Soft magnetic alloy and magnetic component

Abstract

The present invention provides a soft magnetic alloy having a high saturation magnetic flux density Bs and a low coercive force Hc. The soft magnetic alloy contains Fe and at least one chalcogen element. An amorphous phase and a nanocrystal having a crystal grain size of 5 to 30 nm are mixed. The coefficient of determination of the atomic concentration of Fe and the atomic concentration of at least one chalcogen element is 0.700 or more.

Description

Technical Field

[0001] This invention relates to soft magnetic alloys and magnetic components. Background Technology

[0002] Patent document 1 discloses an Fe-based soft magnetic alloy, which precipitates nano-sized crystals with α-Fe as the main component and Si, B, etc. dissolved in solid solution by heat treatment of an amorphous alloy with Fe-Si-B as the basic component.

[0003] Patent document 2 discloses a soft magnetic alloy in which Fe-based nanocrystals are precipitated by heat treatment of an alloy with Fe as the main component and containing Si. This soft magnetic alloy is composed of Fe-based nanocrystals and amorphous materials.

[0004] Non-patent document 1 discloses a feature described later. Figure 4 and Figure 5 The disclosed soft magnetic alloy exhibits a fine-structured microstructure. Specifically, there is... Figure 4 A soft magnetic alloy comprising α-Fe phase 11, amorphous phase 13, and TaC phase (M-Z compound phase 15 described later); and Figure 5 A soft magnetic alloy containing α-Fe compound phase 11 and TaC phase (M-Z compound phase 15, described later) as shown.

[0005] Existing technical documents

[0006] Patent documents

[0007] Patent Document 1: Japanese Patent No. 2713363

[0008] Patent Document 2: Japanese Patent No. 6460276

[0009] Non-patent literature

[0010] Non-patent literature 1: Materials Transactions, JIM, Vol. 36, No. 7 (1995), pp. 952 to 961 Summary of the Invention

[0011] The technical problem that the invention aims to solve

[0012] The purpose of this invention is to provide a soft magnetic alloy with high saturation magnetic flux density Bs and low coercivity Hc.

[0013] Technical solutions for solving technical problems

[0014] To achieve the above objectives, the soft magnetic alloy of the present invention contains Fe and at least one quasi-metallic element, characterized in that:

[0015] Amorphous and nanocrystalline materials with a grain size of 5–30 nm coexist.

[0016] The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element is greater than 0.700.

[0017] The soft magnetic alloy of the present invention, by having the above-mentioned characteristics, can provide a soft magnetic alloy with high saturation magnetic flux density Bs and low coercivity Hc.

[0018] It may also contain at least one type of metal, M, which is a transition metal from group 4 to 6.

[0019] The coefficients of determination for the atomic concentration of Fe and the atomic concentration of at least one type of M can also be greater than 0.700.

[0020] It can also be a soft magnetic alloy with an Fe-M-Z system composition.

[0021] M is selected from one or more transition metals from groups 4 to 6, and Z is selected from two or more of C, P, Si, B, and Ge.

[0022] The element with the highest proportion in Z relative to the total number of atoms in the aforementioned soft magnetic alloys is designated as Z1, and the element with the highest proportion other than Z1 is designated as Z2.

[0023] Alternatively, the coefficients of determination for the atomic concentrations of M and Z1 can be greater than 0.600, or the coefficients of determination for the atomic concentrations of M and Z2 can be greater than 0.600.

[0024] The coefficients of determination for the atomic concentrations of Z1 and Z2 can also be less than 0.400.

[0025] It can also be a soft magnetic alloy with an Fe-M-Z system composition.

[0026] M is selected from one or more transition metals from groups 4 to 6, and Z is selected from two or more of C, P, Si, B, and Ge.

[0027] The element with the highest proportion in Z relative to the total number of atoms in the aforementioned soft magnetic alloys is designated as Z1, and the element with the highest proportion other than Z1 is designated as Z2.

[0028] Alternatively, the coefficient of determination for the atomic concentrations of M and Z1 can be less than 0.500, or the coefficient of determination for the atomic concentrations of M and Z2 can be less than 0.500.

[0029] The coefficients of determination for the atomic concentrations of Z1 and Z2 can also be less than 0.400.

[0030] The composition of the above Fe-M-Z system can also be expressed by the formula (Fe (1－(α+β)) X1 α X2 β ) (1－(a+b+c)) M1 a Z b Cr c express,

[0031] X1 is selected from one or more of Co and Ni.

[0032] X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, Cu, Bi, N, O, S, and rare earth elements.

[0033] M1 is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W.

[0034] Alternatively, it can be 0.030 ≤ a ≤ 0.140.

[0035] 0.030≤b≤0.275

[0036] 0.000≤c≤0.030

[0037] 0≤α(1-(a+b+c))≤0.400

[0038] β≥0

[0039] 0≤α+β≤0.50.

[0040] Alternatively, it can be 0.050≤b≤0.200.

[0041] Alternatively, it can be 0.730≤1-(a+b+c)≤0.930.

[0042] It can also be a soft magnetic alloy with an Fe-M-C system composition.

[0043] Alternatively, the XRD patterns of the aforementioned soft magnetic alloys may not show peaks for M-C compounds.

[0044] The aforementioned soft magnetic alloy may also have a first region where the total concentration of Fe, Co and Ni is 85 at% or more and a second region where the total concentration of Fe, Co and Ni is 80 at% or less. In the second region, the average value of M / C, which is the atomic concentration of M divided by the atomic concentration of C, may also be greater than 1.0.

[0045] The composition of the above Fe-M-C system can also be expressed by the formula (Fe (1－(α+β)) X1 α X2 β ) (1－(a+b1+b2+c)) M1 a C b3Z3 b4 Cr c express,

[0046] X1 is selected from one or more of Co and Ni.

[0047] X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, S, and rare earth elements.

[0048] M1 is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W.

[0049] Z3 is selected from one or more of P, B, Si, and Ge.

[0050] Alternatively, it can be 0.030 ≤ a ≤ 0.140.

[0051] 0.005≤b3≤0.200

[0052] 0.000≤b4≤0.180

[0053] 0.000≤c≤0.030

[0054] 0≤α(1-(a+b3+b4+c))≤0.400

[0055] β≥0

[0056] 0≤α+β≤0.50.

[0057] It can also be 0.040≤b3≤0.120.

[0058] Alternatively, it can be 0.730≤1-(a+b3+b4+c)≤0.930.

[0059] It can also be 0.050≤a≤0.140.

[0060] It may also contain Fe-based nanocrystals.

[0061] It can also be in the shape of a thin strip.

[0062] It can also be in powder form.

[0063] It can also be in the shape of a thin film.

[0064] The magnetic component of the present invention includes the above-mentioned soft magnetic alloy. Attached Figure Description

[0065] Figure 1 This is an example of a scatter plot made from the atomic concentrations of Fe and Z.

[0066] Figure 2This is an example of a scatter plot made from the atomic concentrations of Fe and Z.

[0067] Figure 3 This is a schematic diagram of the microstructure of the soft magnetic alloy 1 in this embodiment.

[0068] Figure 4 This is a schematic diagram of the microstructure of the existing soft magnetic alloy 101.

[0069] Figure 5 This is a schematic diagram of the microstructure of the existing soft magnetic alloy 201.

[0070] Figure 6 This is an example of a graph obtained by analyzing the crystal structure of a soft magnetic alloy using XRD.

[0071] Figure 7 Through the Figure 6 An example of a pattern obtained by contour fitting of a chart.

[0072] Figure 8 This is a mapping image of Fe obtained by 3DAP measurement.

[0073] Figure 9 This is a mapping image of Ta obtained through 3DAP measurement.

[0074] Figure 10 This is a mapping image of C obtained by 3DAP measurement. Detailed Implementation

[0075] The present invention will now be described based on the embodiments shown in the accompanying drawings.

[0076] The soft magnetic alloy of this embodiment contains Fe and at least one quasi-metallic element, characterized in that:

[0077] Amorphous and nanocrystalline materials with a grain size of 5–30 nm coexist.

[0078] The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element is greater than 0.700.

[0079] The soft magnetic properties of a soft magnetic alloy can be altered by changing the microscopic segregation and dispersion state of the elements contained within it. Furthermore, the microscopic segregation and dispersion state of the elements in a soft magnetic alloy varies depending on the alloy's composition and heat treatment conditions (the alloy's thermal history).

[0080] The method for confirming the microscopic segregation and dispersion state of two elements contained in soft magnetic alloys is explained.

[0081] The atomic concentrations of two elements were measured at multiple locations within the soft magnetic alloy. Then, the atomic concentrations of the two elements were plotted at each measurement location using the x-axis and y-axis as the respective axes, resulting in a scatter plot. Regression analysis was then performed to obtain a linear regression equation (y = ax + b).

[0082] When 'a' is positive, the two elements tend to coexist relatively well and are prone to aggregation. When 'a' is negative, the two elements tend to repel each other relatively well and are prone to separation. Moreover, the two elements are prone to segregation.

[0083] In soft magnetic alloys containing Fe and quasi-metallic elements, and where amorphous and nanocrystalline materials coexist, the a-value tends to be negative when scatter plots are obtained based on the atomic concentrations of Fe and quasi-metallic elements. That is, in such soft magnetic alloys, Fe and quasi-metallic elements tend to repel each other and are easily separated. Specifically, nanocrystalline materials tend to contain Fe but are less likely to contain quasi-metallic elements, while amorphous materials tend to contain quasi-metallic elements but are less likely to contain Fe.

[0084] Figure 1 , Figure 2 The image shows an example of a scatter plot. Furthermore, in the scatter plot, the x-axis (horizontal axis) is set to the atomic concentration of Fe, and the y-axis (vertical axis) is set to the atomic concentration of the metalloid element. Additionally, the metalloid element is represented by Z.

[0085] Here, the coefficient of determination R can be obtained from the first regression equation. 2 Furthermore, the larger the coefficient of certainty, the easier it is for the two elements to aggregate or disperse. That is, the greater the influence of each element relative to itself. Conversely, the smaller the coefficient of certainty, the smaller the influence of each element relative to itself.

[0086] Figure 1 It is a scatter plot with a coefficient of determination of around 0.9. Figure 2 It is a scatter plot with a coefficient of determination of approximately 0.6. (And...) Figure 2 compared to, Figure 1 Nanocrystals readily contain Fe but rarely Z. Additionally, with Figure 2 compared to, Figure 1 Amorphous materials tend to contain Z but are less likely to contain Fe. That is, compared to... Figure 2 compared to, Figure 1 The Fe and Z atoms are separated. Furthermore, the inventors have discovered that in soft magnetic alloys containing a mixture of Fe and Z, and of amorphous and nanocrystalline forms, the larger the coefficient of determination is when a scatter plot is obtained based on the atomic concentrations of Fe and Z, the easier it is to improve the magnetic properties. In other words, the more separated Fe and Z are, the easier it is to improve the magnetic properties. In other words, as Fe condenses in the nanocrystalline form and Z condenses in the amorphous form, the magnetic properties are more easily improved.

