Amorphous nanocrystalline soft magnetic alloy powder, preparation method thereof and magnetic powder core

Abstract

The application provides an amorphous nanocrystalline soft magnetic alloy powder and a preparation method and a magnetic powder core thereof, and relates to the technical field of soft magnetic materials. The preparation method of the amorphous nanocrystalline soft magnetic alloy powder adopts high-energy electric pulse technology to realize instantaneous rapid heating and explosion of the amorphous alloy material, and realizes accurate control of the powder particle size by accurately controlling energy input parameters and interval parameters, thereby preparing high-sphericity soft magnetic powder with a median particle size of 0.5-5 mu m, significantly improving the uniformity and dispersity of the powder, and solving the problem of low particle size control accuracy in the prior art. Moreover, the preparation method has a simple process flow and low energy consumption, avoids impurities and defects introduced in the traditional multi-step process, and improves the purity and performance of the material. The prepared amorphous nanocrystalline soft magnetic alloy powder has the characteristics of small particle size, high sphericity, high saturation magnetization, low coercivity and high yield, and is particularly suitable for the field of high-frequency magnetic elements and precision electronic devices.

Description

Technical Field

[0001] This invention relates to the field of soft magnetic materials technology, specifically to an amorphous nanocrystalline soft magnetic alloy powder, its preparation method, and a magnetic powder core. Background Technology

[0002] With the rapid development of electronic information technology, electric vehicles, 5G communication and new energy applications, the market has put forward higher requirements for the performance of soft magnetic powders, especially products with small particle size, high sphericity, low loss, good dispersibility and stable amorphous / nanocrystalline structure, in order to meet the performance requirements of high frequency and high power devices.

[0003] Existing methods for preparing soft magnetic powders mainly include water atomization, gas atomization, mechanical ball milling, electrical discharge machining (EDM), and chemical methods, but all have significant limitations. While gas atomization and water atomization can prepare amorphous powders, the powder particle size is typically 5-150 μm, with a wide particle size distribution. The yield of fine powders with a particle size below 5 μm is extremely low (<1%). Furthermore, the alloy droplets are constrained by surface tension, requiring extremely high crushing energy to refine them to the micron or submicron level, which is difficult to achieve with conventional processes, resulting in poor magnetic domain structure and limited magnetic properties. Mechanical ball milling relies on mechanical force to crush raw materials, easily introducing impurities and strain defects, resulting in irregular powder morphology and poor flowability. Subsequent heat treatment easily leads to recrystallization or grain coarsening, resulting in poor stability of soft magnetic properties. Simultaneously, fine powders have a large specific surface area, making them prone to oxidation and moisture absorption, increasing the difficulty of insulating coating and pressing. For example, Chinese patent document CN117766249A discloses Fe-based amorphous powder prepared by ball milling, with an average particle size of 85 μm, which is unfavorable for subsequent coating and pressing, and results in high magnetic loss of the magnetic powder core. The energy release of the electrical discharge machining (EDM) method is difficult to control precisely, leading to uneven powder chemical composition and particle sizes typically in the tens of micrometers, which cannot meet the requirements of high-precision applications. Chemical methods are limited by reaction conditions, making it difficult to precisely control powder morphology and particle size, and also pose environmental pollution problems. In summary, existing technologies have significant shortcomings in particle size control, morphology regulation, structural stability, and preparation efficiency of soft magnetic powders. There is an urgent need to develop a novel preparation process to overcome existing technological bottlenecks and meet the industrialization needs of high-performance soft magnetic materials. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides an amorphous nanocrystalline soft magnetic alloy powder, its preparation method, and a magnetic powder core. The preparation method uses an instantaneous high-energy electrical pulse to rapidly bring the amorphous / nanocrystalline alloy material into a three-phase critical state, followed by explosive sputtering and ultra-rapid cooling to form the amorphous nanocrystalline soft magnetic alloy powder. The amorphous nanocrystalline soft magnetic alloy powder has the characteristics of small particle size, high sphericity, high yield, and excellent soft magnetic properties, and can maintain a stable amorphous nanocrystalline structure.

[0005] The specific technical solution of this invention is as follows:

[0006] In a first aspect, the present invention provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, comprising the following steps:

[0007] S1. Place the amorphous alloy material in the chamber of the high-energy electric pulse device, and maintain a distance of 5-10 cm between the high-voltage electrode and the ground electrode;

[0008] S2. In an inert gas environment, apply a high-energy electrical pulse with a voltage of 5-15 kV and a capacitance of 1-15 μF to the amorphous alloy material described in step S1, causing the amorphous alloy material to undergo melting, dynamic phase transformation, and cooling under the action of transient energy, wherein the cooling rate is ≥1×10⁻⁶. 6 K / s, to obtain amorphous nanocrystalline soft magnetic alloy powder, the median particle size of the amorphous nanocrystalline soft magnetic alloy powder is... D 50 The thickness is 0.5-5 μm and the sphericity is ≥0.85.

