Amorphous nanocrystalline soft magnetic composite powder material and preparation method thereof

Abstract

The invention discloses an amorphous nanocrystalline soft magnetic composite powder material and a preparation method thereof, and relates to the field of amorphous nanocrystalline soft magnetic composite powder materials, and the amorphous nanocrystalline soft magnetic composite powder material is prepared from Fe-Si-B series amorphous alloy powder raw materials through melting, modification, crystallization, screening, composite insulation coating and environment-friendly recovery processes. Compared with the prior art, the nanoscale amorphous / nanocrystalline soft magnetic composite powder material prepared by the method has higher magnetic conductivity, lower coercive force, more excellent insulating property and more uniform particle size distribution, and is suitable for electromagnetic application with higher frequency and higher performance.

Description

Technical Field

[0001] The present invention relates to the field of amorphous nanocrystalline soft magnetic composite powder materials, in particular to an amorphous nanocrystalline soft magnetic composite powder material and a preparation method thereof. Background Art

[0002] Amorphous / nanocrystalline soft magnetic composite powder materials have broad application prospects in the fields of electronic information, energy, automobiles, and intelligent manufacturing due to their excellent electromagnetic properties. However, the amorphous alloy powders prepared in existing technologies have large particle sizes, making them difficult to meet the requirements of high-performance soft magnetic composite materials. In addition, the crystallization treatment of amorphous alloy powders in existing technologies is not precise enough, resulting in unstable material properties. Therefore, it is necessary to propose an amorphous / nanocrystalline soft magnetic composite powder material and its preparation method to address these issues. Summary of the Invention

[0003] The purpose of the present invention is to provide an amorphous nanocrystalline soft magnetic composite powder material and a preparation method thereof, and to prepare a nano-scale amorphous alloy powder with smaller particle size and better performance by modifying the alloy powder intermediate, and to further optimize the material performance by screening out the crystallized part.

[0004] To achieve the above-mentioned purpose, the present invention provides the following technical solution: an amorphous nanocrystalline soft magnetic composite powder material, comprising an amorphous nanocrystalline soft magnetic composite powder material made from Fe-Si-B amorphous alloy powder raw materials through melting, modification, crystallization, screening, composite insulation coating and environmentally friendly recycling processes.

[0005] The present invention also discloses a method for preparing an amorphous nanocrystalline soft magnetic composite powder material, which is used to prepare the amorphous nanocrystalline soft magnetic composite powder material, and further comprises the following steps:

[0006] S1: Nano-scale modification of the alloy powder intermediate, melting the raw materials for forming the amorphous alloy powder to obtain a molten alloy, and atomizing the molten alloy with an inert gas jet under vacuum or a protective atmosphere to obtain an alloy powder intermediate;

[0007] The alloy powder intermediate is surface modified using nano-surfactants, and the adhesion of the surfactant is further enhanced through plasma treatment technology, so that the surfactant is evenly coated on the powder surface;

[0008] Ultrasonic dispersion technology combined with high-energy ball milling process is used to process the modified alloy powder intermediate to make its particle size reach nanometer level. High-energy ball milling process can achieve nano-size of powder in a short time and reduce agglomeration.

[0009] S2: Precise crystallization treatment pre-screening, the nano-sized amorphous alloy powder is subjected to precise heat treatment, using the segmented heating mode, first heating to 450℃ at a heating rate of 5℃ / min, holding for 1 hour; then heating to 773K at a heating rate of 2℃ / min, holding for 1 hour;

[0010] The amorphous alloy powder after crystallization is screened by using intelligent screening technology. By setting the particle size threshold, the crystallized part is automatically screened out, and the nano-sized amorphous alloy powder of the uncrystallized part is retained.

[0011] S3: Optimization of composite insulation coating, the nano-sized amorphous alloy powder of the uncrystallized part is subjected to surface activation treatment, using 1wt% silane solution combined with ultraviolet light curing technology to further enhance the bonding force between the surface active agent and the powder.

[0012] The nano-sized amorphous alloy powder after surface activation is subjected to multi-layer composite insulation coating by sol-gel method. First, an acidic aluminum isopropyl alcohol precursor solution is used for primary coating, and then a silicon dioxide precursor solution is used for secondary coating to form a double-layer insulation structure.

