CN113539663A - Soft magnetic composite material and preparation method and application thereof - Google Patents
Soft magnetic composite material and preparation method and application thereof Download PDFInfo
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- CN113539663A CN113539663A CN202110826932.1A CN202110826932A CN113539663A CN 113539663 A CN113539663 A CN 113539663A CN 202110826932 A CN202110826932 A CN 202110826932A CN 113539663 A CN113539663 A CN 113539663A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/33—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
Abstract
The invention belongs to the technical field of preparation of magnetic functional materials, and particularly relates to a soft magnetic composite material and a preparation method and application thereof. The method comprises (1) carrying out particle size classification on the alloy raw material by adopting an aerosol method to obtain alloy matrix powder; (2) adding an insulating agent and a binder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating until the slurry is dried, and obtaining magnetic powder coated by an insulating layer, wherein the insulating agent comprises a nano oxide suspension, and the nano oxide suspension comprises an oxide containing lead and palladium; (3) and carrying out hydraulic forming and heat treatment on the magnetic powder coated by the insulating layer to obtain the soft magnetic composite material. The soft magnetic composite material prepared by the method has the advantages of high resistivity, low magnetic loss, low eddy current loss, low noise and the like, and can meet the working requirement of power frequency (50-100Hz), and the noise of the iron core of the reactor prepared by the soft magnetic composite material is lower than 45 dB.
Description
Technical Field
The invention belongs to the technical field of preparation of magnetic functional materials, and particularly relates to a soft magnetic composite material and a preparation method and application thereof.
Background
Soft magnetic materials are the earliest developed magnetic functional materials by man. Since the end of the 19 th century, the development has gone through systems such as electrical pure iron, Fe-Si alloys (silicon steel), Fe-Ni alloys (permalloy), Fe-Al alloys, Fe-Si-Al alloys, Fe-Co alloys, soft magnetic ferrites, and amorphous nanocrystalline alloys. At present, silicon steel and soft magnetic ferrite are soft magnetic materials most applied, and amorphous alloy is the most popular direction for research in the soft magnetic field two decades ago. However, as described above, silicon steel and amorphous soft magnetic alloys have significant disadvantages as soft magnetic cores, and ferrite has low saturation magnetic flux density, poor thermal stability, and a high magnetostriction coefficient, although it has high resistivity, low eddy current loss, and low cost. Silicon steel, ferrite and amorphous traditional soft magnetic core materials cannot meet the development requirements of high-power low-loss low-noise power electronic equipment.
The soft magnetic composite material has the high saturation magnetic flux density, the high Curie temperature, the high resistivity of oxides and the good anti-saturation capacity of metal magnetic materials, so that the soft magnetic composite material gradually draws the attention of researchers at home and abroad, particularly, the soft magnetic composite material starts to replace a large amount of silicon steel, amorphous and ferrite materials in open air gap iron core magnetic circuits along with the improvement of power density and the improvement of conversion efficiency requirements of power electronic equipment in the last five years, and is rapidly developed in the fields of new energy and energy conservation.
The soft magnetic composite material is a novel composite material formed by compounding metal soft magnetic powder and an insulating medium, and can be widely used in the fields of electronic communication, industrial power supplies, new energy power generation, rail transit, smart power grids and the like as an iron core of magnetic elements such as inductors, reactors, flyback transformers and the like. At present, the research of the soft magnetic composite material successively goes through the stages of an iron powder core, a permalloy iron core, a molybdenum permalloy powder core, an iron-silicon-aluminum powder core, an iron-silicon powder core, an amorphous nanocrystalline powder core, a gas atomization iron-silicon-aluminum powder core, a composite powder core and the like.
