CN113053610A - Soft magnetic alloy powder, magnetic core, magnetic component, and electronic device - Google Patents

Soft magnetic alloy powder, magnetic core, magnetic component, and electronic device Download PDF

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Publication number
CN113053610A
CN113053610A CN202011464043.7A CN202011464043A CN113053610A CN 113053610 A CN113053610 A CN 113053610A CN 202011464043 A CN202011464043 A CN 202011464043A CN 113053610 A CN113053610 A CN 113053610A
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soft magnetic
alloy powder
magnetic alloy
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Inventor
梶浦良纪
长谷川晓斗
吉留和宏
松元裕之
熊冈广修
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TDK Corp
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Priority claimed from JP2020170481A external-priority patent/JP2021107575A/en
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    • 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
    • H01F1/15308Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • 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
    • H01F1/15341Preparation processes therefor
    • H01F1/1535Preparation processes therefor by powder metallurgy, e.g. spark erosion

Abstract

The invention provides a soft magnetic alloy powder which can obtain a magnetic core with good magnetic permeability. The soft magnetic alloy powder of the present invention has a specific composition with a high Co content. The soft magnetic alloy powder has a glass transition temperature Tg and a melting point Tm, and Tm is 900 ℃ or more and 1200 ℃ or pressure X is applied to the soft magnetic alloy powderPCoercive force at time YHIt will be beneficial toUsing least square method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXPWhen l is more than or equal to 0, k (unit: Oe/MPa) is more than or equal to 0 and less than or equal to 0.00100.

Description

Soft magnetic alloy powder, magnetic core, magnetic component, and electronic device
Technical Field
The invention relates to a soft magnetic alloy powder, a magnetic core, a magnetic component and an electronic device.
Background
In recent years, low power consumption and high efficiency have been demanded in electronic, information, and communication apparatuses, and the like, particularly in electronic apparatuses. In addition, the demand is more intense for the low-carbon society. Therefore, reduction of energy loss and improvement of power supply efficiency are required also in power supply circuits of electronic, information, and communication devices, particularly electronic devices.
Therefore, in order to reduce energy loss and improve power supply efficiency, it is necessary to obtain a soft magnetic alloy powder which is excellent in soft magnetic characteristics and can improve a filling ratio when used for a magnetic core.
Patent document 1 describes a soft magnetic metal powder with improved waddel sphericity. Further, it is described that an excellent power inductor can be manufactured by improving the sphericity.
Patent document 2 describes a Co-based amorphous alloy ribbon. Further, it is described that the magnetic permeability and squareness ratio are improved by making the S content 30ppm or less and the Al content 40ppm or less.
Further, as a method for filling the soft magnetic alloy powder at a high density, the methods described in patent documents 3 and 4 are known to be effective.
Patent document 3 describes that an inductor having excellent relative permeability can be produced by using soft magnetic alloy powder having a high sphericity.
Patent document 4 describes that by using 2 types of particles having different particle diameters and setting the particle diameter ratio of the 2 types of particles within a specific range, the particles can be packed at a high density and the relative permeability can be improved.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2016 + 25352
Patent document 2: japanese laid-open patent publication No. 3-173750
Patent document 3: japanese laid-open patent application No. 2010-212442
Patent document 4: japanese patent laid-open publication No. 2011-192729
Disclosure of Invention
Technical problem to be solved by the invention
The invention aims to provide soft magnetic alloy powder capable of obtaining a magnetic core with good magnetic permeability.
Technical solution for solving technical problem
In order to achieve the above object, a soft magnetic alloy powder according to a first aspect of the present invention has a composition formula (Co)(1-(α+β))X1αX2β)(1-(a+b+c+d+e+f))MaBbPcSidCreSf(atomic ratio), wherein,
x1 is at least one member selected from the group consisting of Fe and Ni,
x2 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0≤f≤0.010,
0.160<b+c+d+e+f≤0.430,
0.500<1-(a+b+c+d+e+f)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
the soft magnetic alloy powder has a glass transition temperature Tg and a melting point Tm,
and Tm is more than or equal to 900 ℃ and less than or equal to 1200 ℃.
The soft magnetic alloy powder according to the first aspect of the present invention may contain powder particles having an average circularity of 0.93 or more, and the cumulative number proportion of the powder particles from the lowest circularity to 0.50 may be 2.0% or less.
The soft magnetic alloy powder according to the first aspect of the present invention may contain powder particles having an average circularity of 0.95 or more, and the cumulative number proportion of the powder particles from the lowest circularity to 0.50 may be 1.5% or less.
The value obtained by dividing the content ratio of Co by the content ratio of B in the soft magnetic alloy powder according to the first aspect of the present invention may be greater than 2.000 and less than 5.000.
The soft magnetic alloy powder according to the first aspect of the present invention may have an amorphous state.
The soft magnetic alloy powder according to the first aspect of the present invention may have nanocrystallites.
In order to achieve the above object, a soft magnetic alloy powder according to a second aspect of the present invention has a composition formula (Co)(1-(α+β))X1αX3β)(1-(a+b+c+d+e))MaBbPcSidCre(atomic ratio), wherein,
x1 is at least one member selected from the group consisting of Fe and Ni,
x3 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C, S and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0.160<b+c+d+e≤0.430,
0.500<1-(a+b+c+d+e)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
applying pressure X to the soft magnetic alloy powderPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXPWhen l is more than or equal to 0, k (unit: Oe/MPa) is more than or equal to 0 and less than or equal to 0.00100.
The soft magnetic alloy powder according to the second aspect of the present invention may have a structure containing an amorphous substance.
The soft magnetic alloy powder according to the second aspect of the present invention may have a structure containing heterogeneous amorphous (Hetero amorphous).
The soft magnetic alloy powder according to the second aspect of the present invention may have a structure containing nanocrystals.
The following description is common to the soft magnetic alloy powder according to the first aspect and the soft magnetic alloy powder according to the second aspect.
The soft magnetic alloy powder according to the present invention may have an amorphization ratio X of 85% or more.
The magnetic core according to the present invention contains the soft magnetic alloy powder.
The magnetic member according to the present invention contains the soft magnetic alloy powder.
The electronic device according to the present invention contains the soft magnetic alloy powder.
Drawings
Fig. 1 shows an example of a pattern obtained by X-ray crystal structure analysis.
Fig. 2 shows an example of a pattern obtained by pattern fitting the graph of fig. 1.
Fig. 3 is an observation result of Morphologi G3 of powder particles having a high circularity.
Fig. 4 is an observation result of Morphologi G3 of powder particles having a low circularity.
Fig. 5 is a graph showing a relationship between circularity and cumulative number ratio.
FIG. 6 is a graph showing a portion of FIG. 5 having a circularity of 0.4 to 0.6.
FIG. 7 is a graph showing melting points Tm.
Fig. 8 is a graph showing the glass transition temperature Tg and the crystallization start temperature Tx.
FIG. 9 is a graph showing a portion of the temperature range of 450 to 600 ℃ in FIG. 8.
Fig. 10A is a schematic view of a metal powder manufacturing apparatus.
Fig. 10B is an enlarged schematic view of a main portion of fig. 10A.
Description of the symbols
1. 2: the result of the particle shape measurement; 10: an atomizing device; 20: a molten metal supply section; 21: melting a metal; 21 a: dropping molten metal; 30: a cooling section; 36: a coolant introduction section; 38a 1: an outward convex portion; 50: a flow of cooling liquid.
Detailed Description
Hereinafter, embodiments of the present invention will be described.
(first embodiment)
The soft magnetic alloy powder of the present embodiment has a composition formula (Co)(1-(α+β))X1αX2β)(1-(a+b+c+d+e+f))MaBbPcSidCreSfA soft magnetic alloy powder containing (in atomic ratio) a main component, wherein,
x1 is at least one member selected from the group consisting of Fe and Ni,
x2 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0≤f≤0.010,
0.160<b+c+d+e+f≤0.430,
0.500<1-(a+b+c+d+e+f)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
the soft magnetic alloy powder has a glass transition temperature Tg and a melting point Tm,
and Tm is more than or equal to 900 ℃ and less than or equal to 1200 ℃.
In general, soft magnetic alloy powder having a composition containing a large amount of Co has a higher relative magnetic permeability than soft magnetic alloy powder having a composition containing a large amount of Fe. In addition, the soft magnetic alloy powder having a composition containing a large amount of Co tends to have high corrosion resistance and high electric resistance, and the dielectric loss tends to be low. The soft magnetic alloy powder having a composition containing much Co has a lower melting point than the soft magnetic alloy powder having a composition containing much Fe. As a result, when the soft magnetic alloy powder is produced by an atomization method such as gas atomization described later, the atomization temperature is easily lowered. The melting point of the melt containing the soft magnetic alloy before atomization is generally the same as the melting point of the soft magnetic alloy powder obtained by atomization.
The soft magnetic alloy powder according to the present embodiment has the above-described composition, and has the glass transition temperature and the above-described melting point, and therefore the particle shape of the powder particles can be made good. Specifically, by having the above composition, and having the glass transition temperature and the above melting point, a soft magnetic alloy powder containing powder particles having a high average sphericity can be obtained. In addition, a soft magnetic alloy powder with a small number of powder particles having a particle shape with a low circularity, that is, a soft magnetic alloy powder with a small proportion of irregularly shaped particles can be obtained.
