CN113539663B - 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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- 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
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- 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
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- 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
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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) grading the granularity of alloy raw materials 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 to dry the slurry to obtain magnetic powder coated with an insulating layer, wherein the insulating agent comprises a nano oxide suspension, and the nano oxide suspension comprises oxides 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, can meet the working requirement of power frequency (50-100 Hz), and has the iron core noise of the reactor lower than 45dB.
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 magnetic functional materials that were originally developed by humans. From the end of the 19 th century, the development thereof has undergone systems such as electrical pure iron, fe-Si alloy (silicon steel), fe-Ni alloy (permalloy), fe-Al alloy, fe-Si-Al alloy, fe-Co alloy, soft magnetic ferrite, amorphous nanocrystalline alloy, and the like. At present, silicon steel and soft magnetic ferrite are the most widely used soft magnetic materials, and amorphous alloy is the most popular direction of research in the soft magnetic field for the last two decades. However, as described above, the soft magnetic alloys such as silicon steel and amorphous have significant drawbacks as soft magnetic cores, and ferrite has a low saturation magnetic flux density, poor thermal stability, and a high magnetostriction coefficient, although it has a high resistivity, a small eddy current loss, and a low cost. Silicon steel, ferrite and amorphous three traditional soft magnetic core materials can not meet the development requirements of high-power low-loss low-noise power electronic equipment.
The soft magnetic composite material gradually draws attention of researchers at home and abroad due to the high saturation magnetic flux density, the high curie temperature, the high resistivity of oxide and the good saturation resistance of the metal magnetic material, and particularly, the soft magnetic composite material starts to replace silicon steel, amorphous and ferrite materials in an open air gap iron core magnetic circuit in a large quantity along with the improvement of power density of power electronic equipment and the improvement of conversion efficiency requirements in recent five years, so that the soft magnetic composite material has been 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 as an iron core of magnetic elements such as an inductor, a reactor, a flyback transformer and the like in the fields of electronic communication, industrial power supply, new energy power generation, rail transit, intelligent power grid and the like. At present, the research of the soft magnetic composite material sequentially goes through the stages of iron powder core, permalloy iron core, molybdenum permalloy powder core, iron silicon aluminum powder core, iron silicon powder core, amorphous nanocrystalline powder core, gas atomization iron silicon aluminum powder core, composite powder core and the like.
In a plurality of soft magnetic composite materials, the iron powder core has low price, better magnetic conductivity frequency stability and excellent direct current superposition characteristics, but has large high-frequency loss, and is easy to age because the insulating medium adopts organic resin; permalloy powder core has higher saturation magnetic flux density (1.51T), also called high flux powder core, but has the defect of high price and larger magnetostriction coefficient; the molybdenum permalloy is prepared by adding Mo into permalloy, has the advantages of the widest magnetic conductivity range in all magnetic powder cores, the best comprehensive performance, good temperature stability, low iron loss and low noise, but has the defects of the most expensive price and lower saturated system density; the magnetostriction coefficient of the ferrosilicon aluminum powder is close to 0, the saturated magnetic flux density is lower than that of the iron powder core, but the iron loss is 80% lower than that of the iron powder core, the maximum magnetic permeability is higher, the price is lower than that of the high-flux powder core and the molybdenum-slope mullite powder core, and the magnetic flux density is slightly higher than that of the iron powder core, so that the magnetic flux density 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 anti-saturation performance is close to that of the iron nickel powder core, the cost is close to that of the iron silicon powder core, the magnetostriction coefficient is close to 0, and the iron silicon powder core has the advantage of low noise, but the loss is higher than that of the iron nickel powder core and the iron silicon powder core, so that the iron silicon powder core is the current preferred iron core for high-power application occasions with high anti-saturation capability and cost performance; the amorphous nanocrystalline powder core attracts attention due to the excellent soft magnetic property of amorphous microcrystalline alloy, and has the advantages of good magnetic permeability frequency stability and higher magnetic permeability and quality factor at high frequency, but has the disadvantages of low forming density, low effective magnetic permeability, incapacity of overcoming the large magnetostriction defect of amorphous materials after being made into soft magnetic composite materials and high noise; the aerosolised iron-silicon-aluminum powder core is a novel soft magnetic composite material developed in about 2018, alloy components of the aerosolised iron-silicon-aluminum powder core are consistent with those of the iron-silicon-aluminum powder core, but spherical powder prepared by using an aerosolised process and an oxide insulation process with high resistivity are used, so that the anti-saturation capacity of the aerosolised iron-silicon-aluminum powder core is greatly improved on the premise of keeping low loss and low noise of the iron-silicon-aluminum powder core, the aerosolised iron-silicon-aluminum powder core becomes a preferred iron core of a magnetic element in the current new energy field, and the aerosolised iron-silicon-aluminum powder core has better soft magnetic performance in the application range of 10kHz or higher frequency.
At present, related researches at home and abroad are focused on the research fields of reducing the high-frequency loss, improving the magnetic permeability and reducing the high-frequency noise of the soft magnetic composite material, and the research on how to reduce the magnetic loss and noise of the soft magnetic composite material in a power frequency working interval has blank when the material meeting the working requirements of the power frequency has low eddy current loss and low noise and also has low magnetic loss. In addition, in the prior art, substances such as phosphate and the like are generally added when the soft magnetic composite material is prepared, and the substances damage the surface of the magnetic powder after being added, and are also 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 working requirements of power frequency in the prior art, thereby providing a soft magnetic composite material and a preparation method and application thereof.
