WO2019189614A1 - Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same - Google Patents

Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same Download PDF

Info

Publication number
WO2019189614A1
WO2019189614A1 PCT/JP2019/013687 JP2019013687W WO2019189614A1 WO 2019189614 A1 WO2019189614 A1 WO 2019189614A1 JP 2019013687 W JP2019013687 W JP 2019013687W WO 2019189614 A1 WO2019189614 A1 WO 2019189614A1
Authority
WO
WIPO (PCT)
Prior art keywords
iron
soft magnetic
based soft
magnetic powder
crystallinity
Prior art date
Application number
PCT/JP2019/013687
Other languages
French (fr)
Japanese (ja)
Inventor
泰志 木野
慎吾 林
Original Assignee
新東工業株式会社
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 新東工業株式会社 filed Critical 新東工業株式会社
Priority to JP2020511004A priority Critical patent/JP7024859B2/en
Priority to CN201980023114.9A priority patent/CN111971761A/en
Priority to KR1020207019919A priority patent/KR102574343B1/en
Publication of WO2019189614A1 publication Critical patent/WO2019189614A1/en

Links

Images

Classifications

    • 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
    • B22F1/065—Spherical 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
    • B22F1/08—Metallic powder characterised by particles having an amorphous 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/02—Amorphous alloys with iron as the major constituent
    • 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

Definitions

  • the present invention relates to an iron-based soft magnetic powder exhibiting good magnetic properties even under stress and a method for producing the same, and an article containing the iron-based soft magnetic alloy powder and a method for producing the same.
  • a dust core in a choke coil, a reactor coil or the like is manufactured by adding an insulating binder such as an epoxy resin to soft magnetic powder and molding the powder into a predetermined shape by injection molding or press molding. At this time, the dust core is manufactured in a state where stress is applied to the soft magnetic powder.
  • an iron-based nanocrystalline alloy powder described in Patent Document 1 has been used as a soft magnetic powder used in the production of a dust core.
  • Such an iron-based nanocrystalline alloy powder is produced by producing an alloy having an amorphous phase as a whole and then subjecting it to a nanocrystallization by heat treatment.
  • Such a magnetic powder is used, for example, by performing a heat treatment for precipitating the bcc phase on the iron-based soft magnetic alloy powder as disclosed in Patent Document 2 and adjusting the coercive force to be minimized. It is done.
  • Patent Document 1 JP-A-1-79342
  • Patent Document 2 JP-A-2010-280956
  • the present invention provides an iron-based soft magnetic powder that exhibits optimum core magnetic properties as a dust core even in a state in which stress is applied by injection molding, press molding, or the like, and a method for producing the same, and
  • An object of the present invention is to provide an article containing an iron-based soft magnetic alloy powder and a method for producing the same.
  • the inventors of the present invention have developed an iron-based soft magnetic powder having excellent magnetostatic characteristics and optimized magnetostatic characteristics to form a powder magnetic core by applying stress by injection molding or press molding with pressurization. When found, it was found that the optimum core magnetic characteristics were not necessarily exhibited. And, as a result of intensive studies, the inventors have adjusted the crystallinity so that even if stress is applied to the iron-based soft magnetic powder by injection molding or press molding with pressurization, etc. As a result, the inventors have obtained the knowledge that optimum magnetic core characteristics can be obtained as a dust core, and have completed the present invention.
  • the present invention is an iron-based soft magnetic powder obtained by crystallizing a part of an amorphous phase by heat treatment to precipitate crystallites, and the iron-based soft magnetic powder includes Si, B, Cu, Nb and An iron-based soft magnetic powder comprising inevitable impurities and having a crystallinity higher than the crystallinity when coercive force is minimized.
  • the iron-based soft magnetic powder is Fe 100- (x + y + z + r) Si x B y Cu z Nb r [Wherein, x, y, z and r are at%, 3.0 ⁇ x ⁇ 16.0 6.0 ⁇ y ⁇ 13.0 0.5 ⁇ z ⁇ 2.0 0.5 ⁇ r ⁇ 4.0 1.5 ⁇ z + r ⁇ 4.5 11.5 ⁇ y + r ⁇ 14.5 Satisfy the relationship]
  • the above iron-based soft magnetic powder having the following composition is provided:
  • the above iron-based soft magnetic powder having a crystallinity of 80 to 95%.
  • the iron-based soft magnetic powder described above wherein the hardness of the powder measured according to ISO 14577-1 is 1000 to 1250 HV.
  • the iron-based soft magnetic powder having a substantially spherical shape.
  • the above iron-based soft magnetic powder having an average particle diameter of 0.5 to 50 ⁇ m is provided.
  • the above iron-based soft magnetic powder in which 0.5 to 2.0 at% of Fe is replaced with Cr.
  • an article including the iron-based soft magnetic powder that is stressed by pressure molding is provided.
  • the above article that is a dust core.
  • a method for producing an iron-based soft magnetic powder including the following steps.
  • -1st process The process which weighs and melt
  • -2nd process The process of obtaining substantially spherical amorphous particle
  • the first step there is provided a method for producing the above iron-based soft magnetic powder, wherein raw materials are weighed so as to have the following composition and melted to obtain a molten alloy.
  • x, y, z and r are at%, 3.0 ⁇ x ⁇ 16.0 6.0 ⁇ y ⁇ 13.0 0.5 ⁇ z ⁇ 2.0 0.5 ⁇ r ⁇ 4.0 1.5 ⁇ z + r ⁇ 4.5 11.5 ⁇ y + r ⁇ 14.5 Satisfy the relationship.
  • x, y, z and r are at%, 3.0 ⁇ x ⁇ 16.0 6.0 ⁇ y ⁇ 13.0 0.5 ⁇ z ⁇ 2.0 0.5 ⁇ r ⁇ 4.0 1.5 ⁇ z + r ⁇ 4.5 11.5 ⁇ y + r ⁇ 14.5 Satisfy the relationship.
  • the heat treatment temperature in the third step is higher than the heat treatment temperature when the coercive force is minimized, and lower than the crystallization temperature of the amorphous phase.
  • the method for producing the iron-based soft magnetic powder wherein the crystallinity in the third step is 80 to 95%.
  • the hardness of the powder is 1000 to 1250 HV as measured according to ISO 14577-1.
  • the above iron-based soft magnetic powder manufacturing method wherein 0.5 to 2.0 at% of Fe is replaced with Cr in the above-described iron-based soft magnetic powder manufacturing method. Is done.
  • an article manufacturing method including a pressure molding step after the iron-based soft magnetic powder manufacturing method.
  • the iron-based soft magnetic powder of the present invention containing Si, B, Cu, and Nb and crystallizing a part of the amorphous phase by heat treatment to precipitate crystallites.
  • the crystallinity higher than when the coercive force is minimized, it is good as a dust core even when stress is applied to the iron-based soft magnetic powder by injection molding or press molding.
  • Iron-based soft magnetic powder that exhibits excellent magnetic properties.
  • a to B means “A or more and B or less”.
  • the iron-based soft magnetic powder of the present embodiment is an iron-based soft magnetic powder containing Si, B, Cu, and Nb and crystallizing a part of the amorphous phase by heat treatment to precipitate crystallites.
  • a crystallite having a body-centered cubic structure containing Fe as a main component (bcc phase) and a crystallite having a face-centered cubic structure containing Cu as a main component (fcc phase) by heat treatment. ) can be formed, and excellent magnetostatic properties can be obtained.
  • the magnetostatic characteristics of the iron-based soft magnetic powder can be adjusted to a desired state.
  • the iron-based soft magnetic powder when the iron-based soft magnetic powder has the following composition, it exhibits better magnetic properties when used in a state where stress is applied by pressure molding such as injection molding or press molding, such as a dust core. Iron-based soft magnetic powder.
  • the Si improves the amorphous phase forming ability.
  • the Si amount x has a sufficient ability to form an amorphous phase, and in order to obtain good magnetic properties, the amount ratio Si / Fe with Fe is preferably substantially constant, and is preferably 3.0 to 16.0 at%. .
  • B and Nb improve the ability to form an amorphous phase.
  • Nb is an essential component when an iron-based soft magnetic powder is produced by an atomizing method.
  • the amount of B is 6.0 at% or more, the amorphous phase forming ability increases, and if it is 13.0 at% or less, good magnetic characteristics are exhibited, which is preferable.
  • the sum y + r of the B amount y and the Nb amount r is preferably 11.5 ⁇ y + r ⁇ 14.5 (at%). If it is 11.5 at% or more, the ability to form an amorphous phase increases, and if it is 14.5 at% or less, good magnetic properties are exhibited.
  • Cu and Nb are elements that have an effect of controlling the particle size of the deposited nanocrystallites.
  • the effect of controlling the particle size of the nanocrystallite is greatly influenced by the amount of Cu.
  • the amount of Cu z is 0.5 at% or more
  • it can be set as the iron group soft magnetic powder which shows a favorable magnetic characteristic after heat processing.
  • the sum z + r of the Cu amount z and the Nb amount r is preferably 1.5 ⁇ z + r ⁇ 4.5 (at%). If it is 1.5 at% or more, it effectively acts on the control of the particle size of the nanocrystallite, and if it is 4.5 at% or less, good magnetic properties are exhibited.
  • the crystallinity of the iron-based soft magnetic powder is higher than the crystallinity when the coercive force is minimized in the powder state by heat treatment described later.
  • the crystallinity of the iron-based soft magnetic powder is preferably 80 to 95%. According to this, even if it uses for the magnetic component manufactured in the state where the compressive stress was loaded, it can be set as the iron group soft magnetic powder which shows a favorable magnetic characteristic.
  • the “crystallinity” in the present invention is the ratio of the crystal phase precipitated in the powder.
  • “crystallinity 80%” is the ratio of the crystal phase is 80% and the remaining 20% is the amorphous phase. It shows that.
  • the “crystallinity” in the present invention was calculated by the following peak separation using an X-ray diffraction method. (Rigaku Corporation (issued in 2010). X-ray analysis handbook (6th edition) Rigaku Corporation)
  • a dust core in a choke coil, a reactor coil or the like is manufactured by adding an insulating binder such as an epoxy resin to soft magnetic powder and molding the powder into a predetermined shape by injection molding or press molding. At this time, the dust core is manufactured in a state where stress is applied to the soft magnetic powder.
  • the hardness of the iron-based soft magnetic powder is preferably 1000 to 1250 HV. According to this, since fluidity
  • the iron-based soft magnetic powder is formed in a substantially spherical shape. According to this, since the filling rate of the iron-based soft magnetic powder in the dust core can be increased when performing injection molding or press molding, the magnetic characteristics can be improved.
  • not all of the powder shapes may be substantially spherical. For example, when the major axis of the particles is a and the minor axis is b, 70% or more of the particles satisfy the relationship of 1 ⁇ a / b ⁇ 1.2. There should be.
  • the average particle diameter of the iron-based soft magnetic powder is set to 0.5 to 50 ⁇ m, when the dust core is made, the insulation of the dust core can be secured and the filling rate of the iron-based soft magnetic powder can be increased. As a result, the magnetic properties can be improved.
  • the particle diameter is small, the eddy current loss is small when the dust core is used in a high frequency band, so the loss can be reduced.
