High-sphericity amorphous soft magnetic alloy powder and method for preparing the same

Abstract

The application relates to the field of amorphous alloy materials, in particular to a high-sphericity amorphous soft magnetic alloy powder and a preparation method thereof, the structural general formula of which is as follows: (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 100‑x (A a B 1‑a ) x , wherein A and B are the same or different and are selected from rare metals; when A and B are the same, a is 0; when A and B are different, a is 0.1-0.5; and x is 1-5; the amorphous soft magnetic alloy has a saturation magnetization intensity of greater than or equal to 172.7 A.m 2 / kg, a coercive force of only 28.4 A / m, can meet the application requirements of an iron loss Pc < 800 mW / cm m under the test conditions of 100 kHz and B 3 = 100 mT, and has excellent comprehensive soft magnetic performance with a magnetic permeability reduction of less than or equal to 30% under the condition of 100 Oe direct current superposition.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of amorphous alloy materials, in particular to a high-sphericity amorphous soft magnetic alloy powder and a preparation method thereof. BACKGROUND

[0002] Since the discovery of Faraday's law of electromagnetic induction, the application of soft magnetic materials has been continuously developing. The earliest soft magnetic material is iron. Since the advent of oriented silicon steel in the 20th century, the development of metal soft magnetic materials has entered a fast track. Then FeNi, soft magnetic ferrite and amorphous / nanocrystalline materials have emerged in succession. With the continuous improvement of application frequency and response current, amorphous soft magnetic alloys have entered the field of view of developers and have emerged in the fields of 5G, new energy electric vehicles, smart homes, artificial intelligence, big data, etc.

[0003] Fe-Si-B amorphous alloy, as the most commonly used amorphous soft magnetic alloy, has the characteristics of high saturation magnetic induction and good DC superposition characteristics. However, as the most widely studied Fe-Si-B series alloy composition, Fe 75 Si 15 B 10 , Fe 77.5 Si 13.5 B9、Fe 80 Si4B 16 , etc. cannot meet the application requirements of amorphous magnetic powder cores under the test conditions of 100 kHz, B m =100mT, iron loss Pc<800mW / cm 3 , and under the condition of 100Oe DC superposition, the magnetic permeability of the magnetic powder core decreases by ≤30%. SUMMARY

[0004] The present application provides a high-sphericity amorphous soft magnetic alloy powder and a preparation method thereof to solve the above technical problems.

[0005] The technical solutions adopted are as follows:

[0006] A high-sphericity amorphous soft magnetic alloy powder, according to atomic percentage, has the following general structure:

[0007] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 100-x (A a B 1-a ) x

[0008] Wherein, A and B are the same or different and are selected from rare metals;

[0009] when A and B are the same, a is 0;

[0010] when A and B are different, a is 0.1-0.5;

[0011] x is 1-5.

[0012] Further, A and B are the same or different, selected from Ga, Ge, Se or In.

[0013] Further, A and B are different, respectively Ga and Ge.

[0014] Further, a is 0.1, 0.2, 0.3, 0.4 or 0.5.

[0015] Further, a is 0.5.

[0016] Further, x is 1, 2, 3, 4 or 5.

[0017] Further, x is 2.

[0018] The application provides a preparation method of high-sphericity amorphous soft magnetic alloy powder, which comprises the following steps: weighing raw materials according to the proportion in the structural general formula, and placing the raw materials in a vacuum arc furnace, wherein the alloy liquid is obtained by melting under the protection of argon gas with a melting current of 280-300 A; after the alloy liquid is refined, the alloy liquid is placed for 1-3 min, and then cooled to 100-200 DEG C higher than the alloy liquid; the pump is started to begin atomization, the alloy liquid passes through the leakage eye of the intermediate ladle to enter the atomization zone, and the alloy liquid is broken into droplets under the joint action of high-pressure water and gas, and then condensed and collected; after dehydration, drying and screening, the high-sphericity amorphous soft magnetic alloy powder is obtained.

[0019] Further, the atomization pressure is 105-110 MPa.

[0020] Further, the particle size of the high-sphericity amorphous soft magnetic alloy powder obtained after screening is 1-50 mu m.

