixed gas of water vapor and inert gas. Of these, heat treatment in the air is simple and preferable.
- heat treatment in the air is simple and preferable.
- Al having a high affinity for O is also liberated, and an oxide is formed between particles of the Fe-based alloy.
- Cr or Si is included in the Fe-based alloy, Cr or Si is also present between the particles of the Fe-based alloy, but the affinity with O is smaller than that of Al, so the amount thereof is relatively less than that of Al. .
- a compound of Fe 3 Al ordered structure is also formed in the heat treatment. Although it is not possible to determine where the compound is formed, it is presumed that the compound is preferentially formed inside the Fe-based alloy particle.
- the heat treatment in this step may be performed at a temperature at which the oxide layer or the like is formed, but is preferably performed at a temperature at which the Fe-based alloy particles are not significantly sintered. Necking between the alloys during significant sintering causes a portion of the oxide layer to be surrounded by alloy particles and become island-like. Therefore, the function as an insulating layer that separates the particles is lowered.
- the specific heat treatment temperature is preferably in the range of 650 to 850 ° C.
- the holding time in the above temperature range is appropriately set depending on the size of the magnetic core, the processing amount, the allowable range of characteristic variations, and the like, and is set to 0.5 to 3 hours, for example.
- the space factor of the magnetic core may be 80% or more. If it is less than 80%, the desired initial permeability may not be obtained.
- FIG. 2A is a plan view schematically showing the coil component of the present embodiment
- FIG. 2B is a bottom view thereof
- FIG. 2C is a partial cross-sectional view taken along line A-A ′ in FIG. 2A.
- the coil component 10 includes a magnetic core 1 and a coil 20 wound around a conductive wire winding portion 5 of the magnetic core 1.
- the mounting surface of the flange portion 3b of the magnetic core 1 is provided with metal terminals 50a and 50b on the edge portion at the target position across the center of gravity, and one free end of the metal terminals 50a and 50b protruding from the mounting surface is Each of them rises at right angles to the height direction of the magnetic core 1.
- a coil component having such a magnetic core and a coil is used as, for example, a choke, an inductor, a reactor, or a transformer.
- the magnetic core may be manufactured in the form of a single magnetic core obtained by press-molding only the soft magnetic alloy powder mixed with a binder or the like as described above, or may be manufactured in a form in which a coil is arranged inside.
- the latter configuration is not particularly limited.
- a magnetic core of a coil encapsulating structure using a method in which soft magnetic alloy powder and a coil are integrally formed by pressure, or a lamination process such as a sheet lamination method or a printing method is used. It can be manufactured in the form.
- Al is ICP emission analysis method
- Cr is volumetric method
- Si and P are absorptiometry
- C and S are combustion-infrared adsorption method
- O is inert gas melting-infrared absorption method
- N is inert
- the values are analyzed by gas melting and thermal conductivity methods. When the contents of O, C, P, S and N were confirmed, all were less than 0.05% by mass with respect to 100% by mass of the total amount of Fe, Al, Cr and Si.
- the average particle diameter (median diameter d50) of the raw material powder was obtained using a laser diffraction / scattering particle size distribution analyzer (LA-920 manufactured by Horiba, Ltd.).
- a BET specific surface area was obtained by a gas adsorption method using a specific surface area measuring device (Macsorb manufactured by Mounttech).
- the saturation magnetization Ms and the coercive force Hc of each raw material powder were obtained by a VSM magnetic property measuring apparatus (VSM-5-20 manufactured by Toei Industry Co., Ltd.). In the measurement, the capsule was filled with the raw material powder, and a magnetic field (10 kOe) was applied. Further, the saturation magnetic flux density Bs was calculated from the saturation magnetization Ms by the following equation.