[0087] The microscopic segregation and dispersion of elements contained in soft magnetic alloys can be observed and measured using a three-dimensional atomic probe (3DAP).

[0088] The following is an explanation of the three-dimensional atom probe (3DAP).

[0089] 3DAP is an apparatus used to obtain three-dimensional atomic arrangement information. The following describes the sequence of measurements using 3DAP. First, a high voltage is applied to a needle-shaped sample, followed by a laser pulse. This causes electrolytic evaporation at the tip of the sample. A two-dimensional detector detects the ions generated by the electrolytic evaporation, thereby determining the atomic arrangement of the sample. Simultaneously, the ion species can be determined based on the ion's time-of-flight.

[0090] Furthermore, by analyzing the measurement data obtained from 3DAP using software, the observation range can be virtually divided into multiple hexahedral grids of arbitrary size. Each hexahedral grid contains compositional information calculated from the measurement data. Therefore, microscopic compositional information can be statistically processed and analyzed. Thus, by using 3DAP, fluctuations in the microscopic composition of the sample can be observed in three dimensions. Moreover, the atomic configuration within the sample can be observed; that is, the microscopic segregation and dispersion of each element contained in the sample can be observed.

[0091] The inventors used 3DAP to observe the microscopic segregation and dispersion of each element in samples prepared by changing the composition and heat treatment conditions. Then, they measured the magnetic properties (saturation magnetic flux density Bs, coercivity Hc, etc.) using a vibrating sample magnetometer (VSM). The results showed that changing the composition and heat treatment conditions of the soft magnetic alloy altered the concentration distribution of each element within it. Furthermore, they found that changing the composition and heat treatment conditions changed the dependence of each element's concentration distribution relative to the concentration distribution of other elements. They also discovered a significant correlation between the difference in the concentration ratio of Fe and quasi-metallic elements in micro-regions of the soft magnetic alloy and the magnetic properties of the alloy. Examples of quasi-metallic elements include, for instance, B, C, Al, Si, P, Ge, As, Se, Sb, Te, Po, and At.

[0092] The following is an example of the measurement conditions for a sample in 3DAP. A cuboid or cube with sides of at least 40 nm × 40 nm × 50 nm is used as the measurement range. By analyzing the measurement data obtained using software, this cuboid or cube (measurement range) is virtually divided into a grid of cubes with sides of 2 nm. That is, there are at least 10,000 grids containing compositional information in each grid. Furthermore, there are no particular restrictions on the shape of the measurement range, as long as at least 10,000 grids exist continuously. Moreover, it is possible to statistically process and analyze multiple grids, each containing compositional information. The inventors have discovered a coefficient of determination R for obtaining the atomic concentration of Fe and the atomic concentration of at least one metalloid element. 2 The analytical method involves creating a scatter plot based on the atomic concentrations of Fe and at least one other metallic element in each grid cell. Then, a linear regression equation is obtained through regression analysis. Furthermore, the coefficient of determination R can be calculated from the linear regression equation. 2 Hereinafter, the metalloid element will sometimes be designated as Z, and the coefficients of determination for the atomic concentrations of Fe and Z will be denoted as R. 2 (Fe-Z). In addition, other coefficients of determination are sometimes recorded in the same way.

[0093] By R 2 Setting (Fe-Z) to 0.700 or higher allows for the production of soft magnetic alloys with high saturation magnetic flux density Bs and low coercivity Hc. This is because the soft magnetic alloy of this embodiment contains a mixture of amorphous and nanocrystalline phases with a grain size of 5–30 nm. Fe is condensed in the nanocrystalline phase, while the quasi-metallic elements are condensed in the amorphous phase. Therefore, R… 2 (Fe-Z) increases. Conversely, in nanocrystalline phases, the higher the concentration of metalloid elements, the higher the R... 2 The lower (Fe-Z) is, the lower the saturation magnetic flux density Bs is.

[0094] Soft magnetic alloys may also contain at least one metal element (M) in addition to Fe and at least one metalloid. M is a transition metal from group 4 to 6. Furthermore, the deterministic coefficient R can be obtained using the above method based on the atomic concentrations of Fe and at least one metal element in each grid. 2 (Fe-M). R 2 (Fe-M) is preferably 0.700 or higher. (Through R) 2 When the (Fe-M) ratio is 0.700 or higher, the magnetic properties, especially Bs, are easily improved. This is because the soft magnetic alloy of this embodiment contains a mixture of amorphous and nanocrystalline phases with a grain size of 5-30 nm. Fe is condensed in the nanocrystalline phase, while M is condensed in the amorphous phase. Therefore, R... 2(Fe-M) increases. Conversely, in nanocrystalline phases, the higher the concentration of M element, the higher the R... 2 The lower (Fe-M) is, the lower the saturation magnetic flux density Bs is.

[0095] The following provides further explanation of the specific composition determinations. Specifically, the compositions of the Fe-M-Z system and the Fe-M-C system will be explained.

[0096] (1) Composition and coefficient of determination of the Fe-M-Z system

[0097] The soft magnetic alloy of this embodiment may also be a soft magnetic alloy having an Fe-M-Z system composition. M is one or more transition metals selected from groups 4 to 6, and Z is two or more selected from C, P, Si, B, and Ge.

[0098] The Fe-M-Z system is composed primarily of Fe, M, and Z. Additionally, Co and / or Ni can replace a portion of the Fe. Specifically, Co and / or Ni can replace up to 40 at% of the total Fe. Furthermore, the combined content of Fe, Co, and Ni relative to the total soft magnetic alloy can be 73 at% or more. Moreover, in the case of an Fe-M-Z system soft magnetic alloy, the content of elements other than Fe, Co, Ni, M, and Z in the soft magnetic alloy is 25 at% or less relative to the total soft magnetic alloy. Examples of elements other than Fe, Co, Ni, M, and Z include Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, S, and rare earth elements.

[0099] M is one or more transition metals selected from groups 4 to 6. For example, it can also be one or more selected from Ta, V, Zr, Hf, Ti, Nb, Mo, and W. Z is two or more selected from C, P, Si, B, and Ge. In addition, M and Z can combine with each other to form crystals of M-Z compounds. Hereinafter, an element selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W will be designated as M1. Cr can be cited as an example of M other than M1.

[0100] In the soft magnetic alloy of this embodiment, the content of M1 can be 3.0 at% or more and 14.0 at% or less, or 7.0 at% or more and 9.0 at% or less. The content of Z can be 3.0 at% or more and 27.5 at% or less, or 5.0 at% or more and 16.0 at% or less. The content of Cr can also be 0 at% or more and 3.0 at% or less. That is, the soft magnetic alloy of this embodiment may also be Cr-free. In addition, in the soft magnetic alloy of this embodiment, it is particularly easy to increase the saturation magnetic flux density Bs and easily reduce the coercivity Hc by containing 3 at% or more of Ta relative to the total M1, which is therefore preferred. Alternatively, it is also possible to contain 40 at% or more of Ta relative to the total M1.

[0101] There are no particular limitations on the fine structure of the soft magnetic alloy of this embodiment. The soft magnetic alloy of this embodiment contains M and Z, but it is possible to prevent the precipitation of M-Z compounds; preferably, it contains virtually no M-Z compounds. Furthermore, it may contain M and Z as an amorphous material. That is, as... Figure 3 As shown, the soft magnetic alloy 1 of this embodiment contains an α-Fe phase 11 composed of crystals and an amorphous phase 13, but preferably does not actually contain any. Figure 4 , Figure 5 The M-Z compound phase 15 is shown.

[0102] The absence of M-Z compound phase 15 means that there are no peaks of M-Z compounds in the XRD charts obtained for soft magnetic alloys. That is, there is actually no crystallization of M-Z compounds. "No peaks of M-Z compounds in the XRD charts" means that in the chart after removing the background, the intensity of the peak of M-Z compound (200) is less than 5% relative to the intensity of the peak of α-Fe (110). It can also be less than 1%. The precision of quantitative analysis by XRD is usually around 1 to 5% or more relative error, so it is appropriate to consider that the crystallization of M-Z compounds is actually not present.

[0103] Here, the element with the highest proportion in Z relative to the total atomic number of the aforementioned soft magnetic alloy is designated as Z1, and the element with the highest proportion other than Z1 is designated as Z2. That is, Z1 and Z2 are quasi-metallic elements with relatively high concentrations in the composition of the soft magnetic alloy. Furthermore, when the proportions of two or more elements are the same, the proportions increase in the order of C, P, B, Si, and Ge. Moreover, there are no particular restrictions on the total proportion of Z other than Z1 and Z2. For example, the total Z content can be set to 100 at%, or it can be 50 at% or less.

[0104] In soft magnetic alloys with an Fe-M-Z system composition, the soft magnetic properties of the alloy can be altered by changing the microscopic segregation and dispersion state of the various elements contained within it. Furthermore, the microscopic segregation and dispersion state of the elements in the soft magnetic alloy varies depending on the alloy's composition and heat treatment conditions (the alloy's thermal history).

[0105] As mentioned above, the microscopic segregation and dispersion state of each element contained in a soft magnetic alloy can be observed and measured using a three-dimensional atomic probe (3DAP).

[0106] The inventors used 3DAP to observe the microscopic segregation and dispersion of each element in samples prepared by varying the composition and heat treatment conditions. Furthermore, magnetic properties were measured using VSM. The results showed a significant correlation between the difference in the concentration ratio of transition metals and quasi-metals in the micro-regions of the soft magnetic alloy and the magnetic properties of the soft magnetic alloy. Moreover, the observation conditions for 3DAP were the same as those described above.

[0107] The measurement range and grid settings for the sample in 3DAP are as described above. Furthermore, the inventors analyzed the atomic concentrations of the transition metals in each grid, namely the atomic concentrations of M, Z1, and Z2, using the atomic concentrations of M and Z1, M and Z2, and Z1 and Z2 respectively. Hereinafter, the determination coefficients for the atomic concentrations of M and Z1 will sometimes be denoted as R. 2 (M-Z1), the coefficients of determination of the atomic concentrations of M and Z2 are recorded as R. 2 (M-Z2), where the coefficients of determination for the atomic concentrations of Z1 and Z2 are denoted as R. 2 (Z1-Z2).

[0108] You can also use R 2 (M-Z1) is above 0.600 or R 2 (M-Z2) is above 0.600, and R can also be used. 2 (Z1-Z2) is less than 0.400. R 2 (M-Z1) and R 2 In (M-Z2), the side that is not greater than 0.600 can also be less than 0.500.