[0021] The application has the following beneficial effects:

[0022] The application provides a high-sphericity amorphous soft magnetic alloy powder, which mainly comprises ferromagnetic elements Fe and Ni, and metalloid elements such as Si and P, which can improve the amorphous forming ability and thermal stability; the addition of Cu and Mo is beneficial to the formation of amorphous alloy, and the replacement of part of Si by Mo can increase the crystallization temperature of the alloy, that is, the thermal stability of the amorphous alloy is improved; the saturation magnetization of the amorphous soft magnetic alloy is greater than or equal to 172.7 A·m 2 / kg, and the coercive force is only 28.4 A / m, which can meet the requirement that the iron loss Pc is less than 800 mW / cm m under the test condition of 100 kHz and B 3In the condition of 100 Oe direct current superposition, the application requirement of magnetic permeability reduction amplitude ≤30%, and the comprehensive soft magnetic performance is excellent. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 The XRD pattern of the high-sphericity amorphous soft magnetic alloy powder prepared in Example 1-5 of the present application is shown in the figure. As can be seen from the figure, the XRD curve of all the high-sphericity amorphous soft magnetic alloy powders has a wide scattering "steamed bun" peak near 2θ = 45, and no sharp crystallization peak corresponding to the crystal is appeared, which indicates that it is a completely amorphous structure.

[0024] Figure 2 The microstructure morphology of the high-sphericity amorphous soft magnetic alloy powder prepared in Example 1 of the present application is shown in the figure. The powder has high sphericity and smooth surface. DETAILED DESCRIPTION

[0025] The specific conditions not mentioned in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not marked with the manufacturer, which are all conventional products that can be purchased on the market.

[0026] Example 1:

[0027] A high-sphericity amorphous soft magnetic alloy powder, according to atomic percentage, has the following general structure formula:

[0028] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 98 (Ga 0.5 Ge 0.5 )2

[0029] The preparation method is as follows:

[0030] The raw materials are weighed according to the proportion in the general structure formula, and placed in a vacuum arc furnace. The vacuum is extracted to 5×10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 300 A. After refining the alloy liquid, it is placed for 3 min, and the temperature is reduced to 200℃ above the alloy liquid. The pump is started to begin atomization, and the atomization pressure is 110 MPa. The alloy liquid passes through the leakage eye of the intermediate ladle into the atomization zone, and the leakage eye diameter is 4 mm. Under the joint action of high-pressure water and gas, it is broken into droplets, and after condensation, it is collected. After dehydration, drying and screening, the high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50 μm is obtained.

[0031] Example 2:

[0032] ​A high-sphericity amorphous soft magnetic alloy powder, according to the atomic percentage, has the general structure as follows:

[0033] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 98 Ga2

[0034] The preparation method is as follows:

[0035] The raw materials are weighed according to the proportions in the general structure, and are placed in a vacuum arc furnace. The vacuum is extracted to 5*10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 280 A. After refining, the alloy liquid is placed for 1 min, and is cooled to 100℃ overheat of the alloy liquid. The pump is started to begin atomization, the atomization pressure is 105 MPa, the alloy liquid passes through the leakage eye of the intermediate ladle into the atomization zone, the leakage eye diameter is 4 mm, and is broken into liquid drops under the joint action of high-pressure water and gas. After condensation, it is collected, dehydrated, dried, and screened to obtain a high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50μm.

[0036] Example 3:

[0037] A high-sphericity amorphous soft magnetic alloy powder, according to the atomic percentage, has the general structure as follows:

[0038] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 98 Ge2

[0039] The preparation method is as follows:

[0040] The raw materials are weighed according to the proportions in the general structure, and are placed in a vacuum arc furnace. The vacuum is extracted to 5*10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 280 A. After refining, the alloy liquid is placed for 1 min, and is cooled to 100℃ overheat of the alloy liquid. The pump is started to begin atomization, the atomization pressure is 105 MPa, the alloy liquid passes through the leakage eye of the intermediate ladle into the atomization zone, the leakage eye diameter is 4 mm, and is broken into liquid drops under the joint action of high-pressure water and gas. After condensation, it is collected, dehydrated, dried, and screened to obtain a high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50μm.

[0041] Example 4:

[0042] A high-sphericity amorphous soft magnetic alloy powder, according to atomic percentage, has a general structure as follows:

[0043] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 98 (Ga 0.4 Ge 0.6 )2

[0044] A preparation method is as follows:

[0045] The raw materials are weighed according to the proportions in the general structure, placed in a vacuum arc furnace, vacuumed to 5x10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 300A. After refining, the alloy liquid is left for 1 min, cooled to 200℃ of superheat of the alloy liquid, and atomized by starting the pump. The atomization pressure is 105MPa, the alloy liquid enters the atomization zone through the leakage eye of the intermediate ladle with a diameter of 4mm, and is broken into droplets under the joint action of high-pressure water and gas. After condensation, it is collected, dehydrated, dried, and screened to obtain a high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50μm.