- Saturation magnetic flux density Bs (T) 4 ⁇ ⁇ Ms ⁇ ⁇ t ⁇ 10 ⁇ 4 ( ⁇ t : true density of Fe-based alloy)
- the true density ⁇ t of the Fe-based alloy was determined by measuring the apparent density from each of the alloy ingots used as the raw material powders A to D by a submerged weighing method, and setting it as the true density. Specifically, an ingot having an outer diameter of 30 mm and a height of 200 mm cast with the composition of the Fe-based alloy of the raw material powders A to D is evaluated with a sample cut to a height of 5 mm with a cutting machine. Table 2 shows the measurement results.
- a magnetic core was produced as follows. For each of the raw material powders A to D, PVA (Poval PVA-205 manufactured by Kuraray Co., Ltd .; solid content: 10%) was used as a binder, ion-exchanged water was added as a solvent, and the mixture was stirred and mixed to form a slurry. .
- the slurry concentration is 80% by mass.
- the binder was 0.75 part by weight with respect to 100 parts by weight of the raw material powder, spray drying was performed with a spray dryer, and the mixed powder after drying was passed through a sieve to obtain granulated powder. To this granulated powder, zinc stearate was added and mixed at a ratio of 0.4 parts by weight with respect to 100 parts by weight of the raw material powder.
- press molding is performed at room temperature, and a toroidal (annular) shaped molded body and a disk shaped molded body as a sample for measuring X-ray diffraction intensity are used.
- the molded body was heated at 250 ° C./hour in the air, and was subjected to heat treatment at a heat treatment temperature of 670 ° C., 720 ° C., 730 ° C., 770 ° C., 820 ° C. and 870 ° C. for 45 minutes to obtain a magnetic core. It was.
- the outer dimensions of the magnetic core were an outer diameter of 13.4 mm, an inner diameter of 7.7 mm, and a height of 2.0 mm.
- a magnetic core for measuring the X-ray diffraction intensity was a sample having an outer diameter of 13.5 mm and a height of 2.0 mm.
- FIG. 4 is a diagram showing the relationship between the peak strength ratio (P1 / P2) and the initial permeability ⁇ i
- FIG. 5 is a diagram showing the relationship between the peak strength ratio (P3 / P2) and the initial permeability ⁇ i.
- FIG. 6 shows a SEM image of a cross section of the magnetic core of No. 6
- FIGS. 6B to 6F show sample Nos.
- EDX Electronic Dispersive X-ray Spectroscopy
- A. Space factor Pf (relative density) The density (kg / m 3 ) was calculated from the dimensions and mass of the annular magnetic core by the volume weight method, and was defined as the density ds. The density ds was divided by the true density of each Fe-based alloy to calculate the space factor (relative density) [%] of the magnetic core. The true density here is the same as the true density used to calculate the saturation magnetic flux density Bs.
- the object to be measured is such that the magnetic core of the annular body is the object to be measured and the load direction is the radial direction between the surface plates of a tensile / compression tester (Autograph AG-1 manufactured by Shimadzu Corporation). Then, a load was applied in the radial direction of the magnetic core of the annular body, the maximum load P (N) at the time of fracture was measured, and the crushing strength ⁇ r (MPa) was obtained from the following equation.
- Magnetic core loss Pcv The magnetic core of the annular body is the object to be measured, and the primary side winding and the secondary side winding are wound by 15 turns, respectively, and the maximum magnetic flux density is 30 mT and the frequency is 300 kHz by BH analyzer SY-8232 manufactured by Iwatatsu Measurement Co., Ltd.
- the magnetic core loss Pcv (kW / m 3 ) was measured at room temperature.
- Incremental permeability ⁇ An LCR meter (with a DC magnetic field of up to 10 kA / m applied by a DC application device (42841A: manufactured by Hewlett-Packard Company) with a coil of an annular body as the object to be measured and 30 turns of a conducting wire to form a coil component.
- the inductance L was measured at room temperature at a frequency of 100 kHz using Agilent Technologies Inc. 4284A).
- Incremental permeability ⁇ was determined from the obtained inductance in the same manner as the initial permeability ⁇ i.