[0109] From other perspectives, it is also possible to R 2 (M-Z1) less than 0.500 or R 2 (M-Z2) is less than 0.500, and R can also be used. 2 (Z1-Z2) is less than 0.400. R 2 (M-Z1) and R 2In (M-Z2), the side that is not less than 0.500 can also be greater than 0.600.

[0110] In R 2 (M-Z1) or R 2 When (M-Z2) is less than 0.500, or R 2 (M-Z1) or R 2 When (M-Z2) is above 0.600, the coercivity Hc decreases. In addition, the saturation magnetic flux density Bs increases.

[0111] Additionally, in R 2 When (Z1-Z2) is small, the coercivity Hc becomes lower.

[0112] The inventors have discovered that by making the amorphous phase contained in a soft magnetic alloy non-uniform and controlling the local differences in the concentrations of M and Z, the saturation magnetic flux density Bs of the soft magnetic alloy becomes higher and the coercivity Hc becomes lower. Specifically, it was found that in R 2 (M-Z1) or R 2 (M-Z2) is above 0.600, and R 2 When (Z1-Z2) is less than 0.400, the saturation magnetic flux density Bs of the soft magnetic alloy increases, while the coercivity Hc decreases. Furthermore, it was found that in R… 2 (M-Z1) or R 2 (M-Z2) is less than 0.500, and R 2 When (Z1-Z2) is less than 0.400, the saturation magnetic flux density Bs of the soft magnetic alloy becomes higher and the coercivity Hc becomes lower.

[0113] Furthermore, for R 2 (M-Z1) and R 2 There are no particular restrictions on the upper and lower limits of (M-Z2). For example, it can be below 0.750. Alternatively, it can be above 0.308. Moreover, for R… 2 There is no particular restriction on the lower limit of (Z1-Z2). 2 (Z1-Z2) can be greater than 0.100 or greater than 0.203.

[0114] Furthermore, in the soft magnetic alloy of this embodiment, the composition of the Fe-M-Z system described above is based on the formula (Fe (1－(α+β)) X1 α X2 β ) (1－(a+b+c)) M1 a Z b Cr c express,

[0115] X1 is selected from one or more of Co and Ni.

[0116] X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, Cu, Bi, N, O, S, and rare earth elements.

[0117] M1 can also be one or more selected from Ta, V, Zr, Hf, Ti, Nb, Mo, and W.

[0118] Alternatively, it can be 0.030 ≤ a ≤ 0.140.

[0119] 0.030≤b≤0.275

[0120] 0.000≤c≤0.030

[0121] 0≤α(1-(a+b+c))≤0.400

[0122] β≥0

[0123] 0≤α+β≤0.50.

[0124] The content (a) of M1 can satisfy 0.050≤a≤0.140 or 0.070≤a≤0.090. Regardless of whether a is large or small, the coercivity Hc tends to increase and the saturation magnetic flux density Bs tends to decrease.

[0125] Regarding the inclusion of Ta in M1, it is particularly advantageous because the saturation flux density Bs tends to be higher and the coercivity Hc tends to be lower. Alternatively, it may contain more than 3 at% or more of Ta relative to the total M1, or it may contain more than 40 at% or more of Ta.

[0126] The Z content (b) can satisfy 0.050≤b≤0.200 or 0.050≤b≤0.160. Regardless of whether b is large or small, the coercivity Hc tends to increase. When b is large, the saturation flux density Bs tends to decrease more easily.

[0127] Z1 can be C, and Z2 can be P, B, or Si, or Z1 can be C, and Z2 can be P. The coercivity Hc tends to decrease. Furthermore, the content of Z2 relative to the content of Z, in terms of atomic ratio, can be 0.0375 or more and 1.00 or less, or 0.125 or more and 1.00 or less. When the content of Z2 relative to the content of Z is 0.125 or more and 1.00 or less, the coercivity Hc tends to decrease.

[0128] The Cr content (c) can also satisfy 0.000≤c≤0.010. When the Cr content is high, the coercivity Hc tends to be higher, and the saturation magnetic flux density Bs tends to be lower.

[0129] The Fe content (1-(a+b+c)) can be 0.585≤1-(a+b+c)≤0.930, 0.730≤1-(a+b+c)≤0.930, or 0.730≤1-(a+b+c)≤0.890. By setting 1-(a+b+c) within the above range, the amorphous formation ability of the soft magnetic alloy becomes higher, making it difficult to produce crystals with a grain size greater than 30nm during the manufacture of the soft magnetic alloy.

[0130] In addition, in the soft magnetic alloy of this embodiment, a portion of Fe can be replaced by X1 and / or X2.

[0131] X1 can be one or more selected from Co and Ni. When X1 is Ni, it has the effect of reducing the coercivity Hc; when it is Co, it easily increases the saturation magnetic flux density Bs. The type of X1 can be appropriately selected. It can also be α = 0, that is, it can also contain no X1. Alternatively, the total number of atoms in the composition can be set to 100 at%, and the number of X1 atoms can be 40 at% or less. That is, it can also satisfy 0 ≤ α{1-(a+b+c)} ≤ 0.400, or 0 ≤ α{1-(a+b+c)} ≤ 0.100. When the number of X1 atoms increases, the magnetostriction increases, and the coercivity Hc tends to increase.

[0132] X2 is selected from one or more elements chosen from Al, Mn, Ag, Zn, Sn, Cu, Bi, N, O, S, and rare earth elements. Furthermore, the content of X2 can also be β = 0. That is, X2 can be absent. Additionally, it is preferable to set the total number of atoms in the composition to 100 at%, and the number of X2 atoms to 3.0 at% or less. That is, it is preferable to satisfy 0 ≤ β{1-(a+b+c)} ≤ 0.030.

[0133] The range of substitutions for Fe with X1 and / or X2 can also be set to less than half of Fe in terms of atomic number. That is, it can also be set to 0 ≤ α + β ≤ 0.50.

[0134] Furthermore, the soft magnetic alloy of this embodiment may also contain elements other than those described above as unavoidable impurities. For example, each element may contain 0.1% by weight or less relative to 100% by weight of the soft magnetic alloy.

[0135] In addition, the soft magnetic alloy of this embodiment may also have a structure containing Fe-based nanocrystals.

[0136] Here, Fe-based nanocrystals are crystals with a particle size in the nanometer range and a bcc (body-centered cubic) crystalline structure of Fe. In this embodiment, Fe-based nanocrystals with an average particle size of 5–30 nm are preferably precipitated.

[0137] Furthermore, when the soft magnetic alloy composed of amorphous material is heat-treated, Fe-based nanocrystals are easily precipitated in the soft magnetic alloy. In other words, the soft magnetic alloy having the above composition and being composed of amorphous material can easily be used as the initial raw material for the soft magnetic alloy of this embodiment having a structure containing Fe-based nanocrystals.

[0138] Furthermore, the soft magnetic alloy before heat treatment can have a structure composed solely of amorphous material, or it can have a nanostructure with microcrystals present within the amorphous material. Moreover, the average particle size of the aforementioned microcrystals can also be 0.3–10 nm.

[0139] The following section explains the amorphization rate of soft magnetic alloys.

[0140] In the case where the soft magnetic alloy of this embodiment is a granular material as described later, the soft magnetic alloy with an amorphization rate X of 85% or more as shown in the following formula (1) has a structure composed of amorphous material, and the soft magnetic alloy with an amorphization rate X of less than 85% has a structure composed of crystal.

[0141] X=100-(Ic / (Ic+Ia)×100)…(1)

[0142] Ic: Integral intensity of crystalline scattering

[0143] Ia: Integral intensity of amorphous scattering

[0144] Regarding the amorphization rate X, the crystal structure of the soft magnetic alloy is analyzed by XRD, the phase is identified, and the peaks of the crystallized Fe or compound are read (Ic: integrated intensity of crystallization scattering, Ia: integrated intensity of amorphous scattering). The crystallization rate is calculated based on the peak intensity, and the amorphization rate X is calculated using the above formula (1). The calculation method is explained in more detail below.

[0145] The soft magnetic alloy of this embodiment was subjected to XRD crystal structure analysis, and the results were obtained. Figure 6 The graph shown is used. The contour is fitted using the Lorentz function of equation (2) below to obtain... Figure 7 The crystalline composition pattern α shown represents the integral intensity of crystalline scattering. c α represents the amorphous composition pattern representing the integral intensity of amorphous scattering. a and the pattern α that combines them c+a The amorphization rate X is obtained by using equation (1) above, based on the crystalline and amorphous scattering integral intensities of the obtained pattern. Furthermore, the measurement range is set to the range where the diffraction angle 2θ = 30° to 60° from the amorphous halo can be confirmed. Within this range, the error between the measured integral intensity of the XRD and the integral intensity calculated using the Lorentz function is kept within 1%.

[0146]

[0147] h: Peak height

[0148] u: Peak position

[0149] w: half-width

[0150] b: Background height

[0151] In the case where the soft magnetic alloy in this embodiment is a thin film (described later), XRD crystal structure analysis can also be performed using In-Plane diffraction. In this case, the same graph as when performing XRD crystal structure analysis on a granular material using conventional methods is obtained. By performing the same analysis on the graph of the thin film as on the graph of the granular material, the amorphization rate X can be calculated.

[0152] (2) Composition of the Fe-M-C system and M / C

[0153] The soft magnetic alloy in this embodiment can also be a soft magnetic alloy with an Fe-M-C system composition.

[0154] The Fe-M-C system is composed primarily of Fe, M, and C. Additionally, Co and / or Ni can be used to replace a portion of the Fe. Specifically, Co and / or Ni can replace up to 40 at% of the total Fe content. Furthermore, the combined content of Fe, Co, and Ni can be 70 at% or more relative to the total soft magnetic alloy content. Moreover, when the soft magnetic alloy has an Fe-M-C system composition, the content of elements other than Fe, Co, Ni, M, and C in the soft magnetic alloy is 25 at% or less relative to the total soft magnetic alloy content. Examples of elements other than Fe, Co, Ni, M, and C include P, B, Si, Ge, Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Cr, Bi, N, O, S, and rare earth elements.

[0155] M is a metallic element that can combine with C to form crystalline M-C compounds. Examples of M include one or more selected from Ta, V, Zr, Hf, Ti, Nb, Mo, and W. In the soft magnetic alloy of this embodiment, the content of M can be 3 at% or more, 3 at% or more but less than 14 at% or less, or 5 at% or more but less than 12 at% or less. Furthermore, in the soft magnetic alloy of this embodiment, it is particularly easy to increase the saturation magnetic flux density Bs and easily reduce the coercivity Hc, relative to the total content of Ta, and is therefore preferred. Alternatively, it is also possible to have 40 at% or more of Ta relative to the total content of M.