Therefore, the soft magnetic alloy powder according to the present embodiment includes the above-described powder particles having a particle shape, and thus can improve the filling factor of a magnetic core or the like using the soft magnetic alloy powder, and can improve various properties such as the relative permeability of the magnetic core or the like. Hereinafter, the powder particles may be simply referred to as particles.
When the soft magnetic alloy powder of the present embodiment is heat-treated, nanocrystals having a crystal grain size of 100nm or less or 50nm or less are likely to precipitate. Whether to contain nanocrystals and whether to contain amorphousness can be confirmed by XRD. Further, confirmation by TEM is also possible.
A structure containing amorphous is a structure having only amorphous or a structure containing heterogeneous amorphous. A structure containing a heterogeneous amorphous is a structure in which initial crystallites are present in the amorphous. The average crystal grain size of the primary crystallites is not particularly limited, and may be 0.3nm or more and 10nm or less. Further, the amorphous ratio of the structure including an amorphous substance, which can be confirmed by XRD, is 85% or more. Note that whether the structure has only an amorphous structure or a structure including a heterogeneous amorphous structure can be confirmed by TEM. A structure comprising nanocrystals is a structure comprising predominantly nanocrystals. In the structure including crystals (nanocrystals), the amorphization ratio that can be confirmed by XRD is less than 85%. Further, the average crystal grain size of the nanocrystals in the structure containing the nanocrystals is 5nm or more and 100nm or less. In the structure containing a hetero amorphous and the structure containing a nanocrystal, a crystal having a crystal particle size exceeding 100nm is not contained. Among these, in the present embodiment, the soft magnetic alloy powder preferably has a structure containing an amorphous substance, and particularly preferably has a structure containing a heterogeneous amorphous substance.
In the present embodiment, the soft magnetic metal powder having an amorphization ratio X of 85% or more represented by the following formula (1) has a structure containing only amorphous material or a structure containing heterogeneous amorphous material, and the soft magnetic metal powder having an amorphization ratio X of less than 85% has a structure containing crystals.
X=100-(Ic/(Ic+Ia)×100)…(1)
Ic: integrated intensity of crystallinity scattering
Ia: integrated intensity of amorphous scattering
The soft magnetic metal powder was subjected to X-ray crystal structure analysis by XRD, identified in phase, read the peaks (Ic: crystalline scattering integrated intensity, Ia: amorphous scattering integrated intensity) of crystallized Fe or compound, and calculated the crystallization ratio from the peak intensities, and the amorphous ratio X was calculated by the above formula (1). The calculation method will be described in more detail below.
For the present embodimentThe soft magnetic metal powder of this embodiment was subjected to X-ray crystal structure analysis by XRD, and the pattern shown in fig. 1 was obtained. The Lorentz function of the following formula (2) was subjected to a pattern fitting to obtain a crystal composition pattern α showing the integrated intensity of the crystal scattering shown in FIG. 2cAnd an amorphous component pattern alpha representing an integrated intensity of amorphous scatteringaAnd a pattern alpha obtained by combining themc+a. From the integrated intensity of crystalline scattering and the integrated intensity of amorphous scattering of the obtained pattern, the amorphous content X is obtained by the above formula (1). The measurement range is a range in which diffraction angle 2 θ from an amorphous halo can be confirmed to be 30 ° to 60 °. Within this range, the error between the integrated intensity measured by XRD and the integrated intensity calculated by the lorentz function is within 1%.
Figure BDA0002833535380000071
h: peak degree of fashion
u: peak position
w: half width
b: height of background
In addition, when the soft magnetic alloy powder of the present embodiment contains nanocrystals, each particle contains a plurality of nanocrystals. That is, the particle size of the soft magnetic alloy powder described later is different from the crystal particle size of the nanocrystal.
Hereinafter, each component of the soft magnetic alloy powder according to the present embodiment will be described in detail.
M is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V.
The content (a) of M satisfies 0 < a < 0.140. Or a is more than or equal to 0.001 and less than or equal to 0.140. Further, a may be 0.003. ltoreq. a.ltoreq.0.140, or 0.040. ltoreq. a.ltoreq.0.100. In the absence of M, the soft magnetic alloy powder hardly has a glass transition temperature Tg. As a result, the circularity of the particles is easily reduced, and the relative permeability is reduced. When a is too large, the melting point Tm of the soft magnetic alloy powder tends to decrease. As a result, the circularity of the particles is easily reduced, the proportion of the irregularly shaped particles in the soft magnetic alloy powder increases, and the relative permeability decreases. In addition, the saturation magnetic flux density is liable to decrease. Among them, 0.010. ltoreq. a.ltoreq.0.140 is preferable from the viewpoint of easiness in lowering the coercive force.
The content (B) of B is more than 0.160 and less than or equal to 0.250. B can also be more than or equal to 0.180 and less than or equal to 0.250. When b is too small, the melting point Tm of the soft magnetic alloy becomes too high, and the molten liquid cannot be ejected, and thus the soft magnetic alloy powder cannot be produced in some cases. When b is too large, the melting point Tm becomes too low, the proportion of the irregular particles in the soft magnetic alloy powder increases, the coercive force increases, and the relative permeability decreases.
The content (c) of P satisfies that c is more than or equal to 0 and less than or equal to 0.200. That is, P may not be contained. More preferably, 0. ltoreq. c.ltoreq.0.150 is satisfied, and still more preferably, 0.010. ltoreq. c.ltoreq.0.050 is satisfied. When c is too large, the melting point Tm of the soft magnetic alloy powder becomes too low, the proportion of the irregular particles in the soft magnetic alloy powder increases, the coercive force increases, and the relative permeability decreases.
The content (d) of Si satisfies that d is more than or equal to 0 and less than or equal to 0.250. That is, Si may not be contained. More preferably, d is 0. ltoreq. d.ltoreq.0.200. When d is too large, the melting point Tm of the soft magnetic alloy powder becomes too low, the circularity decreases, the proportion of the irregular particles in the soft magnetic alloy powder increases, the coercive force increases, and the relative permeability decreases.
The content (e) of Cr satisfies that e is more than or equal to 0 and less than or equal to 0.030. That is, Cr may not be contained. More preferably, 0.001. ltoreq. e.ltoreq.0.010. By containing Cr, the corrosion resistance of the soft magnetic alloy powder is easily increased. When e is too large, the proportion of the irregular particles in the soft magnetic alloy powder increases, the coercive force increases, and the relative permeability decreases.
The content (f) of S satisfies that f is more than or equal to 0 and less than or equal to 0.010. That is, S may not be contained. The larger f is, the smaller the proportion of the irregular particles in the soft magnetic alloy powder is, but when f is too large, the coercive force increases and the relative permeability decreases.
The soft magnetic alloy powder according to the present embodiment satisfies 0.160 < b + c + d + e + f < 0.430. Or b + c + d + e + f is more than or equal to 0.190 and less than or equal to 0.430. When b + c + d + e + f is too large, a soft magnetic alloy powder having a high relative permeability cannot be obtained.
Further, the soft magnetic alloy powder according to the present embodiment satisfies 0.500 < 1- (a + b + c + d + e + f) < 0.840. Can also meet the requirement that the sum of. If 1- (a + b + c + d + e + f) is too small or too large, a soft magnetic alloy powder having high relative permeability cannot be obtained.
In the soft magnetic alloy powder of the present embodiment, a part of Co may be replaced with X1 and/or X2.
X1 is at least 1 selected from Fe and Ni. The content of X1 may be α ═ 0. That is, X1 may not be included. When the number of atoms of all the components is 100 at%, the number of atoms of X1 is preferably 40 at% or less. That is, it is preferable to satisfy 0. ltoreq. α { 1- (a + b + c + d + e + f) } 0.400. Further, it is more preferable to satisfy 0. ltoreq. α { 1- (a + b + c + d + e + f) } 0.100. In addition, when a small amount of Fe is contained, the coercive force is likely to be lowered and the relative permeability is likely to be increased, as compared with the case where Fe is not contained at all. In particular, when the atomic ratio of Co/Fe is 5 or more and 20 or less, the coercive force is likely to decrease and the relative permeability is likely to increase.
X2 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C and rare earth elements. The content of X2 may be β ═ 0. That is, X2 may not be included. When the number of atoms of all the components is 100 at%, the number of atoms of X2 is preferably 5.0 at% or less. That is, it is preferable to satisfy 0. ltoreq. beta { 1- (a + b + c + d + e + f + g) } 0.050.
The range of the substitution amount for Co with X1 and/or X2 is less than half of Co in terms of atomic number. I.e., 0. ltoreq. alpha. + beta. < 0.50. Also can be more than or equal to 0 and less than or equal to alpha and beta and less than or equal to 0.40. If α + β is too large, particularly if α + β is not less than 0.50, the melting point of the soft magnetic alloy tends to be too high, and the molten liquid cannot be ejected, and thus the soft magnetic alloy powder may not be produced.
Even when the melting point of the soft magnetic alloy is high, the melt can be ejected by raising the atomizing temperature. However, when the atomization temperature is high, the circularity of the soft magnetic alloy powder tends to decrease, the proportion of irregular particles in the soft magnetic alloy powder tends to increase, the coercive force tends to increase, and the relative permeability tends to decrease.
The value obtained by dividing the content ratio of Co by the content ratio of B (hereinafter, sometimes referred to as Co/B) may be greater than 2.000 and less than 5.250, may be greater than 2.000 and less than 5.000, and may be 2.340 to 4.000. When the Co/B ratio is within the above range, the melting point Tm of the soft magnetic alloy powder described later is likely to be lowered, and the atomization temperature is likely to be lowered.