[0009] In one possible implementation, the composition of the amorphous alloy material in step S1 is selected from one of the following: Fe-B alloy, Fe-Si-B alloy, Fe-Si-BP alloy, Fe-Si-BC alloy, Fe-Si-B-Cu-Nb alloy, Fe-Co-Si-BP alloy, Fe-Ni-Si-BP alloy, Fe-Co-Ni-Si-B alloy, Fe-Si-BC-Cr alloy, Fe-Zr-B alloy, Fe-Zr-B-Cu alloy, Fe-Nb-B alloy, Fe-Hf-B alloy, Fe-BC alloy, Fe-PC alloy, Fe-Mo-B-Si alloy, and Fe-Si-BP-Ni-Cu-Mo alloy.

[0010] In one possible implementation, the atomic percentage composition of the amorphous alloy material in step S1 is selected from Fe. 73.5 Cu1Nb3Si 13.5 B9, Fe 80 B 20 Fe 85 B 15 Fe 78 Si9B 13 Fe 80 Si 10 B 10 Fe 75 Si 15 B 10 Fe 76 Si 10 B 10 P4, Fe 78 Si8B 10 P4, Fe 75 Si10 B 10 C5, Fe 74 Cu1Nb2Si 13 B 10 Fe 72 Cu1Nb4Si 14 B9, Fe 60 Co 20 Si 10 B5P5, Fe 55 Co 25 Si 10 B5P5, Fe 65 Co 15 Si 10 B5P5, Fe 65 Ni 10 Si 10 B 10 P5, Fe 70 Ni5Si 10 B 10 P5, Fe 69 Co 16 Ni1Si3B 11 Fe 70 Si 10 B 10 C5Cr5, Fe 68 Si 12 B 10 C5Cr5, Fe 72 Si8B 10 C5Cr5, Fe 78 Zr7B 15 Fe 75 Zr 10 B 15 Fe 77 Zr7B 15 Cu1, Fe 80 Nb5B 15、 Fe 78 Nb7B 15 Fe 78 Hf7B 15 Fe 86 Hf7B7, Fe 80 B 15 C5, Fe 85 P 10 C5, Fe 70 Mo5Si5B 20 Japanese Fe 82 Si 3.6 B 8.4 P 3.6 Ni1Mo 0.4 Cu1 medium type.

[0011] In one possible implementation, the amorphous alloy material in step S1 is a strip with a thickness of 10-100 μm and a width of 1-50 mm.

[0012] In one possible implementation, the high-voltage electrode and the grounding electrode are kept at a distance of 6-8 cm in step S1.

[0013] In one possible implementation, the discharge period of the high-energy electrical pulse in step S2 is 0.1-10 s.

[0014] Furthermore, the voltage of the high-energy electrical pulse in step S2 is 6-10 kV and the capacitance is 4-10 μF.

[0015] In one possible implementation, the pressure of the inert gas in the inert gas environment described in step S2 is 0.08-0.12 MPa.

[0016] Secondly, the present invention provides an amorphous nanocrystalline soft magnetic alloy powder, which is prepared by the above-described preparation method.

[0017] In one possible implementation, the saturation magnetization of the amorphous nanocrystalline soft magnetic alloy powder M s ≥105 emu / g.

[0018] Thirdly, the present invention provides a magnetic powder core made of the above-mentioned amorphous nanocrystalline soft magnetic alloy powder.

[0019] The positive and progressive effects of this invention are as follows:

[0020] This invention provides an amorphous nanocrystalline soft magnetic alloy powder, its preparation method, and a magnetic powder core. The preparation method employs high-energy electric pulse technology to achieve instantaneous and rapid heating and explosion of the amorphous alloy material, overcoming the limitations of melt surface tension and liquid viscosity in traditional methods. By precisely controlling energy input parameters (such as energy input voltage and energy storage capacitor) and spacing parameters, precise control of powder particle size is achieved, producing a high-sphericity soft magnetic powder with a median particle size of 0.5-5 μm. This significantly improves the uniformity and dispersibility of the powder, solving the problem of low particle size control accuracy in existing technologies. Furthermore, this preparation method has a simple process flow, low energy consumption, and avoids impurities and defects introduced in traditional multi-step processes, improving the purity and performance of the material. The prepared amorphous nanocrystalline soft magnetic alloy powder has the characteristics of small particle size, high sphericity, high saturation magnetization, low coercivity, and high yield, making it particularly suitable for high-frequency magnetic components and precision electronic devices. Attached Figure Description

[0021] Figure 1This is a schematic diagram illustrating the preparation method of amorphous nanocrystalline soft magnetic alloy powder in Examples 1-31;

[0022] Figure 2 This is a scanning electron microscope image of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1;

[0023] Figure 3 This is a particle size distribution curve of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1;

[0024] Figure 4 The X-ray diffraction patterns of the amorphous alloy ribbon and the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1 are shown below.

[0025] Figure 5 Differential scanning calorimetry (DSC) curves of the amorphous alloy strip and amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1;

[0026] Figure 6 The magnetometer curve of the vibrating sample of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1 is shown. Detailed Implementation

[0027] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described in detail below. It should be noted that the following embodiments are only used to illustrate the implementation methods and typical parameters of the present invention, and are not intended to limit the parameter range described in the present invention. Reasonable variations derived therefrom are still within the protection scope of the present invention.

[0028] It should be noted that the endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0029] Unless otherwise defined, all terms, symbols, and other scientific terms used herein are intended to have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. In some instances, terms having a conventional meaning are defined herein for clarification or ease of reference, and such definitions should not be construed as indicating a significant difference from conventional understanding in the art. The technical methods described or referenced herein are generally well understood by those skilled in the art and employed by conventional methods. Unless otherwise stated, the use of commercially available kits, reagents, and instruments shall be performed according to the manufacturer's instructions and parameters.

