AMORPHOUS NANOCRYSTALLINE SOFT MAGNETIC MATERIAL, PREPARATION METHOD THEREFOR AND USE THEREOF, AMORPHOUS RIBBON MATERIAL, AMORPHOUS NANOCRYSTALLINE RIBBON MATERIAL, AND AMORPHOUS NANOCRYSTALLINE MAGNETIC SHEET

Abstract

Disclosed are an amorphous nanocrystalline soft magnetic material, a preparation method therefor and an application thereof, an amorphous ribbon material, an amorphous nanocrystalline ribbon material, and an amorphous nanocrystalline magnetic sheet. The soft magnetic material comprises an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles distributed in the amorphous matrix phase and the nanocrystalline phase. The amorphous matrix phase comprises Fe, Si, and B, the fine crystalline particles comprise metal carbides, and the soft magnetic material comprises Fe, Si, B, P, and Cu.

Claims

1. An amorphous nanocrystalline soft magnetic material, comprising an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and a fine crystalline particle distributed in the amorphous matrix phase and the nanocrystalline phase, wherein the amorphous matrix phase comprises Fe, Si and B; the fine crystalline particle comprises metal carbides; and the amorphous nanocrystalline soft magnetic material comprises Fe, Si, B, P and Cu.

2. The amorphous nanocrystalline soft magnetic material according to claim 1, wherein the amorphous nanocrystalline soft magnetic material has a molecular formula of Fe.sub.aSi.sub.bB.sub.cCu.sub.dP.sub.eM.sub.f(XC).sub.h, wherein M is selected from any one or a combination of at least two of Ta, W, Mo, Ge, Zr, Hf or Y; X is Nb and/or V; 1≤b≤12, 3≤c≤10, 0.5≤d≤3, 1≤e≤7, 0≤f≤8, 0.1≤h≤2, and a+b+c+d+e+f+h=100.

3. The amorphous nanocrystalline soft magnetic material according to claim 2, wherein the amorphous matrix phase further comprises M.

4. The amorphous nanocrystalline soft magnetic material according to claim 2, wherein the amorphous matrix phase further comprises P and Cu; optionally, the nanocrystalline phase comprises α-Fe; optionally, the metal carbide is XC.

5. The amorphous nanocrystalline soft magnetic material according to claim 1, wherein the nanocrystalline phase has an average particle size of less than or equal to 30 nm; optionally, the nanocrystalline phase has the average particle size of 10 nm to 20 nm; optionally, the fine crystalline particle has an average particle size of less than or equal to 10 nm; optionally, the fine crystalline particle has the average particle size of 5 nm to 8 nm; optionally, in the amorphous nanocrystalline soft magnetic material, the nanocrystalline phase has an atomic percentage of 50 at % to 70 at %; optionally, in the amorphous nanocrystalline soft magnetic material, the fine crystalline particle has an atomic percentage of 0.1 at % to 2 at %.

6. A preparation method for the amorphous nanocrystalline soft magnetic material according to claim 1, wherein the method comprises the following steps: (1) proportioning a raw material of formulation amount followed by preparing an amorphous alloy; and (2) subjecting the amorphous alloy described in step (1) to a two-stage crystallization under a protective condition, and cooling to obtain the amorphous nanocrystalline soft magnetic material, wherein the crystallization temperature of the second stage is higher than the crystallization temperature of the first stage.

7. The preparation method according to claim 6, wherein the crystallization temperature of the first stage in step (2) is 5° C. to 20° C. below the onset temperature of the first crystallization peak of the amorphous alloy in step (1).

8. The preparation method according to claim 6, wherein, optionally, the crystallization temperature of the second stage in step (2) is 30° C. to 100° C. above the onset temperature of the first crystallization peak of the amorphous alloy in step (1).

9. The preparation method according to claim 6, wherein a method of preparing the amorphous alloy in step (1) comprises the following steps: (11) melting the proportioned raw material under a protective condition to obtain an alloy liquid or an alloy ingot; (12) cooling the alloy liquid in step (11) to obtain the amorphous alloy; or remelting the alloy ingot in step (11) and cooling to obtain the amorphous alloy; optionally, a purity of the raw material in step (11) is greater than 99 wt. %; optionally, the protective condition in step (11) includes vacuum or protective gas; optionally, the protective gas includes nitrogen or argon; optionally, a temperature of melting in step (11) is 1300° C. to 1500° C.; optionally, a method of melting in step (11) includes any one of arc melting, intermediate frequency induction melting or high frequency induction melting; optionally, a cooling rate of cooling in step (12) is greater than or equal to 10.sup.6° C./s; optionally, a method of cooling in step (12) includes a single-roll cold method, a copper mold blow-casting method, a copper mold suction casting method or a Taylor method, and optionally, the single-roll cold method; optionally, the protective condition in step (2) includes vacuum or protective gas; optionally, the protective gas includes nitrogen and/or argon; optionally, a heating rate to the crystallization temperature of the first stage in step (2) is 5° C./min to 10° C./min; optionally, a holding time at the crystallization temperature of the first stage in step (2) is 5 min to 30 min; optionally, the onset temperature of the first crystallization peak of the amorphous alloy is measured and obtained by a differential scanning calorimetry; optionally, a heating rate to the crystallization temperature of the second stage in step (2) is 5° C./min to 10° C./min; optionally, a holding time at the crystallization temperature of the second stage in step (2) is 30 min to 60 min.