The soft magnetic alloy powder of the present embodiment may contain, as inevitable impurities, elements other than the elements contained in the above-described main components, within a range that does not greatly affect the properties such as the relative permeability. For example, the content may be 0.1 mass% or less with respect to 100 mass% of the soft magnetic alloy powder.
Next, a method of evaluating the particle shape and particle diameter of the soft magnetic alloy powder according to the present embodiment will be described.
The evaluation of the sphericity of the soft magnetic alloy powder can be performed by evaluating the circularity of a pattern obtained by projecting the particle shape of the soft magnetic alloy powder.
In the present embodiment, the particle shape was evaluated using Morphologi G3(Malvern Panalytical). Morphologi G3 is a device that disperses powder with air and projects the shape of each particle for evaluation. The shape of the particles having a particle diameter in the range of about 0.5 μm to several mm was evaluated by an optical microscope or a laser microscope. Specifically, as can be seen from the particle shape measurement results 1 and 2 shown in fig. 3 and 4, a plurality of particle shapes can be projected at a time and evaluated. However, in practice, much more particle shapes than described in the particle shape measurement results 1 and 2 shown in fig. 3 and 4 can be projected at once and evaluated. Fig. 3 shows the projection results of the powder particles having a good particle shape and a high degree of circularity, and fig. 4 shows the projection results of the powder particles having a poor particle shape and a low degree of circularity.
Morphologi G3 can create projection views of a plurality of particles at a time and evaluate them, and can evaluate the shapes of a plurality of particles in a shorter time than the conventional evaluation method using SEM observation or the like. For example, in the example described later, a projection view is created for 20000 particles, the circularity of each particle is automatically calculated, and the average circularity is calculated on a number basis. In contrast, in the conventional SEM observation, since the circularity is calculated for 1 particle of 1 by using the SEM image, it is difficult to evaluate the shape of a plurality of particles in a short time.
When the area of the projection is S and the length around the projection is L, the circularity of the particle is 2(π S)1/2and/L represents. The circularity of the circle is 1, and the closer the circularity of the particle is to 1, the higher the sphericity of the particle.
The soft magnetic alloy powder according to the present embodiment can improve the average circularity by having the above-described composition, and specifically, can be 0.93 or more. The average circularity is preferably 0.95 or more.
The proportion of the irregularly shaped particles was evaluated in the following manner.
For 20000 particles after the circularity measurement, the cumulative number ratio (cumulative number) from the time of low circularity was calculated. The smaller the cumulative number ratio from the lowest circularity to 0.50, the smaller the ratio of the irregularly shaped particles.
The soft magnetic alloy powder according to the present embodiment, having the above-described composition, can have a melting point Tm in the range of 900 ℃ to 1200 ℃, and can reduce the proportion of irregular particles. The cumulative number ratio from the lowest circularity to 0.50 can be made specifically 2.5% or less or 2.0% or less. The cumulative number ratio of 0.50 from the lowest circularity is preferably 1.5% or less. The lower limit of the cumulative number ratio from the lowest circularity to 0.50 is not particularly limited. For example, it may be 0.05% or more.
Fig. 5 and 6 show examples of graphs obtained with the circularity on the horizontal axis and the cumulative number ratio on the vertical axis. In the case of the solid line, the cumulative number ratio from the minimum circularity to 0.50 is 1.5% or less. In contrast, in the case of the broken line, the cumulative number ratio from the lowest circularity to 0.50 is more than 1.5% and 2.0% or less. That is, it can be evaluated that the proportion of the irregularly shaped particles is smaller in the case of the solid line than in the case of the broken line.
The method for evaluating the particle size is shown below.
In the present embodiment and examples described later, the particle size was evaluated on a volume basis. The method for measuring the average particle diameter (D50) on a volume basis is not particularly limited. For example, the average particle diameter (D50) on a volume basis can be obtained by a laser diffraction particle size distribution measuring apparatus.
In the present embodiment, the average particle diameter of the soft magnetic metal powder is not particularly limited. For example, it may be 5 μm to 50 μm.
Hereinafter, the glass transition temperature Tg, the melting point Tm, and the like will be described with reference to the drawings.
In fig. 7, the solid line shows the results of the Differential Scanning Calorimeter (DSC) measurement of the soft magnetic alloy powder of the present embodiment for the thermophysical properties (hereinafter also simply referred to as DSC measurement results), and the broken line shows the results of the DSC measurement of the soft magnetic alloy powder containing amorphous Fe. The rate of temperature rise is constant. Generally, the melting point is sometimes the temperature at which the soft magnetic alloy starts to melt (Tm 1 in fig. 7), and the melting point is sometimes the temperature at which the melting ends (Tm 2 in fig. 7). In the present invention, the temperature at which melting ends (Tm 2 in fig. 7) is defined as the melting point Tm. This is because the temperature at the end of melting has a greater influence on the atomization temperature and the temperature of the molten metal when an atomization method such as gas atomization described later is performed, and has a greater influence on the properties of the soft magnetic alloy powder obtained by the atomization method.
When the temperature of the soft magnetic alloy powder of the present embodiment containing an amorphous substance is increased, a glass transition reaction (endothermic reaction) occurs at a specific temperature. This temperature is the glass transition temperature Tg. When the temperature further reaches a high temperature, a crystallization reaction (exothermic reaction) occurs at a certain temperature. This temperature is the crystallization start temperature Tx. At this time, supercooled liquid region Δ T is represented by Tx-Tg.
The supercooled liquid region is associated with stabilization of amorphous substance, and the wider the supercooled liquid region, the larger Δ T, the higher amorphous substance forming ability. In contrast, when the supercooled liquid region is narrow, the amorphous forming ability is low. The Δ T is preferably 20 ℃ or higher.
In fig. 8 and 9, the solid line shows the results of the thermal property measurement by DSC of the soft magnetic alloy powder according to the present embodiment, and the broken line shows the results of the DSC of the soft magnetic alloy powder containing amorphous Fe. The rate of temperature rise is constant. The soft magnetic alloy powder of the present embodiment has a glass transition temperature Tg and a crystallization start temperature Tx. In contrast, the Fe-based soft magnetic alloy powder containing amorphous does not have a glass transition temperature Tg. The crystallization starting temperature of the Fe-based soft magnetic alloy powder containing amorphous is not shown.
The soft magnetic alloy powder of the present embodiment has a characteristic that Tm is lower and Tg is higher than a soft magnetic alloy powder containing amorphous Fe. This can reduce the atomization temperature. Further, the coercive force of the soft magnetic alloy powder can be reduced, the relative permeability of the soft magnetic alloy powder itself can be improved, the average circularity of the soft magnetic alloy powder can be increased, and the proportion of irregular particles in the soft magnetic alloy powder can be reduced. Further, the filling factor of the magnetic core using the soft magnetic alloy powder can be improved, and the relative permeability can be improved.
The method for producing the soft magnetic alloy powder of the present embodiment will be described below.
The method for producing the soft magnetic alloy powder of the present embodiment includes, for example, a gas atomization method.
Hereinafter, a method for producing a soft magnetic alloy powder by a gas atomization method will be described.
The inventors of the present invention have found that when the atomizing device shown in fig. 10A and 10B is used as the atomizing device, soft magnetic metal powder having a good particle shape can be easily obtained.
As shown in fig. 10A, the atomizing device 10 includes a molten metal supply unit 20 and a cooling unit 30 disposed below the molten metal supply unit 20 in the vertical direction. In the drawings, the vertical direction is a direction along the Z axis.
The molten metal supply unit 20 includes a heat-resistant container 22 for containing molten metal 21. In the heat-resistant container 22, the raw materials of the respective metal elements weighed so as to have the composition of the finally obtained soft magnetic alloy powder are melted by the heating coil 24 to form the molten metal 21. The temperature at the time of melting, that is, the temperature of the molten metal 21 may be determined in consideration of the melting point of the raw material of each metal element and the melting point (Tm) of the molten metal 21, and may be, for example, 1200 to 1600 ℃.
Molten metal 21 is discharged from discharge port 23 to cooling unit 30 as dropped molten metal 21 a. High-pressure gas is jetted from the gas jet nozzle 26 toward the discharged molten drop 21a, and the molten drop 21a forms a plurality of droplets and moves toward the inner surface of the cylindrical body 32 along the flow of the gas.
The gas injected from the gas injection nozzle 26 is preferably an inert gas or a reducing gas. As the inert gas, for example, nitrogen, argon, helium, or the like can be used. As the reducing gas, for example, ammonia decomposition gas or the like can be used. However, when the molten metal 21 is a metal that is difficult to oxidize, the gas injected from the gas injection nozzle 26 may be air.
The molten metal 21a dropped onto the inner surface of the cylindrical body 32 collides with the coolant flow 50 formed in an inverted conical shape inside the cylindrical body 32, and is further divided and refined, and is cooled and solidified to become solid alloy powder. The axial center O of the cylinder 32 is inclined at a predetermined angle θ 1 with respect to the lead line Z. The predetermined angle θ 1 is not particularly limited, and is preferably 0 to 45 degrees. By setting the angle to such a range, the dropped molten metal 21a from the discharge port 23 can be easily discharged toward the coolant flow 50 formed in an inverted conical shape inside the cylindrical body 32.