  • the particle diameter is too small, a sufficient magnetic permeability ⁇ cannot be obtained. The above is preferable.
  • the average particle diameter of the iron-based soft magnetic powder is 10 ⁇ m or less, eddy current loss can be reduced when a dust core is used in a high frequency band of 1 MHz or more, and a necessary and sufficient magnetic permeability ⁇ is obtained. More preferably.
  • the article according to this embodiment includes the iron-based soft magnetic powder that is stressed by pressure molding.
  • the article according to the present embodiment is a soft magnetic part used for various purposes such as electronics and automotive parts, and is particularly a dust core. Due to the characteristics of the iron-based soft magnetic powder described above, an article including the iron-based soft magnetic powder that is stressed by pressure molding such as injection molding or press molding, particularly a dust core, has good core magnetic characteristics. (Permeability, core loss) is expressed.
  • raw materials are weighed and melted to obtain a molten alloy of Fe, Si, B, Cu, and Nb so as to have a predetermined composition, for example, the following preferable composition.
  • substantially spherical amorphous particles are obtained from the molten alloy obtained in the first step by an atomizing method.
  • a known water atomization method is employed.
  • the molten alloy obtained in the first step is dropped from the molten orifice, and the raw material melted by the water film sprayed from the atomizing nozzle is rapidly cooled and solidified.
  • the powder is recovered, dried, and classified to obtain amorphous particles having a predetermined particle size and having a substantially spherical particle shape.
  • the amorphous particles obtained in the second step are heat-treated to crystallize a part of the amorphous phase.
  • the crystallinity of the powder is set higher than the crystallinity when the coercive force is minimized.
  • the heat treatment in the present invention is performed in order to adjust the magnetic characteristics by isothermally maintaining a predetermined temperature in a nitrogen atmosphere, crystallizing a part of the amorphous phase, and precipitating nanocrystallites of several tens of nanometers.
  • heat treatment can be performed in the air.
  • the low-temperature exothermic peak temperature Tx is the bcc phase precipitation temperature at which the body-centered cubic crystal phase precipitates
  • the high-temperature exothermic peak temperature T1 is the amorphous phase crystallization temperature.
  • a crystallite having a body-centered cubic structure containing Fe as a main component (bcc phase) and a crystallite having a face-centered cubic structure containing Cu as a main component (fcc phase) by heat treatment. ) can be formed, and excellent magnetostatic properties can be obtained.
  • the magnetostatic characteristics of the iron-based soft magnetic powder can be adjusted to a desired state.
  • Permeability ⁇ and core loss Pcv are important as magnetic characteristics reflecting the characteristics of the dust core.
  • the magnetic permeability ⁇ is high and the core loss Pcv is low.
  • the heat treatment temperature exceeds the heat treatment temperature T2 at which the coercive force Hc is minimized, the coercive force Hc is increased and the magnetostatic characteristics of the powder are not optimal. At this time, the crystallinity increases and the hardness decreases.
  • the present inventors set the heat treatment temperature to T3 higher than the heat treatment temperature T2 when the coercive force Hc is minimized and lower than the crystallization temperature T1 of the amorphous phase, and adjust the crystallinity, hardness, etc.
  • the present inventors have found an iron-based soft magnetic powder that exhibits optimum core magnetic properties (permeability, core loss).
  • the heat treatment temperature T3 is preferably set so that the crystallinity of the iron-based soft magnetic powder is 80 to 95%.
  • the heat treatment temperature T3 is preferably set to be 1000 to 1250 HV.
  • the method for manufacturing an article according to this embodiment includes a pressure molding step after the above-described method for manufacturing an iron-based soft magnetic powder.
  • Articles obtained by the method for manufacturing a dust core according to the present embodiment, particularly a dust core exhibit good core magnetic properties (permeability, core loss) due to the properties of the iron-based soft magnetic powder described above.
  • Example of change When using a dust core for electronic parts, a material having high corrosion resistance against moisture and the like is required. In the iron-based soft magnetic powder, 0.5 to 2.0 at% of Fe can be replaced with Cr. According to this, corrosion resistance can be improved while maintaining good magnetic properties.
  • atomizing method a gas atomizing method, an oil atomizing method, or the like can be adopted.
  • the iron-based soft magnetic powder of the present invention can be obtained by injection molding or press molding by making the crystallinity higher than the crystallinity when the coercive force is minimized. Even when stress is applied to the iron-based soft magnetic powder, the powder magnetic core can exhibit good core magnetic properties.
  • the mixed materials prepared in the respective compositions shown in Table 1 were melted in a high frequency induction furnace, and soft magnetic powder was obtained by a water atomization method.
  • the measurement results of the bcc phase precipitation temperature Tx and the saturation magnetization (Bs) are also shown. Evaluation powder preparation conditions are as follows.
  • the obtained soft magnetic powder was collected and dried with a vibration vacuum dryer (VU-60: manufactured by Chuo Kako Co., Ltd.). Since drying is performed in a reduced pressure atmosphere, drying can be performed in a low oxygen atmosphere as compared with a drying method performed in an atmospheric pressure atmosphere, and drying can be performed in a short time at a low temperature. Further, by applying vibration to the soft magnetic powder during drying, drying can be performed in a shorter time, and aggregation and oxidation of the powder can be prevented.
  • the drying temperature was 100 ° C.
  • the pressure in the drying chamber was ⁇ 0.1 MPa (gauge pressure)
  • the drying time was 60 minutes.
  • the obtained soft magnetic powder was classified by an airflow classifier (turbo classifier: manufactured by Nisshin Engineering Co., Ltd.) to obtain a powder material (6 ⁇ m, 2 ⁇ m) having a target average particle diameter.
  • the particle size distribution of the powder material was measured with a laser diffraction type particle size distribution measuring device (MT3300EXII: manufactured by Microtrack Bell Co., Ltd.).
  • the crystallite diameter and crystallinity measuring devices and measurement conditions are as follows.
  • Measurement device Powder X-ray diffraction device (MinFlex 600: manufactured by Rigaku Corporation) Measurement conditions: voltage 40 kV, current 15 mA, step 0.01 deg, speed 1 deg / min
  • the crystallite diameter was calculated by using the Scherrer equation shown below for the bcc FeSi peak. Here, a peak around 78 ° was used as the FeSi peak.
  • the hardness measuring device and measuring method are as follows.
  • -Measuring device Nanoindenter (ENT-2000: manufactured by Elionix Co., Ltd.)
  • Measurement method Based on ISO 14577-1, the powder hardness was calculated by measuring the size of the indentation after applying a load of 5 ⁇ N to 100 mN to the particle cross section.
  • the measuring method and measuring method of the coercive force Hc are as follows.
  • ⁇ Measuring device Vibrating sample magnetometer (VSM-C7: manufactured by Toei Kogyo Co., Ltd.)
  • Measurement method VSM measurement capsules filled with 200 mg of the obtained powder material having each particle size distribution, fixed with paraffin, applied with a maximum magnetic field of 10000 Oe, saturation magnetization measurement (Bs) and coercive force measurement (Hc) went.
  • the obtained powder material having each particle size distribution was mixed with an epoxy resin (binder) and toluene (organic solvent) to obtain a mixture.
  • the addition amount of the epoxy resin was 3 wt% with respect to the soft magnetic powder material.
  • the mixture thus prepared was dried by heating at a temperature of 80 ° C. for 30 minutes to obtain a lump-like dried body.
  • the dried product was passed through a sieve having an opening of 200 ⁇ m to prepare a powder material (granulated product).
  • the powder material was filled into a mold, and a molded body (dust core) was obtained under the following conditions.
  • ⁇ Measurement conditions and evaluation> The core magnetic characteristics ( ⁇ , Pcv) of the choke coil manufactured under the above conditions were evaluated under the following conditions.
  • compositions 7 and 8 the heat treatment conditions were set to the following six levels, and the coercive force Hc and hardness HV in the powder state and the core magnetic properties (permeability ⁇ , core loss) of the powder magnetic core were used. evaluated.
  • the results are shown in Table 2 and FIGS.
  • test 1 corresponds to the result of composition 7
  • test 2 corresponds to the result of composition 8.
  • the degree of crystallinity increased with increasing heat treatment temperature, and all amorphous phases were crystallized at 600 ° C.
  • the crystallization temperature of the amorphous phase is considered to be about 600 ° C.
  • the reason why crystallization has started from 500 ° C. below the bcc phase precipitation temperature Tx is presumed to be a portion where the temperature is locally higher than the set temperature due to the exothermic reaction of the powder.
  • the best magnetic characteristics with a low coercive force Hc were obtained when heat treatment was performed at 530 ° C. (Test 1-3, Test 2-3). At this time, the crystallinity was 76 in Test 1-3 and 74 in Test 2-3. The hardness HV was 1250 HV in Test 1-3 and 1270 HV in Test 2-3, and each showed the highest value.
  • this state is the target state, and the heat treatment temperature is set to 530 ° C.
  • the heat treatment temperature exceeds 530 ° C., which is the heat treatment temperature at which the coercive force Hc is minimized, the coercive force Hc is increased and the magnetostatic characteristics of the powder are not optimal.
  • the heat treatment temperature exceeds 530 ° C.
  • the crystallinity increases.
  • the grain size of the precipitated crystallites increases and the hardness HV decreases.
  • the magnetic permeability ⁇ showed the maximum value and the core loss showed the minimum value at the heat treatment temperature of 570 ° C.
  • the crystallinity showing the same permeability as that of the crystallinity at which the coercive force Hc is minimum (heat treatment temperature 530 ° C.) is 94% in Test 1 and 93% in Test 2. It was.
  • the crystallinity showing the same core loss as the crystallinity having the minimum coercive force Hc was 91% in both Test 1 and Test 2.
  • the conditions under which the core magnetic properties of the dust core are optimal are that the heat treatment temperature is higher than the heat treatment temperature when the coercive force is minimized, lower than the crystallization temperature of the amorphous phase, and the crystallinity is the coercive force Hc. It was confirmed that the crystallinity was higher than the crystallinity at the time of minimum. It was also confirmed that when the heat treatment was performed at an excessive temperature, the degree of crystallinity became too high and the core magnetic properties deteriorated. Accordingly, it was confirmed that the crystallinity is preferably 80 to 95%.
  • the iron-based soft magnetic powder becomes a material having optimum core magnetic properties when it becomes a dust core in the composition, crystallinity, and hardness defined in the present invention.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