[0013] S4: Environmental protection and recycling process, green solvent substitution, in the sol-gel method, a green solvent is used instead of a traditional organic solvent to reduce the emission of volatile organic compounds.

[0014] The crystallized part powder screened out in the screening process is subjected to recycling treatment. Through mechanical grinding and chemical reduction process, it is reconverted into amorphous powder and used again to prepare nano-sized amorphous alloy powder.

[0015] Preferably, the nano-sized surface active agent includes nano-sized silane coupling agent.

[0016] Preferably, the particle size of the modified alloy powder intermediate after treatment in S1 is between 10-50nm.

[0017] Preferably, the intelligent screening technology in S2 uses a laser particle size analyzer combined with an automatic screening device.

[0018] Preferably, the particle size threshold in S2 is 100nm.

[0019] Preferably, the green solvent in S4 includes ethanol instead of anhydrous ethanol or a bio-based solvent.

[0020] Technical effects and advantages of the present application:

[0021] 1. Nano-sized modification technology: By using nano-sized surface active agent and plasma treatment technology, the surface activity and uniformity of the alloy powder intermediate are significantly improved, and the particle size is smaller and more uniform.

[0022] 2. Precise crystallization and screening: The segmented heating heat treatment method and intelligent screening technology can more accurately control the crystallization process, improve screening efficiency and reduce material waste.

[0023] 3. Multi-layer composite insulation coating: The use of multi-layer composite insulation coating technology significantly improves the insulation performance and mechanical strength of the material, making it suitable for higher frequency and higher performance electromagnetic applications.

[0024] 4. Environmental protection and recycling process: The use of green solvents and powder recovery process reduces environmental pollution, improves resource utilization, and meets the requirements of sustainable development. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a diagram of the preparation method of the amorphous nanocrystalline soft magnetic composite powder material of the present invention. DETAILED DESCRIPTION

[0026] Example 1:

[0027] The present invention provides Figure 1 The method for preparing an amorphous nanocrystalline soft magnetic composite powder material shown includes the following steps:

[0028] The first step is the preparation of alloy powder intermediate;

[0029] The raw materials for forming the amorphous alloy powder are melted to obtain a molten alloy, and the molten alloy is atomized by using an inert gas jet under vacuum or a protective atmosphere to obtain an alloy powder intermediate.

[0030] Specifically, 10 g of Fe-Si-B amorphous alloy powder raw material was melted to obtain a molten alloy; the molten alloy was atomized by a nitrogen jet under vacuum conditions with an atomizing gas pressure of 6 MPa to obtain an alloy powder intermediate.

[0031] The second step is the preparation of nano-scale amorphous alloy powder;

[0032] The alloy powder intermediate was surface modified and coated with nano-surfactant. The modified alloy powder intermediate was treated with ultrasonic dispersion technology to make its particle size reach nano-level. The nano-level alloy powder intermediate was rapidly cooled at a cooling rate of 10 6 ~10 8 K / s, and nano-scale amorphous alloy powder was obtained.

[0033] Specifically, the surface of the alloy powder intermediate is modified by using 1wt% of nano-silane coupling agent; the modified alloy powder intermediate is treated by ultrasonic dispersion technology to make its particle size reach 50-100nm; the nano-alloy powder intermediate is rapidly cooled at a cooling rate of 10 8 K / s, and nano-scale amorphous alloy powder was obtained.

[0034] The third step is crystallization treatment and screening;

[0035] The nano-scale amorphous alloy powder is heat-treated to nano-crystallize a portion of the amorphous material. The crystallized amorphous alloy powder is screened out using a screening technique to retain the uncrystallized portion of the nano-scale amorphous alloy powder.

[0036] Specifically, the nano-scale amorphous alloy powder is heat treated at 773K for 1 hour at a heating rate of 5°C / min. Screening technology is used to screen out the crystallized portion with a particle size greater than 200nm, and retain the uncrystallized portion of the nano-scale amorphous alloy powder.

[0037] The fourth step is composite insulation coating;

[0038] The nano-scale amorphous alloy powder of the non-crystallized part is subjected to surface activation treatment; the surface-activated nano-scale amorphous alloy powder is subjected to composite insulation coating by a sol-gel method to obtain a nano-scale amorphous / nanocrystalline soft magnetic composite powder material with a uniform coating on the surface.