A discharge portion 34 is provided below along the axial center O of the cylindrical body 32, and is capable of discharging the alloy powder contained in the coolant flow 50 to the outside together with the coolant. The alloy powder discharged together with the coolant is separated from the coolant in an external storage tank or the like and taken out. The coolant is not particularly limited, and cooling water may be used.
Therefore, the average circularity of the soft magnetic alloy powder finally obtained can be adjusted by adjusting the water pressure of the cooling water. The lower the water pressure, the higher the average circularity of the finally obtained soft magnetic alloy powder, but when the water pressure is too low, the cooling water flow 50 formed in an inverted conical shape cannot be obtained. However, even if the water pressure is changed, the proportion of the irregular particles does not change greatly. The method of adjusting the water pressure is not particularly limited. The method of supplying the cooling water may be determined as appropriate. For example, when the cooling water is supplied by a pump, the pressure of the cooling water can be adjusted by adjusting the pump pressure.
In the present embodiment, since the dropped molten metal 21a collides with the coolant flow 50 formed in the inverted conical shape, the flight time of the molten drop of the dropped molten metal 21a is shortened as compared with the case where the coolant flow is along the inner surface 33 of the cylindrical body 32. If the flight time is shortened, the quenching effect is promoted, and the amorphization ratio X of the obtained soft magnetic alloy powder is increased. Further, the average circularity tends to be high. Further, if the flight time is shortened, the droplets of molten metal 21a are less likely to be oxidized, so that the miniaturization of the obtained soft magnetic alloy powder is promoted and the quality of the soft magnetic alloy powder is improved.
In the present embodiment, in order to form the coolant flow in the cylindrical body 32 into an inverted conical shape, the flow of the coolant in the coolant introduction portion (coolant discharge portion) 36 for introducing the coolant into the cylindrical body 32 is controlled. Fig. 10B shows the structure of the coolant introduction portion 36.
As shown in fig. 10B, an outer portion (outer space portion) 44 located outside the cylindrical body 32 in the radial direction and an inner portion (inner space portion) 46 located inside the cylindrical body 32 in the radial direction are defined by the frame body 38. The outer portion 44 and the inner portion 46 are partitioned by the partition 40, and the outer portion 44 and the inner portion 46 are communicated with each other by a passage portion 42 formed at an upper portion of the partition 40 in the axial direction O, through which the coolant can flow.
A single or multiple nozzles 37 are connected to the outer side 44, and the cooling liquid enters the outer side 44 from the nozzles 37. Further, a coolant discharge portion 52 is formed below the inner portion 46 in the axial center O direction, and the coolant in the inner portion 46 is discharged (guided) into the interior of the cylinder 32.
The outer peripheral surface of the frame 38 serves as a flow path inner peripheral surface 38b for guiding the flow of the coolant in the inner portion 46, and an outer protrusion 38a1 that continues from the flow path inner peripheral surface 38b of the frame 38 and protrudes radially outward is formed at the lower end 38a of the frame 38. Therefore, the annular gap between the distal end of the outer convex portion 38a1 and the inner surface 33 of the cylindrical body 32 serves as the coolant discharge portion 52. The flow path side upper surface of the outer convex portion 38a1 is formed with a flow path deflecting surface 62.
As shown in fig. 10B, the radial width D1 of the coolant discharge portion 52 is narrower than the radial width D2 of the main body portion of the inner portion 46 due to the outer protrusion 38a 1. Since D1 is narrower than D2, the coolant flowing downward along the flow path inner peripheral surface 38b toward the lower side of the axial center O inside the inner portion 46 flows along the flow path deflecting surface 62 of the frame 38, and collides with the inner surface 33 of the cylindrical body 32 to be reflected. As a result, as shown in fig. 10A, the coolant is discharged from the coolant discharge portion 52 into the interior of the cylindrical body 32 in an inverted conical shape, forming the coolant flow 50. When D1 is D2, the coolant discharged from the coolant discharge unit 52 forms a coolant flow along the inner surface 33 of the cylindrical body 32.
D1/D2 is preferably 2/3 or less, more preferably 1/2 or less, and most preferably 1/10 or more.
The coolant flow 50 flowing out of the coolant discharge portion 52 is a reverse cone flow that linearly advances from the coolant discharge portion 52 toward the axis O, but may be a spiral reverse cone flow.
The gas ejection temperature, gas ejection pressure, and the like may be appropriately set according to the particle size of the target soft magnetic alloy powder. The gas injection temperature may be, for example, room temperature or higher and 200 ℃ or lower. The gas injection pressure may be, for example, 0.5MPa or more and 19MPa or less.
The soft magnetic alloy powder according to the present embodiment can be obtained by the above method. In order to appropriately control the particle shape and particle diameter, it is preferable that the soft magnetic alloy powder contains an amorphous state and does not contain crystals (nanocrystals).
The soft magnetic alloy powder containing amorphous obtained by the above-described gas atomization method is preferably subjected to heat treatment. For example, by performing heat treatment at 350 to 575 ℃ for 0.1 to 2 hours, the powders are prevented from being sintered to each other and from being coarsened, diffusion of elements is promoted, and a thermodynamic equilibrium state is achieved in a short time, and deformation and stress can be removed. Further, nanocrystals may be precipitated at this time.
The use of the soft magnetic alloy powder according to the present embodiment is not particularly limited, and is suitable for use in applications requiring high relative permeability. For example, a magnetic core can be cited. The magnetic core is particularly suitable for power inductors. In addition, the powder is also suitable for magnetic parts using soft magnetic alloy powder, such as thin film inductors and magnetic heads. Further, a magnetic core and a magnetic component using the soft magnetic alloy powder can be applied to an electronic device.
Further, the smaller the average particle size of the soft magnetic alloy powder is, the lower the loss of high frequency can be. Therefore, the soft magnetic alloy powder having a small average particle size is particularly suitable for use in high-frequency parts. In addition, the larger the average particle size of the soft magnetic alloy powder is, the more easily the magnetic permeability of the core is increased. Therefore, the soft magnetic alloy powder having a large average particle size is suitable for use in a member requiring a high magnetic permeability.
(second embodiment)
The second embodiment will be described below, and the same contents as those of the first embodiment will be described without specific description.
The soft magnetic alloy powder of the present embodiment has a composition formula (Co)(1-(α+β))X1αX3β)(1-(a+b+c+d+e))MaBbPcSidCreA soft magnetic alloy powder containing a main component (atomic ratio),
x1 is at least one member selected from the group consisting of Fe and Ni,
x3 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C, S and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0.160<b+c+d+e≤0.430,
0.500<1-(a+b+c+d+e)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
applying pressure X to the soft magnetic alloy powderPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXPWhen l is more than or equal to 0, k (unit: Oe/MPa) is more than or equal to 0 and less than or equal to 0.00100.
In general, the coercive force of a soft magnetic alloy powder having a composition containing a large amount of Co tends to be lower than that of a soft magnetic alloy powder having a composition containing a large amount of Fe.
In addition, the magnetic core can be produced by molding the soft magnetic alloy powder. The higher the pressure at the time of molding, the more the soft magnetic alloy powder can be filled at a high density. By filling the soft magnetic alloy powder at a high density, the relative permeability of the magnetic core can be improved.
However, when a magnetic core is produced by molding a soft magnetic alloy powder, when the soft magnetic alloy powder is filled at a high density by setting the pressure at the time of molding to a high pressure, the inside of the magnetic body (soft magnetic alloy powder) is deformed. Therefore, the coercive force of the magnetic core tends to increase and the relative permeability tends to decrease.
The soft magnetic alloy powder according to the present embodiment has the above-described composition, and the change in coercive force when the soft magnetic alloy powder is pressurized is small. Specifically, pressure X is applied to the soft magnetic alloy powderPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXPWhen l is more than or equal to 0, k (unit: Oe/MPa) is more than or equal to 0 and less than or equal to 0.00100. Further, k may be 0.00015. ltoreq. k.ltoreq. 0.00095.
When k is out of the above range, the higher the pressure at the time of molding, the smaller the ratio of increase in relative permeability of the magnetic core to increase in pressure. In contrast, when k is within the above range, the ratio of the increase in relative permeability of the core with respect to the increase in pressure is less likely to decrease than when k is outside the above range. That is, when the soft magnetic alloy powder having k within the above range is used as compared with the soft magnetic alloy powder having k outside the above range, the higher the pressure at the time of molding, the larger the difference in relative permeability of the obtained magnetic core.
Hereinafter, each component of the soft magnetic alloy powder according to the present embodiment will be described in detail.
The content (a) of M satisfies 0 < a < 0.140. Or a is more than or equal to 0.001 and less than or equal to 0.140. In addition, a may satisfy 0.003. ltoreq. a.ltoreq.0.100, may satisfy 0.003. ltoreq. a.ltoreq.0.040, and may satisfy 0.020. ltoreq. a.ltoreq.0.040. When M is not contained, the coercive force of the soft magnetic alloy powder becomes too high, and the relative permeability of the magnetic core decreases. When a is too large, k becomes too large. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where a is within the above range and k is small, if the filling ratio of the core is the same.
The content (B) of B is more than 0.160 and less than or equal to 0.250. B can also be more than or equal to 0.180 and less than or equal to 0.250, and b can also be more than or equal to 0.180 and less than or equal to 0.220. When b is too small or too large, k becomes too high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where b is within the above range and k is small, if the filling ratio of the core is the same.
