WO2023127198A1 - 軟磁性合金および磁性部品 - Google Patents

軟磁性合金および磁性部品 Download PDF

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WO2023127198A1
WO2023127198A1 PCT/JP2022/032824 JP2022032824W WO2023127198A1 WO 2023127198 A1 WO2023127198 A1 WO 2023127198A1 JP 2022032824 W JP2022032824 W JP 2022032824W WO 2023127198 A1 WO2023127198 A1 WO 2023127198A1
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sample
poor
rich
content ratio
soft magnetic
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French (fr)
Japanese (ja)
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拓也 塚原
健輔 荒
暁斗 長谷川
和宏 吉留
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TDK Corp
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TDK Corp
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals

Definitions

  • the present invention relates to soft magnetic alloys and magnetic parts.
  • Patent Document 1 in a nanocrystalline alloy containing Fe, B, P and Cu, various parameters measurable by an atom probe (for example, the density of Cu clusters, the slope of the Fe concentration in the vicinity of the crystal region) are adjusted to specific ranges. It is described that the soft magnetic properties of the nanocrystalline alloy are improved by setting the content within.
  • An object of the present invention is to provide a soft magnetic alloy that has a high saturation magnetic flux density Bs and that can be used to manufacture magnetic parts with reduced core loss.
  • the soft magnetic alloy according to the present invention is A soft magnetic alloy containing at least Fe and Co
  • the soft magnetic alloy consists of a rich portion and a poor portion, the rich portion being a portion having a content ratio of Fe and Co equal to or higher than the content ratio of Fe and Co in the soft magnetic alloy, and the poor portion being a content ratio of Fe and Co. is less than the content of Fe and Co in the soft magnetic alloy,
  • the standard deviation of ((content ratio of Co)/(content ratio of Fe and Co)) in the rich portion is ⁇ rich
  • ((content ratio of Co)/(content ratio of Fe and Co)) in the poor portion Assuming the standard deviation is ⁇ poor , ⁇ poor is greater than or equal to 1.05 times ⁇ rich .
  • the content ratio of Fe and Co in the soft magnetic alloy may be 70 at % or more and 90 at % or less.
  • V rich is the volume ratio of the rich portion and V poor is the volume ratio of the poor portion
  • V rich /V poor may be 0.80 or more and 2.00 or less.
  • the soft magnetic alloy may be ribbon-shaped.
  • the soft magnetic alloy may be in powder form.
  • the magnetic component according to the present invention is made of the above soft magnetic alloy.
  • the soft magnetic alloy according to the present embodiment is a soft magnetic alloy containing at least Fe and Co, which are elements exhibiting ferromagnetism at room temperature.
  • the soft magnetic alloy has a rich portion in which the content ratio of Fe and Co is equal to or higher than the content ratio of Fe and Co in the soft magnetic alloy, and the content ratio of Fe and Co is less than the content ratio of Fe and Co in the soft magnetic alloy. It consists of a poor part.
  • the rich portion is a portion where the total ratio of Fe and Co is the same or higher than the total ratio of Fe and Co in the average composition of the entire soft magnetic alloy.
  • the poor portion is a portion where the total ratio of Fe and Co is low relative to the total ratio of Fe and Co in the average composition of the entire soft magnetic alloy.
  • the standard deviation of ((content ratio of Co)/(content ratio of Fe and Co)) in the rich portion is ⁇ rich
  • ((content ratio of Co)/(content ratio of Fe and Co)) in the poor portion is 1.05 times or more of ⁇ rich
  • ⁇ poor is the standard deviation.
  • ⁇ poor / ⁇ rich is 1.05 or more.
  • a 3DAP observation range is set for a soft magnetic alloy for which ⁇ rich and ⁇ poor are to be measured.
  • the size of the observation range is not particularly limited, but should be at least 3200 nm 3 or more, preferably 20000 nm 3 or more.
  • the shape of the observation range is not particularly limited. For example, it may be a rectangular parallelepiped of 10 nm ⁇ 10 nm ⁇ 200 nm.
  • the number of grids shall be at least 400 or more.
  • the shape of the observation range is a rectangular parallelepiped of 10 nm ⁇ 10 nm ⁇ 200 nm, the set observation range is divided into 2500 grids.