[0039] Specifically, a 1 wt% silane solution is used to perform surface activation treatment on the uncrystallized portion of the nano-scale amorphous alloy powder; a sol-gel method is used to perform composite insulation coating on the surface-activated nano-scale amorphous alloy powder, the precursor solution is an acidic aluminum isopropoxide precursor solution, the stirring speed is 600 r / min, and the reaction is carried out for 1 hour, followed by washing and drying.

[0040] Comparative Example 1:

[0041] The first step is the preparation of alloy powder intermediate;

[0042] 10g of Fe-Si-B amorphous alloy powder raw material was melted to obtain a molten alloy; the molten alloy was atomized by a nitrogen jet under vacuum conditions with an atomizing gas pressure of 6 MPa to obtain an alloy powder intermediate.

[0043] The second step is the preparation of nano-scale amorphous alloy powder;

[0044] The surface of the alloy powder intermediate was modified by using 1wt% nano-silane coupling agent; the modified alloy powder intermediate was treated by ultrasonic dispersion technology to make its particle size reach 50-100nm; the nano-alloy powder intermediate was rapidly cooled at a cooling rate of 10 6 K / s, and nano-scale amorphous alloy powder was obtained.

[0045] The third step is crystallization treatment and screening;

[0046] The nano-scale amorphous alloy powder was heat treated at 773K for 1 hour at a heating rate of 5°C / min. The composite insulation coating was directly performed without screening.

[0047] The fourth step is composite insulation coating;

[0048] The surface of the nano-scale amorphous alloy powder was activated using a 1wt% silane solution; the surface-activated nano-scale amorphous alloy powder was composite-insulated and coated using a sol-gel method. The precursor solution was an acidic aluminum isopropoxide precursor solution, the stirring speed was 600 r / min, and the powder was reacted for 1 hour before washing and drying.

[0049] The present invention successfully prepares nano-scale amorphous alloy powder with smaller particle size and better performance through the modification of nano-scale surfactants and ultrasonic dispersion technology; by screening out the crystallized part, the performance of the amorphous nano-crystalline soft magnetic composite powder material is further optimized; compared with the existing technology, the material prepared by the present invention has higher magnetic permeability, lower coercive force and better insulation performance, and is suitable for higher frequency and higher performance electromagnetic applications.

[0050] Example 2:

[0051] The present invention provides Figure 1 The method for preparing an amorphous nanocrystalline soft magnetic composite powder material shown includes the following steps:

[0052] The first step is nano-scale modification of the alloy powder intermediate;

[0053] S101: melting and atomizing raw materials, melting raw materials for forming amorphous alloy powder to obtain molten alloy, and atomizing the molten alloy using an inert gas jet under vacuum or protective atmosphere to obtain an alloy powder intermediate;

[0054] S102: Nano-scale surface modification, using nano-scale surfactants (such as nano-scale silane coupling agents) to perform surface modification treatment on the alloy powder intermediate, and further enhance the adhesion of the surfactant through plasma treatment technology (Plasma Treatment), so that the surfactant is evenly coated on the powder surface;

[0055] S103: Ultrasonic dispersion and ball milling, using ultrasonic dispersion technology combined with high-energy ball milling (HEBM) process to process the modified alloy powder intermediate to make its particle size reach the nano level (10-50nm). The high-energy ball milling process can achieve powder nano-sizing in a short time and reduce agglomeration.

[0056] Specifically, 10g of Fe-Si-B amorphous alloy powder raw material is melted to obtain a molten alloy; the molten alloy is atomized using a nitrogen jet under vacuum conditions with an atomizing gas pressure of 6 MPa to obtain an alloy powder intermediate; the alloy powder intermediate is surface-modified using 1wt% of a nano-silane coupling agent, and a plasma treatment technology is used to uniformly coat the surface of the surfactant; and the modified alloy powder intermediate is treated using an ultrasonic dispersion technology combined with a high-energy ball milling process to achieve a particle size of 30-50nm.

[0057] The second step is precise crystallization treatment and screening;

[0058] S201: Precision heat treatment: Precision heat treatment of nano-scale amorphous alloy powder is performed using a staged heating method. The temperature is first raised to 450°C at a heating rate of 5°C / min and kept at this temperature for 1 hour. The temperature is then raised to 773K at a heating rate of 2°C / min and kept at this temperature for 1 hour. This staged heating method can more accurately control the crystallization process and reduce over-crystallization.