In a plurality of soft magnetic composite materials, the iron powder core has low price, good magnetic conductivity and frequency stability and excellent direct current superposition characteristic, but has large high-frequency loss and is easy to age because the insulating medium adopts organic resin; the permalloy powder core has higher saturation magnetic flux density (1.51T), also called high flux powder core, but has the defects of high price and larger magnetostriction coefficient; the molybdenum permalloy powder core is prepared by adding Mo into permalloy, has the widest magnetic conductivity range and the best comprehensive performance in all magnetic powder cores, has good temperature stability, low iron loss and low noise, but has the defects of the most expensive price and lower saturation system density; the magnetostriction coefficient of the ferrosilicon aluminum powder is close to 0, the ferrosilicon aluminum powder has the advantage of low noise, although the saturation magnetic flux density is lower than that of the iron powder core, the iron loss is 80 percent lower than that of the iron powder core, the maximum magnetic conductivity is higher, the price is lower than that of the high-flux powder core and the molybdenum permalloy powder core, and is only slightly higher than that of the iron powder core, so that the ferrosilicon aluminum powder is a soft magnetic composite material with higher cost performance at present; the saturation magnetic flux density of the iron-silicon powder core is highest (1.6-1.9T), the saturation resistance is close to that of the iron-nickel powder core, the cost is close to that of the iron-silicon-aluminum powder core, the magnetostriction coefficient is close to 0, the low-noise advantage is achieved, the loss is higher than that of the iron-nickel and iron-silicon-aluminum powder cores, and the iron-silicon-aluminum powder core is a currently preferred iron core for high-power application occasions with the emphasis on saturation resistance and cost performance; the amorphous nanocrystalline powder core attracts attention due to the excellent soft magnetic property of the amorphous microcrystalline alloy, has the advantages of good magnetic permeability and frequency stability, and still has higher magnetic permeability and quality factor at high frequency, but has the disadvantages of low forming density, low effective magnetic permeability, large magnetostriction of the amorphous material which cannot be overcome after being made into a soft magnetic composite material, and high noise; the gas atomization sendust powder core is a novel soft magnetic composite material developed in about 2018, the alloy components of the gas atomization sendust powder core are consistent with those of the sendust powder core, but spherical powder prepared by using a gas atomization process and an oxide insulation process with high resistivity greatly improve the anti-saturation capacity of the sendust powder core on the premise of keeping low loss and low noise of the sendust powder core, become a preferred iron core of a magnetic element in the current new energy field, and have excellent soft magnetic performance in the application range of 10kHz and even higher frequency.
At present, relevant research at home and abroad is mostly focused in the research field of reducing the high-frequency loss, improving the magnetic conductivity and reducing the high-frequency noise of the soft magnetic composite material, the material meeting the power frequency working requirement has low eddy current loss and low noise and simultaneously has low magnetic loss, and a blank exists in the research on how to reduce the magnetic loss, noise and the like of the soft magnetic composite material in the power frequency working interval. In addition, in the prior art, when the soft magnetic composite material is prepared, substances such as phosphate are generally added, and the substances can damage the surface of the magnetic powder after being added, and are not suitable for being compounded with the magnetic powder with poor corrosion resistance.
Disclosure of Invention
Therefore, the invention aims to overcome the defects of high magnetic loss, high noise and the like of the soft magnetic composite material meeting the power frequency working requirement in the prior art, and provides the soft magnetic composite material and the preparation method and application thereof.
Therefore, the invention provides the following technical scheme.
The present invention provides a method for preparing a soft magnetic composite material, comprising the steps of,
(1) carrying out particle size classification on the alloy raw material by adopting an aerosol method to obtain alloy matrix powder;
(2) adding an insulating agent and a binder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, and heating until the slurry is dried to obtain magnetic powder coated by an insulating layer; wherein the insulating agent comprises a nano-oxide suspension; the nano-oxide suspension comprises an oxide containing lead and palladium;
(3) and carrying out hydraulic forming and heat treatment on the magnetic powder coated by the insulating layer to obtain the soft magnetic composite material.
The mass concentration of the lead-palladium-containing oxide in the nano oxide suspension is 10-15%.