  • each grid is a rich part or a poor part.
  • the content ratio of Fe and Co in the above soft magnetic alloy is the average value of the content ratio of Fe and Co in all grids.
  • the standard deviation ⁇ rich is calculated from ((content ratio of Co)/(content ratio of Fe and Co)) in all grids that are rich portions.
  • the standard deviation ⁇ poor is calculated from ((content ratio of Co)/(content ratio of Fe and Co)) in all the grids which are poor portions.
  • ⁇ poor is 1.05 times or more as large as ⁇ rich .
  • the horizontal axis is ((Content ratio of Co) / (Content ratio of Fe and Co)), and the vertical axis is the number of grids.
  • a histogram is shown in FIG.
  • the horizontal axis is ((content ratio of Co) / (content ratio of Fe and Co)), and the vertical axis is the number of grids.
  • a histogram is shown in FIG.
  • ⁇ rich is small, that is, the variation in ((content ratio of Co)/(content ratio of Fe and Co)) in the rich portion is small means that Fe and Co are in an appropriate mixed state in a relatively large number of rich portions. It shows that The smaller ⁇ rich is, the easier it is to improve Bs.
  • a large ⁇ poor that is, a large variation in ((content ratio of Co) / (content ratio of Fe and Co)) in the poor part causes a large variation in the composition in the poor part, especially in the content ratio of Co. It is shown that. Due to the large variation in composition in the poor portion, the electrical resistance in the poor portion increases. As a result, eddy current loss is reduced, and the core loss of magnetic parts produced using the soft magnetic alloy is improved.
  • ⁇ poor may be 1.10 times or more of ⁇ rich
  • ⁇ poor may be 1.20 times or more of ⁇ rich . That is, ⁇ poor / ⁇ rich ⁇ 1.10 or ⁇ poor / ⁇ rich ⁇ 1.20. As the difference between ⁇ poor and ⁇ rich increases, the above effect increases.
  • ⁇ poor / ⁇ rich there is no particular upper limit for ⁇ poor / ⁇ rich .
  • ⁇ poor / ⁇ rich ⁇ 2.00 or ⁇ poor / ⁇ rich ⁇ 1.93.
  • V rich /V poor may be 0.66 or more and 9.00 or less.
  • V rich /V poor may be 0.66 or more and 9.00 or less.
  • V rich /V poor is smaller than the above range, that is, when V rich /V poor is smaller than 0.66, Bs of the magnetic parts manufactured using the soft magnetic alloy becomes small.
  • V rich /V poor is greater than the above range, that is, when V rich /V poor is greater than 9.00, the eddy current loss of the magnetic parts produced using the soft magnetic alloy increases, and the core loss worsens.
  • V rich /V poor may be 0.66 or more and 4.00 or less, and V rich /V poor may be 0.80 or more and 2.00 or less. Core loss is further improved by setting V rich /V poor within the above range.
  • composition of the soft magnetic alloy according to this embodiment is not particularly limited except that it contains at least Fe and Co.
  • the soft magnetic alloy according to the present embodiment may be represented by the composition formula (Fe 1-( ⁇ + ⁇ ) Co ⁇ Ni ⁇ ) 1-(a + b + c) M a X 1 b X 2 c in terms of atomic ratio
  • X1 is one or more selected from Cu, Al, Mn, Ag, Zn, Sn, As, Sb, Ga, Bi, S, N, O, Ca, Mg, Au, rare earth elements, and platinum group elements
  • M is one or more selected from Nb, Hf, Zr, Ta, Mo, V, Ti, W and Cr
  • X2 is one or more selected from B, P, Si and C, 0 ⁇ a ⁇ 0.200 0 ⁇ b ⁇ 0.050 0 ⁇ c ⁇ 0.300 0.700 ⁇ 1-(a+b+c) ⁇ 0.900 ⁇ > 0 ⁇ 0 0 ⁇ + ⁇ 0.500 may be satisfied.
  • composition of the soft magnetic alloy can be specified by a diffraction (XRD) method, X-ray fluorescence spectroscopy (XRF), inductively coupled plasma emission spectroscopy (ICP-AES), or the like.