[0030] Terminology Explanation

[0031] High-energy electrical pulse: The "high-energy electrical pulse" mentioned in this invention refers to an instantaneous electrical power pulse generated by storing energy in a high-voltage capacitor and discharging it instantaneously. When this pulse acts on amorphous or nanocrystalline alloy materials, it can cause the energy absorbed by a unit mass of material to far exceed the energy required for melting and vaporization within a time range of milliseconds to microseconds. This forces the material to rapidly undergo melting, vaporization, and enter a solid-liquid-gas three-phase critical state, ultimately resulting in explosive expansion due to system instability. This provides the necessary conditions for subsequent ultra-fast cooling and the formation of amorphous and nanocrystalline powders.

[0032] The specific technical solution of this invention is as follows:

[0033] In a first aspect, the present invention provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, comprising the following steps:

[0034] S1. Place the amorphous alloy material in the chamber of the high-energy electric pulse device, and maintain a distance of 5-10 cm between the high-voltage electrode and the ground electrode;

[0035] S2. In an inert gas environment, apply a high-energy electrical pulse with a voltage of 5-15 kV and a capacitance of 1-15 μF to the amorphous alloy material described in step S1, causing the amorphous alloy material to undergo melting, dynamic phase transformation, and cooling under the action of transient energy, wherein the cooling rate is ≥1×10⁻⁶. 6 K / s, to obtain amorphous nanocrystalline soft magnetic alloy powder, the median particle size of the amorphous nanocrystalline soft magnetic alloy powder is... D 50 The thickness is 0.5-5 μm and the sphericity is ≥0.85.

[0036] The method for preparing amorphous nanocrystalline soft magnetic alloy powder provided by this invention employs high-energy electric pulse technology. By precisely controlling the voltage of the high-energy electric pulse to 5-15 kV and the capacitance to 1-15 μF, the energy density applied to the amorphous material is ensured to be sufficient for instantaneous melting and vaporization, entering a "solid-liquid-gas" three-phase critical state, while avoiding excessive plasmaization that could lead to component volatilization. Under this critical state, the inherent high surface tension and high viscosity of the melt are overcome by the explosive energy input, laying the foundation for the formation of micro-droplets. After the material destabilizes and explodes, it is torn into countless micron / submicron-sized molten droplets. During the splashing of these droplets, the surface tension spontaneously causes them to contract into a spherical shape with the lowest energy, forming highly spherical powder particles. The molten droplets in an inert gas environment have a velocity of not less than 1 × 10⁻⁶ kV. 6 Solidification occurs at a cooling rate of K / s. This process is so rapid that the droplets, while maintaining their spherical shape, do not have time for crystal growth or morphological distortion, thus preserving the small particle size and high sphericity, ultimately achieving a median particle size. D 50The powder used is an amorphous nanocrystalline soft magnetic alloy powder with a particle size of 0.5-5 μm and a sphericity ≥0.85. By controlling the distance between the high-voltage electrode and the grounding electrode to maintain 5-10 cm, energy loss in the medium is minimized, ensuring that most of the electrical energy is effectively absorbed by the material through the Joule heating effect, avoiding energy waste, and thus improving the yield (conversion rate) of the amorphous alloy material to the powder. A particle size of not less than 1×10⁻⁶ is used. 6 The extremely high cooling rate of K / s inhibits the long-range ordered arrangement of atoms (i.e., crystallization), forcing the alloy to solidify into an amorphous state. Simultaneously, the extremely high undercooling and stress generated during the explosion may induce the uniform precipitation of fine nanocrystalline phases within the amorphous matrix, forming an amorphous-nanocrystalline composite structure. Meanwhile, the median grain size... D 50 Amorphous nanocrystalline soft magnetic alloy powders with a thickness of 0.5-5 μm and a sphericity ≥0.85 can effectively reduce eddy current losses and exhibit higher stacking density and better flowability during subsequent preparation of magnetic powder cores, which is beneficial for obtaining superior magnetic properties. The amorphous phase is isotropic, while the uniformly distributed nanocrystalline phase can pin magnetic domain walls. Together, they enable the amorphous nanocrystalline soft magnetic alloy powder to possess both high saturation magnetization and low coercivity.

[0037] In one possible implementation, the amorphous alloy material in step S1 is composed of one of the following: Fe-B alloy, Fe-Si-B alloy, Fe-Si-BP alloy, Fe-Si-BC alloy, Fe-Si-B-Cu-Nb alloy, Fe-Co-Si-BP alloy, Fe-Ni-Si-BP alloy, Fe-Co-Ni-Si-B alloy, Fe-Si-BC-Cr alloy, Fe-Zr-B alloy, Fe-Zr-B-Cu alloy, Fe-Nb-B alloy, Fe-Hf-B alloy, Fe-BC alloy, Fe-PC alloy, Fe-Mo-B-Si alloy, and Fe-Si-BP-Ni-Cu-Mo alloy. All of these alloy systems possess excellent amorphous forming ability and readily form uniform amorphous structures during rapid solidification. This ensures that energy is uniformly absorbed during electrical explosion, achieving an overall critical phase transition rather than non-uniform localized melting, which is beneficial for improving the yield of amorphous nanocrystalline soft magnetic alloy powder.