The granularity of the alloy matrix powder is 100-400 meshes;
the alloy matrix powder comprises Fe, Si, Al, B, Ni, Nb and N;
the atomic percentages of Fe, Si, Al, B, Ni, Nb and N are respectively expressed as a, B, c, d, e, f and g based on 100% of the total atomic percentage of the alloy matrix powder; b is more than or equal to 3.0 and less than or equal to 7.0, c is more than or equal to 2 and less than or equal to 10, d is more than or equal to 0.1 and less than or equal to 0.9, e is more than or equal to 2 and less than or equal to 10, f is more than or equal to 0.1 and less than or equal to 3, g is more than or equal to 0.1 and less than or equal to 5, and the balance is a. Wherein N is added in the form of SiN powder.
The nano-oxide suspension further comprises silica;
the mass concentration of silicon dioxide in the nano oxide suspension is 5-10%.
PbPdO2And/or SiO2Dispersing in water to form a nano oxide suspension; the nanometer oxide suspension has high dispersibility and adsorptivityThe insulating coating process can realize controllable uniform insulating coating of magnetic powder particles, greatly improves the electromagnetic performance of soft magnetic composite materials, and greatly reduces loss.
The raw material of the soft magnetic composite material further comprises a lubricant;
in the step (3), the step of uniformly mixing the magnetic powder coated by the insulating layer and the lubricant is further included before the hydraulic forming.
The pressure of the hydraulic forming is 1000-2000 MPa;
the pressure of the hydraulic forming is 1500 MPa.
And (2) screening by a 50-100 mesh sieve to obtain magnetic powder coated by an insulating layer.
The specific steps of the heat treatment comprise that the temperature is raised to 140 ℃ and 160 ℃ at the heating rate of 8-12 ℃/min and is kept for 8-12 min; then heating to 480-520 ℃ at the heating rate of 8-12 ℃/min and preserving the heat for 8-12 min; then raising the temperature to 650-750 ℃ at a heating rate of 8-12 ℃/min and preserving the temperature for 30-50 min.
The invention also provides the soft magnetic composite material prepared by the method.
In addition, the invention also provides a reactor, which comprises the soft magnetic composite material prepared by the method or the soft magnetic composite material.
The technical scheme of the invention has the following advantages:
1. the invention provides a method for preparing a soft magnetic composite material, which comprises the following steps of (1) carrying out particle size classification on an alloy raw material by adopting an aerosol method to obtain alloy matrix powder; (2) adding an insulating agent and a binder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating until the slurry is dried, and obtaining magnetic powder coated by an insulating layer, wherein the insulating agent comprises a nano oxide suspension, and the nano oxide suspension comprises an oxide containing lead and palladium; (3) and carrying out hydraulic forming and heat treatment on the magnetic powder coated by the insulating layer to obtain the soft magnetic composite material. The soft magnetic composite material prepared by the method has the advantages of high resistivity, low magnetic loss, low eddy current loss, low noise and the like, and can meet the working requirement of power frequency (50-100Hz), and the noise of the iron core of the reactor prepared by the soft magnetic composite material is lower than 45 dB.
The oxide containing lead and palladium is used as an insulating agent to coat the alloy matrix powder, an insulating layer can be generated on the surface of the alloy matrix powder, the powder is coated to obtain magnetic powder coated by the insulating layer, the defects that the surface of the magnetic powder is damaged by a phosphate passivation process in the prior art and cannot be used in combination with the magnetic powder with poor corrosion resistance can be overcome, and the resistivity of the soft magnetic composite material is far higher than that of the material obtained by the traditional oxide process; meanwhile, lead-palladium-containing oxide is used as an insulating agent, and can be uniformly coated on the surface of the powder to form a uniform insulating layer, so that the magnetism of the magnetic powder is not influenced, and the eddy current loss of the soft magnetic composite material is favorably reduced.
