WO2023135933A1 - 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物 - Google Patents

軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物 Download PDF

Info

Publication number
WO2023135933A1
WO2023135933A1 PCT/JP2022/042779 JP2022042779W WO2023135933A1 WO 2023135933 A1 WO2023135933 A1 WO 2023135933A1 JP 2022042779 W JP2022042779 W JP 2022042779W WO 2023135933 A1 WO2023135933 A1 WO 2023135933A1
Authority
WO
WIPO (PCT)
Prior art keywords
resin composite
soft magnetic
less
metal flat
flat powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2022/042779
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
宏 安井
信彦 日笠
信一 西山
直也 行吉
けんた 鶴崎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MATE Co Ltd
Original Assignee
MATE Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by MATE Co Ltd filed Critical MATE Co Ltd
Priority to KR1020247026961A priority Critical patent/KR102851552B1/ko
Publication of WO2023135933A1 publication Critical patent/WO2023135933A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • 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
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • 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
    • 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
    • B22F3/006—Amorphous articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • 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
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields

Definitions

  • the present invention relates to noise suppression parts used as countermeasures against unwanted electromagnetic waves in communication equipment and various electronic devices, magnetic shield parts used in electromagnetic induction devices, and soft magnetic metal flats used for cores for electronic parts such as inductors and reactors.
  • the present invention relates to a powder, a resin composite sheet using the same, and a resin composite composition for molding.
  • Soft magnetic metal flat powders are used in resin composite sheets and molded products used for electromagnetic wave noise suppression and magnetic shielding. This is because flat processing reduces the demagnetizing coefficient, increases the magnetic permeability in the in-plane direction, and makes it possible to maintain the magnetic permeability up to higher frequencies beyond the Snake limit.
  • the imaginary permeability ⁇ '' indicating the magnetic loss of the permeability is used, and the magnetic shield uses the real permeability ⁇ ' of the magnetic permeability.
  • the mounting space for electromagnetic noise suppression and magnetic shielding parts has become limited. There is an increasing demand for a resin composite sheet using flat soft magnetic metal powder having high magnetic properties and a resin composite composition for molding.
  • Patent Document 2 proposes a higher magnetic permeability can be obtained by positively adjusting the composition of Al and Si.
  • Patent Document 3 proposes that a higher magnetic permeability can be obtained by positively adjusting the composition of Al and Si.
  • nanocrystalline soft magnetic metal flat powders have been proposed in Japanese Patent No. 2702757 (Patent Document 4) and Japanese Patent Laid-Open No. 11-269509 (Patent Document 5).
  • Patent Document 6 a Fe-Al-Si system soft magnetic material that can obtain a high magnetic permeability with little change in magnetic permeability in the temperature range where various devices actually operate Metal flat powders have been proposed.
  • the resin composite sheet and the molded article stably secure high electromagnetic wave noise suppression and magnetic shielding performance, or soft magnetic properties as a core material, in a temperature range of -40 to 85°C at the lowest.
  • the module in contactless power supply using electromagnetic induction, the module generates heat due to magnetic loss in the battery and coil components including magnetic materials during charging. This creates a vicious cycle in which the temperature rises further and performance declines, resulting in a problem of reduced charging efficiency.
  • measurements of soft magnetic properties including magnetic permeability are performed only at room temperature.
  • Patent Documents 4 and 5 an Fe-based amorphous ribbon is processed into a flat shape using a powder pulverized after an embrittlement treatment, and a nanocrystalline soft magnetic metal flat powder subjected to a nanocrystallization treatment is used to achieve high soft magnetism. Although it is described that characteristics can be obtained, Patent Document 4 focuses on coercive force and saturation magnetic flux density, and does not describe magnetic permeability.
  • the D50 average particle diameter is small and the aspect ratio is also low.
  • Patent Document 5 there is no description about coercive force, and it cannot be said that magnetic permeability has a sufficiently high value.
  • resin composite sheets are required to have low core loss while maintaining magnetic permeability, realize thin-walled products with high flexibility, and products with higher magnetic permeability and low core loss.