[0038] In one possible implementation, the atomic percentage composition of the amorphous alloy material in step S1 is selected from Fe. 73.5 Cu1Nb3Si 13.5 B9, Fe 80 B 20 Fe 85 B 15 Fe 78 Si9B 13 Fe80 Yes 10 B 10 、Fe 75 Yes 15 B 10 、Fe 76 Yes 10 B 10 P4、Fe 78 Si8B 10 P4、Fe 75 Yes 10 B 10 C5、Fe 74 Cu1Nb2Si 13 B 10 、Fe 72 Cu1Nb4Si 14 B9、Fe 60 Co 20 Yes 10 B5P5、Fe 55 Co 25 Yes 10 B5P5、Fe 65 Co 15 Yes 10 B5P5、Fe 65 Ni 10 Yes 10 B 10 P5、Fe 70 Ni5Si 10 B 10 P5、Fe 69 Co 16 Ni1Si3B 11 、Fe 70 Yes 10 B 10 C5Cr5、Fe 68 Yes 12 B 10 C5Cr5、Fe 72 Si8B 10 C5Cr5、Fe 78 Zr7B 15 、Fe 75 Zr 10 B 15 、Fe 77 Zr7B 15 Cu1、Fe 80 Nb5B 15、 Fe 78 Nb7B 15 、Fe 78 Hf7B 15 、Fe 86 Hf7B7、Fe80 B 15 C5, Fe 85 P 10 C5, Fe 70 Mo5Si5B 20 and Fe 82 Si 3.6 B 8.4 P 3.6 Ni1Mo 0.4 One of Cu1. Amorphous alloy materials with the above atomic percentage composition are in the optimal range of amorphous formation capability of the alloy system, which is beneficial for obtaining completely amorphous and non-crystalline materials when preparing initial amorphous alloy materials by rapid quenching.

[0039] In one possible implementation, the amorphous alloy material in step S1 is a strip with a thickness of 10-100 μm and a width of 1-50 mm. When the thickness of the amorphous alloy strip is in the range of 10-100 μm, the huge current (Joule heating) generated by the high-energy electric pulse can instantly penetrate the entire cross-section of the strip, ensuring that the material is heated synchronously and uniformly in the thickness direction; the width of 1-50 mm matches the electrode structure, ensuring that the plasma channel can be stably formed and expanded along the width direction of the strip during the electric pulse process, thereby triggering a uniform and controllable explosion; uniform heating and uniform explosion are beneficial to obtaining amorphous nanocrystalline soft magnetic alloy powder with a more uniform particle size distribution.

[0040] In one possible implementation, the high-voltage electrode and the grounding electrode in step S1 are maintained at a distance of 6-8 cm. When the distance between the high-voltage electrode and the grounding electrode is within the range of 6-8 cm, the plasma channel formed after breakdown can quickly and stably bridge the two electrodes, forming a low-resistance path. This ensures that the enormous energy stored in the capacitor can be efficiently and centrally released onto the amorphous alloy material through this channel, converting it into effective Joule heat for the melting and phase transition of the material. This efficient energy utilization is beneficial for improving the median particle size. D 50 The yield of amorphous nanocrystalline soft magnetic alloy powder with a diameter of 2-5 μm and a sphericity ≥0.85.

[0041] In one possible implementation, the discharge period of the high-energy electrical pulse in step S2 is 0.1-10 s. Each electrical explosion generates instantaneous high temperature and shock wave within the cavity. The 0.1-10 s discharge period allows the inert gas flow to remove excess heat and restores the temperature, pressure, and airflow field within the cavity to a stable initial state before the next discharge, further ensuring an extremely high cooling rate for the explosively ejected droplets.

[0042] Further, in step S2, the voltage of the high-energy electrical pulse is 6-10 kV and the capacitance is 4-10 μF. Controlling the voltage of the high-energy electrical pulse to 6-10 kV and the capacitance to 4-10 μF ensures that the energy density input to the amorphous alloy material precisely matches the heat capacity and phase transition threshold of the alloy material, thereby controlling the median particle size of the powder. D 50 It is stable at 2-5 μm.

[0043] In one possible implementation, the pressure of the inert gas in the inert gas environment described in step S2 is 0.08-0.12 MPa. When the inert gas pressure is 0.08-0.12 MPa, on the one hand, the molecular density of the inert gas ensures sufficient heat exchange efficiency, controlling the cooling rate of the molten droplets to within 1×10⁻⁶. 6 K / s-2×10 7 The K / s range is conducive to the formation of high-performance structures with fine nanocrystals and a high proportion of amorphous materials; on the other hand, it allows the molten droplets to shrink into regular spheres under the balance of their own surface tension and the gas resistance of the inert gas, which is beneficial to improving the sphericity of amorphous nanocrystalline soft magnetic alloy powder.

[0044] Secondly, the present invention provides an amorphous nanocrystalline soft magnetic alloy powder, which is prepared by the above-described preparation method. The amorphous nanocrystalline soft magnetic alloy powder prepared by the above-described preparation method not only maintains a stable amorphous nanocrystalline structure, but also has the advantages of small particle size, high sphericity, high yield, and excellent soft magnetic properties.