- composition distribution A toroidal magnetic core was cut, and the cut surface was observed with a scanning electron microscope (SEM / EDX: Scanning Electron Microscope / Energy Dispersive X-ray Spectroscopy), and element mapping was performed (magnification: 2000 times). ).
- the X-ray diffraction intensity measurement conditions were X-ray Cu-K ⁇ , applied voltage 40 kV, current 100 mA, divergence slit 1 °, scattering slit 1 °, light receiving slit 0.3 mm, scanning continuously, scanning speed 2 ° / min, The scanning step was 0.02 ° and the scanning range was 20 to 110 °.
- the peak intensity ratio (P3 / P2) between the peak intensity P3 and the peak intensity P2 of the superlattice peak of the Fe 3 Al ordered structure is 0.015 or more and 0.050 or less, and higher initial permeability than the sample of the comparative example.
- the magnetic core was obtained. It has been found that the configuration according to the above example is extremely advantageous in obtaining excellent magnetic characteristics. Further, the magnetic core loss, the specific resistance ⁇ v, and the crushing strength were the same or higher than those of the comparative sample.
- the X-ray diffraction spectrum of * 9 also shows the X-ray diffraction spectrum of the compact (not heat-treated).
- Fe oxide or a compound derived from Fe 3 Al is formed by heat treatment, and the peak intensity of the diffraction peak varies with the heat treatment temperature. That is, the target peak intensity ratio (P1 / P2, P3 / P2) can be obtained by adjusting the heat treatment temperature, so that a magnetic core having excellent magnetic properties can be efficiently produced.
- the initial permeability ⁇ i tends to increase as the peak intensity ratio (P1 / P2) between the peak intensity P1 and the peak intensity P2 decreases. Further, as shown in FIG. 5, the initial permeability ⁇ i changes in a parabolic shape and has an extreme value with respect to the peak intensity ratio (P3 / P2) between the peak intensity P3 and the peak intensity P2 in the X-ray diffraction spectrum. I understand that.
- FIG. 6A the evaluation results of cross-sectional observation using a scanning electron microscope (SEM) are shown in FIG. 6A, and the evaluation results of the distribution of each constituent element by EDX are shown in FIGS. 6B to 6F.
- FIGS. 6B to 6F are mappings showing the distribution of Fe (iron), Al (aluminum), Cr (chromium), Si (silicon), and O (oxygen), respectively.