10. The preparation method according to claim 6, wherein the method comprises the following steps: (11) proportioning the raw material with a purity of more than 99% in a formulation amount, melting the proportioned raw material into alloy ingot at a temperature of 1300° C. to 1500° C. under a condition of vacuuming and/or filling with protective gas; (12) remelting the alloy ingot in step (11) and then cooling the melt by the single-roll cold method, wherein a cooling rate of the cooling is greater than or equal to 10.sup.6° C./s, to obtain an amorphous alloy; and (2) under a condition of vacuuming or filling with protective gas, heating the amorphous alloy in step (12) to a crystallization temperature of the first stage at a heating rate of 5° C./min to 10° C./min, keeping the temperature for 5 min to 30 min, then heating to a crystallization temperature in the second stage at a heating rate of 5° C./min to 10° C./min, keeping the temperature for 30 min to 60 min, and cooling to obtain the amorphous nanocrystalline soft magnetic material; wherein the crystallization temperature in the first stage is 5° C. to 20° C. below the onset temperature of the first crystallization peak of the amorphous alloy in step (12), and the crystallization temperature in the second stage is 30° C. to 100° C. above the onset temperature of the first crystallization peak of the amorphous alloy in step (12).

11. An amorphous ribbon, wherein the amorphous ribbon is composed of the amorphous alloy prepared in step (1) of the preparation method according to claim 6.

12. An amorphous nanocrystalline ribbon, wherein the amorphous nanocrystalline ribbon is composed of the amorphous nanocrystalline soft magnetic material according to claim 1.

13. An amorphous nanocrystalline magnetic sheet, wherein the amorphous nanocrystalline magnetic sheet is prepared from the amorphous nanocrystalline soft magnetic material according to claim 1.

14. (canceled)

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0063] FIG. 1 is a schematic diagram of the influencing principle of NbC on crystal grains during the crystallization process of the amorphous alloy in the preparation method of Example 1 in the present application.

[0064] FIG. 2 is the DSC curve of the amorphous alloy obtained after cooling in the preparation methods of Example 1 and Comparative Example 1 in the present application.

[0065] FIG. 3 is the DSC curve of the amorphous alloy obtained after cooling in the preparation methods of Example 7 and Comparative Example 7 of in the present application.

DETAILED DESCRIPTION

[0066] .In order to better explain the present application and facilitate the understanding of the technical solutions of the present application, the present application will be further described in detail hereinafter. However, the following embodiments are only simple examples of the present application, and do not represent or limit the protection scope of the claims of the present application. The protection scope of the present application is defined by the appended claims.

[0067] The following are typical but non-limiting examples of the present application.

EXAMPLE 1

[0068] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0069] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0070] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted at 1500° C. by arc melting in an argon atmosphere to obtain an alloy ingot with uniform composition.

[0071] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and cooled by a single-roll cold method in a cooling rate above 10.sup.6° C./s to obtain ribbon-shaped amorphous alloy.

[0072] The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection, and the DSC curve was obtained as shown by the thick line in FIG. 2. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 428.93° C.

[0073] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0074] the first stage: according to the results of the DSC detecting on the amorphous alloy obtained in step 3, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 428.93° C.; the amorphous alloy was put into the heat treatment furnace; the inside of heat treatment furnace was heated at a heating rate of 8° C./min to 415° C. under high vacuum and kept temperature for 15 minutes; and

[0075] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated at a heating rate of 8° C./min to 480° C. and kept temperature for 50 minutes; then the heat treatment furnace was turn off and the amorphous alloy, after the first stage crystallization and the second stage crystallization, was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0076] X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM) were used to characterize the microstructure of the amorphous nanocrystalline soft magnetic material obtained in this example, and the results are as follows.

[0077] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 11.89 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 8.15 nm.

[0078] The structural characterization methods in other examples are the same as in this example.