An iron-based soft magnetic powder obtained by precipitating a crystallite by crystallizing part of an amorphous phase by heat processing. The iron-based soft magnetic powder is characterized in that the iron-based soft magnetic powder includes Si, B, Cu, Nb, and unavoidable impurities, and has a crystallinity higher than a crystallinity when the coercive force is at a minimum.

Description

鉄基軟磁性粉末及びその製造方法、並びに鉄基軟磁性合金粉末を含む物品及びその製造方法Iron-based soft magnetic powder and method for producing the same, and article containing iron-based soft magnetic alloy powder and method for producing the same
　本発明は、応力が負荷された状態であっても良好な磁気特性を示す鉄基軟磁性粉末及びその製造方法、並びに鉄基軟磁性合金粉末を含む物品及びその製造方法に関する。 The present invention relates to an iron-based soft magnetic powder exhibiting good magnetic properties even under stress and a method for producing the same, and an article containing the iron-based soft magnetic alloy powder and a method for producing the same.
　チョークコイルやリアクトルコイル等における圧粉磁心は、軟磁性粉末にエポキシ系樹脂等、絶縁性の結合剤を添加し、射出成型やプレス成型等により所定の形状に成型されて製造される。このとき、軟磁性粉末には応力が負荷された状態で、圧粉磁心が製造される。 A dust core in a choke coil, a reactor coil or the like is manufactured by adding an insulating binder such as an epoxy resin to soft magnetic powder and molding the powder into a predetermined shape by injection molding or press molding. At this time, the dust core is manufactured in a state where stress is applied to the soft magnetic powder.
　圧粉磁心の製造に用いられる軟磁性粉末として、従来、例えば、特許文献１に記載のような鉄基ナノ結晶合金粉末が用いられてきた。このような鉄基ナノ結晶合金粉末は、全体がアモルファス相である合金を製造した後、熱処理を施してナノ結晶化させることにより製造される。 Conventionally, for example, an iron-based nanocrystalline alloy powder described in Patent Document 1 has been used as a soft magnetic powder used in the production of a dust core. Such an iron-based nanocrystalline alloy powder is produced by producing an alloy having an amorphous phase as a whole and then subjecting it to a nanocrystallization by heat treatment.
　そして、このような磁性粉体は、例えば、特許文献２に開示されているように鉄基軟磁性合金粉末にｂｃｃ相を析出させる熱処理を行い、保磁力が最小となるように調整されて用いられる。 Such a magnetic powder is used, for example, by performing a heat treatment for precipitating the bcc phase on the iron-based soft magnetic alloy powder as disclosed in Patent Document 2 and adjusting the coercive force to be minimized. It is done.
　［特許文献１］特開平１－７９３４２号公報
　［特許文献２］特開２０１０－２８０９５６号公報 [Patent Document 1] JP-A-1-79342 [Patent Document 2] JP-A-2010-280956
　しかし、得られた磁性粉末の静磁気特性（保磁力）を最適化した場合でも、射出成型やプレス成型等の加圧を伴う圧粉磁心製造プロセスを経て磁性粉末に応力が負荷され圧粉磁心となったときには、必ずしも最適なコア磁気特性（透磁率、コアロス）を発現するものではないという問題があった。 However, even when the magnetostatic properties (coercivity) of the obtained magnetic powder are optimized, stress is applied to the magnetic powder through a dust core manufacturing process involving pressurization such as injection molding or press molding, and the dust core When it became, there existed a problem that the optimal core magnetic characteristic (permeability, core loss) was not necessarily expressed.
　そこで、本発明では、射出成型やプレス成型等により応力が負荷された状態においても、圧粉磁心として最適なコア磁気特性を発現する鉄基軟磁性粉末及びその製造方法を提供すること、更には、鉄基軟磁性合金粉末を含む物品及びその製造方法を提供することを目的とする。 Therefore, the present invention provides an iron-based soft magnetic powder that exhibits optimum core magnetic properties as a dust core even in a state in which stress is applied by injection molding, press molding, or the like, and a method for producing the same, and An object of the present invention is to provide an article containing an iron-based soft magnetic alloy powder and a method for producing the same.
　本発明者らは、優れた静磁気特性を有し、更に静磁気特性を最適化した鉄基軟磁性粉末が、加圧を伴う射出成型やプレス成型等により応力が負荷され圧粉磁心となったときには、必ずしも最適なコア磁気特性を発現するものではないことを見出した。そして、本発明者らは、鋭意研究の結果、結晶化度を調整することにより、加圧を伴う射出成型やプレス成型等により、鉄基軟磁性粉末に応力が負荷された状態であっても、圧粉磁心等として最適なコア磁気特性を発現するとの知見を得て、本発明を完成するに至った。 The inventors of the present invention have developed an iron-based soft magnetic powder having excellent magnetostatic characteristics and optimized magnetostatic characteristics to form a powder magnetic core by applying stress by injection molding or press molding with pressurization. When found, it was found that the optimum core magnetic characteristics were not necessarily exhibited. And, as a result of intensive studies, the inventors have adjusted the crystallinity so that even if stress is applied to the iron-based soft magnetic powder by injection molding or press molding with pressurization, etc. As a result, the inventors have obtained the knowledge that optimum magnetic core characteristics can be obtained as a dust core, and have completed the present invention.
　すなわち、本発明は、熱処理によりアモルファス相の一部を結晶化させて結晶子を析出させてなる鉄基軟磁性粉末であって、当該鉄基軟磁性粉末は、Ｓｉ、Ｂ、Ｃｕ、Ｎｂ及び不可避不純物を含み、結晶化度が、保磁力が最小となるときの結晶化度より高いことを特徴とする鉄基軟磁性粉末である。 That is, the present invention is an iron-based soft magnetic powder obtained by crystallizing a part of an amorphous phase by heat treatment to precipitate crystallites, and the iron-based soft magnetic powder includes Si, B, Cu, Nb and An iron-based soft magnetic powder comprising inevitable impurities and having a crystallinity higher than the crystallinity when coercive force is minimized.
　本発明の一態様によれば、鉄基軟磁性粉末が、
Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
３．０≦ｘ≦１６．０
６．０≦ｙ≦１３．０
０．５≦ｚ≦２．０
０．５≦ｒ≦４．０
１．５≦ｚ＋ｒ≦４．５
１１．５≦ｙ＋ｒ≦１４．５
の関係を満たす］
の組成を有する、上記の鉄基軟磁性粉末が提供される。 According to one aspect of the present invention, the iron-based soft magnetic powder is
Fe 100- (x + y + z + r) Si x B y Cu z Nb r
[Wherein, x, y, z and r are at%,
3.0 ≦ x ≦ 16.0
6.0 ≦ y ≦ 13.0
0.5 ≦ z ≦ 2.0
0.5 ≦ r ≦ 4.0
1.5 ≦ z + r ≦ 4.5
11.5 ≦ y + r ≦ 14.5
Satisfy the relationship]
The above iron-based soft magnetic powder having the following composition is provided:
　本発明の一態様によれば、結晶化度が、８０～９５％である、上記の鉄基軟磁性粉末が提供される。 According to an aspect of the present invention, there is provided the above iron-based soft magnetic powder having a crystallinity of 80 to 95%.
　本発明の一態様によれば、ＩＳＯ１４５７７－１に準拠して測定した粉末の硬度が、１０００～１２５０ＨＶである、上記の鉄基軟磁性粉末が提供される。 According to one aspect of the present invention, there is provided the iron-based soft magnetic powder described above, wherein the hardness of the powder measured according to ISO 14577-1 is 1000 to 1250 HV.
　本発明の一態様によれば、略球形である、上記の鉄基軟磁性粉末が提供される。 According to one aspect of the present invention, there is provided the iron-based soft magnetic powder having a substantially spherical shape.
　本発明の一態様によれば、平均粒子径が０．５～５０μｍである、上記の鉄基軟磁性粉末が提供される。 According to one aspect of the present invention, the above iron-based soft magnetic powder having an average particle diameter of 0.5 to 50 μm is provided.
　本発明の一態様によれば、Ｆｅのうち０．５～２．０ａｔ％がＣｒで置換されている、上記の鉄基軟磁性粉末が提供される。 According to one aspect of the present invention, there is provided the above iron-based soft magnetic powder in which 0.5 to 2.0 at% of Fe is replaced with Cr.
　本発明の一態様によれば、加圧成型により応力が負荷されている上記の鉄基軟磁性粉末を含む物品が提供される。 According to one aspect of the present invention, an article including the iron-based soft magnetic powder that is stressed by pressure molding is provided.
　本発明の一態様によれば、圧粉磁心である、上記の物品が提供される。 According to an aspect of the present invention, there is provided the above article that is a dust core.
　本発明の一態様によれば、以下の工程を含む、鉄基軟磁性粉末の製造方法が提供される。
・第１工程
　鉄基軟磁性粉末を構成するＦｅ、Ｓｉ、Ｂ、Ｃｕ、Ｎｂを所定の組成となるように原料を秤量し、溶解して合金溶湯を得る工程。
・第２工程
　第１工程で得られた合金溶湯からアトマイズ法により略球形のアモルファス粒子を得る工程。
・第３工程
　第２工程で得られたアモルファス粒子に熱処理を行い、アモルファス相の一部を結晶化させて結晶子を析出させる工程であって、結晶化度を、保磁力が最小となるときの結晶化度より高くする工程。 According to one aspect of the present invention, a method for producing an iron-based soft magnetic powder including the following steps is provided.
-1st process The process which weighs and melt | dissolves a raw material so that Fe, Si, B, Cu, and Nb which comprise an iron group soft magnetic powder may become a predetermined composition, and obtains a molten alloy.
-2nd process The process of obtaining substantially spherical amorphous particle | grains by the atomizing method from the molten alloy obtained at the 1st process.
Third step A step of heat-treating the amorphous particles obtained in the second step to crystallize a part of the amorphous phase to precipitate crystallites, when the crystallinity is minimized and the coercive force is minimized. The step of making the crystallinity higher than.
　本発明の一態様によれば、第１工程では、以下の組成となるように原料を秤量し、溶解して合金溶湯を得る、上記の鉄基軟磁性粉末の製造方法が提供される。
Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
３．０≦ｘ≦１６．０
６．０≦ｙ≦１３．０
０．５≦ｚ≦２．０
０．５≦ｒ≦４．０
１．５≦ｚ＋ｒ≦４．５
１１．５≦ｙ＋ｒ≦１４．５
の関係を満たす。］ According to one aspect of the present invention, in the first step, there is provided a method for producing the above iron-based soft magnetic powder, wherein raw materials are weighed so as to have the following composition and melted to obtain a molten alloy.
Fe 100- (x + y + z + r) Si x B y Cu z Nb r
[Wherein, x, y, z and r are at%,
3.0 ≦ x ≦ 16.0
6.0 ≦ y ≦ 13.0
0.5 ≦ z ≦ 2.0
0.5 ≦ r ≦ 4.0
1.5 ≦ z + r ≦ 4.5
11.5 ≦ y + r ≦ 14.5
Satisfy the relationship. ]
　本発明の一態様によれば、前記第３工程における熱処理温度を、保磁力が最小となるときの熱処理温度より高く、アモルファス相の結晶化温度より低くする、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, the heat treatment temperature in the third step is higher than the heat treatment temperature when the coercive force is minimized, and lower than the crystallization temperature of the amorphous phase. A method is provided.
　本発明の一態様によれば、第３工程における結晶化度を８０～９５％とする、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, there is provided the method for producing the iron-based soft magnetic powder, wherein the crystallinity in the third step is 80 to 95%.
　本発明の一態様によれば、粉末の硬度を、保磁力が最小となるときの硬度より小さくする、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, there is provided a method for producing the above iron-based soft magnetic powder, wherein the hardness of the powder is smaller than the hardness when the coercive force is minimized.
　本発明の一態様によれば、粉末の硬度を、ＩＳＯ１４５７７－１に準拠して測定した粉末の硬度で１０００～１２５０ＨＶとする、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, there is provided a method for producing the above iron-based soft magnetic powder, wherein the hardness of the powder is 1000 to 1250 HV as measured according to ISO 14577-1.
　本発明の一態様によれば、平均粒子径を０．５～５０μｍとする、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, there is provided a method for producing the above iron-based soft magnetic powder having an average particle size of 0.5 to 50 μm.
　本発明の一態様によれば、上記の鉄基軟磁性粉末の製造方法において、Ｆｅのうち０．５～２．０ａｔ％をＣｒで置換する、上記の鉄基軟磁性粉末の製造方法が提供される。 According to one aspect of the present invention, there is provided the above iron-based soft magnetic powder manufacturing method, wherein 0.5 to 2.0 at% of Fe is replaced with Cr in the above-described iron-based soft magnetic powder manufacturing method. Is done.