  • nanocrystalline soft magnetic metal flat powders that have high soft magnetic properties even if the particle size is small, and reduce the amount of powder blended.
  • the present invention has been made to solve the above problems, and the temperature range of -40 ° C to 150 ° C of a resin composite sheet or a resin composite composition molded product using nanocrystalline soft magnetic metal flat powder A nanocrystalline soft magnetic metal flat powder that has a small change in the temperature coefficient of magnetic permeability and has high magnetic permeability and low core loss, and a resin composite sheet using the material and having high magnetic permeability and low core loss and for molding. It is intended to provide a resin composite composition of An object of the present invention is to solve the problems associated with the above-described conventional soft magnetic metal flat powder, resin composite sheet using the material, and resin composite composition for molding.
  • the nanocrystalline particles have a particle size of 5 nm to less than 30 nm, a crystallinity of 65% to less than 95%, and an aspect ratio of the powder having a particle size near the average particle size D50 of 20 to less than 80.
  • the temperature coefficient of magnetic permeability Kn (n is 1, 2, 3) is expressed by the following formulas (1) (2) (3) in the range of -40 ° C to 150 ° C or less, and 0 ⁇ K1 ⁇ 0.20 , ⁇ 0.10 ⁇ K2 ⁇ 0.10, and ⁇ 0.15 ⁇ K3 ⁇ 0.05.
  • K1 ( ⁇ (0°C) ⁇ ( ⁇ 40°C))/ ⁇ ( ⁇ 40°C) (1)
  • K2 ( ⁇ (85°C) ⁇ ( ⁇ 40°C))/ ⁇ ( ⁇ 40°C) (2)
  • K3 ( ⁇ (150°C)- ⁇ (-40°C))/ ⁇ (-40°C) (3)
  • ⁇ magnetic permeability ( ⁇ ′: real magnetic permeability, ⁇ ′′: imaginary magnetic permeability), ⁇ (0 ° C.): magnetic permeability at 0 ° C.
  • the nanocrystalline soft magnetic metal flat powder has an average grain size
  • the diameter D50 is 20 ⁇ m to less than 40 ⁇ m
  • the average thickness near the D50 average particle size is 0.2 ⁇ m to less than 1.5 ⁇ m
  • the resin composite sheet using the nanocrystalline soft magnetic metal flat powder has a coercive force of 20 A. /m to less than 100 A/m, a nanocrystalline soft magnetic metal flat powder is obtained.
  • the nanocrystalline soft magnetic metal flat powder has an average particle size D50 of 40 ⁇ m to less than 100 ⁇ m and an average thickness near the D50 average particle size of 1.5 ⁇ m to less than 5 ⁇ m, and the nanocrystal A nanocrystalline soft magnetic metal flat powder is obtained using the soft magnetic metal flat powder, characterized in that the resin composite sheet has a coercive force of 20 A/m to less than 80 A/m.
  • a ring-shaped sample made of the nanocrystalline soft magnetic metal flat powder and resin having a coercive force of 20 A/m to less than 100 A/m, and having an outer diameter of 20 mm, an inner diameter of 10 mm, and a thickness of 0.15 mm
  • a resin composite sheet characterized by having a core loss of 50 kW/m to less than 300 kW/m when measured under the conditions of Bm and frequency of 50 mT-100 kHz using three layers of .
  • a product made of the nanocrystalline soft magnetic metal flat powder and resin which is molded to have an outer diameter of 12.8 mm, an inner diameter of 7.5 mm, and a thickness of 5 mm, is used to obtain Bm and a frequency of 50 mT-100 kHz.
  • a resin composite composition for molding is obtained, characterized by having a core loss of 100 kW/m 3 to less than 600 kW/m 3 when measured under conditions.
  • the present invention provides a resin composite sheet or resin composite composition molded product using nanocrystalline soft magnetic metal flat powder, which has a small change in the temperature coefficient of magnetic permeability within the range of -40 ° C to 150 ° C and has high permeability.
  • An object of the present invention is to provide a nanocrystalline soft magnetic metal flat powder having a magnetic permeability and a low core loss, a resin composite sheet having a high magnetic permeability and a low core loss using the material, and a resin composite composition for molding.
  • FIG. 2 is a graph showing the temperature dependence of magnetic permeability of resin composite sheets using flat soft magnetic metal powders of Examples 4 and 9 and Comparative Examples 10 and 11.
  • Amorphous alloy which is the raw material for nanocrystalline soft magnetic metal flat powder, can be produced by a rapid cooling method such as a single roll method, a twin roll method, or a melt spin method, or by a water atomization method, a gas atomization method, or the like. However, it is not particularly limited as long as a nanocrystalline phase is not generated.
  • the amorphous alloy is an Fe-based alloy, and for example, Fe--Si--B--Nb--Cu composition or Fe--Si--B--P--Cu composition can be used.
  • Hf, Ti, Ni, and C may be included, but are not particularly limited as long as a nanocrystalline phase can be obtained by the crystallization treatment.