The content (c) of P satisfies that c is more than or equal to 0 and less than or equal to 0.200. That is, P may not be contained. C can be more than or equal to 0 and less than or equal to 0.150, c can be more than or equal to 0 and less than or equal to 0.050, and c can be more than or equal to 0 and less than or equal to 0.010. When c is too large, k rises. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where c is within the above range and k is small, if the filling ratio of the core is the same.
The content (d) of Si satisfies that d is more than or equal to 0 and less than or equal to 0.250. That is, Si may not be contained. D is more than or equal to 0 and less than or equal to 0.200, d is more than or equal to 0 and less than or equal to 0.100, and d is more than or equal to 0.050 and less than or equal to 0.070. When d is too large, k becomes too high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where d is within the above range and k is small, if the filling ratio of the core is the same.
The content (e) of Cr satisfies that e is more than or equal to 0 and less than or equal to 0.030. That is, Cr may not be contained. E is more than or equal to 0 and less than or equal to 0.020, e is more than or equal to 0 and less than or equal to 0.010, and e is more than or equal to 0 and less than or equal to 0.001. When e is too large, k becomes too high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core is reduced when the filling factor of the core is the same, as compared with the case where e is within the above range and k is small.
The soft magnetic alloy powder according to the present embodiment satisfies 0.160 < b + c + d + e.ltoreq.0.430. B + c + d + e is more than or equal to 0.180 and less than or equal to 0.430, and b + c + d + e is more than or equal to 0.180 and less than or equal to 0.400. When b + c + d + e is too large, k becomes too high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where b + c + d + e is within the above range and k is small, if the filling ratio of the core is the same.
The soft magnetic alloy powder according to the present embodiment satisfies 0.500 < 1- (a + b + c + d + e) < 0.840. Can satisfy the condition that 0.550 is not less than 1- (a + b + c + d + e) not less than 0.800, and can also satisfy the condition that 0.580 is not less than 1- (a + b + c + d + e) not less than 0.800. When 1- (a + b + c + d + e) is too small, the saturation magnetic flux density tends to be low. When 1- (a + b + c + d + e) is too large, the coercive force tends to be high.
In the soft magnetic alloy powder of the present embodiment, a part of Co may be replaced with X1 and/or X3.
X1 is at least 1 selected from Fe and Ni. The content of X1 may be α ═ 0. That is, X1 may not be included. When the number of atoms of all the components is 100 at%, the number of atoms of X1 may be 40 at% or less. That is, 0. ltoreq. α { 1- (a + b + c + d + e) } 0.400 can be satisfied. In addition, 0. ltoreq. alpha { 1- (a + b + c + d + e) } 0.360 may be satisfied, and 0. ltoreq. alpha { 1- (a + b + c + d + e) } 0.144 may be satisfied. In addition, when a small amount of Fe is contained, the coercive force is more likely to decrease and the relative permeability is more likely to increase, as compared with the case where Fe is not contained at all. In particular, when the atomic ratio of Co/Fe is 5 or more and 20 or less, the coercive force is liable to decrease and the relative permeability is liable to increase.
X3 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C, S and rare earth elements. X3 may be at least 1 selected from the group consisting of Al, Zn, Sn, Cu, Bi, La, Y, N, O, C and S. The content of X3 may be β ═ 0. That is, X3 may not be included. When the number of atoms in the entire composition is 100 at%, the number of atoms of X3 may be 5.0 at% or less. That is, 0. ltoreq. beta { 1- (a + b + c + d + e) } 0.050 can be satisfied.
The range of the substitution amount for Co with X1 and/or X3 is 0. ltoreq. alpha. + beta. < 0.50. At α + β > 0.50, k becomes too high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases as compared with the case where the filling ratio of the core is the same and k is small and 0 ≦ α + β < 0.50. In addition, 0. ltoreq. alpha. + β. ltoreq.0.50 may be used.
The soft magnetic alloy powder of the present embodiment may contain, as inevitable impurities, elements other than the elements contained in the above-described main components, within a range that does not greatly affect the properties such as the relative permeability. For example, the content may be 0.1 mass% or less with respect to 100 mass% of the soft magnetic alloy powder.
Hereinafter, a method for measuring k in the soft magnetic alloy powder of the present embodiment will be described. First, a method for producing a pressurized soft magnetic alloy powder will be described.
The soft magnetic alloy powder of the present embodiment was weighed 2 g. Too much or too little amount of powder may cause the result to become inaccurate.
Subsequently, the weighed powder was poured into a mold of Φ 8 mm. Too large or too small a diameter of the die may cause the result to become inaccurate.
Then, using a manual press, the powder poured into the mold is pressed at a specific pressure XPPressurization was carried out for 30 seconds.
Next, the pressurized powder is taken out of the die to obtain pressurized powder.
In the measurement of k, the pressure X at the time of pressurization is preparedP400MPa, 800MPa and unpressurized powders. Will not be pressurizedX of powderPRecorded as 0 MPa. Then, the coercive force (unit: Oe) of each powder was measured. Then, a pressure X will be appliedPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXP+ l, calculating the slope k (unit: Oe/MPa) of the approximate straight line. In addition, even if X is addedpThe soft magnetic alloy powder of the present embodiment is not solidified even when pressurized at 400MPa or 800MPa for 30 seconds.
In the present embodiment, the average particle diameter of the soft magnetic metal powder is not particularly limited. For example, it may be 5 μm to 50 μm.
The method for producing the soft magnetic alloy powder by the gas atomization method is the same as that of the first embodiment. In order to appropriately control k, it is preferable that the soft magnetic alloy powder contains an amorphous state and does not contain crystals (nanocrystals).
The soft magnetic alloy powder containing amorphous obtained by the gas atomization method described above may be subjected to heat treatment. In the heat treatment, for example, by performing the heat treatment at 250 to 600 ℃, preferably 250 to 550 ℃, and more preferably 250 to 450 ℃ for 0.1 to 2 hours, the powders are prevented from being sintered to each other to coarsen the powders, the diffusion of elements is promoted, a thermodynamic equilibrium state is reached in a short time, and deformation and stress can be removed. Further, although crystallization may progress by heat treatment, it is preferable to perform heat treatment at a low temperature to such an extent that crystals having a crystal grain size of more than 100nm do not precipitate. Further, by performing the heat treatment at an appropriate temperature and for an appropriate time, k can be lowered, and the relative permeability of the magnetic core can be particularly improved when the pressure is high at the time of molding. In addition, nanocrystals can be precipitated at this time. However, in the case where the heat treatment temperature is excessively high or in the case where the heat treatment time is excessively long, k becomes excessively high. When the pressure at the time of molding the soft magnetic alloy powder is high, the relative permeability of the core decreases when the filling factor of the core is the same as compared with a case where the heat treatment temperature and the heat treatment time are appropriate and k is small.
The use of the soft magnetic alloy powder according to the present embodiment is not particularly limited, and is suitable for use in applications where high relative permeability is required. For example, a magnetic core can be cited. The magnetic core is particularly suitable for power inductors. In addition, the present invention can be suitably used for magnetic parts using soft magnetic alloy powder, for example, thin film inductors and magnetic heads. Further, a magnetic core and a magnetic component using the soft magnetic alloy powder are suitably used for electronic devices.
[ examples ] A method for producing a compound
The present invention will be specifically described below based on examples.
(Experimental example 1)
Ingots of various materials were prepared and weighed to obtain master alloys of the compositions shown in table 1. Then, the crucible was placed in a gas atomizing device.
Next, the master alloy is stored in a heat-resistant container 22 disposed in the atomizing device 10. Next, after the inside of the cylindrical body 32 is evacuated, the heat-resistant container 22 is heated by high-frequency induction using the heating coil 24 provided outside the heat-resistant container 22, and the raw material metals in the heat-resistant container 22 are melted and mixed to obtain a molten metal (melt).
The obtained melt was injected into the frame 32 of the cooling unit 30 at an atomization temperature shown in table 1, and argon gas was injected at an injection gas pressure of 7MPa, thereby forming a plurality of droplets. The droplets were collided with an inverted conical cooling water flow of cooling water supplied at a pump pressure of 10MPa to form fine powder, which was then recovered. Among them, samples No.3 and 4 in Table 1 had too low an atomization temperature to spray the melt.
In the atomizing device 10 shown in fig. 10A and 10B, the inner diameter of the inner surface of the cylinder 32 is 300mm, D1/D2 is 1/2, and the angle θ 1 is 20 degrees.
In addition, in Experimental example 1, the heat treatment was performed at 475 ℃ for 60 minutes. In addition, ICP analysis confirmed that the composition of the master alloy substantially agrees with that of the soft magnetic alloy powder.
It was confirmed whether or not each of the obtained soft magnetic alloy powders contained an amorphous state and a nanocrystal. The degree of amorphousness X was calculated by XRD. Soft magnetic metal powder with X of 85% or more is amorphous in the fine structure. When the amorphization ratio was less than 85%, it was confirmed by XRD that the crystallite size was evaluated by the scherrer equation, and whether crystals larger than nanocrystals were included. When the crystal containing more than nano-crystal is not contained, the crystal is marked as amorphous and nano-crystal; when crystals larger than nanocrystals are included, they are referred to as crystals. The results are shown in Table 1.