　本発明の一態様によれば、上記の鉄基軟磁性粉末の製造方法の後に、加圧成型工程を含む、物品の製造方法が提供される。 According to one aspect of the present invention, there is provided an article manufacturing method including a pressure molding step after the iron-based soft magnetic powder manufacturing method.
　本発明の一態様によれば、物品が圧粉磁心である、上記の物品の製造方法が提供される。 According to one aspect of the present invention, there is provided the above method for manufacturing an article, wherein the article is a dust core.
　本発明の鉄基軟磁性粉末及びその製造方法によれば、Ｓｉ、Ｂ、Ｃｕ、Ｎｂを含み、熱処理によりアモルファス相の一部を結晶化させて結晶子を析出させてなる鉄基軟磁性粉末において、保磁力が最小となるときの結晶化度より高くすることで、射出成型やプレス成型などにより、鉄基軟磁性粉末に応力が負荷された状態であっても、圧粉磁心等として良好な磁性特性を発現する鉄基軟磁性粉末とすることができる。 According to the iron-based soft magnetic powder of the present invention and the method for producing the same, the iron-based soft magnetic powder containing Si, B, Cu, and Nb and crystallizing a part of the amorphous phase by heat treatment to precipitate crystallites. In this case, by making the crystallinity higher than when the coercive force is minimized, it is good as a dust core even when stress is applied to the iron-based soft magnetic powder by injection molding or press molding. Iron-based soft magnetic powder that exhibits excellent magnetic properties.
実施例における結晶化度と透磁率との関係を示す説明図である。It is explanatory drawing which shows the relationship between the crystallinity and the magnetic permeability in an Example. 実施例における結晶化度とコアロスとの関係を示す説明図である。It is explanatory drawing which shows the relationship between the crystallinity in an Example, and a core loss.
　以下、本発明の一実施形態について詳細に説明する。本発明は、以下の実施形態に限定されるものではなく、本発明の効果を阻害しない範囲で適宜変更を加えて実施することができる。なお、以下の説明において、「Ａ～Ｂ」は、「Ａ以上かつＢ以下」を意味する。 Hereinafter, an embodiment of the present invention will be described in detail. The present invention is not limited to the following embodiments, and can be implemented with appropriate modifications within a range that does not impair the effects of the present invention. In the following description, “A to B” means “A or more and B or less”.
　本実施形態の鉄基軟磁性粉末は、Ｓｉ、Ｂ、Ｃｕ、Ｎｂを含み、熱処理によりアモルファス相の一部を結晶化させて結晶子を析出させてなる鉄基軟磁性粉末である。このような鉄基軟磁性粉末では、熱処理により、アモルファス相にＦｅを主成分とする体心立方構造の結晶子（ｂｃｃ相）、Ｃｕを主成分とする面心立方構造の結晶子（ｆｃｃ相）が分散した合金を形成することができ、優れた静磁気特性が得られる。 The iron-based soft magnetic powder of the present embodiment is an iron-based soft magnetic powder containing Si, B, Cu, and Nb and crystallizing a part of the amorphous phase by heat treatment to precipitate crystallites. In such an iron-based soft magnetic powder, a crystallite having a body-centered cubic structure containing Fe as a main component (bcc phase) and a crystallite having a face-centered cubic structure containing Cu as a main component (fcc phase) by heat treatment. ) Can be formed, and excellent magnetostatic properties can be obtained.
　そして、熱処理温度により、ナノ結晶子の析出形態を変えることができるので、鉄基軟磁性粉末の静磁気特性を所望の状態に調整することができる。 Since the nanocrystallite precipitation form can be changed by the heat treatment temperature, the magnetostatic characteristics of the iron-based soft magnetic powder can be adjusted to a desired state.
　特に、鉄基軟磁性粉末が下記の組成を有するときに、圧粉磁心等、射出成形やプレス成型等の加圧成型により応力が負荷された状態で用いる際に、より良好な磁性特性を発現する鉄基軟磁性粉末とすることができる。 In particular, when the iron-based soft magnetic powder has the following composition, it exhibits better magnetic properties when used in a state where stress is applied by pressure molding such as injection molding or press molding, such as a dust core. Iron-based soft magnetic powder.
Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
３．０≦ｘ≦１６．０
６．０≦ｙ≦１３．０
０．５≦ｚ≦２．０
０．５≦ｒ≦４．０
１．５≦ｚ＋ｒ≦４．５
１１．５≦ｙ＋ｒ≦１４．５
の関係を満たす。］ Fe 100- (x + y + z + r) Si x B y Cu z Nb r
[Wherein, x, y, z and r are at%,
3.0 ≦ x ≦ 16.0
6.0 ≦ y ≦ 13.0
0.5 ≦ z ≦ 2.0
0.5 ≦ r ≦ 4.0
1.5 ≦ z + r ≦ 4.5
11.5 ≦ y + r ≦ 14.5
Satisfy the relationship. ]
　Ｓｉは、アモルファス相形成能を向上させる。Ｓｉ量ｘは、十分なアモルファス相形成能を有するとともに、良好な磁気特性を得るために、Ｆｅとの量比Ｓｉ／Ｆｅはほぼ一定とし、３．０～１６．０ａｔ％とすることが好ましい。 Si improves the amorphous phase forming ability. The Si amount x has a sufficient ability to form an amorphous phase, and in order to obtain good magnetic properties, the amount ratio Si / Fe with Fe is preferably substantially constant, and is preferably 3.0 to 16.0 at%. .
　Ｂ及びＮｂは、アモルファス相形成能を向上させる。特に、Ｎｂはアトマイズ法により鉄基軟磁性粉末を製造するときには必須成分となる。ここで、Ｂ量は、６．０ａｔ％以上とするとアモルファス相形成能が大きくなり、１３．０ａｔ％以下とすると良好な磁気特性を示すため好ましい。 B and Nb improve the ability to form an amorphous phase. In particular, Nb is an essential component when an iron-based soft magnetic powder is produced by an atomizing method. Here, if the amount of B is 6.0 at% or more, the amorphous phase forming ability increases, and if it is 13.0 at% or less, good magnetic characteristics are exhibited, which is preferable.
　Ｂ量ｙとＮｂ量ｒとの和ｙ＋ｒは、１１．５≦ｙ＋ｒ≦１４．５（ａｔ％）であることが好ましい。１１．５ａｔ％以上とすると、アモルファス相の形成能が大きくなり、１４．５ａｔ％以下とすると良好な磁気特性を示す。 The sum y + r of the B amount y and the Nb amount r is preferably 11.5 ≦ y + r ≦ 14.5 (at%). If it is 11.5 at% or more, the ability to form an amorphous phase increases, and if it is 14.5 at% or less, good magnetic properties are exhibited.
　Ｃｕ及びＮｂは、析出するナノ結晶子の粒径を制御する効果がある元素である。ここで、ナノ結晶子の粒径を制御する効果は、Ｃｕ量の影響が大きく、Ｃｕ量ｚは、０．５ａｔ％以上とすると、アモルファス相中に粒径数１０ｎｍに制御されたナノ結晶子が分散した組織を容易に得ることができる。これにより、熱処理後に良好な磁気特性を示す鉄基軟磁性粉末とすることができる。また、２．０ａｔ％以下とすると良好な磁気特性を示すため好ましい。 Cu and Nb are elements that have an effect of controlling the particle size of the deposited nanocrystallites. Here, the effect of controlling the particle size of the nanocrystallite is greatly influenced by the amount of Cu. When the amount of Cu z is 0.5 at% or more, the nanocrystallite whose particle size is controlled to several tens of nm in the amorphous phase. Can be easily obtained. Thereby, it can be set as the iron group soft magnetic powder which shows a favorable magnetic characteristic after heat processing. Moreover, it is preferable to set it to 2.0 at% or less because good magnetic characteristics are exhibited.
　更に、Ｃｕ量ｚとＮｂ量ｒとの和ｚ＋ｒは、１．５≦ｚ＋ｒ≦４．５（ａｔ％）であることが好ましい。１．５ａｔ％以上とするとナノ結晶子の粒径制御に有効に作用し、４．５ａｔ％以下とすると良好な磁気特性を示す。 Furthermore, the sum z + r of the Cu amount z and the Nb amount r is preferably 1.5 ≦ z + r ≦ 4.5 (at%). If it is 1.5 at% or more, it effectively acts on the control of the particle size of the nanocrystallite, and if it is 4.5 at% or less, good magnetic properties are exhibited.
　鉄基軟磁性粉末の結晶化度は、後述する熱処理により、粉末の状態で保磁力が最小となるときの結晶化度より高く形成されている。 The crystallinity of the iron-based soft magnetic powder is higher than the crystallinity when the coercive force is minimized in the powder state by heat treatment described later.
　鉄基軟磁性粉末の結晶化度は、８０～９５％とすることが好ましい。これによれば、圧縮応力が負荷された状態で製造される磁性部品に用いても良好な磁気特性を示す鉄基軟磁性粉末とすることができる。 The crystallinity of the iron-based soft magnetic powder is preferably 80 to 95%. According to this, even if it uses for the magnetic component manufactured in the state where the compressive stress was loaded, it can be set as the iron group soft magnetic powder which shows a favorable magnetic characteristic.
　本発明における「結晶化度」は、粉末中に析出した結晶相の割合であり、例えば、「結晶化度８０％」とは、結晶相の割合が８０％で残部２０％がアモルファス相であることを示す。本発明における「結晶化度」は、Ｘ線回折法を用い、下記のピーク分離により算出した。（株式会社リガク（２０１０年発行）．Ｘ線解析ハンドブック（第６版）　株式会社リガク） The “crystallinity” in the present invention is the ratio of the crystal phase precipitated in the powder. For example, “crystallinity 80%” is the ratio of the crystal phase is 80% and the remaining 20% is the amorphous phase. It shows that. The “crystallinity” in the present invention was calculated by the following peak separation using an X-ray diffraction method. (Rigaku Corporation (issued in 2010). X-ray analysis handbook (6th edition) Rigaku Corporation)
（１）バックグラウンドの分離
　低角度側から高角度側に直線近似により直線を引き、当該直線の下方の面積をバックグラウンドとして設定する。 (1) Separation of background A straight line is drawn by linear approximation from the low angle side to the high angle side, and the area below the straight line is set as the background.
（２）ハローの分離
　アモルファス成分によるハローパターンを推定し、バックグラウンドを減じた散乱曲線からハロー部分を分離する。 (2) Separation of halo A halo pattern due to an amorphous component is estimated, and a halo portion is separated from a scattering curve with reduced background.
（３）結晶性回折線の分離
　上記（２）と同様の方法により、結晶性回折線を分離する。 (3) Separation of crystalline diffraction lines Crystalline diffraction lines are separated by the same method as in (2) above.
（４）結晶化度の算出
　全散乱曲線から分離した、非晶成分及び結晶成分の回折曲線の曲線下の面積（積分強度）を用い、下式により結晶化度を算出する。 (4) Calculation of crystallinity Using the area (integrated intensity) under the diffraction curve of the amorphous component and the crystal component separated from the total scattering curve, the crystallinity is calculated by the following equation.
（数１）
　Ｘｃ＝Ｉｃ／（Ｉｃ＋Ｉａ）
　Ｘｃ：結晶化度、Ｉｃ：結晶性散乱強度、Ｉａ：非晶性散乱強度 (Equation 1)
Xc = Ic / (Ic + Ia)
Xc: crystallinity, Ic: crystalline scattering intensity, Ia: amorphous scattering intensity
　チョークコイルやリアクトルコイル等における圧粉磁心は、軟磁性粉末にエポキシ系樹脂等、絶縁性の結合剤を添加し、射出成型やプレス成型等により所定の形状に成型されて製造される。このとき、軟磁性粉末には応力が負荷された状態で、圧粉磁心が製造される。 A dust core in a choke coil, a reactor coil or the like is manufactured by adding an insulating binder such as an epoxy resin to soft magnetic powder and molding the powder into a predetermined shape by injection molding or press molding. At this time, the dust core is manufactured in a state where stress is applied to the soft magnetic powder.
　鉄基軟磁性粉末の硬度は、１０００～１２５０ＨＶとすることが好ましい。これによれば、射出成形やプレス成型を行うときに流動性が良いので、圧粉磁心等としたときに良好な磁気特性を示す鉄基軟磁性粉末とすることができる。 The hardness of the iron-based soft magnetic powder is preferably 1000 to 1250 HV. According to this, since fluidity | liquidity is good when performing injection molding or press molding, it can be set as the iron-based soft magnetic powder which shows a favorable magnetic characteristic when it is set as a dust core.
　鉄基軟磁性粉末は略球形に形成されている。これによれば、射出成形やプレス成型を行うときに、圧粉磁心での鉄基軟磁性粉末の充填率を高くすることができるので、磁気特性を向上させることができる。ここで、すべての粉末形状が略球形でなくてもよく、例えば、粒子の長径をａ、短径をｂとした場合、１≦ａ／ｂ≦１．２の関係を満たす粒子が７０％以上あるとよい。 The iron-based soft magnetic powder is formed in a substantially spherical shape. According to this, since the filling rate of the iron-based soft magnetic powder in the dust core can be increased when performing injection molding or press molding, the magnetic characteristics can be improved. Here, not all of the powder shapes may be substantially spherical. For example, when the major axis of the particles is a and the minor axis is b, 70% or more of the particles satisfy the relationship of 1 ≦ a / b ≦ 1.2. There should be.