[0079] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

[0080] FIG. 1 is a schematic diagram of the influence principle of NbC on crystal grains during the crystallization process of the amorphous alloy in this example. It can be seen from this figure that in the amorphous alloy prepared in step 3, due to the very fast cooling rate during the manufacturing process of the amorphous alloy, the fine crystalline particles (NbC phase) were solid-dissolved in the amorphous matrix. In the first stage crystallization in step 4, the solid solubility of the fine crystalline particles (NbC phase) in the amorphous matrix was reduced due to the holding temperature, and the fine crystalline particles (NbC phase) gradually solid-solution precipitated from the amorphous matrix. Due to the low holding temperature, the aging of fine crystalline particles (NbC phase) was not obvious. The size of the fine crystalline particles (NbC phase) could be maintained at a few nanometers and dispersed in the amorphous matrix. During this process, because the holding temperature was lower than the onset temperature of the first crystallization peak of the amorphous alloy, Fe will not undergo phase transformation, that is, the α-Fe nanocrystalline phase would not undergo crystallization and precipitation. In the second stage of the crystallization in step 4, the α-Fe nanocrystalline phase began to precipitate and grow, but was inhibited from growing since the pinning effect of the dispersed small fine crystalline particles (NbC phase) on the grain boundary hindered the migration of the grain boundary. The finally obtained α-Fe crystal grain size could be maintained at a relatively small nanometer level.

COMPARATIVE EXAMPLE 1

[0081] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 1, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.5Zr.sub.2alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (427.74° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and under high vacuum protection, the inside of heat treatment furnace was heated to 485° C. at a heating rate of 10° C./min, and kept for 45 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature.

[0082] The specific conditions of the other operation steps of this comparative example are the same as those in Example 1.

[0083] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

[0084] Differential scanning calorimeter (DSC) detection was performed on the amorphous alloy prepared in step 3 of this comparative example, and the DSC curve was obtained as shown by the thin line in FIG. 2. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 427.74° C.

EXAMPLE 2

[0085] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0086] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.79Si.sub.1B.sub.10Cu.sub.0.5P.sub.6Zr.sub.1Mo.sub.2(NbC).sub.0.5, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0087] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted at 1300° C. by arc melting under vacuum to obtain an alloy ingot with uniform composition.

[0088] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 388.06° C.

[0089] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0090] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 388.06° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 379° C. at a heating rate of 10° C./min under high vacuum or inert gas protection and kept temperature for 20 minutes; and

[0091] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 468° C. at a heating rate of 10° C./min and kept temperature for 30 minutes; then the heat treatment furnace was turn off; the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0092] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.79Si.sub.1B.sub.10Cu.sub.0.5P.sub.6Zr.sub.1Mo.sub.2(NbC).sub.0.5, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr, Mo and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 24.57 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 7.79 nm.

[0093] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 2

[0094] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 2, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.79Si.sub.1B.sub.10Cu.sub.0.5P.sub.6.5Zr.sub.1Mo.sub.2 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (390.3° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated under the protection of high vacuum to 470° C. at a heating rate of 10° C./min, and kept temperature for 50 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, then taken out and subjected to air-cooling to room temperature.

[0095] The specific conditions of the other operation steps of this comparative example are the same as those in Example 2.

[0096] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 3

[0097] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0098] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.79.5Si.sub.2B.sub.7Cu.sub.3P.sub.4Ta.sub.1W.sub.1Ge.sub.0.5Hf.sub.1.5(VC).sub.0.5, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, V was added in the form of ferro-vanadium alloy, and C was added in the form of ferro-carbon alloy.

[0099] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted under vacuum at 1400° C. by the medium-frequency induction melting method to obtain an alloy ingot with uniform composition.

[0100] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 398.69° C.

[0101] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0102] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 398.69° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 390° C. at a heating rate of 7° C./min under the protection of high vacuum and kept temperature for 5 minutes; and

[0103] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 465° C. at a heating rate of 7° C./min and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0104] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.79.5Si.sub.2B.sub.7Cu.sub.3P.sub.4Ta.sub.1W.sub.1Ge.sub.0.5Hf.sub.1.5(VC).sub.0.5, wherein the amorphous matrix phase included Fe, Si, B, Cu, Ta, W, Ge, Hf and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 22.19 nm; the fine crystalline particles included VC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 7.7 nm.

[0105] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 3

[0106] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 3, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.79.5Si.sub.2B.sub.7Cu.sub.3P.sub.4.5Ta.sub.1W.sub.1Ge.sub.0.5Hf.sub.1.5 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (397.23° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated under the protection of high vacuum to 470° C. at a heating rate of 10° C./min, and kept temperature for 50 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, then taken out and subjected to air-cooling to room temperature.

[0107] The specific conditions of the other operation steps of this comparative example are the same as those in Example 3.

[0108] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 4

[0109] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0110] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.78.9Si.sub.4B.sub.6Cu.sub.1P.sub.2Zr.sub.2Y.sub.1W.sub.2Mo.sub.2Ge.sub.1(NbC).sub.0.1, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0111] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted under vacuum at 1400° C. by the high-frequency induction melting method to obtain an alloy ingot with uniform composition.