[0045] In one possible implementation, the saturation magnetization of the amorphous nanocrystalline soft magnetic alloy powder M s ≥105 emu / g. Saturation magnetization of amorphous nanocrystalline alloy powder prepared by high-energy electric pulse technology. M s ≥105 emu / g, no need to increase powder saturation magnetization by adding rare earth elements (such as Nd, Sm) M s This helps reduce costs.

[0046] Thirdly, the present invention provides a magnetic powder core made of the above-mentioned amorphous nanocrystalline soft magnetic alloy powder.

[0047] The technical solution of the present invention will be further described below with reference to specific embodiments and comparative examples. All reagents used in the embodiments are commercially available or synthesized by conventional methods and can be used directly without further processing. The instruments used in the embodiments are also commercially available.

[0048] Example 1

[0049] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0050] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 73.5 Cu1Nb1Si 13.5 B9, with a thickness of 30 μm and a width of 10 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the ground electrode in the chamber was 8 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the ground electrode was 2 mm.

[0051] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 10 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 8.8 μF, and the discharge cycle of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to expand, melt, and vaporize rapidly. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it solidifies rapidly, with a cooling rate reaching 10 kV / s. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0052] Example 2

[0053] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0054] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 80 B 20 The amorphous alloy strip, with a thickness of 25 μm and a width of 10 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 8 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 3 mm.

[0055] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, an 8 kV voltage is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 6.6 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to rapidly expand, melt, and vaporize. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it rapidly solidifies, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0056] Example 3

[0057] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0058] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 85 B 15 The amorphous alloy strip, with a thickness of 22 μm and a width of 12 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 5 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 1.5 mm.

[0059] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 12 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 10 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to rapidly expand, melt, and vaporize. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it rapidly solidifies, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0060] Example 4

[0061] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0062] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 78 Si9B 13 The amorphous alloy strip, with a thickness of 28 μm and a width of 9 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 6 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 2.5 mm.

[0063] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 9 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 8.8 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to expand, melt, and vaporize rapidly. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it solidifies rapidly, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0064] Example 5

[0065] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0066] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 80 Si 10 B 10 The amorphous alloy strip, with a thickness of 26 μm and a width of 11 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 °C for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 6 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 1.8 mm.

[0067] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, an 11 kV voltage is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 9.2 μF, and the discharge cycle of the high-energy electrical pulse is 2 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to rapidly expand, melt, and vaporize. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it rapidly solidifies, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0068] Example 6

[0069] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0070] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 75 Si 15 B 10 The amorphous alloy strip, with a thickness of 32 μm and a width of 7 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 °C for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 6 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 2 mm.

[0071] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 7 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 5.5 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to expand, melt, and vaporize rapidly. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it solidifies rapidly, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0072] Example 7

[0073] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0074] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 76 Si 10 B 10 P4, with a thickness of 20 μm and a width of 14 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the ground electrode in the chamber was 9 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the ground electrode was 1.2 mm.

[0075] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 13 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 11 μF, and the discharge cycle of the high-energy electrical pulse is 3 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to rapidly expand, melt, and vaporize. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it rapidly solidifies, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0076] Example 8

[0077] This embodiment provides a method for preparing amorphous / nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0078] S1. Cut the amorphous alloy strip into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 78 Si8B 10 P4, with a thickness of 35 μm and a width of 6 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the ground electrode in the chamber was 6 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the ground electrode was 3.5 mm.

[0079] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 6 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 4.4 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to expand, melt, and vaporize rapidly. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it solidifies rapidly, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0080] Example 9

[0081] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0082] S1. Cut the amorphous alloy wire into 1 m long segments. The atomic percentage formula of the amorphous alloy wire is Fe. 75 Si 10 B 10 C5 is ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60 ℃ for 2 h. It is then wound onto a wire feeding wheel and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber is 10 cm, and the distance between the amorphous alloy wire and the high-voltage electrode and the grounding electrode is 1 mm.

[0083] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a voltage of 14 kV is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 10.5 μF, and the discharge cycle of the high-energy electrical pulse is 5 s. This ionizes the inert gas between the electrode and the amorphous alloy wire, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to expand, melt, and vaporize rapidly. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it solidifies rapidly, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline soft magnetic alloy powder.

[0084] Example 10

[0085] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0086] S1. Cut the amorphous alloy strip obtained in step S0 into 1 m long segments. The atomic percentage formula of the amorphous alloy strip is Fe. 74 Cu1Nb2Si 13 B 10 The amorphous alloy strip, with a thickness of 38 μm and a width of 15 mm, was ultrasonically cleaned with anhydrous ethanol for 12 min and vacuum dried at 60℃ for 2 h. It was then wound onto a feed roller and placed in the chamber of a high-energy electric pulse device. The distance between the high-voltage electrode and the grounding electrode in the chamber was 8 cm, and the distance between the amorphous alloy strip and the high-voltage electrode and the grounding electrode was 5 mm.