  • embrittlement treatment is performed at temperatures above 200°C and below the nanocrystallization temperature in the atmosphere, nitrogen gas atmosphere, inert gas atmosphere, or vacuum, followed by a ball mill, vibration mill, pin mill, hammer mill, or the like. By pulverizing, a raw material powder for flattening with a predetermined particle size can be obtained.
  • the embrittlement treatment is not particularly necessary, and the metal foil strip may be pulverized as it is. Further, when the metal foil strip can be flattened, embrittlement treatment and pulverization can be omitted.
  • the powder obtained by the water atomization method, the gas atomization method, etc. does not particularly need to be embrittled, but in order to adjust the workability into flat powder, it may be used as a raw material for flattening after embrittlement treatment. .
  • the flattening process is not particularly limited, but can be carried out in the presence of distilled water or an organic solvent using an attritor, ball mill, vibration mill, or the like.
  • Toluene, hexane, alcohol, ethylene glycol, or the like can be used as the organic solvent, and the atmosphere in the apparatus may be adjusted during processing.
  • stearic acid or the like may be added as a flattening aid.
  • the amorphous alloy flat powder is heat-treated in a nitrogen gas atmosphere, an inert gas atmosphere, or in a vacuum at a temperature higher than the crystallization temperature to generate a nanocrystalline phase.
  • the heat treatment apparatus and conditions are not particularly limited as long as the target crystal grain size and crystallinity can be achieved by self-fracture due to shrinkage to reduce the diameter.
  • the powder near the average particle size D50 of the nanocrystalline soft magnetic metal flat powder has an aspect ratio of 20 to less than 80 and a coercive force of 20 A/m to less than 150 A/m. If the aspect ratio is less than 20, the diamagnetic field coefficient becomes large, and if it is 80 or more, the workability deteriorates. However, even if the aspect ratio is less than 20 to 80, the coercive force becomes 150 A/m or more when the proportion of fine powder is increased, and the magnetic permeability of the resin composite sheet and molded product is lowered. Therefore, the coercive force may be adjusted by removing fine powder by air classification or the like.
  • the average particle size D50 of the nanocrystalline soft magnetic metal flat powder was measured using R4 with HELOS/BR-multi manufactured by Sympatec.
  • a flat powder having a particle size range of ⁇ 10% of the obtained average particle size D50 was extracted by air classification, embedded in an epoxy resin, and mirror-polished to obtain a sample for thickness measurement. Since the flat powder is generally disk-shaped, the aspect ratio is represented by diameter/thickness.
  • the diameter is the value of the average particle size D50, and the thickness of the flat powder is measured with a scanning electron microscope to obtain the aspect ratio. .
  • the aspect ratio may be obtained by embedding a resin composite sheet or molded article in an epoxy resin, measuring the average length and thickness with a scanning electron microscope, and correcting the length to the diameter.
  • the magnetic permeability was measured in a temperature range of -40°C to 150°C in a thermo-hygrostat using an impedance analyzer E4991B, a magnetic material test fixture 16454A and a heat resistance test kit manufactured by Keysight.
  • a resin composite sheet and a molded resin composite composition were used as a measurement sample.
  • a measurement sample of the resin composite sheet was prepared by punching a ring-shaped sample with an outer diameter of 20 mm and an inner diameter of 10 mm from a sheet with a thickness of 0.15 mm.
  • a sample having an outer diameter of 20 mm, an inner diameter of 20 mm, and a thickness of 0.6 mm was used as the molded product.
  • the shape of the sample for magnetic permeability measurement is not particularly limited as long as the magnetic permeability can be measured. Furthermore, it may be measured in the state of a resin composite sheet, a molded product, or in the state of powder using a vibrating sample magnetometer (VSM), BH analyzer, LCR meter, or the like.
  • VSM vibrating sample magnetometer
  • the coercive force was measured with an applied magnetic field of 148 kA/m using an automatic measuring coercive force meter K-HC1000 manufactured by Tohoku Steel. About 10 mg of the flat powder was covered with a non-magnetic tape so as not to scatter and used as a sample for measurement.
  • a sample for magnetic permeability measurement was used to measure the coercive force of the resin composite sheet and the molded product of the resin composite composition.
  • Coercive force may be measured using a vibrating sample magnetometer (VSM), BH analyzer, or the like.