　鉄基軟磁性粉末の平均粒子径を０．５～５０μｍにすると、圧粉磁心等とした時に、圧粉磁心等の絶縁を確保しつつ、且つ鉄基軟磁性粉末の充填率高くすることができるので、磁気特性を向上させることができる。粒子径が小さいと、圧粉磁心を高周波帯で用いるときに渦電流損失が小さくなるため、低損失とすることができるが、小さ過ぎると十分な透磁率μが得られなくなるため、０．５μｍ以上とすることが好ましい。また、鉄基軟磁性粉末の平均粒子径を１０μｍ以下にすると、１ＭＨｚ以上の高周波帯で圧粉磁心を使用するときに、渦電流損失を低減させる事ができ、必要十分な透磁率μを得ることができるので更に好ましい。 When the average particle diameter of the iron-based soft magnetic powder is set to 0.5 to 50 μm, when the dust core is made, the insulation of the dust core can be secured and the filling rate of the iron-based soft magnetic powder can be increased. As a result, the magnetic properties can be improved. When the particle diameter is small, the eddy current loss is small when the dust core is used in a high frequency band, so the loss can be reduced. However, if the particle diameter is too small, a sufficient magnetic permeability μ cannot be obtained. The above is preferable. Moreover, when the average particle diameter of the iron-based soft magnetic powder is 10 μm or less, eddy current loss can be reduced when a dust core is used in a high frequency band of 1 MHz or more, and a necessary and sufficient magnetic permeability μ is obtained. More preferably.
　本実施形態に係る物品は、加圧成型により応力が負荷されている上記の鉄基軟磁性粉末を含む。本実施形態に係る物品は、エレクトロニクスや自動車用の部品など様々な用途で用いられる軟磁性を有する部品等であり、特に圧粉磁心である。上述の鉄基軟磁性粉末の特性により、射出成形やプレス成型等の加圧成型により応力が負荷されている上述の鉄基軟磁性粉末を含む物品、特に圧粉磁心は、良好なコア磁性特性（透磁率、コアロス）を発現する。 The article according to this embodiment includes the iron-based soft magnetic powder that is stressed by pressure molding. The article according to the present embodiment is a soft magnetic part used for various purposes such as electronics and automotive parts, and is particularly a dust core. Due to the characteristics of the iron-based soft magnetic powder described above, an article including the iron-based soft magnetic powder that is stressed by pressure molding such as injection molding or press molding, particularly a dust core, has good core magnetic characteristics. (Permeability, core loss) is expressed.
（製造方法）
　上述の鉄基軟磁性粉末の製造方法について説明する。 (Production method)
A method for producing the iron-based soft magnetic powder will be described.
　第１工程では、Ｆｅ、Ｓｉ、Ｂ、Ｃｕ、Ｎｂを所定の組成、例えば、以下の好ましい組成となるように原料を秤量し、溶解して合金溶湯を得る。 In the first step, raw materials are weighed and melted to obtain a molten alloy of Fe, Si, B, Cu, and Nb so as to have a predetermined composition, for example, the following preferable composition.
Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
３．０≦ｘ≦１６．０
６．０≦ｙ≦１３．０
０．５≦ｚ≦２．０
０．５≦ｒ≦４．０
１．５≦ｚ＋ｒ≦４．５
１１．５≦ｙ＋ｒ≦１４．５
の関係を満たす。］ Fe 100- (x + y + z + r) Si x B y Cu z Nb r
[Wherein, x, y, z and r are at%,
3.0 ≦ x ≦ 16.0
6.0 ≦ y ≦ 13.0
0.5 ≦ z ≦ 2.0
0.5 ≦ r ≦ 4.0
1.5 ≦ z + r ≦ 4.5
11.5 ≦ y + r ≦ 14.5
Satisfy the relationship. ]
　続く第２工程では、第１工程で得られた合金溶湯からアトマイズ法により略球形のアモルファス粒子を得る。 In the subsequent second step, substantially spherical amorphous particles are obtained from the molten alloy obtained in the first step by an atomizing method.
　本実施形態では、公知の水アトマイズ法を採用する。第１工程で得られた合金溶湯を溶湯オリフィスより落下させ、アトマイズノズルから噴射される水膜にて溶融した原材料を急冷凝固させる。この粉末を回収し、乾燥、および分級を経て、粒子形状が略球形である所定の粒径のアモルファス粒子を得ることができる。 In this embodiment, a known water atomization method is employed. The molten alloy obtained in the first step is dropped from the molten orifice, and the raw material melted by the water film sprayed from the atomizing nozzle is rapidly cooled and solidified. The powder is recovered, dried, and classified to obtain amorphous particles having a predetermined particle size and having a substantially spherical particle shape.
　続く第３工程では、第２工程で得られたアモルファス粒子に熱処理を行い、アモルファス相の一部を結晶化させる。このとき、粉末の結晶化度を、保磁力が最小となるときの結晶化度より高くする。 In the subsequent third step, the amorphous particles obtained in the second step are heat-treated to crystallize a part of the amorphous phase. At this time, the crystallinity of the powder is set higher than the crystallinity when the coercive force is minimized.
　本発明における熱処理は、窒素雰囲気にて所定の温度に等温保持し、アモルファス相の一部を結晶化させて、数１０ｎｍのナノ結晶子を析出させて、磁気特性を調整するために行う。ここで、粉末酸化防止等を考慮する必要がない場合であれば大気中で熱処理することもできる。 The heat treatment in the present invention is performed in order to adjust the magnetic characteristics by isothermally maintaining a predetermined temperature in a nitrogen atmosphere, crystallizing a part of the amorphous phase, and precipitating nanocrystallites of several tens of nanometers. Here, if it is not necessary to consider powder oxidation prevention or the like, heat treatment can be performed in the air.
　鉄基軟磁性粉末の熱分析（ＤＳＣ）曲線を行うと、２つの発熱ピークが認められる。低温側の発熱ピークの温度Ｔｘは体心立方構造の結晶相が析出するｂｃｃ相析出温度であり、高温側の発熱ピークの温度Ｔ１はアモルファス相結晶化温度である。 When a thermal analysis (DSC) curve of the iron-based soft magnetic powder is performed, two exothermic peaks are observed. The low-temperature exothermic peak temperature Tx is the bcc phase precipitation temperature at which the body-centered cubic crystal phase precipitates, and the high-temperature exothermic peak temperature T1 is the amorphous phase crystallization temperature.
　本発明の鉄基軟磁性粉末では、熱処理により、アモルファス相にＦｅを主成分とする体心立方構造の結晶子（ｂｃｃ相）、Ｃｕを主成分とする面心立方構造の結晶子（ｆｃｃ相）が分散した合金を形成することができ、優れた静磁気特性が得られる。 In the iron-based soft magnetic powder of the present invention, a crystallite having a body-centered cubic structure containing Fe as a main component (bcc phase) and a crystallite having a face-centered cubic structure containing Cu as a main component (fcc phase) by heat treatment. ) Can be formed, and excellent magnetostatic properties can be obtained.
　そして、熱処理温度により、ナノ結晶子の析出形態を変えることができるので、鉄基軟磁性粉末の静磁気特性を所望の状態に調整することができる。 Since the nanocrystallite precipitation form can be changed by the heat treatment temperature, the magnetostatic characteristics of the iron-based soft magnetic powder can be adjusted to a desired state.
　圧粉磁心の特性を反映する磁気特性として、透磁率μ、コアロスＰｃｖが重要である。ここで、透磁率μは高い方がよく、コアロスＰｃｖは低い方がよい。 Permeability μ and core loss Pcv are important as magnetic characteristics reflecting the characteristics of the dust core. Here, it is preferable that the magnetic permeability μ is high and the core loss Pcv is low.
　粉末体の状態では、保磁力Ｈｃが低いと透磁率μは高くなり、コアロスを低くすることができるため、従来は、保持力Ｈｃが最小となるように熱処理が行われてきた。 In the state of powder, when the coercive force Hc is low, the magnetic permeability μ becomes high and the core loss can be reduced. Conventionally, heat treatment has been performed so that the coercive force Hc is minimized.
　しかし、得られた磁性粉末の静磁気特性（保磁力）を最適化した場合でも、射出成型やプレス成型等の圧粉磁心製造プロセスを経て磁性粉末に応力が負荷され圧粉磁心となったときには、必ずしも最適なコア磁気特性（透磁率、コアロス）を発現するものではないという問題があった。 However, even when the magnetostatic properties (coercive force) of the obtained magnetic powder are optimized, when the magnetic powder is subjected to a stress magnetic core manufacturing process such as injection molding or press molding to become a powder magnetic core. However, there is a problem that the optimum core magnetic properties (permeability, core loss) are not necessarily exhibited.
　熱処理温度が、保磁力Ｈｃが最小となる熱処理温度Ｔ２を超えると、保持力Ｈｃは増大し、粉末の静磁気特性としては最適条件ではなくなる。このとき、結晶化度は増大し、硬度は低下する。 When the heat treatment temperature exceeds the heat treatment temperature T2 at which the coercive force Hc is minimized, the coercive force Hc is increased and the magnetostatic characteristics of the powder are not optimal. At this time, the crystallinity increases and the hardness decreases.
　一方、保磁力Ｈｃが最小となる熱処理温度Ｔ２以上の熱処理温度で、圧粉磁心のコア磁気特性を示す透磁率μが最大値を示し、コアロスが最小値を示す熱処理温度Ｔ３が存在する。 On the other hand, at a heat treatment temperature equal to or higher than the heat treatment temperature T2 at which the coercive force Hc is minimized, there is a heat treatment temperature T3 at which the magnetic permeability μ indicating the core magnetic characteristics of the dust core has a maximum value and the core loss has a minimum value.
　本発明者らは、熱処理温度を、保磁力Ｈｃが最小となるときの熱処理温度Ｔ２より高く、アモルファス相の結晶化温度Ｔ１より低いＴ３に設定し、結晶化度、硬度などを調整することにより、最適なコア磁気特性（透磁率、コアロス）を発現する鉄基軟磁性粉末を見出した。 The present inventors set the heat treatment temperature to T3 higher than the heat treatment temperature T2 when the coercive force Hc is minimized and lower than the crystallization temperature T1 of the amorphous phase, and adjust the crystallinity, hardness, etc. The present inventors have found an iron-based soft magnetic powder that exhibits optimum core magnetic properties (permeability, core loss).
　熱処理温度Ｔ３は、鉄基軟磁性粉末の結晶化度が、８０～９５％となるように設定することが好ましい。 The heat treatment temperature T3 is preferably set so that the crystallinity of the iron-based soft magnetic powder is 80 to 95%.
　また、熱処理温度Ｔ３は、１０００～１２５０ＨＶとなるように設定することが好ましい。 The heat treatment temperature T3 is preferably set to be 1000 to 1250 HV.
　これによれば、圧粉磁心製造プロセスである射出成型やプレス成型等により応力が負荷され、圧粉磁心となったときに、最適なコア磁気特性を有する鉄基軟磁性粉末とすることができる。 According to this, when a stress is applied by a dust core manufacturing process, such as injection molding or press molding, and a dust core is formed, an iron-based soft magnetic powder having optimum core magnetic characteristics can be obtained. .
　本実施形態に係る物品の製造方法は、上述の鉄基軟磁性粉末の製造方法の後に、加圧成型工程を含む。本実施形態に係る圧粉磁心の製造方法により得られる物品、特に圧粉磁心は、上述の鉄基軟磁性粉末の特性により、良好なコア磁性特性（透磁率、コアロス）を発現する。 The method for manufacturing an article according to this embodiment includes a pressure molding step after the above-described method for manufacturing an iron-based soft magnetic powder. Articles obtained by the method for manufacturing a dust core according to the present embodiment, particularly a dust core, exhibit good core magnetic properties (permeability, core loss) due to the properties of the iron-based soft magnetic powder described above.
（変更例）
　電子部品等で圧粉磁心を使用する場合、湿気等に対する耐食性が高い材料が求められる。鉄基軟磁性粉末において、Ｆｅの０．５～２．０ａｔ％をＣｒで置換することもできる。これによれば、良好な磁気特性を維持しつつ、耐食性を向上させることができる。 (Example of change)
When using a dust core for electronic parts, a material having high corrosion resistance against moisture and the like is required. In the iron-based soft magnetic powder, 0.5 to 2.0 at% of Fe can be replaced with Cr. According to this, corrosion resistance can be improved while maintaining good magnetic properties.
　アトマイズ法として、ガスアトマイズ法、油アトマイズ法、など採用することもできる。 As the atomizing method, a gas atomizing method, an oil atomizing method, or the like can be adopted.
　本発明の鉄基軟磁性粉末及びその製造方法によれば、結晶化度を、保磁力が最小となるときの結晶化度より高くすることで、射出成型やプレス成型により、鉄基軟磁性粉末に応力が負荷された状態であっても、圧粉磁心が良好なコア磁性特性を発現する鉄基軟磁性粉末とすることができる。 According to the iron-based soft magnetic powder of the present invention and the method for producing the same, the iron-based soft magnetic powder can be obtained by injection molding or press molding by making the crystallinity higher than the crystallinity when the coercive force is minimized. Even when stress is applied to the iron-based soft magnetic powder, the powder magnetic core can exhibit good core magnetic properties.
　以下に本発明の実施例を示す。本発明の内容はこれらの実施例により限定して解釈されるものではない。 Examples of the present invention are shown below. The contents of the present invention are not construed as being limited by these examples.
　表１に示される各組成に調製した混合材料を高周波誘導炉にて溶融し水アトマイズ法にて軟磁性粉末を得た。表中には、ｂｃｃ相析出温度Ｔｘ及び飽和磁化（Ｂｓ）の測定結果を併せて示す。評価粉末作製条件は以下の通りである。 The mixed materials prepared in the respective compositions shown in Table 1 were melted in a high frequency induction furnace, and soft magnetic powder was obtained by a water atomization method. In the table, the measurement results of the bcc phase precipitation temperature Tx and the saturation magnetization (Bs) are also shown. Evaluation powder preparation conditions are as follows.