The shape of the powder particles of each of the obtained soft magnetic alloy powders was evaluated. Specifically, the circularities of 20000 particles were measured, and the average circularity on a number basis and the cumulative number ratio from the lowest circularity to 0.50 were calculated. The results are shown in Table 1. In each of examples and comparative examples, when the cumulative number ratio is 2.0% or less, the amount of the irregularly shaped particles is small; when the cumulative number ratio is 1.5% or less, the number of irregular particles is particularly small. In each of examples and comparative examples, it was confirmed that the average particle diameter (D50) on a volume basis was about 25 μm by a laser diffraction particle size distribution measuring apparatus (HELOS & RODOS (Sympatec)).
The obtained soft magnetic alloy powders were subjected to DSC measurement (STA449F3(NETZSCH corporation)) to confirm the presence or absence of Tg. Then, Tm and Δ T were measured. The results are shown in Table 1.
The coercive force HC of each of the obtained soft magnetic alloy powders was measured by using a (K-HC 1000 type (northeast special steel corporation)). The results are shown in Table 1. Hc is not particularly limited. Hc may be 0.50Oe or less. Hc is preferably 0.20Oe or less.
Next, a toroidal core was produced from each soft magnetic alloy powder. Specifically, a phenolic resin as an insulating binder was mixed with each of the soft magnetic alloy powders so that the amount of the phenolic resin was 3 mass% of the total amount, and the mixture was granulated by using a general planetary mixer as a stirrer to obtain a granulated powder having a particle size of about 500 μm. Then, the surface pressure was set to 4ton/cm2(392MPa) the granulated powder thus obtained was molded to give an appearance
Figure BDA0002833535380000211
Inner diameter
Figure BDA0002833535380000212
An annular shaped body having a height of 6 mm. The obtained molded article was cured at 150 ℃ to prepare a toroidal core.
Then, a UEW wire was wound around the toroidal core, and μ (relative permeability) was measured at 100kHz using 4284A PRECISION LCR METER (Hewlett-Packard Company). The results are shown in Table 1. Among them, the case where the relative permeability μ was 30 or more was evaluated as good.
[ TABLE 1 ]
Figure BDA0002833535380000221
According to Table 1, as sample Nos. 1 to 4 and 1a each containing an amorphous Fe-based soft magnetic alloy, the Tm is high, and hence the atomization temperature required for the ejection is as high as 1500 ℃ or higher. That is, the range of the atomization temperature at which the soft magnetic alloy powder can be produced is narrow. In addition, the obtained soft magnetic alloy powder does not have Tg. Therefore, the coercive force of the soft magnetic alloy powder is increased, the circularity is lowered, and many irregular particles are formed. Further, the relative permeability μ of the toroidal core made using the soft magnetic alloy powder is reduced.
In contrast, sample Nos. 5 to 8 and 5a, which had a composition containing much Co, had a low Tm, and therefore had a low atomization temperature required for injection, and could be injected at an atomization temperature of 1300 ℃. That is, the range of the atomization temperature at which the soft magnetic alloy powder can be produced is wide. In addition, the obtained soft magnetic alloy powder has Tg. Therefore, the soft magnetic alloy powder has a low coercive force, a high circularity, and few irregular particles. Further, the relative permeability μ of the toroidal core made using the soft magnetic alloy powder is increased.
(Experimental example 2)
In experimental example 2, the soft magnetic alloy powders and toroidal cores of samples nos. 9 and 10 were produced under the conditions described in experimental example 1, except that the pump pressure for supplying the cooling water was changed from sample No. 1. The results are shown in Table 2.
[ TABLE 2 ]
Figure BDA0002833535380000241
According to table 2, the average circularity of the particles of the soft magnetic alloy powder is increased by lowering the pump pressure. However, the change in the ratio of the cumulative number is small, and the change in the ratio of the irregularly shaped particles is also small. Since samples 9 and 10 are soft magnetic alloys containing amorphous Fe, Tm is high. In addition, the obtained soft magnetic alloy powder does not have Tg. Therefore, the coercivity of the soft magnetic alloy powder increases and the number of irregular particles increases. Further, the relative permeability μ of the toroidal core made using the soft magnetic alloy powder is reduced.
(Experimental example 3)
In experimental example 3, soft magnetic alloy powders and toroidal cores of samples nos. 9 to 16 were produced under the conditions described in experimental example 1, except that part of Co was replaced with Fe in sample No. 8. The results are shown in Table 3.
Soft magnetic alloy powders and toroidal cores of sample nos. 8a to 8e were produced under the same conditions as in sample No.8 except that the compositions were changed. The results are shown in Table 3A.
[ TABLE 3 ]
Figure BDA0002833535380000261
[ TABLE 3A ]
Figure BDA0002833535380000271
According to Table 3, sample Nos. 11 to 14 having compositions within the predetermined range had good particle shapes and good relative magnetic permeability μ of the toroidal core. According to samples 11 to 14, as the amount of Fe increases, Tm increases, coercive force increases, and relative permeability μ decreases. In sample No.16, in which α + β > 0.500 and the content of Co was too small, the melting point of the soft magnetic alloy was too high, and the melt could not be ejected at the atomizing temperature of 1300 ℃. However, sample No.11, which has a Co/Fe atomic ratio of 5 to 20, has a lower coercive force and a higher relative permeability μ than samples Nos. 8 and 12, which are outside the above-described ranges.
According to table 3A, as each sample having a composition within a predetermined range, Tg and Tm within a predetermined range, the atomization temperature required for the injection was low, and the injection could be performed at an atomization temperature of 1300 ℃. That is, the range of the atomization temperature at which the soft magnetic alloy powder can be produced is wide. In addition, the obtained soft magnetic alloy powder has Tg. Therefore, the coercivity of the soft magnetic alloy powder is reduced, the circularity is increased, and the number of irregular particles is small. Further, the relative permeability μ of the toroidal core made using the soft magnetic alloy powder is increased. When the Co/B ratio is higher than that of sample No.8, the higher the Co/B ratio, the higher the Tm, the smaller the average circularity, the higher the coercive force, and the lower the relative permeability μ tend to be.
(Experimental example 4)
In experimental example 4, a soft magnetic alloy powder and a toroidal core were produced under the same conditions as in experimental example 3 and sample No.11, except that the contents of the elements contained in the main components were changed. The results are shown in tables 4to 7.
[ TABLE 4 ]
Figure BDA0002833535380000291
[ TABLE 5 ]
Figure BDA0002833535380000301
[ TABLE 6 ]
Figure BDA0002833535380000311
[ TABLE 7 ]
Figure BDA0002833535380000321
In Table 4, examples of experiments in which the contents of Co, Fe and M (Nb) were changed are shown. Sample Nos. 18 to 22 having a composition within the predetermined range have Tg and have Tm within the predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. In addition, the relative permeability of the toroidal core increases.
In contrast, sample No.17, which does not contain M (Nb), does not have Tg. As a result, the average circularity of the soft magnetic alloy powder is low, the number of irregular particles is large, and the coercive force is increased. And, the relative permeability of the toroidal core is increased. In addition, the Tm of sample No.23 containing an excessive amount of M becomes too low. As a result, the average circularity of the soft magnetic alloy powder is low, the number of irregular particles is large, and the coercive force is increased. And, the relative permeability of the toroidal core is increased.
In Table 5, samples No.24 to 27 are experimental examples in which the contents (B) of Co, Fe and B were changed from sample No. 11. Sample Nos. 25 and 26 having a composition within the specified range have Tg and have Tm within the specified range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. In addition, the relative permeability of the toroidal core increases. In contrast, the soft magnetic alloy of sample No.24, in which the B content was too small, had too high a melting point, and it was not possible to spray the melt at the atomizing temperature of 1300 ℃. The Tm of sample No.27 containing an excessive amount of B becomes too low. As a result, the soft magnetic alloy powder has a large number of irregular particles and a high coercive force. Also, the relative permeability of the toroidal core decreases.
In Table 5, samples No.28 to 34 are experimental examples in which the contents (c) of Co, Fe and P were changed from sample No. 11. Sample Nos. 28 to 33 having a composition within a predetermined range have Tg and have Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. In addition, the relative permeability of the toroidal core increases. In contrast, sample No.34 having an excessive P content has an excessively low Tm. As a result, the average circularity of the soft magnetic alloy powder is low, the number of irregular particles is large, and the coercive force is increased. Also, the relative permeability of the toroidal core decreases.
In Table 5, samples No.35 to 41 are experimental examples in which the contents (d) of Co, Fe and Si were changed from sample No. 11. Sample Nos. 35 to 40 having a composition within a predetermined range have Tg and have Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. In addition, the relative permeability of the toroidal core increases. In contrast, sample No.41, which has an excessive Si content, has an excessively low Tm. As a result, the average circularity of the soft magnetic alloy powder is low, the number of irregular particles is large, and the coercive force is increased. Also, the relative permeability of the toroidal core decreases.
In Table 6, samples 42 to 46 are experimental examples in which the contents (e) of Co, Fe and Cr are mainly changed from sample 11. Sample Nos. 42 to 45 having a composition within a predetermined range have Tg and have Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. And, the relative permeability of the toroidal core is increased. In contrast, the soft magnetic alloy powder of sample No.46, in which the Cr content was too large, had a large number of irregular grains, and the coercive force was high. Also, the relative permeability of the toroidal core decreases.
In Table 7, samples 47 to 49 are experimental examples in which the contents (f) of Co, Fe and S were mainly changed from sample 11. Sample Nos. 47 and 48 having compositions within the specified range have Tg and have Tm within the specified range. The soft magnetic alloy powder has a high average circularity and few irregular particles. In contrast, the soft magnetic alloy powder of sample No.49, in which the content of S is too large, has a high coercive force. Also, the relative permeability of the toroidal core decreases.
