US20200291507A1 - Soft magnetic alloy and magnetic component - Google Patents

Soft magnetic alloy and magnetic component Download PDF

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US20200291507A1
US20200291507A1 US16/809,919 US202016809919A US2020291507A1 US 20200291507 A1 US20200291507 A1 US 20200291507A1 US 202016809919 A US202016809919 A US 202016809919A US 2020291507 A1 US2020291507 A1 US 2020291507A1
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soft magnetic
magnetic alloy
alloy
heat treatment
magnetostriction
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Kensuke Ara
Hajime Amano
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TDK Corp
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TDK Corp
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    • H01F1/147Alloys characterised by their composition
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    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15341Preparation processes therefor
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    • 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
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    • C22C2202/02Magnetic

Definitions

  • the present invention relates to a soft magnetic alloy and a magnetic component.
  • Patent Document 1 a Fe—B-M soft magnetic alloy is disclosed.
  • M denotes at least one element selected from Ti, Zr, Hf, V, Nb, Ta, Mo, and W.
  • Patent Document 1 describes that the soft magnetic properties and the saturation magnetic flux density of the soft magnetic alloy can be improved by performing a heat treatment on an amorphous metal produced by liquid phase cooling to deposit fine crystalline phase. However, it is necessary to reduce coercivity in order to improve the soft magnetic properties of the soft magnetic alloy, but reduction in the coercivity has not been sufficiently considered in Patent Document 1.
  • the coercivity is mainly derived from magnetocrystalline anisotropy and magnetoelastic effect.
  • the coercivity derived from the magnetoelastic effect appears when stress is applied to a magnetic material having a large magnetostriction.
  • the coercivity derived from the magnetocrystalline anisotropy can be reduced by isotropically depositing nanometer scale fine Fe-based crystal phase.
  • the present invention has been made in view of the above circumstances, and an objective thereof is to provide a soft magnetic alloy capable of achieving both low coercivity and high saturation magnetic flux density by reducing both the magnetostriction and the magnetocrystalline anisotropy.
  • a magnetic component comprising the soft magnetic alloy according to any one of [1] to [4].
  • the soft magnetic alloy of the present embodiment has Fe-based nanocrystals and amorphous.
  • the Fe-based nanocrystal is a crystal of which the crystal grain size is in the nanometer scale and which has a bcc (body-centered cubic lattice) structure.
  • many Fe-based nanocrystals are deposited and dispersed in the amorphous.
  • a soft magnetic alloy in which the Fe-based nanocrystals are dispersed in the amorphous is easy to exhibit high saturation magnetic flux density and low coercivity.
  • the average crystal grain size of the Fe-based nanocrystal is preferably 5 nm or more and 30 nm or less. With the average crystal grain size in the above range, it is easy to achieve low magnetostriction, high saturation magnetic flux density, and low coercivity.
  • composition of the soft magnetic alloy of the present embodiment is represented by a composition formula (Fe (1 ⁇ ( ⁇ + ⁇ )) X1 ⁇ X2 ⁇ ) (1 ⁇ (a+b+c+d+e+f)) M a B b P c Si d C e Zn f .
  • M denotes at least one element selected from the group consisting of Ti, V, Cr, Zr, Nb, Mo, Hf, Ta, and W.
  • a represents the content ratio of M.
  • “a” is determined by the relationship with “f” (described later) representing the content ratio of Zn.
  • “b” represents the content ratio of B (boron), and “b” satisfies 0.080 ⁇ b ⁇ 0.150.
  • the content ratio (b) of B is preferably 0.130 or less.
  • “c” represents the content ratio of P (phosphorus), and “c” satisfies 0 ⁇ c ⁇ 0.060. That is, P is an optional component.
  • the content ratio (c) of P is preferably 0.005 or more, and more preferably 0.010 or more. In addition, the content ratio (c) of P is preferably 0.040 or less.
  • the sum of the content ratios of B and P satisfies b+c ⁇ 0.100.
  • the soft magnetic alloy having the above composition region tends to have large positive magnetostriction.
  • the coercivity is affected by not only the magnetocrystalline anisotropy but also the magnetoelastic effect. If the magnetoelastic effect is great, that is, when the magnetostriction is large, the coercivity may not be sufficiently reduced.
  • a predetermined amount of Zn (zinc) is contained in the soft magnetic alloy.
  • Zn zinc
  • the soft magnetic alloy of the present embodiment exhibits small coercivity and high saturation magnetic flux density, because both the magnetocrystalline anisotropy and the magnetoelastic effect are reduced.
  • f represents the content ratio of Zn
  • f satisfies 0.003 ⁇ f ⁇ 0.080
  • a and “f” satisfy 0.003 ⁇ a+f ⁇ 0.080. That is, in the present embodiment, M is substituted with Zn (zinc). Zn may substitute all of M, or may substitute a part of M within the above range.