[0156] In the soft magnetic alloy of this embodiment, the C content can be 0.5 at% or more, or 4 at% or more.

[0157] The soft magnetic alloy of this embodiment does not exhibit any peaks of the M-C compound in the XRD chart. That is, it does not actually contain M-C compound crystals. "No peaks of the M-C compound in the XRD chart" means that, in the chart after background removal, the intensity of the M-C compound (200) peak is less than 5% relative to the intensity of the α-Fe (110) peak. It may also be less than 1%. The precision of quantitative analysis by XRD is typically around 1 to 5% or more relative error; therefore, it is appropriate to consider that it does not actually contain the crystals of this M-C compound.

[0158] The soft magnetic alloy of this embodiment contains M and C, but the M-C compound does not crystallize and therefore does not actually contain an M-C compound. Furthermore, it contains M and C as an amorphous material. That is, as... Figure 3 As shown, the soft magnetic alloy 1 of this embodiment contains an α-Fe phase 11 composed of crystals and an amorphous phase 13, but does not actually contain M-C compounds.

[0159] In contrast, such as Figure 4 and Figure 5 As shown, existing soft magnetic alloys contain an M-C compound phase 15 composed of M-C compounds. Figure 4 The soft magnetic alloy 101 shown contains amorphous phase 13 and Figure 5 The separate fabrication of the soft magnetic alloy 201, which does not contain the amorphous phase 13, can be achieved by primarily controlling the atomic ratio of M / C throughout the soft magnetic alloy. When the atomic ratio of M / C throughout the soft magnetic alloy is greater than 1.0, the soft magnetic alloy 101 tends to contain the amorphous phase 13. When the atomic ratio of M / C is less than or equal to 1.0, the soft magnetic alloy 201 tends to contain virtually only the α-Fe phase 11 and the M-C compound phase 15. Furthermore, in Figure 4 The soft magnetic alloy 101 shown and Figure 5 In the soft magnetic alloy 201 shown, Figure 5 The coercivity of the soft magnetic alloy 201 shown tends to decrease. Furthermore, by changing the heat treatment temperature, in addition to... Figure 4 and Figure 5 In addition to the microstructure shown, it can also become various other microstructures.

[0160] The soft magnetic alloy of this embodiment further comprises a first region having a total concentration of Fe, Co, and Ni of 85 at% or more, and a second region having a total concentration of Fe, Co, and Ni of 80 at% or less. The distinction between the first region, the second region, and the other regions is made using 3DAP. Furthermore, there are no particular limitations on the location for 3DAP measurement. It can be the surface of the soft magnetic alloy or a cut surface obtained by cutting the soft magnetic alloy.

[0161] The following is an example of a method for determining the atomic ratio of M / C using 3DAP. First, a cuboid or cube with sides at least 40 nm × 40 nm × 50 nm is used as the measurement range. By analyzing the measurement data obtained using software, this cuboid or cube (measurement range) is virtually divided into a grid of cubes with sides of 1 nm. That is, there are at least 80,000 grids, each containing compositional information, with a total of 40 × 40 × 50 = 80,000 grids. Furthermore, regarding the measurement range in this embodiment, there are no particular limitations on the shape of the measurement range, as long as there are at least 80,000 grids continuously present. Moreover, it is possible to statistically process and analyze multiple grids, each containing compositional information.

[0162] Grids with a combined Fe, Co, and Ni concentration of 85 at% or higher constitute the first region (first region grids). Grids with a combined Fe, Co, and Ni concentration of 80 at% or lower constitute the second region (second region grids). Furthermore, the first region is predominantly crystalline, while the second region is predominantly amorphous.

[0163] The above-described 3DAP measurements are performed at least twice, preferably at least three times, with different measurement ranges set. Furthermore, the volume ratio of the first region to the soft magnetic alloy is calculated by averaging the volume ratios of the first region obtained in each measurement. The volume ratio of the second region is calculated similarly.

[0164] Furthermore, there are no particular restrictions on the volume percentage of the first region and the second region in the soft magnetic alloy. The volume percentage of the first region can be 5 vol% or more and 90 vol% or less. The volume percentage of the second region can be 10 vol% or more and 90 vol% or less. The volume percentage of the first region in the soft magnetic alloy can also be the same as the number of first region meshes contained in the aforementioned 80,000 or more meshes. The volume percentage of the second region in the soft magnetic alloy can also be the same as the number of second region meshes contained in the aforementioned 80,000 or more meshes.

[0165] 3DAP measurements were performed on the soft magnetic alloy of this embodiment, which contains neither Co nor Ni and has only Ta as M. The results of the elemental mapping images are as follows: Figures 8-10 It can be seen that the higher the Fe content, the lower the Ta and C content.

[0166] Furthermore, in each second-region grid, the atomic concentration of M divided by the atomic concentration of C, i.e., the M / C ratio, is calculated, and the average value is greater than 1.0.

[0167] Based on the above, soft magnetic alloys with an Fe-M-C system composition do not actually contain crystallized M-C compounds, and the average value of the M / C ratio (the ratio of the atomic concentration of M to the atomic concentration of C in the second region) is greater than 1.0. Compared to soft magnetic alloys with the same composition but containing crystallized M-C compounds, and soft magnetic alloys with the same composition but an average M / C ratio of 1.0 or less in the second region, soft magnetic alloys with the above characteristics tend to have higher saturation magnetic flux density Bs and lower coercivity Hc. The average M / C ratio in the second region can be 1.2 or higher and 2.8 or lower, or 1.2 or higher and 2.5 or lower.

[0168] Furthermore, in the soft magnetic alloy of this embodiment, the composition of the Fe-M-C system described above can also be expressed by the formula (Fe (1－(α+β)) X1 α X2 β ) (1－(a+b3+b4+c)) M a C b3 X3 b4 Cr c express,

[0169] X1 can also be one or more selected from Co and Ni.

[0170] X2 can also be one or more elements selected from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, S, and rare earth elements.

[0171] M can also be one or more selected from Ta, V, Zr, Hf, Ti, Nb, Mo, and W.

[0172] X3 can also be one or more selected from P, B, Si, and Ge.

[0173] Alternatively, it can be 0.030 ≤ a ≤ 0.140.

[0174] 0.005≤b3≤0.200

[0175] 0.000≤b4≤0.180

[0176] 0.000≤c≤0.030

[0177] 0≤α(1-(a+b3+b4+c))≤0.400

[0178] β≥0

[0179] 0≤α+β≤0.50.

[0180] M is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W. M is preferably selected from one or more of Ta, V, and W, and more preferably Ta.

[0181] The content of M (a) can also satisfy 0.030≤a≤0.140. The content of M (a) can also be 0.050≤a≤0.140. Regardless of whether a is large or small, the coercivity Hc tends to increase. When a is large, the coercivity Hc tends to increase, and consequently, the saturation magnetic flux density Bs tends to decrease. When a is small, the coercivity Hc tends to increase.

[0182] The C content (b3) can also satisfy 0.005 ≤ b3 ≤ 0.200. Alternatively, it can be 0.040 ≤ b3 ≤ 0.120 or 0.040 ≤ b3 ≤ 0.100. When b3 is small, the coercivity Hc tends to be high. When b3 is large, the saturation magnetic flux density Bs tends to be low, and the coercivity Hc tends to be high.

[0183] X3 can be selected from one or more of P, B, Si, and Ge. It can also be selected from one or more of P, B, and Si.

[0184] The content of X3 (b4) can also satisfy 0.000≤b4≤0.180. It can be 0.003≤b4≤0.180 or 0.010≤b4≤0.080. When b4 is small, the amorphous material forming ability tends to decrease, and the coercivity Hc tends to increase. When b4 is large, the saturation magnetic flux density Bs tends to decrease, and the coercivity Hc tends to increase.

[0185] Furthermore, the total content of C and X3 (b3+b4) can also be 0.080≤b3+b4≤0.130. When b3+b4 is within the above range, the coercivity Hc tends to increase.

[0186] The Cr content (c) can satisfy 0.000≤c≤0.030, or 0.003≤c≤0.030. The larger the c, the more it tends to improve antioxidant properties, but the larger the c, the lower the saturation magnetic flux density Bs tends to be.

[0187] The Fe content (1-(a+b3+b4+c)) can be 0.640≤1-(a+b3+b4+c)≤0.930 or 0.730≤1-(a+b3+b4+c)≤0.930. By setting 1-(a+b3+b4+c) within the above range, the amorphous formation ability of the soft magnetic alloy is increased, making it difficult to produce crystals with a grain size greater than 30nm during the manufacture of the soft magnetic alloy.

[0188] In addition, in the soft magnetic alloy of this embodiment, a portion of Fe can be replaced by X1 and / or X2.

[0189] X1 can be one or more selected from Co and Ni. When X1 is Ni, it has the effect of reducing the coercivity Hc; when it is Co, it easily increases the saturation magnetic flux density Bs after heat treatment. The type of X1 can be appropriately selected. It can also be α = 0, that is, it can also contain no X1. Alternatively, the total number of atoms in the composition can be set to 100 at%, and the number of X1 atoms can be 40 at% or less. That is, it can also satisfy 0 ≤ α{1-(a+b3+b4+c)} ≤ 0.400, or 0 ≤ α{1-(a+b3+b4+c)} ≤ 0.100. When the number of X1 atoms increases, the magnetostriction increases, and the coercivity Hc tends to increase.

[0190] X2 is selected from one or more elements chosen from Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, S, and rare earth elements. Furthermore, the content of X2 can also be β = 0. That is, X2 can be absent. Additionally, it is preferable to set the total number of atoms in the composition to 100 at%, and the number of X2 atoms to 3.0 at% or less. That is, it is preferable to satisfy 0 ≤ β{1-(a+b3+b4+c)} ≤ 0.030.

[0191] The range of substitutions for Fe with X1 and / or X2 can also be set to less than half of Fe in terms of atomic number. That is, it can also be set to 0 ≤ α + β ≤ 0.50.

[0192] Furthermore, the soft magnetic alloy of this embodiment may also contain elements other than those described above as unavoidable impurities. For example, it may contain 0.1% or less of each element relative to 100% by weight of the soft magnetic alloy.

[0193] In addition, the soft magnetic alloy of this embodiment may also have a structure containing Fe-based nanocrystals.

[0194] Here, Fe-based nanocrystals are crystals with a particle size in the nanometer range and a bcc (body-centered cubic) crystalline structure of Fe. In this embodiment, it is preferable to precipitate Fe-based nanocrystals with an average particle size of 5–30 nm.