[0087] S2. Evacuate the chamber until the vacuum level is less than 5 × 10⁻⁶. -3 Pa, then argon gas is introduced into the chamber until the pressure reaches 0.095 MPa. The protective atmosphere of argon gas prevents oxidation of the molten alloy, which is beneficial for obtaining pure powder. Next, a 5 kV voltage is input to the high-voltage electrode through a high-voltage power supply, the energy storage capacitor is set to 2.2 μF, and the discharge period of the high-energy electrical pulse is 1 s. This ionizes the inert gas between the electrode and the amorphous alloy strip, forming a plasma channel. Electrical energy is transferred to the strip through the plasma channel, causing it to rapidly expand, melt, and vaporize. Finally, it destabilizes and explodes, splashing into the argon gas medium at extremely high speed. After contacting the argon gas cooling medium, it rapidly solidifies, with a cooling rate reaching 10. 7 K / s, forming amorphous nanocrystalline alloy powder.

[0088] Example 11

[0089] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 1 in that the alloy composition of the amorphous alloy strip is Fe. 72 Cu1Nb4Si 14 B9.

[0090] Example 12

[0091] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 3 in that the alloy composition of the amorphous alloy strip is Fe. 60 Co 20 Si 10 B5P5.

[0092] Example 13

[0093] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 2 in that the alloy composition of the amorphous alloy strip is Fe. 55 Co 25 Si 10 B5P5.

[0094] Example 14

[0095] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Example 9 in that the alloy composition of the amorphous alloy wire is Fe. 65 Co 15 Si 10 B5P5.

[0096] Example 15

[0097] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 4 in that the alloy composition of the amorphous alloy strip is Fe. 65 Ni 10 Si 10 B 10 P5.

[0098] Example 16

[0099] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 70 Ni5Si 10 B 10 P5.

[0100] Example 17

[0101] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 6 in that the alloy composition of the amorphous alloy strip is Fe. 69 Co 16 Ni1Si3B 11 .

[0102] Example 18

[0103] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 7 in that the alloy composition of the amorphous alloy strip is Fe. 70 Si 10 B 10 C5Cr5.

[0104] Example 19

[0105] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 1 in that the alloy composition of the amorphous alloy strip is Fe. 68 Si 12 B 10 C5Cr5.

[0106] Example 20

[0107] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 3 in that the alloy composition of the amorphous alloy strip is Fe. 72 Si8B 10 C5Cr5.

[0108] Example 21

[0109] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 2 in that the alloy composition of the amorphous alloy strip is Fe. 78 Zr7B 15 .

[0110] Example 22

[0111] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 75 Zr 10 B 15 .

[0112] Example 23

[0113] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 77 Zr7B 15 Cu1.

[0114] Example 24

[0115] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 80 Nb5B 15 .

[0116] Example 25

[0117] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 78 Nb7B 15 .

[0118] Example 26

[0119] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 78 Hf7B 15 .

[0120] Example 27

[0121] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 86 Hf7B7.

[0122] Example 28

[0123] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 80 B 15 C5.

[0124] Example 29

[0125] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 80 P 15 C5.

[0126] Example 30

[0127] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 70 Mo5Si5B 20 .

[0128] Example 31

[0129] This embodiment provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, which differs from Embodiment 5 in that the alloy composition of the amorphous alloy strip is Fe. 82 Si 3.6 B 8.4 P 3.6 Ni1Mo 0.4 Cu1.

[0130] Example 32

[0131] This embodiment provides a magnetic powder core, which is made from amorphous nanocrystalline soft magnetic alloy powder obtained in Example 1, through insulating coating, pressing and annealing.

[0132] Comparative Example 1

[0133] This comparative example provides a method for preparing amorphous nanocrystalline soft magnetic alloy powder, the preparation steps of which are as follows:

[0134] 1. Cut the amorphous ribbon into fragments. The atomic percentage formula of the amorphous alloy ribbon is Fe. 73.5 Cu1Nb3Si 13.5B9, with a thickness of 30 μm and a width of 10 mm, was placed in a vacuum induction melting furnace for remelting. The temperature was controlled at 1550 ℃ and held for 5 min to ensure the homogenization of the molten alloy elements. A nozzle with a diameter of 1.2 mm was used, with 6.0 MPa high-pressure argon gas as the atomizing medium, and the gas pressure in the atomization chamber was maintained at 0.1 MPa. The molten alloy was sprayed vertically downward through the nozzle, and the high-pressure argon gas was sprayed at high speed from the annular nozzle, breaking the molten metal or alloy liquid flow into tiny droplets. The droplets were rapidly cooled in the atomization chamber to form amorphous nanocrystalline soft magnetic alloy powder.

[0135] The amorphous nanocrystalline soft magnetic alloy powders prepared in Examples 1-31 and Comparative Example 1 were subjected to the following performance tests and characterizations: the morphology and size of the powders were observed using a scanning electron microscope (SEM), the median particle size of the powders was measured using a laser particle size analyzer (LDPA), the microstructure of the strips and powders was analyzed using an X-ray diffractometer (XRD), the thermal properties of the strips and powders were analyzed using a differential scanning calorimeter (DSC), and the magnetic properties of the powders were measured using a vibrating sample magnetometer (VSM).