(Experimental example 5)
In experimental example 5, a soft magnetic alloy powder and a toroidal core were produced under the conditions described in experimental example 1, except that part of Co was replaced with X1 and/or X2 in sample No. 8. The results are shown in tables 8 and 9.
[ TABLE 8 ]
Figure BDA0002833535380000351
[ TABLE 9 ]
Figure BDA0002833535380000361
Even if a part of Co is replaced with X1 and/or X2, each sample having a composition within a predetermined range has Tg and Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. And, the relative permeability of the toroidal core is increased.
(Experimental example 6)
In experimental example 6, a soft magnetic alloy powder and a toroidal core were produced under the conditions described in experimental example 1, except that the type of M was changed for sample No. 8. The results are shown in Table 10.
[ TABLE 10 ]
Figure BDA0002833535380000381
Even if the kind of M is changed, each sample having a composition within a predetermined range has Tg and has Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. And, the relative permeability of the toroidal core is increased.
(Experimental example 7)
In experimental example 7, a soft magnetic alloy powder and a toroidal core were produced under the conditions described in experimental example 1, except that the heat treatment conditions were changed for sample No. 8. Specifically, sample No.109 was not heat-treated. The heat treatment temperature was raised to 575 ℃ in sample No. 110. The results are shown in Table 11. Although not shown in table 11, each sample had Tg and Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force.
[ TABLE 11 ]
Figure BDA0002833535380000391
The soft magnetic alloy powder of sample No.109 can be said to be the soft magnetic alloy powder before the heat treatment in the process for producing the soft magnetic alloy powder of sample No. 8. When the heat treatment is carried out at 475 ℃ before and after the heat treatment, it is considered that the relative permeability μ is increased because no crystal is formed in the heat treatment and the strain and stress can be removed.
The soft magnetic alloy powder of sample No.110 was heat-treated at 575 ℃ to form nanocrystals.
(Experimental example 8)
In experimental example 8, the soft magnetic alloy powders and toroidal cores of samples nos. 111 and 112 were produced under the conditions described in experimental example 3, except that the average particle size on a volume basis was changed from that of sample No. 11. Soft magnetic alloy powders and toroidal cores of samples nos. 113 to 115 were produced under the same conditions as in samples nos. 11, 111 and 112 except that the content (B) of B was reduced and the atomization temperature was 1600 ℃. The results are shown in Table 12.
[ TABLE 12 ]
Figure BDA0002833535380000401
According to table 12, the larger the average particle diameter is, the higher the relative permeability of the toroidal core is. In addition, each of samples No.11, 111, and 112 having a composition within a predetermined range has Tg and has Tm within a predetermined range. In addition, the soft magnetic alloy powder has a high average circularity, few irregular particles, and a low coercive force. And, the relative permeability of the toroidal core is increased.
On the other hand, the samples No.113 to 115 in which the B content (B) was too small had no Tg, and Tm was too high. As a result, the average circularity of the soft magnetic alloy powder is low, the number of irregular particles is large, and the coercive force is increased. Also, the relative permeability of the toroidal core decreases.
(Experimental example 9)
To obtain Co0.720Nb0.020B0.180P0.010Si0.070Preparing and weighing ingots of various materials.Then, the crucible was placed in a gas atomizing device.
Next, the master alloy is stored in a heat-resistant container 22 disposed in the atomizing device 10. Next, after the inside of the cylindrical body 32 is evacuated, the heat-resistant container 22 is heated by high-frequency induction using the heating coil 24 provided outside the heat-resistant container 22, and the raw material metals in the heat-resistant container 22 are melted and mixed to obtain a molten metal (melt).
The obtained melt was sprayed into the frame 32 of the cooling unit 30 at an atomization temperature of 1500 ℃, and argon gas was sprayed at a spray gas pressure of 7MPa, thereby forming a plurality of droplets. The droplets were collided with an inverted conical cooling water flow of cooling water supplied at a pump pressure of 10MPa to form fine powder, which was then recovered.
In the atomizing device 10 shown in fig. 10A and 10B, the inner diameter of the inner surface of the cylinder 32 is 300mm, and the angle θ 1 is 20 degrees. In addition, in Experimental example 9, D1/D2 were set to the conditions shown in Table 13.
ICP analysis confirmed that the composition of the master alloy substantially agrees with that of the soft magnetic alloy powder.
It was confirmed whether or not each of the obtained soft magnetic alloy powders had a structure containing amorphous material, a structure containing nanocrystalline material, and a structure containing crystalline material. Whether or not a peak due to the nanocrystal exists was confirmed by XRD, and when the amorphization ratio was 85% or more, it was written as having a structure including an amorphous material; when the content is less than 85%, the structure is regarded as having a structure containing nanocrystals or a structure containing crystals. When the amorphization ratio was 85% or more, whether the structure including amorphous had only amorphous or included heterogeneous amorphous was confirmed by TEM. According to the results confirmed by TEM, a structure having only amorphous is referred to as amorphous, and a structure having a structure containing heterogeneous amorphous is referred to as heterogeneous amorphous. In addition, when the amorphization ratio was less than 85%, it was confirmed whether or not crystals larger than nanocrystals were included by evaluation of the crystallite size by the scherrer equation by XRD. When the crystal containing more than nanocrystal is not contained, it is referred to as having a structure containing nanocrystal. In addition, when having a structure including nanocrystals, the term "nanocrystal" refers to a structure including nanocrystals; when crystals larger than nanocrystals are included, they are referred to as crystals. The results are shown in table 13 as one item of the microstructure.
Subsequently, 2g of the obtained soft magnetic alloy powder was weighed. Subsequently, the weighed powder was poured into a mold of Φ 8 mm. Then, the powder poured into the mold is pressed by a manual press with a pressure XPPressurization was carried out for 30 seconds. Next, the pressurized powder is taken out of the die to obtain pressurized powder.
In the measurement of k, unpressurized powder (X) was prepared in each sampleP0), pressure X at the time of pressurizationP400MPa powder, pressure X at the time of pressurizationP800MPa powder 3 kinds of powders were measured for coercive force (unit: Oe) of each powder by Hc meter (K-HC 1000 type (northeast Special Steel Co., Ltd)). Then, a pressure X will be appliedPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXP+ l, the slope k of the approximate line is measured. The results are shown in Table 13.
Next, a toroidal core was produced from each soft magnetic alloy powder. Specifically, a phenolic resin as an insulating binder was mixed with each of the soft magnetic alloy powders so that the amount of the phenolic resin was 3 mass% of the total amount, and the mixture was granulated by using a general planetary mixer as a stirrer to obtain a granulated powder having a particle size of about 500 μm. Then, the magnetic material was packed at a surface pressure of 6ton/cm so that the magnetic material filled rate became 70 to 72%2(588MPa) to surface pressure of 8ton/cm2(784MPa) the resulting granulated powder was molded to give an appearance
Figure BDA0002833535380000421
Inner diameter
Figure BDA0002833535380000422
An annular shaped body having a height of 6 mm. The obtained molded article was cured at 150 ℃ to prepare a toroidal core.
Then, the coercive force of the toroidal core was measured by using an Hc meter (K-HC 1000 type (manufactured by northeast Special Steel Co., Ltd)). The coercive force of the toroidal core was evaluated as good at 1.00Oe or less, more preferably at 0.50Oe or less, and particularly preferably at 0.30Oe or less.
Then, a UEW wire was wound around the toroidal core, and μ (relative permeability) was measured at 100kHz using 4284A PRECISION LCR METER (Hewlett-Packard Company). The results are shown in Table 13. Among them, the case where the relative permeability μ is 30 or more is evaluated as good, and the case where the relative permeability μ is 35 or more is evaluated as particularly good.
[ TABLE 13 ]
Figure BDA0002833535380000431
According to Table 13, the coercive force and the relative permeability of the magnetic cores of sample Nos. 201 to 203 in which k is 0. ltoreq. k.ltoreq.0.00100 are both good. In contrast, sample No.204, in which D1/D2 is 1, has too large k, resulting in too high coercive force of the magnetic core and too low relative permeability of the magnetic core.
(Experimental example 10)
In experimental example 10, a soft magnetic alloy powder and a toroidal core were produced under the same conditions as in sample No.201 or sample No.204 except that sample No.201 or sample No.204 was heat-treated at the temperature shown in table 14 for 60 minutes. The results are shown in Table 14.
[ TABLE 14 ]
Figure BDA0002833535380000432
According to Table 14, all of the coercive forces and the relative permeabilities of the magnetic cores of sample Nos. 201 and 205 to 209 in which k is 0. ltoreq. k.ltoreq.0.00100 were good. In particular, the fine structure is sample nos. 201, 205 to 208 having only an amorphous structure, a structure containing heterogeneous amorphous, or a structure containing nanocrystalline, and both the coercive force of the magnetic core and the relative permeability of the magnetic core are better than in sample No.209 having a fine structure containing crystals larger than nanocrystalline. Further, the fine structure is sample nos. 201, 205 to 207 having only an amorphous structure or a structure containing heterogeneous amorphous, and both the coercive force of the magnetic core and the relative permeability of the magnetic core are better than those of sample No.208 having a fine structure containing nanocrystals. In contrast, sample No.210 had too large k, and as a result, the coercive force of the magnetic core was too high, and the relative permeability of the magnetic core was too low. In sample No.204 and samples No.211 to 216 obtained by heat-treating sample No.204, k was too large regardless of the microstructure, and as a result, the coercive force of the magnetic core was too high and the relative permeability of the magnetic core was too low.