  • the crystal grain size of the nanocrystalline particles of the nanocrystalline soft magnetic metal flat powder is preferably 5 nm to less than 30 nm, more preferably 5 nm to less than 25 nm. If the crystal grain size is less than 5 nm, the growth of the nanocrystalline grains is insufficient and the soft magnetic properties are lowered. Also, the degree of crystallinity is preferably 65% to less than 95%, more preferably 65% to less than 90%. If the degree of crystallinity is less than 65%, crystal grain formation is insufficient, and if the degree of crystallinity is 95% or more, the crystal grains become coarse and the soft magnetic properties deteriorate.
  • the degree of crystallinity was calculated from the XRD measurement results by profile fitting using Rigaku's SmartLab Studio II application analysis package. For the calculation, as shown in FIG. 1, the areas of diffraction peaks before and after nanocrystallization of bcc Fe(110) were used.
  • the sample for XRD measurement does not have to be a powder, and the sheet and molded product can be set in a folder so that the plane of the nanocrystalline metal flat powder is generally parallel to the measurement surface.
  • the nanocrystalline soft magnetic metal flat powder preferably has an average particle size D50 of 20 ⁇ m to less than 40 ⁇ m. If it is less than 20 ⁇ m, fine powder having a high coercive force increases, making it difficult to obtain a sufficiently high magnetic permeability. If the thickness is 40 ⁇ m or more, the flexibility of the resin composite sheet is lowered.
  • the average thickness near the D50 average particle size is 0.2 ⁇ m to less than 1.5 ⁇ m. If it is less than 0.2 ⁇ m, the specific surface area becomes too large, resulting in deterioration of workability. It is desirable that the resin composite sheet using the nanocrystalline soft magnetic metal flat powder has a coercive force of 20 A/m to less than 100 A/m. When the coercive force is 100 A/m or more, the magnetic permeability decreases.
  • the nanocrystalline soft magnetic metal flat powder preferably has an average particle size D50 of 40 ⁇ m to less than 100 ⁇ m.
  • the thickness is less than 40 ⁇ m, it is not possible to meet the requirement for a particularly high magnetic permeability, and if it exceeds 100 ⁇ m, workability decreases. Furthermore, since the coarse and flat powder contains internal cracks that form magnetic gaps and lead to a decrease in soft magnetism, they may be removed by air classification or mechanical sieving. In addition, it is desirable that the average thickness near the D50 average particle size is from 1.5 ⁇ m to less than 5 ⁇ m. If the particle size is less than 1.5 ⁇ m, fine powder having a high coercive force increases. It is desirable that the resin composite sheet using the nanocrystalline soft magnetic metal flat powder has a coercive force of 20 A/m to less than 80 A/m.
  • the bulk density/true density is preferably in the range of 0.034 to 0.076. If it is smaller than 0.034, the flattening progresses too much, making handling difficult, and the amount of excessively pulverized fine powder increases and the profile becomes uneven, resulting in an increase in coercive force and a decrease in magnetic permeability. On the other hand, when it exceeds 0.076, flattening becomes insufficient, and magnetic permeability decreases. Bulk density was measured according to JISZ2504. The true density was measured using AccuPyc1330 manufactured by Shimadzu Corporation.
  • the resin composite sheet is made by blending nanocrystalline soft magnetic metal flat powder and polymer material in a predetermined ratio, making it into ink by various known methods, and forming a sheet by doctor coating, comma coating, screen printing, etc. Although it is produced, it may be further compressed by various rolls or a press. Alternatively, the resin composite sheet may be produced by kneading with a kneader or the like and roll-molding it, and further compressing this with a press, but the production method of the resin composite sheet is not limited to these. Magnetic permeability can be increased by applying a magnetic field during sheet fabrication to control the orientation of the nanocrystalline soft magnetic metal flat powder.
  • Polyurethane-based, acrylic-based, silicone-based, epoxy-based, chlorinated polyethylene-based, chloroprene-based rubbers, etc. can be used alone or in combination as polymer resins, but are not particularly limited, and have heat resistance of 150°C. It is desirable to have Thermoplasticity and thermosetting properties are also not particularly limited.
  • various additives such as antioxidants, pigments, non-magnetic fillers, thermally conductive fillers, etc., as well as various surface treatments such as coupling agents, dispersants, and anti-rust agents, as long as they do not impair the purpose of the present invention. can be added as needed.