2. According to the method for preparing the soft magnetic composite material, the mass concentration of the lead-palladium-containing oxide determines the coverage condition of the insulating layer on the surface of the magnetic powder, the quality concentration of the lead-palladium-containing oxide can be controlled to ensure that the insulating agent uniformly covers the surface of the magnetic powder, the concentration is too low, effective coating cannot be formed, the concentration is too high, the insulating layer on the surface of the magnetic powder is coated too thickly, the density of the soft magnetic composite material is reduced, and the binding force between the insulating layer and the magnetic powder is also poor to cause falling.
By controlling the granularity of the alloy matrix powder, the soft magnetic composite material can keep proper density, the air gap inside the material is proper, the magnetic loss and noise of the material are not influenced, the air gap inside the magnetic powder can be influenced by too coarse granularity, the magnetic loss is increased, and the noise can be improved by too fine granularity.
The alloy matrix powder comprises Fe, Si, Al, B, Ni, Nb and N with specific dosage, which can help to reduce the eddy current loss of the composite material, improve the magnetic conductivity and ensure the mechanical strength of the composite material; the proper amount of silicon can be added to greatly improve the magnetic permeability and the resistivity of the composite material and reduce the eddy current loss of the soft magnetic composite material, meanwhile, the proper amount of silicon can also reduce the magnetostriction coefficient of the soft magnetic composite material and reduce the noise of the iron core of the soft magnetic composite material, and the excessive amount of silicon can increase the brittleness of the material and reduce the mechanical strength and the magnetic permeability of the material. Proper amount of boron can refine the grain size inside the soft magnetic composite material, improve the resistivity of the powder of the soft magnetic composite material, increase the brittleness of the soft magnetic composite material when the amount of boron is too much, and reduce the mechanical strength and magnetic conductivity of the material. Proper nickel can form an interaction with 3d electrons of the iron element outer layer, the magnetic conductivity of the soft magnetic composite material is improved, loss is reduced, and the use amount of the nickel is too much, so that the cost is increased, and the magnetic conductivity gain effect is weakened. A proper amount of niobium element, iron and boron can form second phase particles, the grain size of the soft magnetic composite material powder is refined, the tissue is uniformly refined, the isotropic soft magnetic performance of the soft magnetic composite material is improved, and excessive niobium can increase the anisotropy of the material, increase the cost and increase the loss. Proper amount of aluminum and nitrogen can be deposited on the grain boundary of the soft magnetic composite material powder by an amorphous matrix to limit the growth of grains, so that the size of the grains is greatly reduced, the exchange coupling among the grains is enhanced, and thus the small effective anisotropy is averagely formed with the magnetocrystalline anisotropy effect, the magnetic conductivity is improved, the loss is reduced, and the soft magnetic performance of the soft magnetic composite material is deteriorated and the mechanical strength is reduced due to excessive use of the two elements.
3. According to the method for preparing the soft magnetic composite material, the proper density of the soft magnetic composite material can be kept by controlling the hydraulic forming pressure, the material is loose due to the fact that the hydraulic forming pressure is too small, the magnetic performance is poor, the air gap of the composite material is reduced due to the fact that the hydraulic forming pressure is too large, and the magnetic loss and the anti-saturation capacity are poor.
And fully grinding the dried powder slurry and screening the powder slurry by 50-100 meshes, wherein the resistivity and magnetostrictive noise of the final soft magnetic composite material sample are influenced by excessively large or excessively small powder particle size, and the optimal powder particle size is 50-100 meshes.
By controlling the heat treatment process, the lubricant can be slowly decomposed in the first temperature rise and heat preservation process, so that the magnetic powder core sample is not broken by too fast decomposition speed; the second heating and heat preservation process can ensure that the sodium silicate reacts completely; the third temperature rise and preservation process is beneficial to improving the density of the soft magnetic composite material product and completely volatilizing the volatile substances.