[0195] Furthermore, when the soft magnetic alloy composed of amorphous material is heat-treated, Fe-based nanocrystals are easily precipitated in the soft magnetic alloy. In other words, the soft magnetic alloy having the above composition and being composed of amorphous material is readily used as the initial raw material for the soft magnetic alloy of this embodiment having a structure containing Fe-based nanocrystals.

[0196] Furthermore, the soft magnetic alloy before heat treatment can also have a structure composed solely of amorphous material, or it can have a nanostructure with microcrystals present within the amorphous material. Moreover, the average particle size of the aforementioned microcrystals can also be 0.3–10 nm.

[0197] The following section explains the amorphization rate of soft magnetic alloys.

[0198] In the case where the soft magnetic alloy of this embodiment is a granular material as described later, the soft magnetic alloy with an amorphization rate X of 85% or more as shown in the following formula (1) has a structure composed of amorphous material, and the soft magnetic alloy with an amorphization rate X of less than 85% has a structure composed of crystal.

[0199] X=100-(Ic / (Ic+Ia)×100)…(1)

[0200] Ic: Integral intensity of crystalline scattering

[0201] Ia: Integral intensity of amorphous scattering

[0202] Regarding the amorphization rate X, the crystal structure of the soft magnetic alloy is analyzed by XRD, the phase is identified, and the peaks of crystallized Fe or compounds (Ic: integrated intensity of crystallization scattering, Ia: integrated intensity of amorphous scattering) are read. The crystallization rate is calculated based on the peak intensity using the above formula (1). The calculation method is explained in more detail below.

[0203] The soft magnetic alloy of this embodiment was subjected to XRD crystal structure analysis, and the results were obtained. Figure 6 The graph shown is used. The contour is fitted using the Lorentz function of equation (2) below to obtain... Figure 7 The crystalline composition pattern α shown represents the integral intensity of crystalline scattering. c α represents the amorphous composition pattern representing the integral intensity of amorphous scattering. a and the pattern α that combines them c+a The amorphization rate X is obtained by using Equation (1) above, based on the crystalline scattering integral intensity and the amorphous scattering integral intensity of the obtained pattern. Furthermore, the measurement range is set to the range where the diffraction angle 2θ = 30° to 60° from the amorphous halo can be confirmed. Within this range, the error between the measured integral intensity using XRD and the integral intensity calculated using the Lorentz function is within 1%.

[0204]

[0205] h: Peak height

[0206] u: Peak position

[0207] w: half-width

[0208] b: Background height

[0209] In the case where the soft magnetic alloy in this embodiment is a thin film (described later), crystal structure analysis can also be performed using In-Plane XRD. In this case, the same graph as that obtained when performing XRD analysis on a granular material using conventional methods is obtained. By performing the same analysis on the graph of the thin film as on the graph of the granular material, the amorphization rate X can be calculated.

[0210] There are no particular limitations on the shape of the soft magnetic alloy in this embodiment. For example, it can be in the form of a strip, powder, or thin film.

[0211] In the following description, both strip-shaped and powder-shaped soft magnetic alloys are sometimes referred to as granules. Furthermore, thin-film soft magnetic alloys are sometimes simply referred to as soft magnetic alloy films or films, strip-shaped soft magnetic alloys are sometimes simply referred to as soft magnetic alloy strips or strips, and powder-shaped soft magnetic alloys are sometimes simply referred to as soft magnetic alloy powders or powders.

[0212] The manufacturing method of the soft magnetic alloy of this embodiment will be described below, but the manufacturing method of the soft magnetic alloy of this embodiment is not limited to the method described below.

[0213] As an example of the method for manufacturing soft magnetic alloy strips according to this embodiment, there is a method for manufacturing soft magnetic alloy strips by a single-roll method. Alternatively, the strip can also be a continuous strip.

[0214] In the single-roller process, firstly, pure metals of each metallic element contained in the final soft magnetic alloy strip are prepared and weighed to achieve the same composition as the final soft magnetic alloy strip. Then, the pure metals of each metallic element are dissolved and mixed to create a master alloy. Furthermore, the method for dissolving the pure metals is arbitrary; for example, it may involve dissolving them by high-frequency heating after evacuating the chamber. Additionally, the master alloy and the final soft magnetic alloy strip typically have the same composition.

[0215] Next, the prepared master alloy is heated to melt it, resulting in molten metal (liquid). There are no particular restrictions on the temperature of the molten metal. For example, it can be set to 1200–1500°C.

[0216] In this embodiment, there are no particular limitations on the temperature of the roller. For example, it can be set to room temperature to 90°C. Furthermore, there are no particular limitations on the pressure difference (injection pressure) between the chamber and the nozzle. For example, it can be set to 20 to 80 kPa.

[0217] In the single-roll method, the thickness of the resulting strip can be adjusted by primarily adjusting the rotational speed of the roller. The thickness can also be adjusted by changing factors such as the nozzle-roller spacing and the temperature of the molten metal. There are no particular limitations on the strip thickness; for example, it can range from 10 to 80 μm.

[0218] The soft magnetic alloy ribbon before heat treatment, as described later, does not contain crystals with a particle size greater than 30 nm. Furthermore, the soft magnetic alloy ribbon before heat treatment can have a structure composed solely of amorphous material, or it can have a nanostructure with microcrystals present within the amorphous material. Moreover, the amorphization rate X can be 85% or higher.

[0219] Furthermore, there are no particular limitations on the method for confirming whether crystals with a diameter greater than 30 nm are present in the thin strip. For example, the presence or absence of crystals with a diameter greater than 30 nm can be confirmed by conventional X-ray diffraction.

[0220] Furthermore, there are no particular limitations on the methods for observing the presence or absence of microcrystals and their average particle size. For example, confined-field diffraction images, nanobeam diffraction images, bright-field images, or high-resolution images can be obtained by using a transmission electron microscope on samples thinned by ion milling. When using confined-field diffraction images or nanobeam diffraction images, in the diffraction pattern, ring-shaped diffraction patterns are formed in the case of amorphous materials, while diffraction spots caused by crystalline structures are formed in the case of non-amorphous materials. Additionally, when using bright-field images or high-resolution images, visual inspection at magnification of 1.00 × 10⁻⁶ is also possible. 5 ~3.00×10 5 By observing the sample multiple times, it is possible to observe the presence or absence of the initial microcrystals and their average particle size.

[0221] The following describes a method for manufacturing the soft magnetic alloy strip of this embodiment by heat treatment of the soft magnetic alloy strip.

[0222] To manufacture soft magnetic alloy strips with all determinant coefficients within a specified range, it is particularly important to control the heat treatment conditions. Preferably, the heating rate during heat treatment is set to a rapid rate such as 100°C / min or higher, the holding temperature after heating is set to 450°C or higher and 650°C or lower, and the holding time is set to a short time such as 0.1 min or higher and 5 min or lower. Furthermore, the cooling rate after holding is set to 50°C / min or higher and 1000°C / min or lower. By controlling these conditions, it is easy to make the determinant coefficients for the atomic concentrations of Fe and at least one metalloid element 0.700 or higher. The determinant coefficients for the atomic concentrations of Fe and at least one metalloid element (M) are also easily made to be 0.700 or higher. Moreover, it is possible to manufacture soft magnetic alloy strips where local differences in M ​​and Z exist within a specific range and each determinant coefficient is within a specified range.

[0223] There are no particular restrictions on the atmosphere during heat treatment. It can be carried out in a reactive atmosphere such as the atmosphere, or in an inactive atmosphere such as Ar, or in a vacuum.

[0224] Furthermore, there are no particular limitations on the method for calculating the average grain size when Fe-based nanocrystals are included in the soft magnetic alloy ribbons obtained through heat treatment. For example, it can be calculated by observation using a transmission electron microscope. Additionally, there are no particular limitations on the method for confirming that the crystal structure is a bcc (body-centered cubic) lattice structure. For example, it can be confirmed using X-ray diffraction.

[0225] As an example of the method for manufacturing soft magnetic alloy powder in this embodiment, there is a method for manufacturing soft magnetic alloy powder using a gas atomization method.

[0226] In the gas atomization method, firstly, pure metals of each metallic element contained in the final soft magnetic alloy are prepared and weighed in a manner that results in the same composition as the final soft magnetic alloy. Then, the pure metals of each metallic element are dissolved and mixed to prepare a master alloy. Furthermore, there are no particular limitations on the method for dissolving the pure metals; for example, a method involving dissolution by high-frequency heating after evacuating a chamber is employed. Moreover, the master alloy and the final soft magnetic alloy typically have the same composition.

[0227] Next, the prepared master alloy is heated to melt it, resulting in molten metal (liquid). There are no particular limitations on the temperature of the molten metal; for example, it can be set to 1200–1500°C. Then, the molten alloy is sprayed through a gas atomizing device to produce powder.

[0228] By controlling the spraying conditions at this time, the particle size of the soft magnetic alloy powder can be appropriately controlled.

[0229] There are no particular limitations on the particle size of soft magnetic alloy powders. For example, D50 can be 1–150 μm. Furthermore, when the soft magnetic alloy powder has a structure composed of Fe-based nanocrystals, each particle typically contains multiple Fe-based nanocrystals. Therefore, the particle size of the aforementioned soft magnetic alloy powder differs from the crystal size of the Fe-based nanocrystals.

[0230] Appropriate spraying conditions vary depending on the composition of the molten metal and the target particle size. For example, the nozzle diameter is 0.5 to 3 mm, the molten metal discharge rate is less than 1.5 kg / min, and the air pressure is 5 to 10 MPa.

[0231] The above method yields soft magnetic alloy powder before heat treatment. To appropriately control the grain size, it is preferable that the soft magnetic alloy powder has an amorphous structure at this point.

[0232] The following describes a method for manufacturing the soft magnetic alloy powder of this embodiment by heat treatment of soft magnetic alloy powder.

[0233] In order to manufacture with Figure 3 The microstructured soft magnetic alloy powder shown, specifically the soft magnetic alloy powder containing α-Fe phase 11 (composed of crystals) and amorphous phase 13, but not M-Z compounds, requires particularly controlled heat treatment conditions. Preferably, the heating rate during heat treatment is set to a fast rate such as 100°C / min or higher, the holding temperature after heating is set to 450°C or higher and 650°C or lower, and the holding time is set to a short time such as 0.1 min or higher and 3 min or lower. Furthermore, the cooling rate after holding is set to 50°C / min or higher and 1000°C / min or lower. By controlling these conditions, it is easy to make the coefficients of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element 0.700 or higher. The coefficients of determination for the atomic concentration of Fe and the atomic concentration of at least one M element are also easily made to be 0.700 or higher. Moreover, it is possible to manufacture soft magnetic alloy ribbons in which local differences in M ​​and Z exist within a specific range and each coefficient of determination is within a specified range.