[0136] Figure 1 This is a schematic diagram illustrating the preparation method of amorphous nanocrystalline soft magnetic alloy powder in Examples 1-31. It mainly includes the following parts:

[0137] (1) Current heating effect and high-voltage explosion effect: A high-energy instantaneous flow is applied to the amorphous alloy strip / wire through electrodes and capacitors. The gas medium between the strip / wire and the electrodes breaks down to form a plasma channel, constituting a high-voltage circuit. A high-density pulsed current passes through the amorphous nanocrystalline alloy strip / wire, according to Joule's law ( Q = I ² Rt ,in Q For heat, I For current intensity, R For resistance, t (For time), the tape / filament rapidly generates a large amount of heat, causing a sharp increase in temperature and pressure, thus entering the three-phase critical state.

[0138] (2) Dynamic phase transition: Amorphous nanocrystalline alloy strips / wires first expand and melt, and then vaporize; under the action of a strong electric field, the vaporization region ionizes to form high temperature and high pressure plasma. The rapid expansion of the plasma and the imbalance of the material's own constraint force cause the system to become unstable, triggering a violent phase transition and generating shock waves that cause the molten or vaporized metal or alloy material to be ejected into the surrounding environment at high speed.

[0139] (3) Powder formation: The sprayed metal or alloy vapor and droplets undergo ultra-rapid cooling in an inert atmosphere, forming ultrafine powder through a nucleation-growth mechanism.

[0140] Figure 2The image shows a scanning electron microscope (SEM) image of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1. Most powder particles exhibit an approximately spherical morphology, without obvious sharp edges or irregular protrusions, with a sphericity ≥ 0.85. This high sphericity improves the powder's flowability, allowing for more uniform insulation coating and cold pressing during the subsequent preparation of the soft magnetic composite magnetic powder core, ensuring the density uniformity and magnetic performance stability of the core. Furthermore, there is minimal agglomeration of the powder particles, with only a few small agglomerates (formed by slight aggregation of extremely fine particles) and no large agglomerates.

[0141] Figure 3 This is a particle size distribution curve of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1. The median particle size of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1 is shown. D 50 =3.44 μm, indicating that the powder particle size is within the micrometer range. Small particle size can reduce eddy current loss and improve high-frequency performance, meeting the requirements of high-frequency soft magnetic powder cores for small particle size powder. The particle size distribution curve shows a bimodal distribution. The first peak is concentrated in the 1.5-4 μm range, which is the main particle size range of the powder, indicating that most particles are uniform in size and within the small particle size range. The second peak is concentrated in the 21-30 μm range, possibly due to powder agglomeration. This distribution feature of small particle size as the main component and large particle size as the minority reflects the advantages of the high-energy electric pulse critical state preparation process in this technical solution: by precisely controlling the electric pulse parameters (voltage, capacitance, and distance between electrodes), a narrow distribution and small size control of powder particle size are achieved, avoiding the defects of wide particle size distribution and large particles in the traditional gas atomization method and the easy generation of ultra-large agglomerates in the mechanical ball milling method.

[0142] Figure 4 The images show the X-ray diffraction patterns of the amorphous alloy ribbon and the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1. The XRD pattern of the amorphous alloy ribbon shows a dome-shaped peak, indicating an amorphous structure. The XRD pattern of the amorphous nanocrystalline soft magnetic alloy powder shows three sharp crystalline diffraction peaks, located at approximately 45°, 65°, and 82.5°, corresponding to the characteristic crystal planes of the α-Fe crystalline phase, indicating that the prepared amorphous nanocrystalline soft magnetic alloy powder is of the α-Fe crystalline phase. Calculations using the Scherrer equation show a grain size of 17 nm, confirming the nanocrystalline structure of the soft magnetic alloy powder. α-Fe nanocrystals provide high saturation magnetization, ensuring the material's magnetic induction capability under strong magnetic fields.

[0143] Figure 5The figures show the differential scanning calorimetry (DSC) curves of the amorphous alloy ribbon and the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1. As can be seen from the figures, the DSC curve of the amorphous alloy ribbon shows a significant exothermic peak in the 500-600 °C range. This is the crystallization peak, representing the transition from an amorphous to a crystalline state, where atoms change from a disordered arrangement to an ordered crystalline structure, releasing heat of crystallization, which manifests as an exothermic peak. The DSC curve of the amorphous nanocrystalline soft magnetic alloy powder does not show a significant crystallization peak at 500-600 °C, but only a weaker exothermic peak appears at higher temperatures above 700 °C. This indicates that after the high-energy electric pulse preparation process, the amorphous nanocrystalline alloy powder has completed the nanocrystalline crystallization process. The weak peak above 700 °C corresponds to the secondary phase transition or grain growth of the nanocrystals, but the temperature required for this process is much higher than the operating temperature of conventional soft magnetic components (usually <300 °C), therefore it has no impact on practical applications.

[0144] Figure 6 The image shows the magnetometer curve of the vibrating sample of the amorphous nanocrystalline soft magnetic alloy powder prepared in Example 1. The curve exhibits a typical soft magnetic hysteresis loop shape, reflecting the easy magnetization and demagnetization characteristics of the amorphous nanocrystalline soft magnetic alloy powder. The saturation magnetization of the amorphous nanocrystalline soft magnetic alloy powder is 130.69 emu / g. Rapid saturation in the low magnetic field range of 0-5000 Oe indicates extremely low coercivity of the amorphous nanocrystalline soft magnetic alloy powder. The curve rises steeply in the 0-5000 Oe low magnetic field region, indicating high permeability and strong response to weak magnetic fields, making it suitable for the high permeability requirements of high-frequency inductor devices (such as 5G base station inductors).