  • XRD diffraction
  • XRF X-ray fluorescence spectroscopy
  • ICP-AES inductively coupled plasma emission spectroscopy
  • the content of elements other than the above, that is, elements other than Fe, Co, Ni, M, X1 and X2 may be 0.1% by mass or less.
  • the content of M (a) may be 0 ⁇ a ⁇ 0.100.
  • the content (b) of X1 may be 0 ⁇ b ⁇ 0.012 or 0.001 ⁇ b ⁇ 0.012.
  • the content (c) of X2 may be 0.050 ⁇ c ⁇ 0.230.
  • the Co content ( ⁇ ) with respect to the total content of Fe, Co and Ni may be 0.050 ⁇ 0.500 or 0.050 ⁇ 0.400.
  • the content ( ⁇ ) of Ni with respect to the total content of Fe, Co and Ni may be 0 ⁇ 0.450.
  • the content ratio of Fe and Co in the soft magnetic alloy may be 70 at % or more and 90 at % or less. That is, (1 ⁇ ) ⁇ (1 ⁇ (a+b+c)) may be 0.700 or more and 0.900 or less. Bs can be further increased by setting the content ratio of Fe and Co in the soft magnetic alloy to 70 at % or more and 90 at % or less.
  • the method of manufacturing the soft magnetic alloy according to the present embodiment is arbitrary, but for example, a method of manufacturing a ribbon of the soft magnetic alloy by a single roll method can be mentioned.
  • the single roll method first, various raw materials such as pure metals of each metal element contained in the finally obtained soft magnetic alloy are prepared and weighed so that they have the same composition as the finally obtained soft magnetic alloy. Then, pure metals of each metal element are melted and mixed to prepare a master alloy.
  • the method of melting the pure metal is arbitrary, but for example, there is a method of melting by high-frequency heating after evacuating the chamber.
  • the master alloy and the finally obtained soft magnetic alloy usually have the same composition.
  • the prepared master alloy is heated and melted to obtain molten metal (molten metal).
  • the temperature of the molten metal is not particularly limited, it can be, for example, 1200-1500.degree.
  • Fig. 5 shows a schematic diagram of the equipment used for the single roll method.
  • the molten metal 2 is jetted from the nozzle 1 to the roll 3 rotating in the direction of the arrow and supplied, whereby the ribbon 4 is formed in the rotation direction of the roll 3. manufactured.
  • the material of the roll 3 is not particularly limited. For example, a roll made of Cu is used.
  • the thickness of the ribbon obtained can be adjusted mainly by adjusting the rotation speed of the roll 3.
  • the gap between the nozzle 1 and the roll 3 and the temperature of the molten metal can be adjusted.
  • the thickness of the obtained ribbon can also be adjusted by Although the thickness of the ribbon is not particularly limited, it can be, for example, 10 to 50 ⁇ m.
  • the temperature of the roll 3 is arbitrary. It may be 30 to 70°C. It is preferably 50 to 70°C.
  • the atmosphere inside the chamber 5 is arbitrary. For example, it may be in a vacuum or in the atmosphere. Alternatively, an argon atmosphere in which the vapor pressure is controlled by adjusting the dew point may be used. Although the vapor pressure is arbitrary, it is preferable to set the vapor pressure inside the chamber 5 to 1 hPa or more.
  • the soft magnetic alloy has a rich portion and a poor portion, and the ⁇ poor / ⁇ rich of the soft magnetic alloy obtained after the hot press treatment described below can be easily increased.
  • the heat treatment temperature may be 400° C. or higher and 650° C. or lower, or may be 450° C. or higher and 600° C. or lower. It is preferably 500° C. or higher and 600° C. or lower.
  • the heat treatment time may be 0.05 hours or more and 5 hours or less. It is preferably 1.0 hours or more and 1.5 hours or less.
  • the preferred heat treatment temperature tends to be low and the preferred heat treatment time tends to be short.
  • the heat treatment temperature is preferably 450° C. or more and 500° C. or less, and the heat treatment time is preferably 0.05 hours or more and 1.5 hours or less.
  • the ⁇ poor / ⁇ rich of the soft magnetic alloy after heat treatment is less than 1.05.
  • ⁇ poor / ⁇ rich can be increased by subjecting this soft magnetic alloy to a hot press treatment.