  • the resin composite sheet preferably has a coercive force of 20 A/m to less than 100 A/m, more preferably less than 80 A/m. If it becomes 100 A/m or more, the magnetic permeability will decrease. Also, the core loss is preferably 50 kW/m 3 to less than 300 kW/m 3 , more preferably less than 200 kW/m 3 . If the core loss is 300 kW/m 3 or more, the magnetic loss increases when used in the magnetic parts of various electronic parts, and the performance of the parts deteriorates. Also, when used as a magnetic shield material for non-contact charging, a reduction in charging efficiency due to magnetic loss and accompanying heat generation pose a serious problem.
  • the content of the nanocrystalline soft magnetic metal flat powder is less than 35 vol % to less than 65 vol % with respect to the total solid content. More preferably, it is less than 40vol% to 55vol%. If it is less than 35 vol %, the magnetic permeability will be low even if the coercive force is less than 100 A/m.
  • the core loss was measured using a BH analyzer SY-8219 manufactured by Iwasaki Tsushinki Co., Ltd. and a high-speed bipolar power source HSA4041 manufactured by N.F.
  • the measurement sample for the resin composite sheet is obtained by punching a ring-shaped sample with an outer diameter of 20 mm and an inner diameter of 10 mm from a sheet with a thickness of 0.15 mm.
  • the primary side had 19 turns and the secondary side had 5 turns.
  • a sample with an outer diameter of 20 mm, an inner diameter of 10 mm and a thickness of 0.6 mm and a sample with an outer diameter of 12.8 mm, an inner diameter of 7.5 mm and a thickness of 5 mm were prepared.
  • a sample with an outer diameter of 12.8 mm was wound with 15 turns on the primary side and 5 turns on the secondary side to prepare a sample for measurement. The measurement was performed at a room temperature of 25° C. under the conditions of Bm and frequency of 50 mT-100 kHz.
  • the resin composite composition can be obtained by mixing flat nanocrystalline soft magnetic metal powder and polymer resin and kneading the mixture with a kneader or a twin-screw kneader, but not limited thereto, and various known methods. can be made with It is desirable that the content of the nanocrystalline soft magnetic metal flat powder is less than 35 vol % to less than 65 vol % with respect to the total solid content. It is more preferably 40 vol % to less than 60 vol %. If it is less than 35 vol%, the magnetic permeability of the molded product will be low, and if it is 65 vol% or more, molding will become difficult and the magnetic permeability will decrease.
  • the core loss is preferably less than 100 kW/m 3 to 600 kW/m 3 , more preferably less than 400 kW/m 3 . Although it can be molded into various shapes, it is not limited to these. At the time of molding, the molding may be performed while applying a magnetic field in order to orient the flattened powder.
  • Fe 83.3 Si 7.7 B having a thickness of 20 ⁇ m prepared by a single roll method was used to prepare the nanocrystalline soft magnetic metal flat powders used in Examples 1 to 12 and Comparative Examples 1 to 4 and 6 to 9 .
  • An amorphous ribbon having a composition of 0 Nb 5.7 Cu 1.3 (wt %) was used as a starting material. This was embrittled in an Ar atmosphere at 420 ° C. for Examples 1 to 5 and Comparative Examples 1 to 4, and at 220 ° C. for Examples 6 to 12 and Comparative Examples 6 to 9 for 1 hour. pulverized into The ground powder was then flattened by wet conditions with ethanol in an attritor.
  • nano-crystallization treatment was performed in an Ar atmosphere at 560° C. for 1 hour.
  • the obtained nanocrystalline soft magnetic metal flat powder was used, and the heat resistance temperature was 150 ° C. so that the total solid content was 50 vol%.
  • a curable acrylic rubber mixed resin was blended in a resin solution diluted with toluene and then dispersed to prepare a coating material for coating. This paint was applied with a comma coater to a thickness of 0.05 mm, and after magnetic field orientation, it was dried at 50° C. to remove the solvent. Six dried sheets were laminated and hot-pressed at 150° C.
  • Comparative Examples 5 and 10 an alloy powder having a composition of Fe 84.8 Al 5.6 Si 9.6 (wt %) produced by a gas atomization method, and in Comparative Example 11, Fe 84.0 Al 7.0 Si 9.0 ( %) composition was used as a starting material, flattened by an attritor under wet conditions using ethanol, and then heat-treated at 700° C. for 1 hour in an Ar atmosphere.
  • a resin composite sheet was prepared using this flat powder and a thermosetting acrylic rubber mixed resin having a heat resistant temperature of 150° C., and the magnetic permeability, coercive force and core loss were measured.
  • the real part ( ⁇ ′) and the imaginary part ( ⁇ ′′) of the magnetic permeability at each temperature were measured at 1 MHz and 10 MHz, respectively.
  • Table 1 shows Examples 1-5 and Comparative Examples 1-5.
  • Examples 1 to 5 focus on the flexibility of the resin composite sheet, and the nanocrystalline metal flat powder has an average particle size of 20 ⁇ m to less than 40 ⁇ m and an average thickness of 0.2 to less than 1.5 ⁇ m.