＜水アトマイズ条件＞
　・水圧：１００ＭＰａ
　・水量：１００Ｌ／ｍｉｎ
　・水温：２０℃
　・オリフィス径：φ４ｍｍ
　・溶湯原材料温度：１８００℃ <Water atomization conditions>
・ Water pressure: 100 MPa
・ Water volume: 100L / min
・ Water temperature: 20 ℃
・ Orifice diameter: φ4mm
-Melt raw material temperature: 1800 ° C
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　次に、得られた軟磁性粉末を回収し、振動真空乾燥機（ＶＵ―６０：中央化工機株式会社製）により乾燥をおこなった。減圧雰囲気下で乾燥を行うため、大気圧雰囲気下で行う乾燥方法に比べ低酸素雰囲気で乾燥を行うことができ、また低温で短時間に乾燥を行うことができる。さらに、乾燥中に軟磁性粉末に振動を加えることでさらに短時間での乾燥が可能となり、粉末の凝集や酸化を防ぐことができる。本実施例では、乾燥温度：１００℃、乾燥室内の圧力：－０．１ＭＰａ（ゲージ圧）、乾燥時間：６０分とした。 Next, the obtained soft magnetic powder was collected and dried with a vibration vacuum dryer (VU-60: manufactured by Chuo Kako Co., Ltd.). Since drying is performed in a reduced pressure atmosphere, drying can be performed in a low oxygen atmosphere as compared with a drying method performed in an atmospheric pressure atmosphere, and drying can be performed in a short time at a low temperature. Further, by applying vibration to the soft magnetic powder during drying, drying can be performed in a shorter time, and aggregation and oxidation of the powder can be prevented. In this example, the drying temperature was 100 ° C., the pressure in the drying chamber was −0.1 MPa (gauge pressure), and the drying time was 60 minutes.
　次に得られた軟磁性粉末を気流分級装置（ターボクラシファイア：日清エンジニアリング株式会社製）により分級して目的の平均粒径を有する粉末材（６μｍ、２μｍ）を得た。該粉末材の粒度分布測定はレーザ回折方式の粒度分布測定装置（ＭＴ３３００ＥＸII：マイクロトラックベル株式会社製）にて行った。 Next, the obtained soft magnetic powder was classified by an airflow classifier (turbo classifier: manufactured by Nisshin Engineering Co., Ltd.) to obtain a powder material (6 μm, 2 μm) having a target average particle diameter. The particle size distribution of the powder material was measured with a laser diffraction type particle size distribution measuring device (MT3300EXII: manufactured by Microtrack Bell Co., Ltd.).
　次に得られた軟磁性粉末について、結晶子径、結晶化度、硬度及び保磁力Ｈｃを評価した。 Next, the crystallite diameter, crystallinity, hardness, and coercive force Hc of the obtained soft magnetic powder were evaluated.
　結晶子径及び結晶化度の測定装置、測定条件は以下のとおりである。
　・測定装置：粉末Ｘ線回折装置（ＭｉｎＦｌｅｘ６００：株式会社リガク製）
　・測定条件：電圧４０ｋＶ、電流１５ｍＡ、ステップ０．０１ｄｅｇ、スピード１ｄｅｇ／ｍｉｎ The crystallite diameter and crystallinity measuring devices and measurement conditions are as follows.
Measurement device: Powder X-ray diffraction device (MinFlex 600: manufactured by Rigaku Corporation)
Measurement conditions: voltage 40 kV, current 15 mA, step 0.01 deg, speed 1 deg / min
　結晶子径は、ｂｃｃ　ＦｅＳｉピークを下記に示すＳｃｈｅｒｒｅｒの式を用いて算出した。ここで、ＦｅＳｉピークとして７８°付近のピークを用いた。 The crystallite diameter was calculated by using the Scherrer equation shown below for the bcc FeSi peak. Here, a peak around 78 ° was used as the FeSi peak.
Figure JPOXMLDOC01-appb-M000002
Figure JPOXMLDOC01-appb-M000002
　硬度測定装置及び測定方法は以下のとおりである。
　・測定装置：ナノインデンター（ＥＮＴ－２０００：株式会社エリオニクス製）
　・測定方法：ＩＳＯ１４５７７－１に準拠し、５μＮ～１００ｍＮの荷重を粒子断面にかけた後に圧痕のサイズを測定することで粉末硬度を算出した。 The hardness measuring device and measuring method are as follows.
-Measuring device: Nanoindenter (ENT-2000: manufactured by Elionix Co., Ltd.)
Measurement method: Based on ISO 14577-1, the powder hardness was calculated by measuring the size of the indentation after applying a load of 5 μN to 100 mN to the particle cross section.
　保磁力Ｈｃの測定方法及び測定方法は以下のとおりである。
　・測定装置：振動式試料型磁力計（ＶＳＭ－Ｃ７：東英工業株式会社製）
　・測定方法：得られた各粒度分布を有する粉末材を、ＶＳＭ測定用カプセルに２００ｍｇ充填しパラフィンにて固定し、最大磁界１００００Ｏｅを印加し飽和磁化測定（Ｂｓ）及び保磁力測定（Ｈｃ）を行った。 The measuring method and measuring method of the coercive force Hc are as follows.
・ Measuring device: Vibrating sample magnetometer (VSM-C7: manufactured by Toei Kogyo Co., Ltd.)
Measurement method: VSM measurement capsules filled with 200 mg of the obtained powder material having each particle size distribution, fixed with paraffin, applied with a maximum magnetic field of 10000 Oe, saturation magnetization measurement (Bs) and coercive force measurement (Hc) went.
　次に得られた各粒度分布を有する粉末材を、エポキシ樹脂（バインダ）およびトルエン（有機溶媒）と混合して混合物を得た。なお、エポキシ樹脂の添加量は軟磁性粉末材に対して３ｗｔ％とした。 Next, the obtained powder material having each particle size distribution was mixed with an epoxy resin (binder) and toluene (organic solvent) to obtain a mixture. The addition amount of the epoxy resin was 3 wt% with respect to the soft magnetic powder material.
　こうして調製した混合物を温度８０℃で３０分加熱して乾燥させ塊状の乾燥体を得た。次いで、乾燥体を目開き２００μｍの篩にかけ、粉末材(造粒体)を調製した。 The mixture thus prepared was dried by heating at a temperature of 80 ° C. for 30 minutes to obtain a lump-like dried body. Next, the dried product was passed through a sieve having an opening of 200 μm to prepare a powder material (granulated product).
　該粉末材を成形型に充填し、下記の条件で成型体（圧粉磁心）を得た。 The powder material was filled into a mold, and a molded body (dust core) was obtained under the following conditions.
＜成形条件＞
　・成形方法：プレス成形
　・成形体の形状：リング状
　・成形体寸法：外形１３ｍｍ、内径８ｍｍ、厚さ２ｍｍ
　・成形圧力：５ｔ／ｃｍ2（４９０ＭＰａ）
　・成形体硬化条件：１５０℃、３０分 <Molding conditions>
・ Molding method: Press molding ・ Shape of molded body: Ring shape ・ Dimension of molded body: External shape 13 mm, internal diameter 8 mm, thickness 2 mm
Molding pressure: 5 t / cm 2 (490 MPa)
-Molded body curing conditions: 150 ° C, 30 minutes
＜コイル作製条件＞
　上述した成型体に導線を下記の条件で巻き付け、チョークコイルを作製した。
　・導線材料：Ｃｕ
　・導線線径：０．２ｍｍ
　・巻き線数：１次４５ターン、２次４５ターン <Coil manufacturing conditions>
A conductive wire was wound around the molded body described above under the following conditions to produce a choke coil.
-Conductor material: Cu
・ Wire diameter: 0.2mm
・ Number of windings: 45 turns for primary, 45 turns for secondary
＜測定条件・評価＞
　上記条件で作製したチョークコイルのコア磁気特性（μ、Ｐｃｖ）を以下の条件で評価した。
　・測定装置：交流磁気特性測定装置（岩通計測製  Ｂ－ＨアナライザＳＹ８２５８）
　・測定周波数：１ＭＨｚ
　・透磁率μ測定条件：印加磁界１０ｍＴ
　・コアロス測定条件：印加磁界２５ｍＴ <Measurement conditions and evaluation>
The core magnetic characteristics (μ, Pcv) of the choke coil manufactured under the above conditions were evaluated under the following conditions.
・ Measuring device: AC magnetic property measuring device (BH analyzer SY8258, manufactured by Iwatori Keisoku)
・ Measurement frequency: 1MHz
・ Permeability μ measurement condition: Applied magnetic field 10 mT
・ Core loss measurement condition: Applied magnetic field 25mT
　評価結果を以下に示す。　組成７、８については、熱処理条件を下記６水準とし、異なる結晶化度としたものについて、粉末状態での保磁力Ｈｃ及び硬度ＨＶ、圧粉磁心のコア磁気特性（透磁率μ、コアロス）を評価した。結果を表２、図１、２に示す。ここで、表２において、試験１が組成７の結果に、試験２が組成８の結果に相当する。 Evaluation results are shown below. For compositions 7 and 8, the heat treatment conditions were set to the following six levels, and the coercive force Hc and hardness HV in the powder state and the core magnetic properties (permeability μ, core loss) of the powder magnetic core were used. evaluated. The results are shown in Table 2 and FIGS. Here, in Table 2, test 1 corresponds to the result of composition 7, and test 2 corresponds to the result of composition 8.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
　試験１、２ともに、結晶化度は熱処理温度の上昇とともに増大し、６００℃ではアモルファス相がすべて結晶化した。ここで、アモルファス相の結晶化温度は約６００℃と考えられる。なお、ｂｃｃ相析出温度Ｔｘ以下の５００℃から結晶化が始まっている理由としては、粉末の発熱反応により局所的に設定温度より温度が高くなる部分があることなどが推定される。 In both tests 1 and 2, the degree of crystallinity increased with increasing heat treatment temperature, and all amorphous phases were crystallized at 600 ° C. Here, the crystallization temperature of the amorphous phase is considered to be about 600 ° C. The reason why crystallization has started from 500 ° C. below the bcc phase precipitation temperature Tx is presumed to be a portion where the temperature is locally higher than the set temperature due to the exothermic reaction of the powder.
　また、粉末の静磁気特性として、保磁力Ｈｃが低く最も良好な磁気特性を示すのは、５３０℃で熱処理を行ったとき（試験１－３、試験２－３）であった。このとき、結晶化度は、試験１－３で７６、試験２－３で７４であった。また、硬度ＨＶは、試験１－３で１２５０ＨＶ、試験２－３で１２７０ＨＶであり、それぞれ最高値を示した。 As the magnetostatic characteristics of the powder, the best magnetic characteristics with a low coercive force Hc were obtained when heat treatment was performed at 530 ° C. (Test 1-3, Test 2-3). At this time, the crystallinity was 76 in Test 1-3 and 74 in Test 2-3. The hardness HV was 1250 HV in Test 1-3 and 1270 HV in Test 2-3, and each showed the highest value.
　従来は、この状態を目的の状態とし、熱処理温度が５３０℃と設定されていた。 Conventionally, this state is the target state, and the heat treatment temperature is set to 530 ° C.
　熱処理温度が保磁力Ｈｃが最小となる熱処理温度である５３０℃を超えると、保持力Ｈｃは増大し、粉末の静磁気特性としては最適条件ではなくなる。 When the heat treatment temperature exceeds 530 ° C., which is the heat treatment temperature at which the coercive force Hc is minimized, the coercive force Hc is increased and the magnetostatic characteristics of the powder are not optimal.
　ここで、熱処理温度である５３０℃を超えると、結晶化度は増大する。また、析出する結晶子の粒径が大きくなり硬度ＨＶが低下する。 Here, when the heat treatment temperature exceeds 530 ° C., the crystallinity increases. In addition, the grain size of the precipitated crystallites increases and the hardness HV decreases.
　一方、圧粉磁心のコア磁気特性は、熱処理温度５７０℃において、透磁率μは最大値を示し、コアロスは最小値を示した。 On the other hand, regarding the core magnetic properties of the dust core, the magnetic permeability μ showed the maximum value and the core loss showed the minimum value at the heat treatment temperature of 570 ° C.
　図１に示すように、保磁力Ｈｃが最小（熱処理温度５３０℃）となる結晶化度の透磁率と同じ透磁率を示す結晶化度は、試験１で９４％、試験２で９３％となった。 As shown in FIG. 1, the crystallinity showing the same permeability as that of the crystallinity at which the coercive force Hc is minimum (heat treatment temperature 530 ° C.) is 94% in Test 1 and 93% in Test 2. It was.
　図２に示すように、保磁力Ｈｃが最小となる結晶化度のコアロスと同じコアロスを示す結晶化度は、試験１、試験２ともに９１％となった。 As shown in FIG. 2, the crystallinity showing the same core loss as the crystallinity having the minimum coercive force Hc was 91% in both Test 1 and Test 2.
　つまり、圧粉磁心のコア磁気特性が最適となる条件は、熱処理温度が、保磁力が最小となるときの熱処理温度より高く、アモルファス相の結晶化温度より低く、結晶化度が、保磁力Ｈｃが最小となるときの結晶化度より高い、ということが確認された。また、過剰な温度で熱処理を行うと結晶化度が高くなりすぎ、コア磁気特性が悪化することも確認された。これにより、結晶化度は８０～９５％とすることが好適であることも確認された。 That is, the conditions under which the core magnetic properties of the dust core are optimal are that the heat treatment temperature is higher than the heat treatment temperature when the coercive force is minimized, lower than the crystallization temperature of the amorphous phase, and the crystallinity is the coercive force Hc. It was confirmed that the crystallinity was higher than the crystallinity at the time of minimum. It was also confirmed that when the heat treatment was performed at an excessive temperature, the degree of crystallinity became too high and the core magnetic properties deteriorated. Accordingly, it was confirmed that the crystallinity is preferably 80 to 95%.
　また、組成１～６においても同様の傾向が認められることを確認した。 Also, it was confirmed that the same tendency was observed in the compositions 1 to 6.
　以上より、鉄基軟磁性粉末が、本発明で規定した組成、結晶化度、硬度において、圧粉磁心となったときに最適なコア磁気特性を有する材料となることが確認された。