  • FIG. 6 shows a schematic diagram of the hot press treatment.
  • the press plate 13 is preheated. Then, the press plate 13 is used to apply pressure to the soft magnetic alloy 11 after the heat treatment in the direction of the arrow and is held.
  • the temperature of the press plate 13 hereinafter sometimes referred to as press temperature
  • the pressure during hot press hereinafter sometimes referred to as press pressure
  • the time held at the pressure during hot press hereinafter referred to as press time ⁇ poor / ⁇ rich of the soft magnetic alloy 11 is increased by appropriately controlling ⁇ . This is because the hot press process promotes the diffusion of the elements contained in the soft magnetic alloy 11, making the composition of the poor portion non-uniform and the composition of the rich portion uniform.
  • the ribbon-shaped soft magnetic alloy may be hot-pressed as it is, or the ribbon-shaped soft magnetic alloy may be processed according to the type of the hot-pressing device.
  • two press plates 13 are used to press the soft magnetic alloy 11 from both sides in FIG. 6, it may be pressed from only one side. Moreover, although it is preferable to heat both the two press plates 13, only one press plate 13 may be heated. Also, the temperatures of the two press plates 13 may be the same or different.
  • the pressing temperature is not particularly limited, but may be 250 to 350°C.
  • the pressing pressure is not particularly limited, but may be from 0.10 to 1.0 MPa.
  • the pressing time is not particularly limited, but may be 1 to 60 minutes. However, if the pressing temperature is low (e.g., less than 250° C.), the pressing pressure is low (e.g., less than 0.10 MPa), and/or the pressing time is short (e.g., less than 1 minute), diffusion of the elements is not sufficiently urged. Also, if the pressing temperature is high (eg, higher than 350° C.), if the pressing pressure is high (eg, higher than 1.0 MPa), and/or if the pressing time is long (eg, longer than 60 minutes), diffusion of the elements is likely to be excessively urged. Therefore, the composition of the poor portion tends to be uniform and the composition of the rich portion tends to be non-uniform compared to the case where the hot press treatment is performed under appropriate conditions. In either case, ⁇ poor / ⁇ rich tends
  • the soft magnetic alloy according to this embodiment there is a method for obtaining powder of the soft magnetic alloy according to this embodiment, for example, by a water atomization method or a gas atomization method, in addition to the above-described single roll method.
  • the gas atomization method will be described below.
  • a molten alloy of 1200 to 1500°C is obtained in the same manner as in the single roll method described above. After that, the molten alloy is injected in the chamber to produce powder.
  • the gas heating temperature may be 4-100°C. It is preferably 4 to 30°C.
  • the atmosphere inside the chamber 5 is arbitrary. For example, it may be in a vacuum or in the atmosphere. Alternatively, an argon atmosphere in which the vapor pressure is controlled by adjusting the dew point may be used.
  • the powder is produced by the gas atomization method
  • heat treatment is performed in the same manner as in the single roll method, so that the soft magnetic alloy has a rich portion and a poor portion, and the ⁇ of the soft magnetic alloy obtained after the hot press treatment described later. It becomes easier to increase poor / ⁇ rich .
  • the heat treatment conditions vary depending on the composition of the soft magnetic alloy, but the heat treatment temperature may be 400°C or higher and 650°C or lower, or may be 450°C or higher and 600°C or lower. It is preferably 500° C. or higher and 600° C. or lower.
  • the heat treatment time may be 0.05 hours or more and 5 hours or less. It is preferably 1.0 hours or more and 1.5 hours or less.
  • the ⁇ poor / ⁇ rich of the soft magnetic alloy after heat treatment is less than 1.05.
  • ⁇ poor / ⁇ rich can be increased by subjecting this soft magnetic alloy to a hot press treatment.
  • heat and pressure may be applied to the powder-shaped soft magnetic alloy after heat treatment.
  • the heat press treatment may be performed using a mold for powder molding.
  • the pressing temperature is not particularly limited, but may be 250 to 350°C.
  • the pressing pressure is not particularly limited, but may be from 0.10 to 1.0 MPa.