[0234] There are no particular restrictions on the atmosphere during heat treatment. It can be carried out in a reactive atmosphere such as the atmosphere, or in an inactive atmosphere such as N2 or Ar, or in a vacuum.

[0235] There are no particular restrictions on the method for forming a thin film. For example, thin films can be formed by sputtering or vapor deposition. The following describes the case of forming a thin film by sputtering.

[0236] Regarding film formation, multiple targets can be used for simultaneous film formation via multi-element sputtering, or film formation can be performed via single-element sputtering while appropriately changing the target. Simultaneous film formation via multi-element sputtering facilitates the production of thin films that reproduce the crystalline state of the dispersed material, and is therefore preferred.

[0237] There are no particular restrictions on the substrate temperature during film formation. For example, it can be set to 25℃~350℃.

[0238] There are no particular restrictions on the type of substrate. For example, thermally oxidized silicon substrates, silicon substrates, glass substrates, ceramic substrates, and resin substrates can be used. Examples of ceramic substrates include barium titanate substrates and ALTIC substrates. Additionally, proper cleaning can be performed before sputtering.

[0239] There are no particular limitations on the film thickness. For example, it can be set to 50 nm to 50 μm. Furthermore, it can be a multilayer film consisting of alternating layers of thin films and films composed of insulating materials and / or high-resistivity materials. There are no particular limitations on the types of insulating and / or high-resistivity materials; examples include SiO2, Al2O3, and AlN. Additionally, the resistivity of the insulating and / or high-resistivity materials should be 1000 μΩ·cm or higher.

[0240] The following describes a method for manufacturing the soft magnetic alloy thin film of this embodiment by heat treatment of the soft magnetic alloy thin film.

[0241] In order to manufacture with Figure 3 The microstructured soft magnetic alloy thin film shown, namely a soft magnetic alloy thin film containing a crystalline α-Fe phase 11 and an amorphous phase 13 but not M-Z compounds, requires particularly controlled heat treatment conditions. Preferably, the heating rate during heat treatment is set to a fast rate such as 100°C / min or higher, the holding temperature after heating is set to 450°C or higher and 650°C or lower, and the holding time is set to a short time such as 0.1 min or higher and 5 min or lower. Furthermore, the cooling rate after holding is set to 50°C / min or higher and 1000°C / min or lower. By controlling these conditions, it is easy to make the coefficients of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element 0.700 or higher. The coefficients of determination for the atomic concentration of Fe and the atomic concentration of at least one M element are also easily made to be 0.700 or higher. Moreover, it is possible to manufacture soft magnetic alloy thin strips in which local differences in M ​​and Z exist within a specific range and each coefficient of determination is within a specified range.

[0242] There are no particular restrictions on the atmosphere during heat treatment. It can be carried out in a reactive atmosphere such as the atmosphere, or in an inactive atmosphere such as N2 or Ar, or in a vacuum.

[0243] There are no particular limitations on the applications of the soft magnetic alloy described in this embodiment. For example, in the case of soft magnetic alloy strips, cores, inductors, transformers, and motors can be used. In the case of soft magnetic alloy powder, pressed powder cores can be used. In particular, it can be appropriately used as pressed powder cores for inductors, especially for power inductors. In addition, it can also be applied to magnetic components that use soft magnetic alloy thin films, such as thin film inductors and magnetic heads.

[0244] Furthermore, the soft magnetic alloy of this embodiment can be used as, for example, a soft magnetic alloy having a higher saturation magnetic flux density Bs than the well-known Fe-Si-B-Nb-Cu soft magnetic alloys. Additionally, the soft magnetic alloy of this embodiment can be used as a soft magnetic alloy having a lower coercivity Hc than the Fe-Nb-B soft magnetic alloys, wherein the Fe-Nb-B soft magnetic alloys are known to have a higher saturation magnetic flux density Bs than the aforementioned Fe-Si-B-Nb-Cu soft magnetic alloys. Moreover, the soft magnetic alloy of this embodiment can easily be configured to have a higher saturation magnetic flux density Bs than the Fe-Nb-B soft magnetic alloys. That is, magnetic components using the soft magnetic alloy of this embodiment, in the case of inductors, can easily achieve improved DC overlap characteristics, reduced core losses, and increased inductance. In other words, by using the soft magnetic alloy of this embodiment, it is easy to obtain magnetic components that are smaller, consume less power, and are more efficient compared to those using well-known Fe-Si-B-Nb-Cu or Fe-Nb-B soft magnetic alloys. Furthermore, when using magnetic components such as transformers that employ the soft magnetic alloy of this embodiment in power supply circuits, it is easy to achieve improved power efficiency by reducing energy loss.

[0245] Example

[0246] The present invention will now be described with reference to more detailed embodiments, but the present invention is not limited to these embodiments.

[0247] (Experimental Example 1)

[0248] In Experiment 1, the soft magnetic alloy thin films described in Tables 1A and 1B were fabricated. The method for manufacturing the soft magnetic alloy thin film shape will be described below. Furthermore, some of the tables described below have blank columns. This indicates that the values ​​entered into the blank columns have not been calculated.

[0249] First, thin films with the compositions described in Tables 1A and 1B were formed by sputtering. For film formation, magnetron sputtering (ES340 manufactured by Eicoh Co., Ltd.) was used. Furthermore, film formation was performed simultaneously using multiple targets via multi-element sputtering.

[0250] In this experimental example, the substrate temperature during film deposition was set to 250°C to deposit multiple thin films. The substrate was a thermally oxidized silicon substrate cut into 6mm × 6mm pieces and ultrasonically cleaned using solvents in the order of water, acetone, and IPA. The film thickness was set to 100nm. The gas flow rate within the chamber was set to 20 sccm, and the gas pressure within the chamber was set to 0.4 Pa.

[0251] For each thin film before heat treatment (described later), the amorphization rate X was measured using XRD. It was confirmed that the amorphization rate X of the thin films before heat treatment was above 85% in all the examples and comparative examples described later. Furthermore, the presence or absence of microcrystals was confirmed by observing confined-field diffraction patterns using transmission electron microscopy and by observing bright-field patterns at 300,000x magnification. As a result, it was confirmed that the thin films before heat treatment did not contain microcrystals in all the examples and comparative examples described later.

[0252] Next, the thin films were subjected to heat treatment. The heat treatment was performed by heating to a specified holding temperature at a specified heating rate and holding at that temperature for a specified holding time. The heating rate, holding temperature, holding time, and subsequent cooling rate for each thin film are shown in Tables 1A and 1B. The atmosphere during heat treatment was set to a vacuum.

[0253] The coercivity Hc and saturation magnetic flux density Bs of each heat-treated film were measured. A vibrating sample magnetometer (VSM) was used to measure the coercivity Hc and saturation magnetic flux density Bs under a maximum applied magnetic field of 1000 Oe. Furthermore, the Bs and Hc of the film varied depending on the composition; however, for Bs, values ​​above 1.40 T were considered good, and values ​​above 1.50 T were considered even better. For Hc, values ​​below 10.0 Oe were considered good, and values ​​below 5.0 Oe were considered even better.

[0254] For the heat-treated films, XRD was used to confirm the presence or absence of α-Fe and M-Z compounds. Specifically, the presence or absence of α-Fe peaks and M-Z compound peaks was investigated in the XRD-obtained graphs. In all the examples described in Tables 1A and 1B, α-Fe peaks were present in the XRD-obtained graphs, but no M-Z compound peaks were observed.

[0255] For the heat-treated thin film, 3DAP was used to determine the coefficients of determination. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, this cuboid (measurement range) was virtually divided into 10,000 continuous cubic grids of 2 nm × 2 nm × 2 nm. Statistical processing and analysis were performed on the 10,000 grids, each containing compositional information, to calculate the concentration of each element. Then, the coefficients of determination R were derived.2 (Fe-Z1), R 2 (Fe-Z2) and R 2 (Fe-M). Table 1A only records R. 2 (Fe-C). In all the comparative examples listed in Table 1A, it was confirmed that not only R 2 (Fe-C), and the coefficient of determination for metalloids other than Fe and C is also less than 0.700.

[0256] Furthermore, in all the examples and comparative examples recorded in Table 1A, the average M / C value was measured in the region (second region) where the combined concentration of Fe, Co, and Ni was 80 at% or less. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, the cuboid (measurement range) was virtually divided into 80,000 grids of continuous 1 nm × 1 nm × 1 nm cube shapes. The 80,000 grids, each with composition information, were statistically processed and analyzed to calculate the concentration of each element in each grid. Then, grids with a combined concentration of Fe, Co, and Ni of 80 at% or less were selected from the 80,000 grids. The M / C of the selected grids was calculated and averaged to obtain the average M / C value. The results are shown in Table 1A. In addition, when a portion of the measurement results was mapped onto a plane, the average M / C value was obtained. Figures 8-10 The mapped image shown.

[0257] Furthermore, in the soft magnetic alloys (thin films, ribbons, powders) of the various experimental examples shown below, unless otherwise specified, a first region containing a total concentration of Fe, Co, and Ni of 85 at% or more was identified by 3DAP. Specifically, a grid containing a total concentration of Fe, Co, and Ni of 85 at% or more was identified within the aforementioned 1 nm × 1 nm × 1 nm grid of 80,000 grids. Moreover, for the 3DAP measurement, each sample was subjected to three trials. Then, in the soft magnetic alloys (thin films, ribbons, powders) of the various experimental examples shown below, unless otherwise specified, the first region was identified as having a volume percentage of 5 vol% or more and 90 vol% or less in the soft magnetic alloy, and the second region was identified as having a volume percentage of 10 vol% or more and 90 vol% or less in the soft magnetic alloy.

[0258] In the experimental examples shown below, unless otherwise specified, α-Fe and amorphous substances were mixed in the heat-treated soft magnetic alloys (thin films, strips, powders). Furthermore, M-C compounds were not present. Moreover, observations using XRD and transmission electron microscopy confirmed that the α-Fe was Fe-based nanocrystals with an average particle size of 5–30 nm and a bcc crystalline structure.

[0259] In addition, in the experimental examples shown below, unless otherwise specified, the composition of the soft magnetic alloys (thin films, strips, powders) remained unchanged before and after heat treatment, as confirmed by ICP analysis.

[0260] [Table 1A]

[0261]

[0262] [Table 1B]

[0263]

[0264] According to Table 1A, the coefficients of determination for each embodiment where the heating rate was sufficiently fast, the holding temperature was sufficiently low, the holding time was sufficiently short, and the cooling rate was sufficiently fast were all within the specified range. Furthermore, the average M / C ratio in the second region was greater than 1.0. In contrast, in the comparative examples where the heating rate was too slow, the holding temperature was too high, the holding time was too long, and the cooling rate was too slow, the coefficients of determination for Fe and each of the metalloid elements were not greater than 0.700. Moreover, in the sample numbers 14-16 of Table 1A, which served as comparative examples, peaks of the M-C compound (TaC) were present in the XRD graphs. Furthermore, the embodiments exhibited good magnetic properties, but the coercivity of the comparative examples was higher. Additionally, the saturation magnetic flux density of some comparative examples was also lower.