- the brighter color tone (which appears white in the figure) indicates that there are more target elements.
- FIG. 6F shows that there are a lot of oxygen between the Fe-based alloy particles, oxides are formed, and the particles of each Fe-based alloy are bonded to each other through the oxides. Further, from FIG. 6C, it was confirmed that the concentration of Al was remarkably higher between particles (grain boundaries) including the surface of alloy particles than other non-ferrous metals.
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Abstract
Description
金属系磁性粉末としては、例えばFe-Si系、Fe-Ni系、Fe-Si-Cr系、Fe-Si-Al系などの磁性合金粉末が用いられている。かかる磁性合金粉末の成形体を圧密化して得られる磁心は、飽和磁束密度が高い反面、合金粉末であるため電気抵抗率が低く、予め水ガラスや熱硬化性樹脂等を用いて磁性合金粉末を絶縁被覆する場合が多い。
前記Fe基合金の粒子同士がFe基合金に由来する酸化物を介して結合され、
CuのKα特性X線を用いて測定された前記磁心のX線回折スペクトルにおける、2θ=33.2°付近に表れるコランダム構造を有するFe酸化物の回折ピークのピーク強度P1と、2θ=44.7°付近に表れるbcc構造を有する前記Fe基合金の回折ピークのピーク強度P2とのピーク強度比(P1/P2)が0.015以下であり、且つX線回折スペクトルにおける、2θ=26.6°付近に表れるFe3Al規則構造の超格子ピークのピーク強度P3と前記ピーク強度P2とのピーク強度比(P3/P2)が0.015以上0.050以下の磁心である。
アトマイズ法によりFe基合金の原料粉末を作製した。その組成分析結果を表1に示す。
飽和磁束密度Bs(T)=4π×Ms×ρt×10-4
(ρt:Fe基合金の真密度)
なおFe基合金の真密度ρtは、原料粉末A~Dのもととなる合金のインゴットのそれぞれから液中秤量法によって見掛け密度を測定し、それを真密度とした。具体的には、原料粉末A~DのFe基合金の組成で鋳造した外径30mm、高さ200mmのインゴットを、切断機で高さ5mmに切断した試料で評価している。測定の結果を表2に示す。
以下のようにして、磁心を作製した。A~Dの原料粉末それぞれに対して、PVA(株式会社クラレ製ポバールPVA-205;固形分10%)をバインダーとし、溶媒としてイオン交換水を投入し、攪拌混合して泥漿(スラリー)とした。スラリー濃度は80質量%である。前記原料粉末100重量部に対して、バインダーは0.75重量部とし、スプレードライヤーで噴霧乾燥を行い、乾燥後の混合粉を篩に通して造粒粉を得た。この造粒粉に、原料粉末100重量部に対して0.4重量部の割合でステアリン酸亜鉛を添加、混合した。
以上の工程により作製した各磁心について以下の評価を行った。評価結果を表3に示す。表3において、比較例の試料には試料No.に*を付与して区別している。また、表中の回折ピーク強度欄で“-”で示す部分は、X線回折スペクトルにおいて回折ピークのピーク強度がノイズレベル以下である場合で、回折ピークの強度がベースラインを形成するノイズレベル(不回避的に得られるX線散乱)と同様か、又はそれより低くて、回折ピークの検出が困難で確認出来ないということを意味する。図3に試料No.5~No.*9のX線回折強度を示す。図4はピーク強度比(P1/P2)と初透磁率μiとの関係を示す図であり、図5はピーク強度比(P3/P2)と初透磁率μiとの関係を示す図である。図6Aに試料No.6の磁心の断面のSEM画像を示し、図6B~FにEDX(Energy Dispersive X-ray Spectroscopy)による試料No.6の磁心の断面の組成マッピング画像を示す。
円環状の磁心に対し、その寸法と質量から体積重量法により密度(kg/m3)を算出し、密度dsとした。密度dsを各Fe基合金の真密度で除して磁心の占積率(相対密度)[%]を算出した。なお、ここでの真密度も飽和磁束密度Bsを算出するのに用いた真密度に同じである。
円板状の磁心を被測定物とし、その対向する二平面に導電性接着剤を塗り、乾燥・固化の後、被測定物を電極の間にセットする。電気抵抗測定装置(株式会社エーディーシー製8340A)を用いて、100Vの直流電圧を印加し、抵抗値R(Ω)を測定する。被測定物の平面の面積A(m2)と厚みt(m)とを測定し、次式により比抵抗ρ(Ωm)を算出した。
比抵抗ρv(Ωm)=R×(A/t)
磁心の代表寸法は、外径φ13.5mm、高さ2mmである。