4. The soft magnetic composite material provided by the invention has the advantages of high resistivity, low magnetic loss, low eddy current loss, low noise and the like, meets the power frequency use requirement, and is suitable for being used in a reactor.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 100 meshes; wherein the alloy matrix powder comprises, in atomic percent, 81.2 wt% Fe, 4 wt% Si, 3 wt% Al, 0.8 wt% B, 6 wt% Ni, 2 wt% Nb, and 3 wt% N; wherein N is added in the form of SiN powder.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 50 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 50-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10 percent of PbPdO by mass fraction2And SiO with the mass fraction of 5%2，PbPdO2And SiO2The nanometer oxide is dispersed in water to form nanometer oxide suspension, and excessive insulating agent and sodium silicate can fall off from the magnetic powder coated by the insulating layer.
(3) Uniformly mixing magnetic powder coated by an insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample under the condition of 1000Mpa and room temperature, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Example 2
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 400 meshes; wherein the alloy matrix powder comprises, in atomic percent, 80.3 wt% Fe, 6 wt% Si, 5 wt% Al, 0.2 wt% B, 8 wt% Ni, 0.3 wt% Nb, and 0.2 wt% N; n is added in the form of SiN powder.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 80 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 100-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 15 percent of PbPdO by mass fraction2And SiO with the mass fraction of 10%2，PbPdO2And SiO2The nanometer oxide is dispersed in water to form nanometer oxide suspension, and excessive insulating agent and sodium silicate can fall off from the magnetic powder coated by the insulating layer.
(3) Uniformly mixing the magnetic powder coated by the insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample at the room temperature of 2000Mpa, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Example 3
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 200 meshes; wherein the alloy matrix powder comprises, in atomic percent, 80 wt% Fe, 3 wt% Si, 9 wt% Al, 0.5 wt% B, 2 wt% Ni, 1.5 wt% Nb, and 4 wt% N; n is added in the form of SiN powder.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 60 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 80-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 13 percent of PbPdO by mass fraction2And 7% by mass of SiO2，PbPdO2And SiO2The nanometer oxide is dispersed in water to form nanometer oxide suspension, and excessive insulating agent and sodium silicate can fall off from the magnetic powder coated by the insulating layer.
(3) Uniformly mixing the magnetic powder coated by the insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample at the room temperature of 1500Mpa, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Example 4
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 500 meshes; wherein the alloy matrix powder comprises, in atomic percent, 81.2 wt% Fe, 4 wt% Si, 3 wt% Al, 0.8 wt% B, 6 wt% Ni, 2 wt% Nb, and 3 wt% N; n is added in the form of SiN powder.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 50 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 50-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10 percent of PbPdO by mass fraction2And SiO with the mass fraction of 5%2，PbPdO2And SiO2The nanometer oxide is dispersed in water to form nanometer oxide suspension, and excessive insulating agent and sodium silicate can fall off from the magnetic powder coated by the insulating layer.
(3) Uniformly mixing magnetic powder coated by an insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample under the condition of 1000Mpa and room temperature, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Comparative example 1
The present comparative example provides a soft magnetic composite material and a method for preparing the same, comprising the steps of,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 100 meshes; wherein the alloy matrix powder comprises, in atomic percent, 81.2 wt% Fe, 4 wt% Si, 3 wt% Al, 0.8 wt% B, 6 wt% Ni, 2 wt% Nb, and 3 wt% N.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 50 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 50-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10 mass percent of sodium phosphate and 5 mass percent of SiO2。
(3) Uniformly mixing magnetic powder coated by an insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample under the condition of 1000Mpa and room temperature, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Comparative example 2
The present comparative example provides a soft magnetic composite material and a method for preparing the same, comprising the steps of,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 100 meshes; wherein the alloy matrix powder comprises, in atomic percent, 81.2 wt% Fe, 4 wt% Si, 3 wt% Al, 0.8 wt% B, 6 wt% Ni, 2 wt% Nb, and 3 wt% N.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 50 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 50-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises SiO with the mass fraction of 5 percent2，SiO2Dispersed in water to form a nano-oxide suspension.