  • Flattening conditions were adjusted so that a flattened powder having a predetermined bulk density/true density was obtained after the flattening treatment. Furthermore, in the flattening process, the generation of fine powder is suppressed so that the coercive force after the nano-crystallization treatment is minimized, and the flattening such as the slurry concentration and the collision energy of the grinding media is adjusted so that the outline of the flattened powder is smooth.
  • the processing conditions were optimized.
  • Table 2 shows Examples 6 to 12 and Comparative Examples 6 to 11.
  • Examples 6 to 12 focus on the magnetic permeability of the resin composite sheet, and the nanocrystalline soft magnetic metal flat powder has an average particle size of 40 ⁇ m to less than 100 ⁇ m and an average thickness of 1.5 to less than 5 ⁇ m.
  • Flattening conditions were adjusted so as to obtain a flattened powder having a predetermined bulk density/true density after the treatment.
  • the generation of fine powder is suppressed so that the coercive force after the nano-crystallization treatment is minimized, and the flattening such as the slurry concentration and the collision energy of the grinding media is adjusted so that the outline of the flattened powder is smooth.
  • the processing conditions were optimized.
  • controlled moderate microcracks were introduced in the plane of the flat powder.
  • air classification was performed to remove 5 wt % of fine powder with high coercive force and 5 wt % of coarse and flat powder whose internal cracks act as magnetic gaps and affect soft magnetic properties. Table 3 shows Examples 13 and 14 and Comparative Examples 12 and 13.
  • Example 13 and 14 and Comparative Examples 12 and 13 the nanocrystalline soft magnetic metal flat powder of Example 4 and the Fe 84.8 Al 5.6 Si 9.6 (wt%) composition of Comparative Example 10 were used.
  • a soft magnetic metal flat powder was used.
  • the flat metal powder was surface-treated with a silane coupling agent, mixed with heat-resistant nylon (PA-9T), and heat-kneaded using a twin-screw kneader to obtain a resin composite composition.
  • a plate-shaped molded article having a thickness of 0.6 mm was produced using an injection molding machine, and the magnetic permeability and coercive force were measured on a sample punched to a thickness of 0.6 mm with an outer diameter of 20 mm and an inner diameter of 10 mm.
  • a ring-shaped molded product with an outer diameter of 12.8 mm, an inner diameter of 7.5 mm, and a thickness of 5 mm was shaped. Prepared as 2.
  • the samples of shape 1 and shape 2 were wound, and the core loss was measured under the conditions of Bm and frequency of 50 mT-100 kHz. From Table 1, all of Examples 1 to 5 have a temperature coefficient K of real (1 MHz) and imaginary permeability (10 MHz) in the range of -40 ° C. to 150 ° C.
  • Examples 6 to 12 have a temperature coefficient K of real (1 MHz) and imaginary permeability (10 MHz) in the range of -40 ° C. to 150 ° C. 0 ⁇ K1 ⁇ 0.20, -0.10 ⁇ K2 ⁇ 0.10 and -0.15 ⁇ K3 ⁇ 0.05 are satisfied, and the influence of the measurement temperature on the magnetic permeability is slight. In addition, they have significantly higher real and imaginary magnetic permeability at 0° C. than those of Comparative Examples 6 to 9, and low core loss. In particular, the magnetic permeability of Examples 8 to 10, in which fine powder and coarse and flat powder were removed by air classification, shows extremely high values.
  • Example 9 has a remarkably high magnetic permeability in the temperature range of -40°C to 150°C.
  • Example 10 has a smaller particle size, it has a higher magnetic permeability than Comparative Examples 10 and 11, and the amount of flat powder compounded to achieve the same magnetic permeability can be reduced. It is possible to realize thinning and improvement of flexibility.
  • both Examples 13 and 14 have a temperature coefficient K of real number (1 MHz) and imaginary number permeability (10 MHz) in the range of -40 ° C. to 150 ° C. 0 ⁇ K1 ⁇ 0.20, -0.10 ⁇ K2 ⁇ 0.10 and -0.15 ⁇ K3 ⁇ 0.05 are satisfied, and the influence of the measurement temperature on the magnetic permeability is slight. Moreover, it has higher real and imaginary magnetic permeability at 0° C. than Comparative Example 12, and Example 14, which contains a large amount of powder, is superior to Comparative Example 12 in moldability. Therefore, it becomes easy to reduce the thickness of the molded product. In Comparative Example 12, the magnetic permeability at 0° C.
  • Comparative Example 13 cannot be molded because the amount of powder blended is too large, and cannot be measured.
  • shape 1 shows a lower value than shape 2, but Examples 13 and 14 are compared. It shows significantly lower values than Example 12.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Power Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
PCT/JP2022/042779 2022-01-13 2022-11-11 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物 Ceased WO2023135933A1 (ja)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020247026961A KR102851552B1 (ko) 2022-01-13 2022-11-11 연자성 금속 편평 분말 및 이를 이용한 수지 복합 시트 및 수지 복합 조성물