(Experimental example 11)
In experimental example 11, a soft magnetic alloy powder and a toroidal core were produced under the same conditions as in sample No.207 except that a part or all of Co was replaced with Fe in sample No. 207. The results are shown in Table 15. Among them, it was confirmed by XRD that the amorphous ratio was 85% or more with respect to the fine structure of the soft magnetic metal powder. That is, although it was confirmed that the structure includes amorphous, it was not confirmed whether the structure including amorphous includes only amorphous or includes hetero-amorphous.
[ TABLE 15 ]
Figure BDA0002833535380000451
According to Table 15, the magnetic cores of sample Nos. 207 and 217 to 220 in which α + β is within a specific range and k is 0. ltoreq. k.ltoreq.0.00100 are excellent in relative permeability. In contrast, the coercive force of the magnetic core of sample nos. 222 and 223 in which α + β is too large and k is too large is too high, and as a result, the relative permeability of the magnetic core is too low. In particular, in sample No.217 in which Co/Fe is 5 to 20 at an atomic ratio, k is smaller than in sample Nos. 207, 218 to 220 in which Co/Fe is outside the above range, the coercive force of the magnetic core is lowered, and the relative permeability of the magnetic core is increased. All of the samples in table 15 had a structure including amorphous.
(Experimental example 12)
In experimental example 12, a soft magnetic alloy powder and a toroidal core were produced under the same conditions as in sample No.217 except that the content (a) of Nb was changed and the contents of Co and Fe were changed from sample No. 217. The results are shown in Table 16. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or had a structure containing heterogeneous amorphous.
[ TABLE 16 ]
Figure BDA0002833535380000471
According to Table 16, the coercive force and the relative permeability of the magnetic core of sample Nos. 217, 225 to 229 satisfying 0.001. ltoreq. a.ltoreq.0.140 and 0.500. ltoreq.1- (a + b + c + d + e) < 0.840 and satisfying 0. ltoreq. k.ltoreq.0.00100 are good. In contrast, sample No.224, which does not contain m (nb) and a is 0.000, has the results that the coercive force of the magnetic core is too high and the relative permeability of the magnetic core is too low. In addition, sample No.230 in which a is too large has too large k, resulting in too high coercive force of the magnetic core and too low relative permeability of the magnetic core. In addition, the sample had a structure including an amorphous material, except for sample No. 224. Sample No.224 contained crystals larger than the nanocrystals.
(Experimental example 13)
In experimental example 13, a soft magnetic alloy powder and a toroidal core were produced under the same conditions as in sample No.217 except that the content (B) of B, the content (c) of P, the content (d) of Si, and the content (e) of Cr were changed from sample No.217, and the contents of Co and Fe were changed. The results are shown in Table 17. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or a structure containing heterogeneous amorphous.
[ TABLE 17 ]
Figure BDA0002833535380000491
According to Table 17, the coercive force and the relative permeability of the magnetic core of each sample were good in which the B content (B), the P content (c), the Si content (d), the Cr content (e), and the B + c + d + e were in specific ranges and k was 0. ltoreq. k.ltoreq.0.00100 was satisfied. On the other hand, when the k of each sample is too large, the coercive force of the magnetic core is too high and the relative permeability of the magnetic core is too low, which is caused by that any one or more of the content (B) of B, the content (c) of P, the content (d) of Si, the content (e) of Cr, and the content (B + c + d + e) of B + c + d + e is out of the specific range. In addition to sample No.231, the material had a structure containing amorphous material. Sample No.231 contained crystals larger than the nanocrystals.
(Experimental example 14)
Soft magnetic alloy powder and toroidal core were produced under the same conditions as in sample No.207 except that a part of Co was replaced with Ni in sample No. 207. The results are shown in Table 18. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or had a structure containing heterogeneous amorphous.
[ TABLE 18 ]
Figure BDA0002833535380000501
According to Table 18, even when a part of Co was replaced with Ni and X1 was Ni, the coercive force of the magnetic core and the relative permeability of the magnetic core of each sample having a composition within a specific range and satisfying 0. ltoreq. k.ltoreq.0.00100 were good. In contrast, sample No.258 in which the Ni content was too large had too large k, resulting in too high coercive force of the magnetic core and too low relative permeability of the magnetic core. All of the samples in table 18 had a structure including amorphous.
(Experimental example 14)
Soft magnetic alloy powder and toroidal cores were produced under the same conditions as in sample No.207 except that part of Co was replaced with X3 in sample No. 207. The results are shown in Table 19. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or had a structure containing heterogeneous amorphous.
[ TABLE 19 ]
Figure BDA0002833535380000511
According to Table 19, even when a part of Co was replaced with X3, the coercive force and the relative permeability of the magnetic core of each sample having a composition within a specific range and satisfying 0. ltoreq. k.ltoreq.0.00100 were good. All of the samples in table 19 had a structure including an amorphous substance.
(Experimental example 15)
Soft magnetic alloy powder and toroidal cores were produced under the same conditions as in sample 207 except that part of Co was replaced with X1 and X3 in sample 207. The results are shown in Table 20. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or had a structure containing heterogeneous amorphous.
[ TABLE 20 ]
Figure BDA0002833535380000521
According to Table 20, even when some of Co was replaced with X1 and X3, the coercive force of the magnetic core and the relative permeability of the magnetic core of each sample having a composition within a specific range and satisfying 0. ltoreq. k.ltoreq.0.00100 were good. All samples in table 20 had a structure including amorphous.
(Experimental example 16)
Soft magnetic alloy powder and toroidal core were produced under the same conditions as in sample No.207 except that the type of M was changed for sample No. 207. The results are shown in Table 21. In addition, with respect to the fine structure of the soft magnetic metal powder, it was not confirmed whether the structure containing amorphous had only an amorphous structure or had a structure containing heterogeneous amorphous.
[ TABLE 21 ]
Figure BDA0002833535380000531
According to Table 21, even when the type of M was changed, the coercive force of the magnetic core and the relative permeability of the magnetic core of each sample having a composition within a specific range and satisfying 0. ltoreq. k.ltoreq.0.00100 were good. All samples in table 21 had a structure including amorphous.

Claims (10)

1. A soft magnetic alloy powder characterized by:
having a composition formula (Co) expressed by an atomic number ratio(1-(α+β))X1αX2β)(1-(a+b+c+d+e+f))MaBbPcSidCreSfThe main components of the composition are as follows,
x1 is at least one member selected from the group consisting of Fe and Ni,
x2 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0≤f≤0.010,
0.160<b+c+d+e+f≤0.430,
0.500<1-(a+b+c+d+e+f)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
the soft magnetic alloy powder has a glass transition temperature Tg and a melting point Tm,
and Tm is more than or equal to 900 ℃ and less than or equal to 1200 ℃.
2. A soft magnetic alloy powder according to claim 1, wherein:
the soft magnetic alloy powder contains powder particles having an average circularity of 0.93 or more, and the powder particles have a cumulative number ratio of 0.50 or less from the lowest circularity of 2.0% or less.
3. A soft magnetic alloy powder according to claim 1, wherein:
the soft magnetic alloy powder contains powder particles having an average circularity of 0.95 or more, and the powder particles have a cumulative number ratio of 0.50 or less from the lowest circularity of 1.5% or less.
4. A soft magnetic alloy powder according to any one of claims 1 to 3, wherein:
the value obtained by dividing the content ratio of Co by the content ratio of B is greater than 2.000 and less than 5.000.
5. A soft magnetic alloy powder according to any one of claims 1 to 3, wherein:
the amorphization rate X is 85% or more.
6. A soft magnetic alloy powder characterized by:
having a composition formula (Co) expressed by an atomic number ratio(1-(α+β))X1αX3β)(1-(a+b+c+d+e))MaBbPcSidCreThe main components of the composition are as follows,
x1 is at least one member selected from the group consisting of Fe and Ni,
x3 is more than 1 selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, C, S and rare earth elements,
m is more than 1 selected from Nb, Hf, Zr, Ta, Mo, W, Ti and V,
0<a≤0.140,
0.160<b≤0.250,
0≤c≤0.200,
0≤d≤0.250,
0≤e≤0.030,
0.160<b+c+d+e≤0.430,
0.500<1-(a+b+c+d+e)<0.840,
α≥0,
β≥0,
0≤α+β<0.50,
applying a pressure X to the soft magnetic alloy powderPCoercive force at time YHWill use the least squares method to XPAnd YHThe straight line obtained by linear approximation of the relationship (A) is represented by YH=kXPWhen the sum of the k and the k is more than or equal to 0 and less than or equal to 0.00100, wherein the unit of the k is Oe/MPa.
7. A soft magnetic alloy powder according to claim 6, wherein:
the amorphization rate X is 85% or more.
8. A magnetic core, characterized by:
a soft magnetic alloy powder comprising the soft magnetic alloy powder according to any one of claims 1 to 7.
9. A magnetic component, characterized by:
a soft magnetic alloy powder comprising the soft magnetic alloy powder according to any one of claims 1 to 7.
10. An electronic device, characterized in that:
a soft magnetic alloy powder comprising the soft magnetic alloy powder according to any one of claims 1 to 7.
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