[0112] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 419.6° C.

[0113] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0114] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 419.6° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 410° C. at a heating rate of 9° C./min under the protection of high vacuum and kept temperature for 18 minutes; and

[0115] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 460° C. at a heating rate of 9° C./min and kept temperature for 45 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0116] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.78.9Si.sub.4B.sub.6Cu.sub.1P.sub.2Zr.sub.2Y.sub.1W.sub.2Mo.sub.2Ge.sub.1(NbC).sub.0.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr, Y, W, Mo, Ge and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 16.64 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 7.55 nm.

[0117] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 4

[0118] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 4, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.78.9Si.sub.4B.sub.6Cu.sub.1P.sub.2.1Zr.sub.2Y.sub.1W.sub.2Mo.sub.2Ge.sub.1 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (420.35° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace; the inside of heat treatment furnace was heated under the protection of high vacuum the to 470° C. at a heating rate of 10° C./min, and kept temperature for 35 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, then taken out and subjected to air-cooling to room temperature.

[0119] The specific conditions of the other operation steps of this comparative example are the same as those in Example 4.

[0120] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 5

[0121] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0122] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.78.5Si.sub.7B.sub.8Cu.sub.1.2P.sub.2Y.sub.1Mo.sub.1Zr.sub.1(NbC).sub.0.3, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0123] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted under vacuum at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0124] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was melted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 458.63° C.

[0125] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0126] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 458.63° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 440° C. at a heating rate of 6° C./min under the protection of high vacuum and kept temperature for 25 minutes; and

[0127] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 510° C. at a heating rate of 6° C./min and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0128] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.78.5Si.sub.7B.sub.8Cu.sub.1.2P.sub.2Y.sub.1Mo.sub.1Zr.sub.1(NbC).sub.0.3, wherein the amorphous matrix phase included Fe, Si, B, Cu, Y, Mo, Zr and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 9.51 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 9.05 nm.

[0129] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 5

[0130] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 5, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.78.5Si.sub.7B.sub.8Cu.sub.1.2P.sub.2.3Y.sub.1Mo.sub.1Zr.sub.1 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (457.69° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace; the inside of heat treatment furnace was heated under the protection of high vacuum to 500° C. at a heating rate of 10° C./min, and kept temperature for 40 minutes; then the heat treatment furnace was turn off, the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, then taken out and subjected to air-cooling to room temperature.

[0131] The specific conditions of the other operation steps of this comparative example are the same as those in Example 5.

[0132] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 6

[0133] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0134] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.76.95Si.sub.4B.sub.7Cu.sub.1.25P.sub.4Mo.sub.1Ge.sub.1Zr.sub.2Y.sub.2(VC).sub.0.8, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, V was added in the form of ferro-vanadium alloy, and C was added in the form of ferro-carbon alloy.

[0135] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted under vacuum at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0136] 3. Amorphous alloy manufacturing: the alloy ingots described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 420.63° C.

[0137] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0138] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 420.63° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 410° C. at a heating rate of 7° C./min under the protection of high vacuum and kept temperature for 20 minutes; and

[0139] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 475° C. at a heating rate of 7° C./min and kept temperature for 45 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to 150° C. accompanying with the furnace, taken out and subjected to air-cooling to room temperature to obtain an amorphous nanocrystalline soft magnetic material.

[0140] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.76.95Si.sub.4B.sub.7Cu.sub.1.25P.sub.4Mo.sub.1Ge.sub.1Zr.sub.2Y.sub.2(VC).sub.0.8, wherein the amorphous matrix phase included Fe, Si, B, Cu, Mo, Ge, Zr, Y and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 16.64 nm; the fine crystalline particles included VC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 8 nm.

[0141] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 6

[0142] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 6, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.76.95Si.sub.4B.sub.7Cu.sub.1.25P.sub.4.8Mo.sub.1Ge.sub.1Zr.sub.2Y.sub.2 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (418.96° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated under the protection of high vacuum to 465° C. at a heating rate of 10° C./min, and kept temperature for 45 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to 150° C. accompanying with the furnace, then taken out and subjected to air-cooling to room temperature.

[0143] The specific conditions of the other operation steps of this comparative example are the same as those in Example 6.

[0144] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 7

[0145] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0146] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.74Si.sub.2B.sub.6Cu.sub.25P.sub.6Mo.sub.2Ge.sub.1Zr.sub.3Y.sub.2(NbC)1.5, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0147] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted in a nitrogen atmosphere at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0148] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method. The prepared amorphous alloy was subjected to differential scanning calorimeter (DSC) detection to obtain the DSC curve shown by the thick line in FIG. 3. The DSC curve showed that the amorphous alloy had two crystallization peaks, wherein the onset temperature of the first crystallization peak was 400.25° C.