  • the pressing time is not particularly limited, but may be 1 to 60 minutes. However, if the pressing temperature is low (e.g., less than 250° C.), the pressing pressure is low (e.g., less than 0.10 MPa), and/or the pressing time is short (e.g., less than 1 minute), diffusion of the elements is not sufficiently urged. Also, when the pressing temperature is high (greater than 350° C.), the pressing pressure is high (greater than 1.0 MPa), and/or the pressing time is long (longer than 60 minutes), the diffusion of the elements is excessive. easily provoked. Therefore, the composition of the poor portion tends to be uniform and the composition of the rich portion tends to be non-uniform compared to the case where the hot press treatment is performed under appropriate conditions. In either case, ⁇ poor / ⁇ rich tends to be small.
  • the shape of the soft magnetic alloy according to this embodiment is not particularly limited. As described above, thin strips and powders are exemplified, but other shapes such as thin films and blocks are also conceivable.
  • the soft magnetic alloy there are no particular restrictions on the use of the soft magnetic alloy according to this embodiment.
  • Examples include magnetic parts such as magnetic cores, thin film inductors, magnetic heads, and transformers.
  • the prepared mother alloy was heated and melted to form a metal in a molten state at 1150 ° C., and the roll temperature, chamber atmosphere, and chamber vapor pressure shown in each table were determined by a single roll method. was jetted onto a roll to prepare a ribbon. Also, the thickness of the ribbon obtained by appropriately adjusting the rotation speed of the roll was set to 20 ⁇ m.
  • each obtained sample an observation range of 10 nm x 10 nm x 200 nm was observed using 3DAP.
  • the set observation range was divided into a grid of 2500 2 nm ⁇ 2 nm ⁇ 2 nm cubes. Then, the content ratio of each element in each grid was measured. It was confirmed that the composition obtained by averaging the content ratio of each element in all grids was consistent with the composition described in each table. Then, it was specified whether each grid is a rich part or a poor part.
  • V rich /V poor was calculated. Specifically, it was calculated by dividing the number of grids in the rich section by the number of grids in the poor section. Results are shown in each table.
  • the Bs of each sample was measured. Specifically, it was measured in a magnetic field of 1000 kA/m using a vibrating sample magnetometer (VSM). Results are shown in each table. A sample with an increase in Bs of 0.01 T or more compared to a sample processed under the same conditions except that the hot press treatment was not performed was evaluated as good.
  • VSM vibrating sample magnetometer
  • a magnetic core (toroidal core) was produced using the soft magnetic alloy ribbon of each sample.
  • five toroidal strips with an outer diameter of 18 mm and an inner diameter of 10 mm were punched out, and the punched strips were stacked to obtain a toroidal core with a height of about 0.1 mm.
  • the core loss was measured for the obtained toroidal core.
  • a BH analyzer SY-8218 manufactured by Iwatsu Keisoku Co., Ltd.
  • the core loss reduction rate was calculated as how much the core loss of the toroidal core produced from each sample decreased relative to the core loss of the toroidal core produced from the sample performed under the same conditions except that the heat press treatment was not performed. . Results are shown in each table. A case where the core loss reduction rate was 3.0% or more was evaluated as good.
  • Table 1 shows examples and comparative examples in which the heat treatment temperature and the presence or absence of hot press treatment were varied.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed had a higher Bs and a lower core loss than the comparative examples performed under the same conditions except that the hot press treatment was not performed. Also, the higher the heat treatment temperature, the larger the ⁇ poor / ⁇ rich , and the higher the core loss reduction rate.
  • Table 2 shows examples and comparative examples in which the heat treatment time and the presence or absence of hot press treatment were changed.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed had a higher Bs and a lower core loss than the comparative examples performed under the same conditions except that the hot press treatment was not performed. Also, when the heat treatment time was 1.0 to 1.5 hours, ⁇ poor / ⁇ rich became relatively large, and the Bs and core loss reduction rate became relatively high.
  • Table 3 shows examples and comparative examples in which the hot press treatment conditions and the presence or absence of the hot press treatment were changed.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed under suitable conditions had a higher Bs and a lower core loss than the comparative examples in which the hot press treatment was performed under the same conditions except that the hot press treatment was not performed. Also, there was a tendency that the higher the ⁇ poor / ⁇ rich , the higher the Bs and core loss reduction rate.