[0059] S202: Intelligent screening technology uses intelligent screening technology (such as a laser particle size analyzer combined with an automatic screening device) to screen the crystallized amorphous alloy powder. By setting a particle size threshold (such as 100nm), the crystallized part is automatically screened out, and the non-crystallized part of the nano-scale amorphous alloy powder is retained. Intelligent screening technology can improve screening efficiency and reduce human errors.

[0060] Specifically, the nano-scale amorphous alloy powder is heat treated by keeping the temperature at 450°C for 1 hour and then raising the temperature to 773K and keeping the temperature for 1 hour; a laser particle size analyzer is used in combination with an automatic screening device, and the particle size threshold is set to 100nm to screen out the crystallized part and retain the non-crystallized part of the nano-scale amorphous alloy powder.

[0061] The third step is the optimization of composite insulation coating;

[0062] S301: Surface activation enhancement: Surface activation treatment is performed on the non-crystallized portion of the nano-scale amorphous alloy powder using a 1wt% silane solution combined with UV curing technology to further enhance the bonding between the surfactant and the powder;

[0063] S302: Multi-layer composite insulation coating, using the sol-gel method to perform multi-layer composite insulation coating on the surface-activated nano-scale amorphous alloy powder. First, an acidic aluminum isopropoxide precursor solution is used for the initial coating; then, a silicon dioxide (SiO2) precursor solution is used for the secondary coating to form a double-layer insulation structure; this multi-layer composite insulation coating can significantly improve the insulation performance and mechanical strength of the material.

[0064] Specifically, a 1wt% silane solution combined with ultraviolet curing technology is used to activate the surface of the uncrystallized part of the nano-scale amorphous alloy powder; a sol-gel method is used for multi-layer composite insulation coating: first, an acidic aluminum isopropoxide precursor solution is used for primary coating, and then a silicon dioxide precursor solution is used for secondary coating to form a double-layer insulation structure.

[0065] Step 4: Environmental protection and recycling process;

[0066] S401: Green solvent replacement: In the sol-gel method, green solvents (such as ethanol instead of anhydrous ethanol, or bio-based solvents) are used instead of traditional organic solvents to reduce the emission of volatile organic compounds (VOCs) and reduce environmental pollution;

[0067] S402: Powder recycling: The crystallized powder removed during the screening process is recycled. Through mechanical grinding and chemical reduction, it is converted back into amorphous powder and reused in the preparation of nano-scale amorphous alloy powder. This recycling process can reduce material waste and improve resource utilization.

[0068] Specifically, in the sol-gel method, ethanol is used instead of anhydrous ethanol as a solvent; the crystallized powder screened out during the screening process is mechanically ground and chemically reduced, and converted back into amorphous powder, which is used again to prepare nano-scale amorphous alloy powder.

[0069] Comparative Example 2:

[0070] The first step is nano-scale modification of the alloy powder intermediate. 10g of Fe-Si-B amorphous alloy powder raw material is melted to obtain a molten alloy. The molten alloy is atomized using a nitrogen jet under vacuum conditions with an atomizing gas pressure of 6 MPa to obtain an alloy powder intermediate. The alloy powder intermediate is surface-modified using 1wt% of a nano-silane coupling agent, but plasma treatment technology is not used. The modified alloy powder intermediate is treated only with ultrasonic dispersion technology, and the particle size reaches 50-100nm.

[0071] The second step is precise crystallization treatment and screening. Heat treatment is carried out directly at 773K for 1 hour at a heating rate of 5°C / min. Intelligent screening technology is not used and the crystallized part is manually screened out.

[0072] The third step is to optimize the composite insulation coating. The surface of the nano-scale amorphous alloy powder is activated using a 1wt% silane solution, but without combining it with UV curing technology; only an acidic aluminum isopropoxide precursor solution is used for single-layer insulation coating.

[0073] The fourth step is environmental protection and recycling process. Green solvents are not used to replace traditional organic solvents; the crystallized powder screened out during the screening process is not recycled.