[0149] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0150] the first stage: according to the DSC curve shown by the thick line in FIG. 3, the onset temperature of the first crystallization peak of the amorphous alloy was 400.25° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 386° C. at a heating rate of 8° C./min in a nitrogen atmosphere and kept temperature for 15 minutes; and

[0151] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 460° C. at a heating rate of 8° C./min and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to room temperature accompanying with the furnace, then taken out to obtain an amorphous nanocrystalline soft magnetic material.

[0152] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.74Si.sub.2B.sub.6Cu.sub.2.5P.sub.6Mo.sub.2Ge.sub.1Zr.sub.3Y.sub.2(NbC).sub.1.5, wherein the amorphous matrix phase included Fe, Si, B, Cu, Mo, Ge, Zr, Y, P, and NbC; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 15.06 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 7.58 nm.

[0153] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 7

[0154] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 7, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.74Si.sub.2B.sub.6Cu.sub.2.5P.sub.7.5Mo.sub.2Ge.sub.1Zr.sub.3Y.sub.2 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (402.25° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated in a nitrogen atmosphere to 450° C. at a heating rate of 10° C./min, and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to room temperature accompanying with the furnace and then taken out.

[0155] The specific conditions of the other operation steps of this comparative example are the same as those in Example 7.

[0156] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

[0157] Differential scanning calorimeter (DSC) detection was performed on the amorphous alloy prepared in step 3 of this comparative example, and the DSC curve shown by the thin line in FIG. 3 was obtained. The DSC curve showed that the amorphous alloy had two crystallization peaks, and the onset temperature of the first crystallization peak was 402.25° C.

EXAMPLE 8

[0158] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0159] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.80.8Si.sub.5B.sub.5Cu.sub.2P.sub.3Zr.sub.2Hf.sub.1(NbC).sub.1(VC).sub.0.2, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, V was added in the form of ferro-vanadium alloy, and C was added in the form of ferro-carbon alloy.

[0160] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted in a nitrogen atmosphere at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0161] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method.

[0162] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0163] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 428.45° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 409° C. at a heating rate of 5° C./min in a nitrogen atmosphere and kept temperature for 30 minutes; and

[0164] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 528° C. at a heating rate of 5° C./min and kept temperature for 30 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to room temperature accompanying with the furnace, and then taken out to obtain an amorphous nanocrystalline soft magnetic material.

[0165] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80.8Si.sub.5B.sub.5Cu.sub.2P.sub.3Zr.sub.2Hf.sub.1(NbC).sub.1(VC).sub.0.2, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr, Hf and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 12.68 nm; the fine crystalline particles included NbC and VC which were both dispersed in the amorphous matrix phase and the nanocrystalline phase, and had the average particle size of 9.32 nm and 9.67 nm respectively.

[0166] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 8

[0167] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 8, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.80.8Si.sub.5B.sub.5Cu.sub.2P.sub.3.2Zr.sub.2Hf.sub.1 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (429.34° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated in a nitrogen atmosphere to 495° C. at a heating rate of 10° C./min, and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to room temperature accompanying with the furnace, and then taken out.

[0168] The specific conditions of the other operation steps of this comparative example are the same as those in Example 8.

[0169] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 9

[0170] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0171] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.75.5Si.sub.4B.sub.8Cu.sub.1.5P.sub.5W.sub.1Mo.sub.1Zr.sub.2(NbC).sub.1(VC).sub.1, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, V was added in the form of ferro-vanadium alloy, and C was added in the form of ferro-carbon alloy.

[0172] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted in a nitrogen atmosphere at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0173] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method.

[0174] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0175] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 421.42° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 408° C. at a heating rate of 7° C./min in a nitrogen atmosphere and kept temperature for 25 minutes; and

[0176] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 470° C. at a heating rate of 7° C./min and kept temperature for 50 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to room temperature accompanying with the furnace, and taken out to obtain an amorphous nanocrystalline soft magnetic material.

[0177] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.75.5Si.sub.4B.sub.8Cu.sub.1.5P.sub.5W.sub.1Mo.sub.1Zr.sub.2(NbC).sub.1(VC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, W, Mo, Zr and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 12.56 nm; the fine crystalline particles included NbC and VC which were dispersed in the amorphous matrix phase and the nanocrystalline phase, and had the average particle size of 7.65nm and 7.93 nm respectively.

[0178] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 9

[0179] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 9, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.7.55Si.sub.4B.sub.8Cu.sub.1.5P.sub.7W.sub.1Mo.sub.1Zr.sub.2 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (421.21° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated in a nitrogen atmosphere to 470° C. at a heating rate of 10° C./min, and kept temperature for 45 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to room temperature accompanying with the furnace, and then taken out.

[0180] The specific conditions of the other operation steps of this comparative example are the same as those in Example 9.