  • Example 2 Sample No. 1 of Experimental Example 1 except that the conditions for producing the ribbon were changed from those of Experimental Example 1. It was carried out under the same conditions as in 1-2. In Experimental Example 2, sample No. 2 was used for comparison with the case where no heat press treatment was performed. The core loss reduction rate for 1-1 was calculated. Furthermore, in order to make a comparison with the case where the ribbon production conditions are the same as in Experimental Example 1, sample No. The core loss reduction rate for 1-2 was calculated. Table 4 shows the results.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed had a higher Bs and a lower core loss than the comparative examples in which the hot press treatment was not performed.
  • ⁇ poor / ⁇ rich tended to decrease as the roll temperature increased. Also, if the roll temperature is the same, there is a tendency that the higher the vapor pressure in the chamber, the larger the ⁇ poor / ⁇ rich .
  • Sample No. 1 was prepared with the exception that various raw material metals and the like were weighed so as to obtain master alloys having the compositions shown in Tables 5, 6, 7A to 7F, 8A to 8B, and 9A to 9D. 1-1 or sample No. It was carried out under the same conditions as in 1-2. Also, it was confirmed that the composition obtained by averaging the content ratio of each element in all grids for each sample was consistent with the composition described in each table.
  • Sample No. in Table 5 7-1, 8-1, 11-1 and 12-1 are sample Nos. These samples were carried out under the same conditions except that the ratio of Fe and Co was changed from 1-1. Sample no. 7-2, 8-2, 11-2 and 12-2 are sample Nos. These samples were carried out under the same conditions as in 1-2, except that the ratio of Fe and Co was changed. Sample no. In 9-1 and 10-1, the types and content ratios of elements other than Fe and Co were also examined. 1-1 and processed at the heat treatment temperatures listed in Table 5 accordingly. Sample no. In 9-2 and 10-2, the types and content ratios of elements other than Fe and Co were also examined. 1-2 and processed at the heat treatment temperatures listed in Table 5 accordingly. Table 5 shows the results.
  • Sample No. in Table 7B. 1a-1 to 1d-1 are sample Nos. 1-1, except that the content ratio of M was changed, but the sample was carried out under the same conditions.
  • Sample no. 1a-2 to 1d-2 are sample Nos. 1-2, except that the content ratio of M was changed, this sample was carried out under the same conditions.
  • Sample no. 18a-1 to 18c-1 are sample Nos. 18-1, except that the content ratio of M was changed, this sample was carried out under the same conditions.
  • Sample no. 18a-2 to 18c-2 are sample Nos. 18-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Results are shown in Table 7B.
  • Sample No. in Table 7C. 19a-1 to 19c-1 are sample Nos. This sample was carried out under the same conditions as in 19-1, except that the content ratio of M was changed. Sample no. 19a-2 to 19c-2 are sample Nos. 19-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Sample no. 20a-1 to 20c-1 are sample Nos. 20-1, except that the content ratio of M was changed, the sample was carried out under the same conditions. Sample no. 20a-2 to 20c-2 are sample Nos. 20-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Results are shown in Table 7C.
  • Sample No. in Table 7D. 21a-1 to 21b-1 are sample Nos. 21-1 was carried out under the same conditions except that the content ratio of M was changed.
  • Sample no. 21a-2 to 21b-2 are sample Nos. 21-2, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 22a-1 to 22b-1 are sample Nos. 22-1, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 22a-2 to 22b-2 are sample Nos. 22-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Results are shown in Table 7D.
  • Sample No. in Table 7E. 23a-1 to 23b-1 are sample Nos. 23-1, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 23a-2 to 23b-2 are sample Nos. 23-2, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 24a-1 to 24c-1 are sample Nos. 24-1, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 24a-2 to 24c-2 are sample Nos. 24-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Results are shown in Table 7E.
  • Sample No. in Table 7F. 25a-1 to 25b-1 are sample Nos. 25-1, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 25a-2 to 25b-2 are sample Nos. 25-2, except that the content ratio of M was changed, the sample was carried out under the same conditions.
  • Sample no. 26a-1 to 26c-1 are sample Nos. 26-1 was carried out under the same conditions except that the content ratio of M was changed.
  • Sample no. 26a-2 to 26c-2 are sample Nos. 26-2, except that the content ratio of M was changed, the sample was carried out under the same conditions. Results are shown in Table 7F.