  • f is preferably 0.010 or more. On the other hand, “f” is preferably 0.050 or less. In addition, a+f is preferably 0.010 or more. On the other hand, a+f is preferably 0.050 or less.
  • One of the factors for the increase in magnetostriction is the expansion in the lattice spacing of bcc caused by solid-solution of M in the Fe-based nanocrystals having a bcc structure. Because Zn has an atomic radius smaller than that of the M element, the expansion of the lattice spacing of bcc can be suppressed when Zn, instead of M, is solid-soluted in the Fe-based nanocrystals. As a result, the positive magnetostriction of the Fe-based nanocrystals is considered to decrease. In addition, the lattice spacing tends to expand when Zn is added excessively, and as a result, the magnetostriction reduction effect is considered to decreases.
  • Zn also has the effect of refinement of the Fe-based nanocrystals, and thus it is possible to obtain a soft magnetic alloy of which the magnetostriction is reduced while the structure having fine nanocrystals is maintained.
  • the lattice spacing of bcc expands when M is solid-soluted in bcc, and thus the expansion in the lattice spacing of bcc is preferably equal to or less than a predetermined value.
  • a (110) plane spacing of bcc is employed as the lattice spacing of bcc. Because pure iron does not contain M, M is not solid-soluted in bcc of pure iron. That is, the expansion in the plane spacing caused by the solid-solution of M in bcc does not occur. Accordingly, it means that the closer the (110) plane spacing of the soft magnetic alloy is to the (110) plane spacing of the pure iron, the lower the solid-solution ratio of M in bcc is.
  • a value obtained by subtracting the (110) plane spacing of pure iron from the (110) plane spacing of the soft magnetic alloy is defined as an expansion value of the (110) plane spacing.
  • the expansion value of the (110) plane spacing is preferably 0.002 angstroms or less.
  • the (110) plane spacing of the soft magnetic alloy and the (110) plane spacing of pure iron can be calculated by XRD (X-Ray Diffraction) measurement. That is, the (110) plane spacing can be calculated from the angle at which a diffraction peak of the (110) plane is observed and the wavelength of X-ray. Then, the expansion value of the (110) plane spacing may be calculated based on the calculated spacing.
  • XRD X-Ray Diffraction
  • the (110) plane spacing of the soft magnetic alloy and the (110) plane spacing of pure iron are preferably measured with the same device and under the same measurement conditions.
  • “d” represents the content ratio of Si (silicon), and “d” satisfies 0 ⁇ d ⁇ 0.060. That is, Si is an optional component.
  • the content ratio (d) of Si is preferably 0.001 or more, and more preferably 0.005 or more.
  • the content ratio (d) of Si is preferably 0.030 or less.
  • e represents the content ratio of C (carbon), and “e” satisfies 0 ⁇ e ⁇ 0.030. That is, C is an optional component.
  • the content ratio (e) of C is preferably 0.001 or more.
  • the content ratio (e) of C is preferably 0.015 or less.
  • 1 ⁇ (a+b+c+d+e+f) represents the total content ratio of Fe (iron), X1 and X2.
  • the total content ratio of Fe, X1 and X2 is not particularly limited as long as “a”, “b”, “c”, “d”, “e” and “f” are within the above ranges.
  • the total content ratio (1 ⁇ (a+b+c+d+e+f)) is preferably 0.73 or more and 0.95 or less. With the total content ratio set to 0.73 or more, high saturation magnetic flux density is obtained easily. In addition, with the total content ratio set to 0.95 or less, crystal phase configured by crystals having a grain size larger than 30 nm is hardly generated. As a result, a soft magnetic alloy in which the Fe-based nanocrystals are deposited by heat treatment tends to be obtained easily.
  • X1 denotes at least one element selected from the group consisting of Co and Ni.
  • “a” represents the content ratio of X1
  • “ ⁇ ” is 0 or more in the present embodiment. That is, X1 is an optional component.
  • the number of atoms of X1 is preferably 40 at % or less. That is, it is preferable to satisfy 0 ⁇ a ⁇ 1 ⁇ (a+b+c+d+e+f) ⁇ 0.40.
  • X2 denotes at least one element selected from the group consisting of Cu, Mg, Al, Mn, Ag, Sn, Bi, O, N, S, and rare earth elements.
  • 0 represents the content ratio of X2
  • is 0 or more in the present embodiment. That is, X2 is an optional component.
  • the number of atoms of X2 is preferably 3.0 at % or less. That is, it is preferable to satisfy 0 ⁇ 1 ⁇ (a+b+c+d+e+f) ⁇ 0.030.
  • the range (substitution ratio) in which X1 and/or X2 substitutes for Fe is set equal to or less than half of the total number of Fe atoms in terms of the number of atoms. That is, 0 ⁇ + ⁇ 0.50 is satisfied.