[0181] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 10

[0182] In this example, the amorphous nanocrystalline soft magnetic material was prepared according to the following method.

[0183] 1. Proportioning: the raw materials with a purity greater than 99% were proportioned according to the alloy composition of Fe.sub.83.2Si.sub.12B.sub.3Cu.sub.0.5Pi(NbC).sub.0.3, wherein B was added in the form of ferro-boron alloy, P was added in the form of ferro-phosphorus alloy, Nb was added in the form of ferro-niobium alloy, and C was added in the form of ferro-carbon alloy.

[0184] 2. Melting: the proportioned raw materials were put into the crucible of the melting furnace, and melted in a nitrogen atmosphere at 1400° C. by the arc melting method to obtain an alloy ingot with uniform composition.

[0185] 3. Amorphous alloy manufacturing: the alloy ingot described in step 2 was remelted, and prepared into ribbon-shaped amorphous alloy by a single-roll cold method.

[0186] 4. Crystallizing: crystallization included the first stage and the second stage, wherein:

[0187] the first stage: according to the DSC curve, the onset temperature of the first crystallization peak of the amorphous alloy was identified as 488.24° C.; the amorphous alloy was put into the heat treatment furnace, and the inside of the heat treatment furnace was heated to 475° C. at a heating rate of 5° C./min in a nitrogen atmosphere and kept temperature for 25 minutes; and

[0188] the second stage: after the first stage crystallization, the inside of heat treatment furnace was heated to 540° C. at a heating rate of 5° C./min and kept temperature for 35 minutes; then the heat treatment furnace was turn off, and the amorphous alloy after the first stage crystallization and the second stage crystallization was cooled to room temperature accompanying with the furnace, and then taken out to obtain an amorphous nanocrystalline soft magnetic material.

[0189] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.83.2Si.sub.12B.sub.3Cu.sub.0.5Pi(NbC).sub.0.3, wherein the amorphous matrix phase included Fe, Si, B, Cu and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 8.19 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 9.95 nm.

[0190] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this example were tested, and the results are shown in Table 1.

COMPARATIVE EXAMPLE 10

[0191] The amorphous nanocrystalline soft magnetic material of this comparative example refers to Example 10, where the difference is that, in step 1, the raw materials with a purity greater than 99% were proportioned according to the Fe.sub.83.2Si.sub.12B.sub.3Cu.sub.0.5P.sub.1.3 alloy composition; in step 4, only one-stage crystallization was performed; the crystallization temperature was calculated according to the onset temperature (487.35° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 of this comparative example; the amorphous alloy was put into the heat treatment furnace, and the inside of heat treatment furnace was heated in a nitrogen atmosphere to 550° C. at a heating rate of 10° C./min, and kept temperature for 40 minutes; then the heat treatment furnace was turn off, and the crystallized amorphous alloy was cooled to room temperature accompanying with the furnace, and then taken out.

[0192] The specific conditions of the other operation steps of this comparative example are the same as those in Example 10.

[0193] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

EXAMPLE 11

[0194] Except that the crystallization temperature of the first stage crystallization in step 4 is 434° C. (5.07° C. above the onset temperature of the first crystallization peak of the amorphous alloy), all other operations and operating parameters, raw material proportions and the like in this example were the same as those in the preparation method of the amorphous nanocrystalline soft magnetic material in Example 1.

[0195] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 15.58 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 8.1 nm.

EXAMPLE 12

[0196] Except that the crystallization temperature of the first stage crystallization in step 4 is 400° C. (28.93° C. below the onset temperature of the first crystallization peak of the amorphous alloy), all other operations and operating parameters, raw material proportions and the like in this example were the same as those in the preparation method of the amorphous nanocrystalline soft magnetic material in Example 1.

[0197] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr and P; the nanocrystalline phase was α-Fe, which was dispersed in the amorphous matrix phase and had the average particle size of 16.11 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 8.15 nm.

EXAMPLE 13

[0198] Except that the crystallization temperature of the first stage crystallization in step 4 is 440° C. (11.07° C. above the onset temperature of the first crystallization peak of the amorphous alloy), all other operations and operating parameters, raw material proportions and the like in this example were the same as those in the preparation method of the amorphous nanocrystalline soft magnetic material in Example 1.

[0199] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr and P; the nanocrystalline phase was α-Fe which was dispersed in the amorphous matrix phase, grew incompletely and had the average particle size of 10.21 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 6.95 nm.

EXAMPLE 14

[0200] Except that the crystallization temperature of the first stage crystallization in step 4 is 560° C. (131.07° C. above the onset temperature of the first crystallization peak of the amorphous alloy), all other operations and operating parameters, raw material proportions and the like in this example were the same as those in the preparation method of the amorphous nanocrystalline soft magnetic material in Example 1.