  From the above, it was confirmed that the iron-based soft magnetic powder becomes a material having optimum core magnetic properties when it becomes a dust core in the composition, crystallinity, and hardness defined in the present invention.

Claims (19)

  1. 　熱処理によりアモルファス相の一部を結晶化させて結晶子を析出させてなる鉄基軟磁性粉末であって、
    　Ｓｉ、Ｂ、Ｃｕ、Ｎｂ及び不可避不純物を含み、
    　結晶化度が、保磁力が最小となるときの結晶化度より高いことを特徴とする鉄基軟磁性粉末。     An iron-based soft magnetic powder obtained by crystallizing a part of an amorphous phase by heat treatment to precipitate crystallites,
    Containing Si, B, Cu, Nb and inevitable impurities,
    An iron-based soft magnetic powder characterized in that the crystallinity is higher than the crystallinity when coercive force is minimized.
  2. 　前記鉄基軟磁性粉末が、Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
    ［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
    ３．０≦ｘ≦１６．０
    ６．０≦ｙ≦１３．０
    ０．５≦ｚ≦２．０
    ０．５≦ｒ≦４．０
    １．５≦ｚ＋ｒ≦４．５
    １１．５≦ｙ＋ｒ≦１４．５
    の関係を満たす］の組成を有することを特徴とする請求項１に記載の鉄基軟磁性粉末。     The iron-based soft magnetic powder, Fe 100- (x + y + z + r) Si x B y Cu z Nb r
    [Wherein, x, y, z and r are at%,
    3.0 ≦ x ≦ 16.0
    6.0 ≦ y ≦ 13.0
    0.5 ≦ z ≦ 2.0
    0.5 ≦ r ≦ 4.0
    1.5 ≦ z + r ≦ 4.5
    11.5 ≦ y + r ≦ 14.5
    The iron-based soft magnetic powder according to claim 1, wherein the iron-based soft magnetic powder has a composition of
  3. 　前記結晶化度が、８０～９５％であることを特徴とする請求項１または請求項２に記載の鉄基軟磁性粉末。 The iron-based soft magnetic powder according to claim 1 or 2, wherein the crystallinity is 80 to 95%.
  4. 　ＩＳＯ１４５７７－１に準拠して測定した粉末の硬度が、１０００～１２５０ＨＶであることを特徴とする請求項１ないし請求項３のいずれか１つに記載の鉄基軟磁性粉末。 The iron-based soft magnetic powder according to any one of claims 1 to 3, wherein the hardness of the powder measured according to ISO 14577-1 is 1000 to 1250 HV.
  5. 　略球形であることを特徴とする請求項１ないし請求項４のいずれか１つに記載の鉄基軟磁性粉末。 The iron-based soft magnetic powder according to any one of claims 1 to 4, wherein the iron-based soft magnetic powder is substantially spherical.
  6. 　平均粒子径が０．５～５０μｍであることを特徴とする請求項１ないし請求項５のいずれか１つに記載の鉄基軟磁性粉末。 6. The iron-based soft magnetic powder according to claim 1, wherein the average particle diameter is 0.5 to 50 μm.
  7. 　Ｆｅのうち０．５～２．０ａｔ％がＣｒで置換されていることを特徴とする請求項１ないし請求項６のいずれか１つに記載の鉄基軟磁性粉末。 The iron-based soft magnetic powder according to any one of claims 1 to 6, wherein 0.5 to 2.0 at% of Fe is substituted with Cr.
  8. 　加圧成型により応力が負荷されている請求項１ないし請求項７のいずれか１つに記載の鉄基軟磁性粉末を含む、物品。 An article comprising the iron-based soft magnetic powder according to any one of claims 1 to 7, which is stressed by pressure molding.
  9. 　圧粉磁心である、請求項８に記載の物品。 The article according to claim 8, which is a dust core.
  10. 　以下の工程を含むことを特徴とする、鉄基軟磁性粉末の製造方法：
    ・第１工程
    　鉄基軟磁性粉末を構成するＦｅ、Ｓｉ、Ｂ、Ｃｕ、Ｎｂを所定の組成となるように原料を秤量し、溶解して合金溶湯を得る工程。
    ・第２工程
    　第１工程で得られた合金溶湯からアトマイズ法により略球形のアモルファス粒子を得る工程。
    ・第３工程
    　第２工程で得られたアモルファス粒子に熱処理を行い、アモルファス相の一部を結晶化させて結晶子を析出させる工程であって、結晶化度を、保磁力が最小となるときの結晶化度より高くする工程。     A method for producing an iron-based soft magnetic powder characterized by comprising the following steps:
    -1st process The process which weighs and melt | dissolves a raw material so that Fe, Si, B, Cu, and Nb which comprise an iron group soft magnetic powder may become a predetermined composition, and obtains a molten alloy.
    -2nd process The process of obtaining substantially spherical amorphous particle | grains by the atomizing method from the molten alloy obtained at the 1st process.
    Third step A step of heat-treating the amorphous particles obtained in the second step to crystallize a part of the amorphous phase to precipitate crystallites, when the crystallinity is minimized and the coercive force is minimized. The step of making the crystallinity higher than.
  11. 　前記第１工程において、以下の組成となるように原料を秤量し、溶解して合金溶湯を得ることを特徴とする請求項１０に記載の鉄基軟磁性粉末の製造方法。
    Ｆｅ１００―（ｘ＋ｙ＋ｚ＋ｒ）ＳｉｘＢｙＣｕｚＮｂｒ
    ［式中、ｘ、ｙ、ｚ、ｒはａｔ％で、
    ３．０≦ｘ≦１６．０
    ６．０≦ｙ≦１３．０
    ０．５≦ｚ≦２．０
    ０．５≦ｒ≦４．０
    １．５≦ｚ＋ｒ≦４．５
    １１．５≦ｙ＋ｒ≦１４．５
    の関係を満たす。］     The method for producing an iron-based soft magnetic powder according to claim 10, wherein in the first step, raw materials are weighed so as to have the following composition and melted to obtain a molten alloy.
    Fe 100- (x + y + z + r) Si x B y Cu z Nb r
    [Wherein, x, y, z and r are at%,
    3.0 ≦ x ≦ 16.0
    6.0 ≦ y ≦ 13.0
    0.5 ≦ z ≦ 2.0
    0.5 ≦ r ≦ 4.0
    1.5 ≦ z + r ≦ 4.5
    11.5 ≦ y + r ≦ 14.5
    Satisfy the relationship. ]
  12. 　前記第３工程における熱処理温度を、保磁力が最小となるときの熱処理温度より高く、アモルファス相の結晶化温度より低くすることを特徴とする請求項１０または請求項１１に記載の鉄基軟磁性粉末の製造方法。 12. The iron-based soft magnetism according to claim 10, wherein the heat treatment temperature in the third step is higher than the heat treatment temperature when the coercive force is minimized and lower than the crystallization temperature of the amorphous phase. Powder manufacturing method.
  13. 　前記第３工程における結晶化度を８０～９５％とすることを特徴とする請求項１０ないし請求項１２のいずれか１つに記載の鉄基軟磁性粉末の製造方法。 The method for producing an iron-based soft magnetic powder according to any one of claims 10 to 12, wherein the crystallinity in the third step is 80 to 95%.
  14. 　粉末の硬度を、保磁力が最小となるときの硬度より小さくすることを特徴とする請求項１０ないし請求項１３のいずれか１つに記載の鉄基軟磁性粉末の製造方法。 The method for producing an iron-based soft magnetic powder according to any one of claims 10 to 13, wherein the hardness of the powder is smaller than the hardness at which the coercive force is minimized.
  15. 　粉末の硬度を、ＩＳＯ１４５７７－１に準拠して測定した粉末の硬度で１０００～１２５０ＨＶとすることを特徴とする請求項１４に記載の鉄基軟磁性粉末の製造方法。 15. The method for producing an iron-based soft magnetic powder according to claim 14, wherein the hardness of the powder is 1000 to 1250 HV in terms of the hardness of the powder measured in accordance with ISO 14577-1.
  16. 　平均粒子径を０．５～５０μｍとすることを特徴とする請求項１０ないし請求項１５のいずれか１つに記載の鉄基軟磁性粉末の製造方法。 The method for producing an iron-based soft magnetic powder according to any one of claims 10 to 15, wherein the average particle diameter is 0.5 to 50 µm.
  17. 　Ｆｅのうち０．５～２．０ａｔ％をＣｒで置換することを特徴とする請求項９ないし請求項１６のいずれか１つに記載の鉄基軟磁性粉末の製造方法。 The method for producing an iron-based soft magnetic powder according to any one of claims 9 to 16, wherein 0.5 to 2.0 at% of Fe is substituted with Cr.
  18. 　請求項１０ないし請求項１７のいずれか１つに記載の鉄基軟磁性粉末の製造方法の後に、加圧成型工程を含む、物品の製造方法。 A method for manufacturing an article comprising a pressure molding step after the method for manufacturing an iron-based soft magnetic powder according to any one of claims 10 to 17.
  19. 　物品が圧粉磁心である、請求項１８に記載の物品の製造方法。