[0265] According to Table 1B, under identical heat treatment conditions, the coefficient of determination varies depending on the composition. Furthermore, the coefficient of determination R... 2 (Fe-Z1), R 2 Examples in which at least one (Fe-Z2) is 0.700 or higher exhibit good properties. Furthermore, the coefficient of determination R... 2 Examples where (Fe-M) is also 0.700 or higher, sample numbers 18-21 and R 2 Compared to samples 25 and 26, where (Fe-M) is less than 0.700, better Bs were obtained. In contrast, the coefficient of determination R… 2 (Fe-Z1), R 2 In comparative examples where (Fe-Z2) values ​​were all less than 0.700, Bs and / or Hc were unfavorable. Furthermore, in sample number 24, peaks of the M-C compound were observed in the XRD plot.

[0266] (Experimental Example 2)

[0267] In Experiment 2, the heat treatment conditions were fixed at a heating rate of 100 °C / min, a holding temperature of 500 °C, a holding time of 1 min, and a cooling rate of 50 °C / min, resulting in a film with altered composition. The results are shown in Tables 2 to 6. In all the samples recorded in Tables 2 to 6, the XRD patterns showed peaks for α-Fe but not for M-Z compounds. Furthermore, in Tables 3 and 4, b1, b2, and b were all rounded to the fourth decimal place; therefore, b1+b2 and b are sometimes inconsistent.

[0268] The coefficients of determination (R0) of the heat-treated thin film were determined using 3DAP. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, the cuboid (measurement range) was virtually divided into 10,000 consecutive cubic grids of 2 nm × 2 nm × 2 nm. By statistically processing and analyzing the 10,000 grids, each containing compositional information, the concentration of each element in each grid was calculated. Then, the coefficients of determination (R0) were derived. 2 (Fe-Z1), R 2 (Fe-Z2), R 2 (Fe-M), R 2 (M-Z1), R 2 (M-Z2) and R 2 (Z1-Z2). In the following examples, all deterministic coefficients R 2 (Fe-Z1), R 2 At least one of (Fe-Z2) is greater than 0.700, and the coefficient of determination R 2 (Fe-M) is also above 0.700. In contrast, in the following comparative examples, the coefficient of determination R... 2 (Fe-Z1), R 2 Both (Fe-Z2) values ​​are less than 0.700.

[0269] Furthermore, the average M / C value was measured in the region (second region) where the combined concentration of Fe, Co, and Ni was below 80 at%. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, the cuboid (measurement range) was virtually divided into 80,000 continuous cubic grids of 1 nm × 1 nm × 1 nm. By statistically processing and analyzing the 80,000 grids, each containing compositional information, the concentration of each element in each grid was calculated. Then, grids with a combined concentration of Fe, Co, and Ni below 80 at% were selected from the 80,000 grids. The M / C value of the selected grids was calculated separately and then averaged to obtain the average M / C value. The results are shown in Tables 2 to 6. In addition, when a portion of the measurement results was mapped onto a plane, the following was obtained: Figures 8-10 The mapped image shown.

[0270] [Table 2]

[0271]

[0272] [Table 3]

[0273]

[0274] [Table 4]

[0275]

[0276] [Table 5A]

[0277]

[0278] [Table 5B]

[0279]

[0280] [Table 6]

[0281]

[0282] Table 2 shows the results for each sample for which the content (a) of Ta was changed for sample number 18 in Table 1B. As mentioned above, the coefficient of determination R... 2 (Fe-Z1), R 2 In embodiments where at least one of (Fe-Z2) is 0.700 or higher, Bs and Hc are favorable. In particular, in embodiments satisfying 0.070≤a≤0.090, Hc is reduced to 5.00e or lower compared to embodiments not satisfying 0.070≤a≤0.090.

[0283] Table 3 shows the results for each sample in Table 1B where the total content of C (b1) and the content of P (b2) (b1 + b2 = b) was fixed at 0.080, and b and c were varied. As mentioned above, the coefficient of determination R... 2 (Fe-Z1), R 2 In the embodiments where at least one of (Fe-Z2) is 0.700 or more, Bs and Hc are favorable. Furthermore, in sample numbers 18, 34-36 of Table 3, Z1 is C and Z2 is P; in sample numbers 37 and 38, Z1 is P and Z2 is C. In particular, in embodiments where Z1 is C, Z2 is P, and the Z2 content relative to the Z content is 0.125 or more and 1.00 or less in atomic ratio, compared to embodiments where Z1 is P, Z2 is C, and the Z2 content relative to the Z content is less than 0.125, Hc is reduced to 5.0 Oe or less.

[0284] Table 4 shows the results for each sample (sample number 18) in Table 1B with variations in the contents of C and P. As mentioned above, the coefficient of determination R... 2 (Fe-Z1), R 2 In embodiments where at least one of (Fe-Z2) is 0.700 or higher, Bs and Hc are favorable. In particular, in embodiments satisfying 0.050≤b≤0.160, Hc is reduced to 5.0Oe or lower compared to embodiments not satisfying 0.050≤b≤0.160.

[0285] Tables 5A and 5B show the results for each sample for which the types and contents of M1, Z1, and Z2 were changed for sample number 18 in Table 1B. As mentioned above, the coefficient of determination R... 2 (Fe-Z1), R 2 In each embodiment where at least one of (Fe-Z2) is 0.700 or higher, Bs and Hc are preferred.

[0286] Table 6 shows the results for each sample (sample number 18) where a portion of Fe was replaced by X1 or X2, and the results for each sample containing Cr. As mentioned above, the determination coefficient R... 2 (Fe-Z1), R 2 In each embodiment where at least one of (Fe-Z2) is 0.700 or higher, Bs and Hc are preferred.

[0287] (Experimental Example 3)

[0288] In Experimental Example 3, a soft magnetic alloy strip with the composition of the Fe-M-Z system as described in Table 7 was fabricated. The method for manufacturing the soft magnetic alloy strip will be explained below.

[0289] First, pure metal materials were weighed to obtain the master alloy with the composition shown in Table 7. Then, after evacuating the chamber, the master alloy was melted by high-frequency heating.

[0290] Then, the prepared master alloy is heated to melt it, producing a molten metal at 1200°C. This metal is then sprayed onto a single-roller method, rotating at 15 m / sec, to create a thin strip. The roller is made of Cu. The roller temperature is set to 25°C, and the pressure difference (injection pressure) between the chamber and the nozzle is set to 40 kPa. Furthermore, the slit width of the nozzle is set to 180 mm, the distance from the slit opening to the roller is set to 0.2 mm, and the roller diameter is set to φ300 mm. This results in a thin strip with a thickness of 20 μm, a width of 5 mm, and a length of several tens of meters.

[0291] The amorphization rate X of each thin strip before heat treatment was measured using XRD. It was confirmed that the amorphization rate X of the thin strips before heat treatment was above 85% in all the examples described below. Furthermore, the presence or absence of crystallites was confirmed by observing confined-field diffraction images and bright-field images at 300,000x magnification using transmission electron microscopy. As a result, it was confirmed that the thin strips before heat treatment did not contain crystallites in any of the examples and comparative examples described below.

[0292] Next, the thin strip was subjected to heat treatment. The heat treatment conditions were set as follows: heating rate 100℃ / min, holding temperature 600℃, holding time 1min, and cooling rate after heat treatment 50℃ / min. In addition, the atmosphere during heat treatment was set to an inert atmosphere (Ar atmosphere).

[0293] The coercivity Hc and saturation magnetic flux density Bs of each heat-treated strip were measured. The coercivity Hc was measured using an Hc meter. The saturation magnetic flux density Bs was measured using a vibrating sample magnetometer (VSM) at a maximum applied magnetic field of 1000 Oe. Furthermore, the Bs and Hc of the strips varied depending on their composition; however, for Bs, values ​​above 1.40 T were considered good, and values ​​above 1.50 T were considered even better. For Hc, values ​​below 0.25 Oe (below 19.9 A / m) were considered good, and values ​​below 0.06 Oe (below 4.8 A / m) were considered even better.

[0294] The presence or absence of α-Fe and M-Z compounds was confirmed using XRD on the heat-treated thin strips. Specifically, the presence or absence of α-Fe peaks and M-Z compound peaks was investigated in the XRD-derived graphs. In all the samples listed in Table 7, α-Fe peaks were present in the XRD-derived graphs, but no M-Z compound peaks were observed.

[0295] The coefficients of determination (R) were determined using 3DAP on the heat-treated ribbon. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, this cuboid (measurement range) was virtually divided into 10,000 continuous cubic grids of 2 nm × 2 nm × 2 nm. By statistically processing and analyzing the 10,000 grids, each containing compositional information, the concentration of each element in each grid was calculated. Then, the coefficients of determination (R) were derived. 2 (Fe-Z1), R 2 (Fe-Z2), R 2 (Fe-M), R 2 (M-Z1), R 2 (M-Z2) and R 2 (Z1-Z2). In the following examples, all deterministic coefficients R 2 (Fe-Z1), R 2 At least one of (Fe-Z2) is greater than 0.700, and the coefficient of determination R 2 (Fe-M) is also above 0.700.

[0296] Furthermore, the average M / C value was measured in the region (second region) where the combined concentration of Fe, Co, and Ni was below 80 at%. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, this cuboid (measurement range) was virtually divided into 80,000 continuous cubic grids of 1 nm × 1 nm × 1 nm. By statistically processing and analyzing the 80,000 grids, each containing compositional information, the concentration of each element in each grid was calculated. Then, grids with a combined concentration of Fe, Co, and Ni below 80 at% were selected from the 80,000 grids. The M / C value of the selected grids was calculated separately and then averaged to obtain the average M / C value. The results are shown in Table 7.

[0297] [Table 7]

[0298]

[0299] All the embodiments described in Table 7 are as described above, with the determination coefficient R. 2 (Fe-Z1), R 2 At least one of (Fe-Z2) is above 0.700, resulting in good magnetic properties.

[0300] (Experimental Example 4)

[0301] In Experiment 4, for the compositions shown in Table 8, the heat treatment conditions were changed to prepare thin film-shaped samples, thin strip-shaped samples, and powder-shaped samples. The method for preparing the thin film-shaped samples was the same as in Experiment 1. The method for preparing the thin strip-shaped samples was the same as in Experiment 3, but the heat treatment conditions were set to the conditions described in Table 8. The method for preparing the powder-shaped samples will be described below.