(3) Uniformly mixing magnetic powder coated by an insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample under the condition of 1000Mpa and room temperature, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Comparative example 3
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) carrying out particle size classification on the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the particle size of the alloy matrix powder after particle size classification is 100 meshes; wherein the alloy matrix powder comprises, in atomic percent, 81.2 wt% Fe, 4 wt% Si, 3 wt% Al, 0.8 wt% B, 6 wt% Ni, 2 wt% Nb, and 3 wt% N.
(2) Adding the suspension of the nano oxide and the instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 50 ℃, keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and screening by a 50-mesh sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10 percent of PbPdO by mass fraction2And SiO with the mass fraction of 5%2The excessive insulating agent and sodium silicate may be released from the magnetic powder coated by the insulating layer.
(3) Uniformly mixing the magnetic powder coated by the insulating layer and a proper amount of zinc stearate powder, putting the mixture into a hydraulic forming machine, pressing the mixture into an annular powder core sample at the room temperature of 2500Mpa, then placing the annular powder core sample in a high-purity nitrogen environment, heating the annular powder core sample to 150 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 10 min; heating to 500 ℃ at the heating rate of 10 ℃/min and preserving the heat for 10 min; and then heating to 700 ℃ at the heating rate of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature to obtain the soft magnetic composite material.
Test examples
The test example provides performance tests and results of the soft magnetic composite materials prepared in examples 1 to 4 and comparative examples 1 to 3, the test method is as follows, and the results are shown in table 1;
the method for testing the resistivity of the soft magnetic composite material comprises the following steps: the volume resistance of the soft magnetic composite was measured using an insulation resistance meter, and then the volume resistivity was calculated.
The method for testing the anti-saturation capacity of the soft magnetic composite material comprises the following steps: testing the change of the inductance along with the external current by using a direct current bias measurement system, then converting the inductance into the magnetic permeability, and converting the current into a magnetic field, thus obtaining the change of the magnetic permeability along with the external magnetic field;
in testing the noise of soft magnetic composites, the materials were prepared into cores for use in reactor preparation, according to standard GBT 1094.10-2003 power transformer part 10: and measuring the sound level, and testing to obtain the noise of the reactor.
The method for testing the loss and the relative permeability of the soft magnetic composite material utilizes a soft magnetic alternating current B-H loop recorder to directly test.
TABLE 1 Performance results of the examples and comparative examples Soft magnetic composites
The results show that the soft magnetic composite material provided by the invention has the advantages of high resistivity, low magnetic loss, low eddy current loss, low noise and the like, and can meet the working requirement of power frequency (50-100 Hz). In addition, the comparative example 1 uses sodium phosphate to replace lead-palladium-containing oxide, which shows that the material obtained by the prior art adopting the sodium phosphate process has low relative permeability and high loss, and the process has certain acid pollution, the magnetic powder can generate chemical reaction, and the reaction process is not easy to control. Comparative example 2 the material obtained after removing the lead-palladium containing oxide had low conductivity and high loss.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (11)
1. A method for producing a soft magnetic composite material, comprising the steps of,
(1) carrying out particle size classification on the alloy raw material by adopting an aerosol method to obtain alloy matrix powder;
(2) adding an insulating agent and a binder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, and heating until the slurry is dried to obtain magnetic powder coated by an insulating layer; wherein the insulating agent comprises a nano-oxide suspension; the nano-oxide suspension comprises an oxide containing lead and palladium;
(3) and carrying out hydraulic forming and heat treatment on the magnetic powder coated by the insulating layer to obtain the soft magnetic composite material.
2. The method of claim 1, wherein the nano-oxide suspension has a concentration of lead-palladium containing oxide in the range of 10-15% by mass.