[0201] The amorphous nanocrystalline soft magnetic material prepared in this example included an amorphous matrix phase, a nanocrystalline phase distributed in the amorphous matrix phase, and fine crystalline particles dispersed in the amorphous matrix phase and the nanocrystalline phase. The molecular formula of the amorphous nanocrystalline soft magnetic material was Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1, wherein the amorphous matrix phase included Fe, Si, B, Cu, Zr and P, and further included a part of the second phase such as Fe.sub.2B and the like; the nanocrystalline phase was α-Fe which was dispersed in the amorphous matrix phase, and had the average particle size of 21.83 nm; the fine crystalline particles included NbC which was dispersed in the amorphous matrix phase and the nanocrystalline phase and had the average particle size of 10.55 nm.

COMPARATIVE EXAMPLE 11

[0202] The preparation method of the amorphous nanocrystalline soft magnetic material in this comparative example refers to Example 1, where the difference is that, in step 1, raw materials with a purity greater than 99% were proportioned according to the Fe.sub.81Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2 alloy composition; the crystallization temperatures of the first and second stages of crystallization in step 4 were both calculated according to the onset temperature (428.33° C.) of the first crystallization peak of the amorphous alloy obtained in step 3 in this comparative example; the specific value, which the crystallization temperature of the first stage in this comparative example was lower than the onset temperature of the first crystallization peak in this comparative example, was the same as the difference value between the first stage crystallization temperature in Example 1 and the onset temperature of the first crystallization peak of the amorphous alloy in Example 1, and the specific value, which the crystallization temperature of the second stage in this comparative example was higher than the onset temperature of the first crystallization peak of the amorphous alloy in this comparative example, was the same as the difference value between the second stage crystallization temperature in Example 1 and the onset temperature of the first crystallization peak of the amorphous alloy in Example 1.

[0203] The specific conditions of the other operation steps of this comparative example are the same as those in Example 1.

[0204] The magnetic properties of the amorphous nanocrystalline soft magnetic material obtained after crystallization in this comparative example were tested, and the results are shown in Table 1.

[0205] Performance Test Method

[0206] A vibrating sample magnetometer (VSM) was used to test the saturation magnetic induction intensity of the amorphous nanocrystalline soft magnetic materials prepared in each example and comparative example at room temperature.

[0207] The coercive force of the amorphous nanocrystalline soft magnetic materials prepared in each example and comparative example was tested by using the soft magnetic direct current magnetic performance measurement system instrument at room temperature.

[0208] The test results are shown in the table below.

TABLE-US-00001 TABLE 1 Saturation magnetic Coercivity No. Molecular formulae induction (T) (A/m) Example 1 Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1 1.71 4.5 Comparative Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.5Zr.sub.2 1.70 18.9 Example 1 Example 2 Fe.sub.79Si.sub.1B.sub.10Cu.sub.0.5P.sub.6Zr.sub.1Mo.sub.2(NbC).sub.0.5 1.94 9.3 Comparative Fe.sub.79Si.sub.1B.sub.10Cu.sub.0.5P.sub.6.5Zr.sub.1Mo.sub.2 1.93 23.4 Example 2 Example 3 Fe.sub.79.5Si.sub.2B.sub.7Cu.sub.3P.sub.4Ta.sub.1W.sub.1Ge.sub.0.5Hf.sub.1.5(VC).sub.0.5 1.88 8.4 Comparative Fe.sub.79.5Si.sub.2B.sub.7Cu.sub.3P.sub.4.5Ta.sub.1W.sub.1Ge.sub.0.5Hf.sub.1.5 1.86 21.6 Example 3 Example 4 Fe.sub.78.9Si.sub.4B.sub.6Cu.sub.1P.sub.2Zr.sub.2Y.sub.1W.sub.2Mo.sub.2Ge.sub.1(NbC).sub.0.1 1.76 6.3 Comparative Fe.sub.78.9Si.sub.4B.sub.6Cu.sub.1P.sub.2.1Zr.sub.2Y.sub.1W.sub.2Mo.sub.2Ge.sub.1 1.74 20.7 Example 4 Example 5 Fe.sub.78.5Si.sub.7B.sub.8Cu.sub.1.2P.sub.2Y.sub.1Mo.sub.1Zr.sub.1(NbC).sub.0.3 1.55 3.6 Comparative Fe.sub.78.5Si.sub.7B.sub.8Cu.sub.1.2P.sub.2.3Y.sub.1Mo.sub.1Zr.sub.1 1.53 17.3 Example 5 Example 6 Fe.sub.76.95Si.sub.4B.sub.7Cu.sub.1.25P.sub.4Mo.sub.1Ge.sub.1Zr.sub.2Y.sub.2(VC).sub.0.8 1.76 6.3 Comparative Fe.sub.76.95Si.sub.4B.sub.7Cu.sub.1.25P.sub.4.8Mo.sub.1Ge.sub.1Zr.sub.2Y.sub.2 1.74 20.8 Example 6 Example 7 Fe.sub.74Si.sub.2B.sub.6Cu.sub.2.5P.sub.6Mo.sub.2Ge.sub.1Zr.sub.3Y.sub.2(NbC).sub.1.5 1.87 5.7 Comparative Fe.sub.74Si.sub.2B.sub.6Cu.sub.2.5P.sub.7.5Mo.sub.2Ge.sub.1Zr.sub.3Y.sub.2 1.84 23.2 Example 7 Example 8 Fe.sub.80.8Si.sub.5B.sub.5Cu.sub.2P.sub.3Zr.sub.2Hf.sub.1(NbC).sub.1(VC).sub.0.2 1.71 4.8 Comparative Fe.sub.80.8Si.sub.5B.sub.5Cu.sub.2P.sub.3.2Zr.sub.2Hf.sub.1 1.70 20.6 Example 8 Example 9 Fe.sub.75.5Si.sub.4B.sub.8Cu.sub.1.5P.sub.5W.sub.1Mo.sub.1Zr.sub.2(NbC).sub.1(VC).sub.1 1.75 4.8 Comparative Fe.sub.75.5Si.sub.4B.sub.8Cu.sub.1.5P.sub.7W.sub.1Mo.sub.1Zr.sub.2 1.72 20.7 Example 9 Example 10 Fe.sub.83.2Si.sub.12B.sub.3Cu.sub.0.5P.sub.1(NbC).sub.0.3 1.38 3.1 Comparative Fe.sub.83.2Si.sub.12B.sub.3Cu.sub.0.5P.sub.1.3 1.35 19.3 Example 10 Example 11 Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1 1.71 5.9 Example 12 Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1 1.71 6.1 Example 13 Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1 1.7 9.0 Example 14 Fe.sub.80Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2(NbC).sub.1 1.7 20.9 Comparative Fe.sub.81Si.sub.5B.sub.7Cu.sub.1P.sub.4Zr.sub.2 1.72 19.3 Example 11