[0145] Table 1 shows the performance data of the amorphous nanocrystalline soft magnetic alloy powders prepared in Examples 1-31 and Comparative Example 1. The data in the table show the median particle size of the amorphous nanocrystalline soft magnetic alloy powders prepared in Examples 1-31. D 50 Saturation magnetization in the range of 1.8–5 μm M s The concentration ranges from 105.5 to 160.5 emu / g, with possible variations between different compositions. The yield is consistently greater than 90%, and the grain size is less than 30 nm. This demonstrates that the high-energy electric pulse critical state preparation process in this technical solution, through precise control of electric pulse parameters (voltage, capacitance, and distance between electrodes), can produce amorphous nanocrystalline soft magnetic alloy powders with small particle size, high sphericity, high yield, and excellent soft magnetic properties.

[0146] Table 1 Performance data of amorphous nanocrystalline soft magnetic alloy powders in Examples 1-31 and Comparative Example 1

[0147] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing amorphous nanocrystalline soft magnetic alloy powder, characterized in that, Includes the following steps: S1. Place the amorphous alloy material in the chamber of the high-energy electric pulse device, and maintain a distance of 5-10 cm between the high-voltage electrode and the ground electrode. S2. In an inert gas environment, a high-energy electrical pulse with a voltage of 5-15 kV and a capacitance of 2-15 μF is applied to the amorphous alloy material described in step S1, causing the amorphous alloy material to undergo melting, dynamic phase transformation, and cooling under transient energy, thereby obtaining amorphous nanocrystalline soft magnetic alloy powder. The median particle size of the amorphous nanocrystalline soft magnetic alloy powder is... D 50 The diameter is 1.8-5 μm, and the sphericity is ≥0.

85.

2. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, The amorphous alloy material mentioned in step S1 is selected from one of the following: Fe-B alloy, Fe-Si-B alloy, Fe-Si-BP alloy, Fe-Si-BC alloy, Fe-Si-B-Cu-Nb alloy, Fe-Co-Si-BP alloy, Fe-Ni-Si-BP alloy, Fe-Co-Ni-Si-B alloy, Fe-Si-BC-Cr alloy, Fe-Zr-B alloy, Fe-Zr-B-Cu alloy, Fe-Nb-B alloy, Fe-Hf-B alloy, Fe-BC alloy, Fe-PC alloy, Fe-Mo-B-Si alloy, and Fe-Si-BP-Ni-Cu-Mo alloy.

3. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 2, characterized in that, The atomic percentage composition formula of the amorphous alloy material in step S1 is selected from Fe. 73.5 Cu1Nb3Si 13.5 B9, Fe 80 B 20 Fe 85 B 15 Fe 78 Si9B 13 Fe 80 Si 10 B 10 Fe 75 Si 15 B 10 Fe 76 Si 10 B 10 P4, Fe 78 Si8B 10 P4, Fe 75 Si 10 B 10 C5, Fe 74 Cu1Nb2Si 13 B 10 Fe 72 Cu1Nb4Si 14 B9, Fe 60 Co 20 Si 10 B5P5, Fe 55 Co 25 Si 10 B5P5, Fe 65 Co 15 Si 10 B5P5, Fe 65 Ni 10 Si 10 B 10 P5, Fe 70 Ni5Si 10 B 10 P5, Fe 69 Co 16 Ni1Si3B 11 Fe 70 Si 10 B 10 C5Cr5, Fe 68 Si 12 B 10 C5Cr5, Fe 72 Si8B 10 C5Cr5, Fe 78 Zr7B 15 Fe 75 Zr 10 B 15 Fe 77 Zr7B 15 Cu1, Fe 80 Nb5B 15、 Fe 78 Nb7B 15 Fe 78 Hf7B 15 Fe 86 Hf7B7, Fe 80 B 15 C5, Fe 85 P 10 C5, Fe 70 Mo5Si5B 20 and Fe 82 Si 3.6 B 8.4 P 3.6 Ni1Mo 0.4 One of Cu1.

4. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, The amorphous alloy material mentioned in step S1 is a strip with a thickness of 10-100 μm and a width of 1-50 mm.

5. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, In step S1, the high-voltage electrode and the grounding electrode are kept at a distance of 6-8 cm.

6. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, The discharge period of the high-energy electrical pulse in step S2 is 0.1-10 s.

7. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, The voltage of the high-energy electrical pulse in step S2 is 6-10 kV and the capacitance is 4-10 μF.

8. The method for preparing amorphous nanocrystalline soft magnetic alloy powder according to claim 1, characterized in that, The pressure of the inert gas in the inert gas environment described in step S2 is 0.08-0.12 MPa.

9. An amorphous nanocrystalline soft magnetic alloy powder, characterized in that, It is prepared by the method for preparing amorphous nanocrystalline soft magnetic alloy powder according to any one of claims 1-8.

10. The amorphous nanocrystalline soft magnetic alloy powder according to claim 9, characterized in that, The saturation magnetization of the amorphous nanocrystalline soft magnetic alloy powder M s ≥105 emu / g.

11. A magnetic powder core, characterized in that, It is made from the amorphous nanocrystalline soft magnetic alloy powder described in claim 9 or 10 through insulating coating, pressing and annealing.

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