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2022-013691 2022-01-13
JP2022013691A JP7565611B2 (ja) 2022-01-13 2022-01-13 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物

Publications (1)

Publication Number Publication Date
WO2023135933A1 true WO2023135933A1 (ja) 2023-07-20

Family

ID=87278876

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2022/042779 Ceased WO2023135933A1 (ja) 2022-01-13 2022-11-11 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物

Country Status (3)

Country Link
JP (1) JP7565611B2 (https=)
KR (1) KR102851552B1 (https=)
WO (1) WO2023135933A1 (https=)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118711970A (zh) * 2024-06-13 2024-09-27 江西大有科技有限公司 一种升压电感及其制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102843410B1 (ko) * 2023-09-27 2025-08-06 주식회사 아모그린텍 연자성 합금 코어 구조체 및 이를 포함하는 전자기기

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269509A (ja) * 1998-03-19 1999-10-05 Hitachi Metals Ltd ノイズ抑制効果に優れた扁平状ナノ結晶軟磁性粉末およびその製造方法
JP2003209010A (ja) * 2001-11-07 2003-07-25 Mate Co Ltd 軟磁性樹脂組成物、その製造方法及び成形体
JP2009059753A (ja) * 2007-08-30 2009-03-19 Hitachi Chem Co Ltd 難燃化ノイズ抑制シート
JP2016094652A (ja) * 2014-11-14 2016-05-26 株式会社リケン 軟磁性合金および磁性部品
JP2021111766A (ja) * 2020-01-11 2021-08-02 株式会社メイト 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに成形加工用樹脂複合コンパウンド