[0302] First, pure metal materials were weighed separately to obtain the master alloy with the composition shown in Table 8. Then, after evacuating the chamber, the master alloy was melted by high-frequency heating.

[0303] The prepared master alloy was then heated to melt it, producing a molten metal at 1500°C. This molten metal was then sprayed using a gas atomization method with the composition shown in Table 8 to produce powder. The nozzle diameter was set to 1 mm, the molten metal discharge rate to 1 kg / min, and the gas pressure to 7.5 MPa.

[0304] The amorphization rate X of each powder before heat treatment (described later) was determined using XRD. It was confirmed that the amorphization rate X of the powder before heat treatment was above 85% in all the examples described later. Furthermore, the presence or absence of crystallites was confirmed by observing confined-field diffraction patterns using transmission electron microscopy and by observing bright-field patterns at 300,000x magnification. As a result, it was confirmed that the powder before heat treatment did not contain crystallites in any of the examples and comparative examples described later.

[0305] Next, the powder was subjected to heat treatment. The heat treatment conditions are shown in Table 8. In addition, the atmosphere during heat treatment was set to an inert atmosphere (Ar atmosphere).

[0306] The coercivity Hc and saturation magnetic flux density Bs of each heat-treated powder were measured. The coercivity Hc was measured using an Hc meter. The saturation magnetic flux density Bs was measured using a vibrating sample magnetometer (VSM) at a maximum applied magnetic field of 1000 Oe. Furthermore, the Bs and Hc of the powder varied depending on its composition; however, for Bs, values ​​above 1.40 T were considered good, and values ​​above 1.50 T were considered even better. For Hc, values ​​below 15.0 Oe (below 1194 A / m) were considered good, and values ​​below 5.0 Oe (below 398 A / m) were considered even better.

[0307] The presence or absence of α-Fe and the M-Z compound was confirmed using XRD on the heat-treated powder. Specifically, the presence or absence of α-Fe peaks and M-Z compound peaks was investigated in the XRD-obtained graphs. In all the examples described in Table 8, the XRD-obtained graphs showed α-Fe peaks but no M-Z compound peaks. In contrast, all the comparative examples described in Table 8 showed both α-Fe peaks and a peak of TaC, one type of M-Z compound.

[0308] The coefficients of determination (R0) of the heat-treated powder were determined using 3DAP. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, this cuboid (measurement range) was virtually divided into 10,000 consecutive cubic grids of 2 nm × 2 nm each. By statistically processing and analyzing the 10,000 grids, each containing compositional information, the concentration of each element in each grid was calculated. Then, the coefficients of determination (R0) were derived. 2 (Fe-Z1), R 2 (Fe-Z2), R 2 (Fe-M), R 2 (M-Z1), R 2 (M-Z2) and R 2 (Z1-Z2). In the following examples, all deterministic coefficients R 2 (Fe-Z1), R 2 At least one of (Fe-Z2) is greater than 0.700, and the coefficient of determination R 2 (Fe-M) is also above 0.700. In contrast, in the following comparative examples, the coefficient of determination R... 2 (Fe-Z1), R 2 Both (Fe-Z2) values ​​are less than 0.700.

[0309] Furthermore, the average M / C value in the region (second region) where the combined concentration of Fe, Co, and Ni is below 80 at% was determined using 3DAP for the heat-treated powder. Specifically, a cuboid with one side length of 40 nm × 40 nm × 50 nm was used as the measurement range. By analyzing the measurement data obtained using software, this cuboid (measurement range) was virtually divided into 80,000 continuous cubic grids of 1 nm × 1 nm × 1 nm. By statistically processing and analyzing the 80,000 grids, each with compositional information, the concentration of each element in each grid was calculated. Then, grids with a combined concentration of Fe, Co, and Ni below 80 at% were selected from the 80,000 grids, and the M / C of the selected grids was calculated and averaged to obtain the average M / C value. The results are shown in Table 8.

[0310] [Table 8]

[0311]

[0312] According to Table 8, in each sample of the embodiment where the heating rate and holding time were sufficiently fast and sufficient, regardless of whether the soft magnetic alloy was in the form of a thin film, a strip, or a powder, the determination coefficient R, as described above, was...2 (Fe-Z1), R 2 At least one of (Fe-Z2) is 0.700 or higher. In contrast, in comparative examples where the heating rate is too slow and the holding time is too long, the coefficient of determination R... 2 (Z1-Z2) is not within the specified range. Furthermore, as mentioned above, the coefficient of determination R... 2 (Fe-Z1), R 2 The (Fe-Z2) values ​​are both less than 0.700. Furthermore, the examples exhibit good magnetic properties, but the comparative examples show higher coercivity.

[0313] Symbol Explanation

[0314] 1…(The soft magnetic alloy of this embodiment)

[0315] 101, 201… (existing) soft magnetic alloys

[0316] 11…α-Fe phase

[0317] 13…Amorphous phase

[0318] 15…M-Z compound phase (M-C compound phase)

Claims

1. A soft magnetic alloy containing Fe and at least one metalloid element, characterized in that: Amorphous and nanocrystalline materials with a grain size of 5–30 nm coexist. The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element is greater than 0.

700. The soft magnetic alloy is composed of the formula (Fe （1－（α＋β）） X1 α X2 β ) （1－（a＋b＋c）） M1 a Z b Cr c express, X1 is selected from one or more of Co and Ni. X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, Cu, Bi, N, O, S, and rare earth elements. M1 is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W. Z represents C and P. 0.030≤a≤0.140 0.030≤b≤0.160 0.000≤c≤0.030 0.730≤1-(a+b+c)≤0.890 0≤α(1-(a+b+c))≤0.400 0≤β{1-(a+b+c)}≤0.010 0≤α＋β≤0.50 The content of Ta relative to M1 is more than 40 at%. The coefficients of determination for the atomic concentrations of M1 and C are greater than or equal to 0.600, or the coefficients of determination for the atomic concentrations of M1 and P are greater than or equal to 0.

600. The coefficients of determination for the atomic concentrations of C and P are less than 0.

400.

2. The soft magnetic alloy according to claim 1, characterized in that: The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one M1 is greater than 0.

700.

3. The soft magnetic alloy according to claim 1 or 2, characterized in that: 0.050≤b≤0.160。 4. The soft magnetic alloy according to claim 1 or 2, characterized in that: 0.050≤a≤0.140。 5. The soft magnetic alloy according to claim 1 or 2, characterized in that: It contains Fe-based nanocrystals.

6. The soft magnetic alloy according to claim 1 or 2, characterized in that: It is in the shape of a thin strip.

7. The soft magnetic alloy according to claim 1 or 2, characterized in that: It is in powder form.

8. The soft magnetic alloy according to claim 1 or 2, characterized in that: It is in the shape of a thin film.

9. A soft magnetic alloy containing Fe and at least one metalloid element, characterized in that: It has the composition of the Fe-M-Z system. M is selected from one or more transition metals from groups 4 to 6, and Z is selected from two or more of C, P, Si, B, and Ge. M is M1, where M1 is selected from one or more elements chosen from Ta, V, Zr, Hf, Ti, Nb, Mo, and W. Amorphous and nanocrystalline materials with a grain size of 5–30 nm coexist. The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element is greater than 0.

700. The soft magnetic alloy is composed of the formula (Fe （1－（α＋β）） X1 α X2 β ) （1－（a＋b＋c）） M1 a Z b Cr c express, X1 is selected from one or more of Co and Ni. X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, Cu, Bi, N, O, S, and rare earth elements. M1 is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W. Z represents C and P. 0.030≤a≤0.140 0.030≤b≤0.160 0.000≤c≤0.030 0.730≤1-(a+b+c)≤0.890 0≤α(1-(a+b+c))≤0.400 0≤β{1-(a+b+c)}≤0.010 0≤α＋β≤0.50 The content of Ta relative to M1 is more than 40 at%. The coefficients of determination for the atomic concentrations of M1 and C are less than 0.500, or the coefficients of determination for the atomic concentrations of M1 and P are less than 0.

500. The coefficients of determination for the atomic concentrations of C and P are less than 0.

400.

10. The soft magnetic alloy according to claim 9, characterized in that: The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one M1 is greater than 0.

700.

11. The soft magnetic alloy according to claim 9 or 10, characterized in that: 0.050≤b≤0.160。 12. The soft magnetic alloy according to claim 9 or 10, characterized in that: 0.050≤a≤0.140。 13. The soft magnetic alloy according to claim 9 or 10, characterized in that: It contains Fe-based nanocrystals.

14. The soft magnetic alloy according to claim 9 or 10, characterized in that: It is in the shape of a thin strip.

15. The soft magnetic alloy according to claim 9 or 10, characterized in that: It is in powder form.

16. The soft magnetic alloy according to claim 9 or 10, characterized in that: It is in the shape of a thin film.

17. A soft magnetic alloy containing Fe and at least one metalloid element, characterized in that: Amorphous and nanocrystalline materials with a grain size of 5–30 nm coexist. The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one metalloid element is greater than 0.

700. The soft magnetic alloy is composed of the formula (Fe （1－（α＋β）） X1 α X2 β ) （1－（a＋b3＋b4＋c）） M a C b3 Z3 b4 Cr c express, X1 is selected from one or more of Co and Ni. X2 is selected from one or more elements including Al, Mn, Ag, Zn, Sn, As, Sb, Cu, Bi, N, O, S, and rare earth elements. M is selected from one or more of Ta, V, Zr, Hf, Ti, Nb, Mo, and W. Z3 is selected from one or more of P, B, Si, and Ge. 0.030≤a≤0.140 0.005≤b3≤0.200 0.000≤b4≤0.180 0.000≤c≤0.030 0≤α(1-(a+b3+b4+c))≤0.400 β≥0 0≤α＋β≤0.50 The content of Ta relative to M is more than 40 at%. No peaks of M-C compounds were found in the XRD crystal structure analysis results of the soft magnetic alloy. The soft magnetic alloy has a first region where the total concentration of Fe, Co and Ni is 85 at% or more, and a second region where the total concentration of Fe, Co and Ni is 80 at% or less, wherein in the second region, the average value of the atomic concentration of M divided by the atomic concentration of C, M / C, is greater than 1.

0.

18. The soft magnetic alloy according to claim 17, characterized in that: The coefficient of determination for the atomic concentration of Fe and the atomic concentration of at least one type of M is greater than 0.

700.

19. The soft magnetic alloy according to claim 17 or 18, characterized in that: 0.040≤b3≤0.120。 20. The soft magnetic alloy according to claim 17 or 18, characterized in that: 0.730≤1-(a+b3+b4+c)≤0.

930.

21. The soft magnetic alloy according to claim 17 or 18, characterized in that: 0.050≤a≤0.140。 22. A magnetic component comprising any one of claims 1 to 21.

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