          The method for manufacturing an article according to claim 18, wherein the article is a dust core.

PCT/JP2019/013687 2018-03-29 2019-03-28 Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same WO2019189614A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2020511004A JP7024859B2 (en) 2018-03-29 2019-03-28 Iron-based soft magnetic powder and its manufacturing method, and articles containing iron-based soft magnetic alloy powder and its manufacturing method
CN201980023114.9A CN111971761A (en) 2018-03-29 2019-03-28 Iron-based soft magnetic powder and method for producing same, and article comprising iron-based soft magnetic alloy powder and method for producing same
KR1020207019919A KR102574343B1 (en) 2018-03-29 2019-03-28 Iron-based soft magnetic powder and manufacturing method thereof, article containing iron-based soft magnetic alloy powder, and manufacturing method thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2018-063624 2018-03-29
JP2018063624 2018-03-29

Publications (1)

Publication Number Publication Date
WO2019189614A1 true WO2019189614A1 (en) 2019-10-03

Family

ID=68058224

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2019/013687 WO2019189614A1 (en) 2018-03-29 2019-03-28 Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same

Country Status (5)

Country Link
JP (1) JP7024859B2 (en)
KR (1) KR102574343B1 (en)
CN (1) CN111971761A (en)
TW (1) TWI834652B (en)
WO (1) WO2019189614A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021141267A (en) * 2020-03-09 2021-09-16 セイコーエプソン株式会社 Magnetic powder, magnetic powder compact, and manufacturing method of magnetic powder
JP2023506960A (en) * 2019-12-19 2023-02-20 アルセロールミタル Metal powders for additive manufacturing

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5940502A (en) * 1982-08-28 1984-03-06 Matsushita Electric Works Ltd Heat treatment of amorphous core
JPH02258957A (en) * 1988-12-20 1990-10-19 Toshiba Corp Fe-base soft-magnetic alloy
JPH05335129A (en) * 1992-05-29 1993-12-17 Mitsui Petrochem Ind Ltd Fe-based soft magnetic alloy particle and manufacturing method thereof
JPH07232926A (en) * 1993-12-27 1995-09-05 Alps Electric Co Ltd Fine-grained ferrite and its production
JP2006118040A (en) * 2004-09-27 2006-05-11 Tohoku Univ Method for producing nanocrystal magnetic material with oriented crystal grain
JP2010280956A (en) * 2009-06-05 2010-12-16 Alps Electric Co Ltd METHOD FOR PRODUCING Fe-BASED SOFT MAGNETIC ALLOY POWDER
JP2013067863A (en) * 2005-09-16 2013-04-18 Hitachi Metals Ltd Soft magnetic alloy powder and magnetic part using the same
JP2016025352A (en) * 2014-07-18 2016-02-08 サムソン エレクトロ−メカニックス カンパニーリミテッド． Soft magnetic metal powder and production method thereof

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6479342A (en) * 1986-12-15 1989-03-24 Hitachi Metals Ltd Fe-base soft magnetic alloy and its production
CN101841404B (en) 2009-03-16 2013-08-07 上海贝尔股份有限公司 Relay communication method, system and device
JP5912349B2 (en) * 2011-09-02 2016-04-27 Ｎｅｃトーキン株式会社 Soft magnetic alloy powder, nanocrystalline soft magnetic alloy powder, manufacturing method thereof, and dust core
JP5940502B2 (en) 2013-09-17 2016-06-29 日本電信電話株式会社 Router, communication system, management method, and management program
JP6530164B2 (en) * 2014-03-04 2019-06-12 株式会社トーキン Nanocrystalline soft magnetic alloy powder and dust core using the same
TWI518932B (en) * 2014-07-24 2016-01-21 茂迪股份有限公司 Solar cell and module comprising the same
JP6651082B2 (en) * 2015-07-31 2020-02-19 Ｊｆｅスチール株式会社 Method for manufacturing soft magnetic powder core
WO2021071246A1 (en) * 2019-10-07 2021-04-15 주식회사 엘지화학 Method for producing super absorbent polymer

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5940502A (en) * 1982-08-28 1984-03-06 Matsushita Electric Works Ltd Heat treatment of amorphous core
JPH02258957A (en) * 1988-12-20 1990-10-19 Toshiba Corp Fe-base soft-magnetic alloy
JPH05335129A (en) * 1992-05-29 1993-12-17 Mitsui Petrochem Ind Ltd Fe-based soft magnetic alloy particle and manufacturing method thereof
JPH07232926A (en) * 1993-12-27 1995-09-05 Alps Electric Co Ltd Fine-grained ferrite and its production
JP2006118040A (en) * 2004-09-27 2006-05-11 Tohoku Univ Method for producing nanocrystal magnetic material with oriented crystal grain
JP2013067863A (en) * 2005-09-16 2013-04-18 Hitachi Metals Ltd Soft magnetic alloy powder and magnetic part using the same
JP2010280956A (en) * 2009-06-05 2010-12-16 Alps Electric Co Ltd METHOD FOR PRODUCING Fe-BASED SOFT MAGNETIC ALLOY POWDER
JP2016025352A (en) * 2014-07-18 2016-02-08 サムソン エレクトロ−メカニックス カンパニーリミテッド． Soft magnetic metal powder and production method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2023506960A (en) * 2019-12-19 2023-02-20 アルセロールミタル Metal powders for additive manufacturing
JP7503137B2 (en) 2019-12-19 2024-06-19 アルセロールミタル Metal Powders for Additive Manufacturing
JP2021141267A (en) * 2020-03-09 2021-09-16 セイコーエプソン株式会社 Magnetic powder, magnetic powder compact, and manufacturing method of magnetic powder
US11948712B2 (en) 2020-03-09 2024-04-02 Seiko Epson Corporation Magnetic powder, magnetic powder molded body, and method for manufacturing magnetic powder

Also Published As

Publication number Publication date
TW201942389A (en) 2019-11-01
JP7024859B2 (en) 2022-02-24
JPWO2019189614A1 (en) 2021-04-22
CN111971761A (en) 2020-11-20
KR20200129089A (en) 2020-11-17
KR102574343B1 (en) 2023-09-04
TWI834652B (en) 2024-03-11

Similar Documents

Publication Publication Date Title
JP6482718B1 (en) Soft magnetic material and manufacturing method thereof
US11081266B2 (en) Soft magnetic alloy powder, dust core, and magnetic component
US10847291B2 (en) Soft magnetic powder, dust core, magnetic compound and method of manufacturing dust core
US11145448B2 (en) Soft magnetic alloy powder, dust core, and magnetic component
CN110225801B (en) Soft magnetic powder, Fe-based nanocrystalline alloy powder, magnetic component, and dust core
JP6669304B2 (en) Crystalline Fe-based alloy powder and method for producing the same
JP6088192B2 (en) Manufacturing method of dust core
JP6493639B1 (en) Fe-based nanocrystalline alloy powder and method for producing the same, Fe-based amorphous alloy powder, and magnetic core
CN111128504B (en) Soft magnetic alloy powder, dust core, magnetic component, and electronic device
CN112004625B (en) Alloy powder, fe-based nanocrystalline alloy powder, and magnetic core
JP2016104900A (en) Metallic soft magnetic alloy, magnetic core, and production method of the same
TWI778112B (en) Fe-BASED ALLOY, CRYSTALLINE Fe-BASED ALLOY ATOMIZED POWDER, AND MAGNETIC CORE
US11276516B2 (en) Magnetic powder for high-frequency applications and magnetic resin composition containing same
WO2019189614A1 (en) Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same
CN111681846B (en) Soft magnetic alloy and magnetic part
JP2016162947A (en) Soft magnetic material, soft magnetic powder, powder magnetic core, and manufacturing methods thereof
JPH0448004A (en) Fe base soft magnetic alloy powder and manufacture thereof and powder compact magnetic core with the same
JP2021150555A (en) Powder magnetic core and method of manufacturing the same

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: 19774397

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2020511004

Country of ref document: JP

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: 19774397

Country of ref document: EP

Kind code of ref document: A1