  • ⁇ + ⁇ is too large, it tends to be difficult to obtain a soft magnetic alloy in which the Fe-based nanocrystals are deposited by heat treatment.
  • the soft magnetic alloy of the present embodiment may include elements other than the above elements as inevitable impurities.
  • the elements other than the above elements may be included in a total of 0.1% by mass or less with respect to 100% by mass of the soft magnetic alloy.
  • the soft magnetic alloy of the present embodiment is manufactured by, for example, depositing Fe-based nanocrystals in an amorphous alloy having the above composition.
  • a method of quenching a molten metal to obtain an amorphous alloy for example, a method of quenching a molten metal to obtain an amorphous alloy is exemplified.
  • a ribbon or flake of the amorphous alloy may be obtained by a single roll method, or powder of the amorphous alloy may be obtained by an atomization method.
  • a method of obtaining the amorphous alloy by the single roll method and a method of obtaining the amorphous alloy by a gas atomization method as an example of the atomization method are described.
  • a raw material (pure metal or the like) of each metal element contained in the soft magnetic alloy is prepared and is weighed so as to obtain a composition of the finally obtained soft magnetic alloy, and the raw material is melted to obtain molten metal.
  • the method for melting the raw material of the metal elements is not particularly limited; for example, a method of melting the material by high-frequency heating in a predetermined atmosphere is exemplified.
  • the temperature of the molten metal may be determined in consideration of the melting point of each metal element and may be, for example, 1200-1500° C.
  • the molten metal is injected and supplied from a nozzle to a cooled rotary roll, and thereby a ribbon-shaped or flaky amorphous alloy is manufactured toward the rotating direction of the rotary roll.
  • the material of the rotary roll include copper.
  • the temperature of the rotary roll, the rotating speed of the rotary roll, the atmosphere inside the chamber, and the like may be determined corresponding to the conditions under which the Fe-based nanocrystals are easily deposited in the amorphous during the heat treatment described later.
  • molten metal is obtained in which the raw material of the soft magnetic alloy is melted.
  • the temperature of the molten metal may be determined in consideration of the melting point of each metal element as in the case of the single roll method, and may be, for example, 1200-1500° C.
  • the obtained molten metal is supplied into the chamber as a linear continuous fluid through a nozzle provided at the bottom of the crucible, and a high-pressure gas is sprayed onto the supplied molten metal to make the molten metal into droplets, and the droplets are quenched to obtain a powder-shaped amorphous alloy.
  • the gas injection temperature, the pressure in the chamber, and the like may be determined corresponding to the conditions under which the Fe-based nanocrystals are easily deposited in the amorphous during the heat treatment described later.
  • the particle size can be adjusted by sieving classification, airflow classification, or the like.
  • the ribbon and powder obtained by the above methods are configured by an amorphous alloy.
  • the amorphous alloy may be an amorphous alloy in which fine crystals are dispersed in an amorphous, or may be an alloy not containing crystals.
  • the obtained ribbon and powder are subjected to a heat treatment (first heat treatment).
  • first heat treatment By performing the first heat treatment, diffusion of the elements constituting the soft magnetic alloy can be promoted, a thermodynamic equilibrium state can be achieved in a short time, and strain or stress existing in the soft magnetic alloy can be removed. As a result, it becomes easy to obtain a soft magnetic alloy in which the Fe-based nanocrystals are deposited.
  • the condition of the first heat treatment is not particularly limited as long as the Fe-based nanocrystals are easily deposited under this condition.
  • the heat treatment temperature can be set to 400-700° C.
  • the holding time can be set to 0.5-10 hours.
  • the present embodiment it is preferable to further perform a heat treatment (second heat treatment) after the first heat treatment.
  • second heat treatment M solid-soluted in the Fe-based nanocrystals can be released out of the crystals.
  • a composition containing a relatively large amount of Zn excessively solid-soluted Zn can be released out of the crystals and the amount of solid-solution Zn in the crystals can be optimized.
  • the (110) plane spacing of the Fe-based nanocrystal decreases and gets close to the (110) plane spacing of pure iron, and thus the magnetostriction can be reduced.
  • the heat treatment temperature of the second heat treatment is preferably lower than the heat treatment temperature of the first heat treatment, and more preferably lower by 50° C. or more.
  • the holding time of the second heat treatment is preferably three hours or longer and ten hours or shorter.
  • the soft magnetic alloy of the present embodiment having a ribbon shape or the soft magnetic alloy of the present embodiment having a powder shape is obtained.
  • the calculation method of the average grain size of the Fe-based nanocrystals contained in the soft magnetic alloy obtained by the heat treatment can be made by a transmission electron microscope observation.
  • a method for confirming that the crystal structure is a bcc (body-centered cubic lattice) structure.