[0046] Example 5:

[0047] A high-sphericity amorphous soft magnetic alloy powder, according to atomic percentage, has a general structure as follows:

[0048] (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 98 (Ga 0.1 Ge 0.9 )2

[0049] A preparation method is as follows:

[0050] The raw materials are weighed according to the proportions in the general structure, placed in a vacuum arc furnace, vacuumed to 5x10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 300A. After refining, the alloy liquid is left for 1 min, cooled to 200℃ of superheat of the alloy liquid, and atomized by starting the pump. The atomization pressure is 105MPa, the alloy liquid enters the atomization zone through the leakage eye of the intermediate ladle with a diameter of 4mm, and is broken into droplets under the joint action of high-pressure water and gas. After condensation, it is collected, dehydrated, dried, and screened to obtain a high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50μm.

[0051] Comparative Example:

[0052] A high-sphericity amorphous soft magnetic alloy powder, according to atomic percentage, has a general structure as follows:

[0053] Fe 65 Ni 10 Si 10 Mo5Cu9P1

[0054] A preparation method is as follows:

[0055] Raw materials are weighed according to the proportion in the general structure, and are placed in a vacuum arc furnace. The vacuum is extracted to 5x10 -3 Pa or below, argon is introduced, and the alloy liquid is obtained by smelting at a current of 300 A under the protection of the argon atmosphere. After refining, the alloy liquid is left for 3 min, and is cooled to 200℃ overheat of the alloy liquid. The pump is started to begin atomization, and the atomization pressure is 110 MPa. The alloy liquid passes through the leakage eye of the intermediate ladle to enter the atomization zone, and the leakage eye diameter is 4 mm. Under the joint action of high-pressure water and gas, the alloy liquid is broken into droplets, and is collected after condensation. After dehydration, drying, and screening, the high-sphericity amorphous soft magnetic alloy powder with a particle size of 1-50μm is obtained.

[0056] Performance test:

[0057] The specific saturation magnetization and coercivity of the amorphous soft magnetic alloy powder in Examples 1-5 and the comparative example are measured by using a Lake Shore 7407 type vibrating magnetometer (VSM).

[0058] The amorphous soft magnetic alloy powder in Examples 1-5 and the comparative example is cold-pressed into a φ27xφ14.5x11 standard 106 magnetic powder core ring at 800 MPa. Under the test conditions of 100 kHz and Bm=100 mT AC, the iron loss is tested, and under the test conditions of 100 Oe DC superposition, the permeability drop is tested. The test results are shown in Table 1 as follows:

[0059] Table 1:

[0060]

[0061] As shown in Table 1 above, the saturation magnetization of the amorphous soft magnetic alloy is ≥172.7 A·m 2 / kg, and the coercivity is only 28.4 A / m. The application requirements of the iron loss Pc<800 mW / cm m under the test conditions of 100 kHz and B 3 =100 mT, and the permeability drop ≤30% under the test conditions of 100 Oe DC superposition are met, and the comprehensive soft magnetic performance is excellent.

[0062] The above examples are only used to illustrate the technical solutions of the present application, and are not intended to limit the present application; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can be modified, or some technical features can be replaced by equivalent features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A high-sphericity amorphous soft magnetic alloy powder, characterized by comprising: According to atomic percentage, the structural general formula is as follows: (Fe 0.65 Ni 0.1 Si 0.1 Mo 0.05 Cu 0.09 P 0.01 ) 100-x (A a B 1-a ) x Wherein, A and B are same or different, selected from Ga, Ge, Se or In; When A and B are same, a is 0; When A and B are different, a is 0.1-0.5; x is 1-5.

2. The high-sphericity amorphous soft magnetic alloy powder according to claim 1, wherein A and B are different, respectively Ga and Ge.

3. The high-sphericity, amorphous soft magnetic alloy powder of claim 1, wherein the alloy powder has a sphericity of at least 0.

90. a is 0.

5.

4. The high-sphericity, amorphous soft magnetic alloy powder of claim 1, wherein the alloy powder has a sphericity of at least 0.

90. x is 2.

5. A method of producing the high-sphericity non-crystalline soft magnetic alloy powder according to any one of claims 1 to 4, characterized by, According to the proportion in the structural general formula, the raw materials are weighed and placed in a vacuum arc furnace, and the alloy liquid is obtained by smelting under the protection of argon atmosphere with a smelting current of 280-300A. After refining, the alloy liquid is placed for 1-3min, and the temperature is reduced to 100-200℃ overheat of the alloy liquid. The pump is started to begin atomization, and the alloy liquid enters the atomization zone through the leakage eye of the intermediate ladle. Under the joint action of high-pressure water and gas, it is broken into droplets, condensed and collected. After dehydration, drying and screening, the high-spherical-degree amorphous soft magnetic alloy powder is obtained. The atomization pressure is 105-110MP; The particle size of the high-spherical-degree amorphous soft magnetic alloy powder obtained after screening is 1-50μm.

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