[0209] Based on the examples and comparative examples hereinabove, it can be seen that in Examples 1-10, due to the existence of metal carbide fine crystalline particles, the phosphorus-containing soft magnetic material provided in the present application solves the problem of excessively high coercivity in the phosphorus-containing soft magnetic material in the prior art, balances the saturation magnetic induction and coercivity of the phosphorus-containing soft magnetic material, and improves the comprehensive magnetic properties of the phosphorus-containing nanocrystalline soft magnetic material.

[0210] The temperature in the first stage crystallization in Example 11 was too high, resulting in the premature precipitation of the nanocrystalline phase, while NbC fine-crystalline particles could not effectively inhibit the growth of the nanocrystalline grains, so as to affect the product performance.

[0211] The temperature in the first stage crystallization in Example 12 was too low, resulting in that the NbC fine crystalline particles failed to precipitate in a large amount, which did not have the effect of inhibiting the growth of nanocrystalline grains and affected the product performance.

[0212] The temperature in the second stage crystallization in Example 13 was too low, resulting in the precipitation of other second phases, such as Fe2B, which were unfavorable to the magnetic properties, and deterioration of the magnetic properties.

[0213] The temperature in the second stage crystallization in Example 14 was too high, resulting in incomplete formation of nanocrystalline grains, and a small content of nanocrystalline phases, which could not obtain the best magnetic properties.

[0214] Comparative Examples 1-11 did not add the raw materials that made up XC, and only carried out one-stage crystallization. This resulted in not having enough fine crystalline particles in the product obtained in Comparative Examples 1-11, so that it was unable to pin the grain boundary during the crystallization stage, and could not hinder the migration of grain boundaries or effectively inhibit the growth of α-Fe nanocrystalline phase. At the same time, Comparative Examples 1-11 failed to use a fast heating rate during the crystallization process due to the difficulty of the process. Therefore, even if P element is added to the alloy composition of Comparative Examples 1-11, P element can hardly hinder the movement of grain boundaries, and the effect of fining crystalline is poor. Therefore, the product performance of Comparative Examples 1-11 cannot reach the excellent level of the corresponding examples, and there is the problem of excessively high coercivity, which is common in existing phosphorus-containing soft magnetic materials.

[0215] Although Comparative Example 11 merely didn't add C and Nb raw materials, which resulted in that the metal carbide could not be formed, this already prevented the Comparative Example 11 from producing enough fine crystalline particles of metal carbide. Although Comparative Example 11 used the same two-stage crystallization as Example 1, the coercivity of the product is too high to reach the level of Example 1.

[0216] The applicant declares that although the detailed methods of the present application are illustrated by the examples described above, the present application is not limited to the detailed methods described above, which means that the present application does not rely on the detailed methods described above to be implemented.