[0074] The present invention significantly improves the surface activity and uniformity of the alloy powder intermediate through nano-surfactant and plasma treatment technology, resulting in a smaller particle size and more uniform distribution; the segmented heating heat treatment method and intelligent screening technology can more accurately control the crystallization process, improve screening efficiency, and reduce material waste; the use of multi-layer composite insulation coating technology significantly improves the insulation performance and mechanical strength of the material, making it suitable for higher frequency and higher performance electromagnetic applications; the use of green solvents and powder recovery processes reduces environmental pollution, improves resource utilization, and meets the requirements of sustainable development.

[0075] Compared with the existing technology, the nano-scale amorphous / nanocrystalline soft magnetic composite powder material prepared by the present invention has higher magnetic permeability, lower coercivity, better insulation performance and more uniform particle size distribution, and is suitable for higher frequency and higher performance electromagnetic applications.

Claims

1. An amorphous nanocrystalline soft magnetic composite powder material, characterized by: It includes amorphous nanocrystalline soft magnetic composite powder materials made from Fe-Si-B series amorphous alloy powder raw materials through melting, modification, crystallization, screening, composite insulation coating and environmentally friendly recycling processes.

2. A method for preparing an amorphous nanocrystalline soft magnetic composite powder material, characterized in that: The method for preparing the amorphous nanocrystalline soft magnetic composite powder material according to claim 1 further comprises the following steps: S1: Nano-scale modification of the alloy powder intermediate, melting the raw materials for forming the amorphous alloy powder to obtain a molten alloy, and atomizing the molten alloy with an inert gas jet under vacuum or a protective atmosphere to obtain an alloy powder intermediate; The alloy powder intermediate is surface modified using nano-surfactants, and the adhesion of the surfactant is further enhanced through plasma treatment technology, so that the surfactant is evenly coated on the powder surface; Ultrasonic dispersion technology combined with high-energy ball milling process is used to process the modified alloy powder intermediate to make its particle size reach nanometer level. High-energy ball milling process can achieve nano-size of powder in a short time and reduce agglomeration. S2: Precise crystallization treatment pre-screening, precise heat treatment of nano-scale amorphous alloy powder, using a staged heating method, first heating to 450 ° C at a heating rate of 5 ° C / min, keeping warm for 1 hour; then heating to 773 K at a heating rate of 2 ° C / min, keeping warm for 1 hour; Adopt intelligent screening technology to screen the crystallized amorphous alloy powder. By setting the particle size threshold, the crystallized part is automatically screened out, and the non-crystallized part of the nano-scale amorphous alloy powder is retained. S3: Optimization of composite insulation coating: Surface activation treatment of the non-crystallized nano-scale amorphous alloy powder was performed, using a 1wt% silane solution combined with UV curing technology to further enhance the bonding strength between the surfactant and the powder; The surface-activated nano-scale amorphous alloy powder is coated with a multilayer composite insulation coating using a sol-gel method. First, an acidic aluminum isopropoxide precursor solution is used for primary coating, and then a silicon dioxide precursor solution is used for secondary coating to form a double-layer insulation structure. S4: Environmental protection and recycling process, green solvent substitution, in the sol-gel method, green solvents are used instead of traditional organic solvents to reduce the emission of volatile organic compounds; The crystallized powder removed during the screening process is recycled and converted back into amorphous powder through mechanical grinding and chemical reduction processes, and is used again to prepare nano-scale amorphous alloy powder.

3. The method for preparing an amorphous nanocrystalline soft magnetic composite powder material according to claim 2, characterized in that: The nano-scale surfactant includes a nano-scale silane coupling agent.

4. The method for preparing an amorphous nanocrystalline soft magnetic composite powder material according to claim 2, characterized in that: The particle size of the modified alloy powder intermediate after processing in S1 is between 10-50 nm.

5. The method for preparing an amorphous nanocrystalline soft magnetic composite powder material according to claim 2, characterized in that: The intelligent screening technology in S2 uses a laser particle size analyzer combined with an automatic screening device.

6. The method for preparing an amorphous nanocrystalline soft magnetic composite powder material according to claim 2, characterized in that: The particle size threshold in S2 is 100 nm.

7. The method for preparing an amorphous nanocrystalline soft magnetic composite powder material according to claim 2, characterized in that: The green solvent in S4 includes ethanol instead of anhydrous ethanol or a bio-based solvent.

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