3. The method as claimed in claim 1 or 2, wherein the alloy matrix powder has a particle size of 100-400 mesh;
the alloy matrix powder comprises Fe, Si, Al, B, Ni, Nb and N;
the atomic percentages of Fe, Si, Al, B, Ni, Nb and N are respectively expressed as a, B, c, d, e, f and g based on 100% of the total atomic percentage of the alloy matrix powder; b is more than or equal to 3.0 and less than or equal to 7.0, c is more than or equal to 2 and less than or equal to 10, d is more than or equal to 0.1 and less than or equal to 0.9, e is more than or equal to 2 and less than or equal to 10, f is more than or equal to 0.1 and less than or equal to 3, g is more than or equal to 0.1 and less than or equal to 5, and the balance is a.
4. The method of any one of claims 1-3, wherein the nano-oxide suspension further comprises silica;
the mass concentration of silicon dioxide in the nano oxide suspension is 5-10%.
5. The method according to any one of claims 1 to 4, wherein the raw material of the soft magnetic composite material further comprises a lubricant;
in the step (3), the step of uniformly mixing the magnetic powder coated by the insulating layer and the lubricant is further included before the hydraulic forming.
6. The method as claimed in any one of claims 1 to 5, wherein the pressure of the hydroforming is 1000-2000 MPa.
7. The method of claim 6, wherein the hydroforming pressure is 1500 MPa.
8. The method according to any one of claims 1 to 7, wherein step (2) is carried out by sieving through a 50-100 mesh sieve to obtain an insulating layer-coated magnetic powder.
9. The method as claimed in any one of claims 1 to 8, wherein the heat treatment comprises raising the temperature to 140 ℃ and 160 ℃ at a temperature raising rate of 8 to 12 ℃/min for 8 to 12 min; then heating to 480-520 ℃ at the heating rate of 8-12 ℃/min and preserving the heat for 8-12 min; then raising the temperature to 650-750 ℃ at a heating rate of 8-12 ℃/min and preserving the temperature for 30-50 min.
10. A soft magnetic composite material obtainable by a process according to any one of claims 1 to 9.
11. An inductor comprising the soft magnetic composite material produced by the method according to any one of claims 1 to 9 or the soft magnetic composite material according to claim 10.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080003126A1 (en) * | 2004-09-06 | 2008-01-03 | Mitsubishi Materials Pmg Corporation | Method for Producing Soft Magnetic Metal Powder Coated With Mg-Containing Oxide Film and Method for Producing Composite Soft Magnetic Material Using Said Powder |
| JP2012156438A (en) * | 2011-01-28 | 2012-08-16 | Fujifilm Corp | Magnetic particle, method of manufacturing the same, magnetic powder for magnetic recording, and magnetic recording medium |
| CN103247403A (en) * | 2013-05-31 | 2013-08-14 | 合肥工业大学 | Preparation method of metal soft magnetic powder core |
| CN112309667A (en) * | 2019-07-31 | 2021-02-02 | Tdk株式会社 | Soft magnetic metal powder and electronic component |
| CN112582125A (en) * | 2019-09-27 | 2021-03-30 | Tdk株式会社 | Soft magnetic alloy and electronic component |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080003126A1 (en) * | 2004-09-06 | 2008-01-03 | Mitsubishi Materials Pmg Corporation | Method for Producing Soft Magnetic Metal Powder Coated With Mg-Containing Oxide Film and Method for Producing Composite Soft Magnetic Material Using Said Powder |
| JP2012156438A (en) * | 2011-01-28 | 2012-08-16 | Fujifilm Corp | Magnetic particle, method of manufacturing the same, magnetic powder for magnetic recording, and magnetic recording medium |
| CN103247403A (en) * | 2013-05-31 | 2013-08-14 | 合肥工业大学 | Preparation method of metal soft magnetic powder core |
| CN112309667A (en) * | 2019-07-31 | 2021-02-02 | Tdk株式会社 | Soft magnetic metal powder and electronic component |
| CN112582125A (en) * | 2019-09-27 | 2021-03-30 | Tdk株式会社 | Soft magnetic alloy and electronic component |
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