  • Sample No. in Table 8B. 41-1 to 44-1 are sample Nos. These samples were carried out under the same conditions except that the type and content ratio of X1 were changed from 1-1.
  • Sample no. 41-2 to 44-2 are sample Nos. 1-2 except that the type and content ratio of X1 were changed, but the samples were carried out under the same conditions. Results are shown in Table 8B.
  • Sample No. in Table 8C. 27-1 to 32-1 are sample Nos. These samples were carried out under the same conditions except that the type and content ratio of X1 were changed from 1-1.
  • Sample no. 27-2 to 32-2 are sample Nos. 1-2 except that the type and content ratio of X1 were changed, but the samples were carried out under the same conditions. Results are shown in Table 8C.
  • Sample No. in Table 8D. 45-1 to 49-1 are sample Nos. These samples were carried out under the same conditions except that the type of X1 was changed from 1-1. Sample no. 45-2 to 49-2 are sample Nos. These samples were carried out under the same conditions as in 1-2, except that the type of X1 was changed. Results are shown in Table 8D.
  • Sample No. in Table 8E. 50-1 to 52-1 are sample Nos. These samples were carried out under the same conditions except that the type and content ratio of X1 were changed from 1-1.
  • Sample no. 50-2 to 52-2 are sample Nos. 1-2 except that the type and content ratio of X1 were changed, but the samples were carried out under the same conditions. Results are shown in Table 8E.
  • Sample No. in Table 9A. 1h-1 to 1m-1 are sample Nos. 1-1 except that the content ratio of B and/or the content ratio of P was changed from 1-1 under the same conditions.
  • Sample no. 1h-2 to 1m-2 are sample Nos. 1-2 except that the content ratio of B and/or the content ratio of P was changed. Results are shown in Table 9A.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the Bs was higher and the core loss was lower than the comparative example performed under the same conditions except that the hot press treatment was not performed.
  • the prepared master alloy is heated and melted to form a metal in a molten state at 1500° C., and then the gas heating temperature is set to 30° C., and the chamber is filled with argon whose dew point is adjusted to bring the vapor pressure in the chamber to 1 hPa.
  • a powder was produced by the gas atomization method. Also, the soft magnetic metal powder obtained was classified by sieving so that the average particle size (D50) of the obtained soft magnetic metal powder was 24 ⁇ m.
  • the heat treatment temperature was 600° C.
  • the heat treatment time was 1.0 hour.
  • each obtained sample an observation range of 10 nm x 10 nm x 200 nm was observed using 3DAP.
  • the set observation range was divided into a grid of 2500 2 nm ⁇ 2 nm ⁇ 2 nm cubes. Then, the content ratio of each element in each grid was measured. It was confirmed that the composition obtained by averaging the content ratio of each element in all grids was consistent with the composition described in Table 10. Then, it was specified whether each grid is a rich part or a poor part.
  • V rich /V poor was calculated. Specifically, it was calculated by dividing the number of grids in the rich section by the number of grids in the poor section. Table 10 shows the results.
  • the Bs of each sample was measured. Specifically, it was measured in a magnetic field of 1000 kA/m using a vibrating sample magnetometer (VSM). Table 10 shows the results. A sample with an increase in Bs of 0.01 T or more compared to a sample processed under the same conditions except that the hot press treatment was not performed was evaluated as good.
  • VSM vibrating sample magnetometer
  • a magnetic core (toroidal core) was produced using the soft magnetic alloy powder of each sample.
  • a phenolic resin as an insulating binder was mixed with each powder so that the amount of the phenolic resin was 3 mass % of the total.
  • the mixture was granulated to obtain a granulated powder of about 500 ⁇ m.
  • the obtained granulated powder was compacted at a surface pressure of 4 tons/cm 2 (392 MPa) to produce a toroidal compact having an outer diameter of 18 mm, an inner diameter of 10 mm and a height of 6.0 mm.
  • the molded body obtained was cured at 150° C. to produce a toroidal core.
  • the core loss was measured for the obtained toroidal core.
  • a BH analyzer SY-8218 manufactured by Iwatsu Keisoku Co., Ltd.