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2702757B2 (ja) 1988-11-01 1998-01-26 日立金属株式会社 扁平状Ｆｅ基軟磁性合金微粉末およびその製造方法
JP3722391B2 (ja) 1996-09-05 2005-11-30 Ｎｅｃトーキン株式会社 複合磁性体およびそれを用いた電磁干渉抑制体
JP2005281783A (ja) 2004-03-30 2005-10-13 Nec Tokin Corp ノイズ抑制用軟磁性粉末、その製造方法及びそれを用いたノイズ抑制シート
JP6592424B2 (ja) 2016-12-22 2019-10-16 山陽特殊製鋼株式会社 軟磁性扁平粉末およびこれを用いた磁性シート

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269509A (ja) * 1998-03-19 1999-10-05 Hitachi Metals Ltd ノイズ抑制効果に優れた扁平状ナノ結晶軟磁性粉末およびその製造方法
JP2003209010A (ja) * 2001-11-07 2003-07-25 Mate Co Ltd 軟磁性樹脂組成物、その製造方法及び成形体
JP2009059753A (ja) * 2007-08-30 2009-03-19 Hitachi Chem Co Ltd 難燃化ノイズ抑制シート
JP2016094652A (ja) * 2014-11-14 2016-05-26 株式会社リケン 軟磁性合金および磁性部品
JP2021111766A (ja) * 2020-01-11 2021-08-02 株式会社メイト 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに成形加工用樹脂複合コンパウンド

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118711970A (zh) * 2024-06-13 2024-09-27 江西大有科技有限公司 一种升压电感及其制备方法

Also Published As

Publication number Publication date
JP7565611B2 (ja) 2024-10-11
JP2023103144A (ja) 2023-07-26
KR102851552B1 (ko) 2025-08-28
KR20240136376A (ko) 2024-09-13

Similar Documents

Publication Publication Date Title
JP5669389B2 (ja) 高周波用磁性材料とその製造方法
EP2518740A1 (en) Reactor and method for producing same
US8974608B2 (en) Powder magnetic core and the method of manufacturing the same
CN103339694A (zh) 复合软磁性粉末及其制造方法以及使用了其的压粉磁心
JP2013051329A (ja) 磁性材料、磁性材料の製造方法および磁性材料を用いたインダクタ素子
KR20050015563A (ko) 철계 비정질 금속 분말의 제조방법 및 이를 이용한 연자성코어의 제조방법
TWI751302B (zh) 鎳系鐵氧體燒結體、線圈零件、及鎳系鐵氧體燒結體的製造方法
WO2023135933A1 (ja) 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに樹脂複合組成物
US10576539B2 (en) Flat soft magnetic powder and production method therefor
WO2011016207A1 (ja) 複合磁性体及びその製造方法
EP4280234A1 (en) Magnetic composite
JP7041819B2 (ja) 軟磁性金属扁平粉末およびそれを用いた樹脂複合シート並びに成形加工用樹脂複合コンパウンド
JP2014204051A (ja) 軟磁性扁平粉末およびこれを用いた磁性シート
TW201426773A (zh) 磁性零件、用於其之軟磁性金屬粉末及其製造方法
US20240177902A1 (en) Magnetic core and magnetic component
CN104036900B (zh) 软磁性金属粉末及压粉磁芯
WO2023090220A1 (ja) 磁性粉体の製造方法、磁場増幅用磁性材料、および超高周波吸収用磁性材料
JP2023103144A5 (https=)
EP4503068A1 (en) Magnetic composite
CN117476331A (zh) 磁芯和磁性部件
WO2022202760A1 (ja) 高周波用磁性材料とその製造法
WO2024038829A1 (ja) α－Ｆｅ含有希土類－鉄－窒素系磁性粉体、その製造方法、磁場増幅用磁性材料、超高周波吸収用磁性材料
JP2023174580A (ja) 被覆希土類－鉄－窒素系磁性粉体、その製造方法、磁場増幅用磁性材料、超高周波吸収用磁性材料
JPWO2022202760A5 (https=)
Lai et al. Mechanically alloyed ultrafine Fe-Si powders for soft magnetic composites

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 22920453

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 20247026961

Country of ref document: KR

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 22920453

Country of ref document: EP

Kind code of ref document: A1