JIS Z2507に基づき、環状体の磁心を被測定物とし、引張・圧縮試験機(株式会社島津製作所製オートグラフAG-1)の定盤間に荷重方向が径方向となる様に被測定物を配置し、環状体の磁心の径方向に荷重をかけ、破壊時の最大加重P(N)を測定し、次式から圧環強度σr(MPa)を求めた。
圧環強度σr(MPa)=P×(D-d)/(I×d2)
[D:磁心の外径(mm)、d:磁心の厚み〔内外径差の1/2〕(mm)、I:磁心の高さ(mm)]
環状体の磁心を被測定物とし、一次側巻線と二次側巻線とをそれぞれ15ターン巻回し、岩通計測株式会社製B-HアナライザーSY-8232により、最大磁束密度30mT、周波数300kHzで磁心損失Pcv(kW/m3)を室温で測定した。
環状体の磁心を被測定物とし、導線を30ターン巻回し、LCRメータ(アジレント・テクノロジー株式会社製4284A)により、周波数100kHzで室温にて測定したインダクタンスから次式により求めた。
初透磁率μi=(le×L)/(μ0×Ae×N2)
(le:磁路長、L:試料のインダクタンス(H)、μ0:真空の透磁率=4π×10-7(H/m)、Ae:磁心の断面積、N:コイルの巻数)
環状体の磁心を被測定物とし、導線を30ターン巻回してコイル部品とし、直流印加装置(42841A:ヒューレットパッカード社製)で10kA/mまでの直流磁界を印加した状態にて、LCRメータ(アジレント・テクノロジー株式会社社製4284A)によりインダクタンスLを周波数100kHzで室温にて測定した。得られたインダクタンスから前記初透磁率μiと同様に増分透磁率μΔを求めた。
トロイダル形状の磁心を切断し、切断面を走査型電子顕微鏡(SEM/EDX:Scanning Electron Microscope/Energy Dispersive X-ray Spectroscopy)により観察し、元素マッピングを行なった(倍率:2000倍)。
X線回折装置(株式会社リガク製Rigaku RINT-2000)を使用し、X線回折法による回折スペクトルから、2θ=33.2°付近に表れるコランダム構造を有するFeの酸化物の回折ピークのピーク強度P1と、2θ=44.7°付近に表れるbcc構造を有するFe基合金の回折ピークのピーク強度P2と、2θ=26.6°付近に表れるFe3Al規則構造の超格子ピークのピーク強度P3とを求め、ピーク強度比(P1/P2、P3/P2)を算出した。X線回折強度測定の条件は、X線Cu-Kα、印加電圧40kV、電流100mA、発散スリット1°、散乱スリット1°、受光スリット0.3mm、走査を連続とし、走査速度2°/min、走査ステップ0.02°、走査範囲20~110°とした。
3a,3b 鍔部
5 導線巻回部
10 コイル部品
20 コイル
25a,25b コイルの端部
50a,50b 金属端子
Claims (4)
- Alを含むFe基合金の粒子を用いた磁心であって、
前記Fe基合金の粒子同士がFe基合金に由来する酸化物を介して結合され、
CuのKα特性X線を用いて測定された前記磁心のX線回折スペクトルにおける、2θ=33.2°付近に表れるコランダム構造を有するFe酸化物の回折ピークのピーク強度P1と、2θ=44.7°付近に表れるbcc構造を有する前記Fe基合金の回折ピークのピーク強度P2とのピーク強度比(P1/P2)が0.015以下であり、且つX線回折スペクトルにおける、2θ=26.6°付近に表れるFe3Al規則構造の超格子ピークのピーク強度P3と、前記ピーク強度P2とのピーク強度比(P3/P2)が0.015以上0.050以下の磁心。 - 請求項1に記載の磁心であって、
初透磁率μiが55以上である磁心。 - 請求項1または2に記載の磁心であって、
前記Fe基合金が、組成式:aFebAlcCrdSiで表され、質量%で、a+b+c+d=100、13.8≦b≦16、0≦c≦7、0≦d≦1である磁心。 - 請求項1~3のいずれかに記載の磁心とコイルを備えたコイル部品。
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EP17851007.9A EP3514809B1 (en) | 2016-09-15 | 2017-09-15 | Magnetic core and coil component |
KR1020197008827A KR102020668B1 (ko) | 2016-09-15 | 2017-09-15 | 자심 및 코일 부품 |
CN201780056825.7A CN109716454B (zh) | 2016-09-15 | 2017-09-15 | 磁芯及线圈部件 |
US16/333,132 US10468174B2 (en) | 2016-09-15 | 2017-09-15 | Magnetic core and coil component |
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US11692250B2 (en) | 2018-08-02 | 2023-07-04 | Kabushiki Kaisha Toshiba | Plurality of flaky magnetic metal particles, pressed powder material, and rotating electric machine |
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US10468174B2 (en) | 2019-11-05 |
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