  • the core loss reduction rate was calculated as how much the core loss of the toroidal core produced from each sample decreased relative to the core loss of the toroidal core produced from the sample performed under the same conditions except that the heat press treatment was not performed.
  • Table 10 shows the results. A case where the core loss reduction rate was 3.0% or more was evaluated as good.
  • Example No. 33r-1, 33r-2 Various raw material metals were weighed so as to obtain a master alloy having a composition of (Fe0.800Co0.200)0.805Nb0.060Cu0.005B0.080P0.030Si0.020 in atomic ratio . Then, after the chamber was evacuated, it was melted by high-frequency heating to produce a master alloy.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed had a higher Bs and a lower core loss than the comparative examples performed under the same conditions except that the hot press treatment was not performed.
  • Sample no. Sample No. 10-1 was obtained by changing the content ratio of X2 and also changing the heat treatment temperature. 60-1 was made.
  • Sample no. Sample No. 10-2 was prepared by changing the content ratio of X2 and also changing the heat treatment temperature and heat treatment time. 60-2 was made. Table 11 shows the results.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed had a higher Bs and a lower core loss than the comparative examples performed under the same conditions except that the hot press treatment was not performed.
  • the examples in which the hot press treatment was performed under suitable conditions had a higher Bs and a lower core loss than the comparative examples in which the hot press treatment was performed under the same conditions except that the hot press treatment was not performed. Also, there was a tendency that the higher the ⁇ poor / ⁇ rich , the higher the Bs and core loss reduction rate.
  • Sample No. in Table 14B. 70-1 to 73-1 are sample Nos. These samples were carried out under the same conditions except that the type and content ratio of X1 were changed from 60-1. Sample no. 70-2 to 73-2 are sample Nos. 1-2 except that the type and content ratio of X1 were changed, but the samples were carried out under the same conditions. Results are shown in Table 14B.
  • Sample No. in Table 14C. 74-1 to 79-1 are sample Nos. These samples were carried out under the same conditions except that the type of X1 was changed from 60-1. Sample no. 74-2 to 79-2 are sample Nos. These samples were carried out under the same conditions except that the type of X1 was changed from 60-2. Results are shown in Table 14C.
  • Sample No. in Table 14D. 80-1 to 82-1 are sample Nos. These samples were carried out under the same conditions except that the type and content ratio of X1 were changed from 60-1.
  • Sample no. 80-2 to 82-2 are sample Nos. 1-2 except that the type and content ratio of X1 were changed, but the samples were carried out under the same conditions. Results are shown in Table 14D.
  • Sample No. in Table 15A. 83-1 to 86-1 are sample Nos. These samples were carried out under the same conditions as in 60-1, except that the content ratio of B was changed. Sample no. 83-2 to 86-2 are sample Nos. These samples were carried out under the same conditions as in 60-2, except that the content ratio of B was changed. Results are shown in Table 15A.
  • Sample No. in Table 15C. 91-1 to 94-1 are sample Nos. This sample was carried out under the same conditions as in 60-1, except that the content ratio of Si was increased. Sample no. 91-2 to 94-2 are sample Nos. This sample was carried out under the same conditions as in 60-2, except that the content ratio of Si was increased. Results are shown in Table 15C.
  • ⁇ poor / ⁇ rich was 1.05 or more.
  • the ⁇ poor / ⁇ rich was less than 1.05 in the comparative example which was carried out under the same conditions except that the hot press treatment was not performed.
  • the Bs was higher and the core loss was lower than the comparative example performed under the same conditions except that the hot press treatment was not performed.

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Publication number Priority date Publication date Assignee Title
WO2003060175A1 (fr) * 2002-01-16 2003-07-24 Mitsui Chemicals, Inc. Materiau de base magnetique, lamine a base de ce materiau de base magnetique et procede de fabrication
JP2021154732A (ja) * 2020-03-25 2021-10-07 日立金属株式会社 軟磁性合金薄帯の積層体の製造方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003060175A1 (fr) * 2002-01-16 2003-07-24 Mitsui Chemicals, Inc. Materiau de base magnetique, lamine a base de ce materiau de base magnetique et procede de fabrication
JP2021154732A (ja) * 2020-03-25 2021-10-07 日立金属株式会社 軟磁性合金薄帯の積層体の製造方法

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