  • the confirmation can be made using X-ray diffraction measurement.
  • the magnetic component of the present embodiment is not particularly limited as long as this magnetic component includes the above soft magnetic alloy as a magnetic material.
  • the magnetic component may have a magnetic core configured by the above soft magnetic alloy.
  • Examples of the method for obtaining a magnetic core from the ribbon-shaped soft magnetic alloy include a method of winding the ribbon-shaped soft magnetic alloy or a method of laminating the ribbon-shaped soft magnetic alloy.
  • a magnetic core with further improved properties can be obtained.
  • Examples of the method for obtaining a magnetic core from the powder-shaped soft magnetic alloy include a method in which the powder-shaped soft magnetic alloy is appropriately mixed with a binder and then molded using a press mold.
  • the magnetic core has an improved resistivity and is adapted to higher frequency regions.
  • the magnetic component of the present embodiment is suitable for a power inductor used in a power supply circuit.
  • applications of the magnetic core include, in addition to the inductor, a transformer, a motor, and the like.
  • raw metal of the soft magnetic alloy was prepared.
  • the prepared raw metal was weighed so as to satisfy the composition shown in Table 1 and was melted by high-frequency heating to prepare a mother alloy.
  • the prepared mother alloy was heated and melted to obtain molten metal having a melting temperature of 1250° C.
  • the molten metal was sprayed on a rotary roll by a single roll method to form a ribbon.
  • the material of the rotary roll was Cu.
  • the standard rotating speed of the rotary roll was 25 m/sec. By adjusting the roll rotating speed, the thickness of the obtained ribbon was set to 20 ⁇ m-30 ⁇ m, the width of the ribbon was set to 4 mm-5 mm, and the length of the ribbon was set to tens of meters.
  • the ribbon had an amorphous or a nanohetero-structure in which initial fine crystals exist in the amorphous.
  • the magnetostriction, saturation magnetic flux density, and coercivity were measured for each ribbon after the heat treatment.
  • the magnetostriction was measured by a strain gauge method.
  • the saturation magnetic flux density (Bs) was measured using a vibrating sample magnetometer (VSM) at a magnetic field of 1000 kA/m.
  • the coercivity (Hc) was measured using a direct current BH tracer at a magnetic field of 5 kA/m.
  • magnetostriction a sample in which the absolute value of magnetostriction is 2.50 ppm or less was judged to be good. A sample in which the absolute value of magnetostriction is 1.50 ppm or less is more preferable.
  • saturation magnetic flux density a sample in which the saturation magnetic flux density was 1.40 T or more was judged to be good. A sample in which the saturation magnetic flux density is 1.60 T or more was more preferable.
  • coercivity a sample in which the coercivity is 2.0 A/m or less was judged to be good. A sample in which the coercivity is 1.5 A/m or less is more preferable. The results are shown in Table 1.
  • the value of the coercivity measured as described above includes both a component derived from the magnetocrystalline anisotropy and a component derived from the magnetoelastic effect caused by the magnetostriction.
  • the component derived from the magnetoelastic effect is the product of the magnetostriction and the stress and thus cannot be detected as coercivity when the internal stress is not applied to the sample. Accordingly, it is necessary to confirm that both the coercivity and the magnetostriction show a low value and the saturation magnetic flux density shows a high value, in order to determine whether the effect of the present invention exists.
  • zero point was allocated when the magnetostriction is greater than 2.50 ppm, one point was allocated when the magnetostriction is greater than 1.50 ppm and equal to or lower than 2.50 ppm, and two points were allocated when the magnetostriction is 1.50 ppm or less.
  • zero point was allocated when the saturation magnetic flux density is less than 1.40 T, one point was allocated when the saturation magnetic flux density is 1.40 T or more and less than 1.60 T, and two points were allocated when the saturation magnetic flux density is 1.60 T or more.
  • the numerical value of the product is equal to or greater than 1 when the content ratios of boron and zinc, the total content ratio of M and zinc, and the total content ratio of boron and phosphorus are within the above-described range.
  • the numerical value of the product is equal to or greater than 4 and particularly good properties are obtained when the content ratio of zinc, the total content ratio of M and zinc, the content ratio of phosphorus, and the content ratio of silicon are within the preferable range described above.
  • the soft magnetic alloy was produced in the same manner as in Example 8.
  • the (110) plane spacing was calculated.
  • the (110) plane spacing was calculated from 20 of the strongest peak belonging to the (110) plane among the diffraction peaks obtained by the XRD measurement and the wavelength of the measurement X-ray.
  • the (110) plane spacing was calculated under the condition under which the above XRD measurement was performed using the same device as that used for the above XRD measurement.
  • the expansion values of the (110) plane spacing in the samples of Example 8 and Examples 35-38 were obtained. The results are shown in Table 3.

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