For this purpose, the invention provides the following technical scheme.
The invention provides a method for preparing a soft magnetic composite material, which comprises the following steps,
(1) Grading the granularity of 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 the slurry 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 oxide containing lead and palladium in the nano oxide suspension is 10-15%.
The granularity of the alloy matrix powder is 100-400 meshes;
the alloy matrix powder includes Fe, si, al, B, ni, nb, N;
fe, si, al, B, ni, nb, N atomic percent, based on 100 percent of the total atomic percent of the alloy matrix powder, is represented by a, b, c, d, e, f and g, respectively; b is more than or equal to 3.0 and less than or equal to 7.0,2, c is more than or equal to 10,0.1, d is more than or equal to 0.9,2 and less than or equal to e is more than or equal to 10,0.1 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 the silicon dioxide in the nano oxide suspension is 5-10%.
PbPdO 2 And/or SiO 2 Dispersing in water to form nano oxide suspension; the nano oxide suspension has high dispersibility and high adsorptivity, is mixed with magnetic powder, the magnetic powder does not react with the nano oxide, the dosage of ferromagnetic components in the powder core product is convenient to control, the controllable uniform insulating coating of the magnetic powder particles can be realized by the insulating coating process, the electromagnetic performance of the soft magnetic composite material is greatly improved, and the loss is greatly reduced.
The raw materials of the soft magnetic composite material also comprise 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 1000-2000MPa;
the pressure of the hydraulic forming is 1500MPa.
And (2) sieving with a 50-100 mesh granularity sieve to obtain the magnetic powder coated with the insulating layer.
The specific steps of the heat treatment comprise heating to 140-160 ℃ at a heating rate of 8-12 ℃/min, and preserving heat for 8-12min; heating to 480-520 ℃ at a heating rate of 8-12 ℃/min, and preserving heat for 8-12min; then heating to 650-750deg.C at a heating rate of 8-12 deg.C/min, and maintaining for 30-50min.
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 steps of (1) adopting an aerosol method to carry out particle size classification on alloy raw materials 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 to dry the slurry to obtain magnetic powder coated with an insulating layer, wherein the insulating agent comprises a nano oxide suspension, and the nano oxide suspension comprises oxides 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, can meet the working requirement of power frequency (50-100 Hz), and has the iron core noise of the reactor lower than 45dB.
The oxide containing lead and palladium is used as an insulating agent to coat 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 defect that the phosphate passivation process in the prior art damages the surface of the magnetic powder and can not 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, the oxide containing lead and palladium is used as an insulating agent, so that the oxide containing lead and palladium can be uniformly coated on the surface of the powder to form a uniform insulating layer, the magnetism of the magnetic powder is not influenced, and the eddy current loss of the soft magnetic composite material is reduced.
2. According to the method for preparing the soft magnetic composite material, the mass concentration of the oxide containing lead and palladium determines the covering condition of the insulating layer on the surface of the magnetic powder, the insulating agent can be ensured to be uniformly covered on the surface of the magnetic powder by controlling the mass concentration of the oxide containing lead and palladium, 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 too thick, the density of the soft magnetic composite material is reduced, the adhesive force between the insulating layer and the magnetic powder is also deteriorated, and the soft magnetic composite material falls off.
The granularity of the alloy matrix powder is controlled, so that the soft magnetic composite material can keep proper density, an air gap inside the material is proper, the magnetic loss and noise of the material are not influenced, the granularity is too thick, the air gap inside the magnetic powder can be influenced, the magnetic loss is increased, and the noise is increased due to too thin.
The alloy matrix powder comprises Fe, si, al, B, ni, nb, N with a specific dosage, which can help to reduce the eddy current loss of the composite material, improve the magnetic permeability and ensure the mechanical strength of the composite material; the magnetic conduction characteristic and the resistivity of the composite material can be greatly improved by adding a proper amount of silicon, the eddy current loss of the soft magnetic composite material is reduced, the magnetostriction coefficient of the soft magnetic composite material is reduced by adding a proper amount of silicon, the noise of a soft magnetic composite material iron core is reduced, the brittleness of the material is increased due to excessive silicon consumption, and the mechanical strength and the magnetic conductivity of the material are reduced. The proper amount of boron can refine the internal grain size of the soft magnetic composite material, improve the powder resistivity of the soft magnetic composite material, and the excessive boron dosage can increase the brittleness of the soft magnetic composite material and reduce the mechanical strength and the magnetic conductivity of the material. And a proper amount of nickel can form interaction with the 3d electrons of the outer layer of the iron element, so that the magnetic permeability of the soft magnetic composite material is improved, the loss is reduced, on one hand, the cost is increased, and on the other hand, the magnetic permeability gain effect is weakened due to excessive nickel consumption. Proper amount of niobium element, iron and boron can form second phase particles, refine the grain size of the soft magnetic composite material powder, lead the structure to be refined uniformly, improve the isotropy soft magnetic property of the soft magnetic composite material, and excessive niobium can increase the anisotropy of the material and increase the cost and loss. Proper amounts of aluminum and nitrogen can be deposited on grain boundaries of the soft magnetic composite material powder in an amorphous matrix, so that the growth of grains is limited, the grain size is greatly reduced, exchange coupling among grains is enhanced, smaller effective anisotropism is formed on average due to the action of magnetocrystalline anisotropism, the magnetic permeability is improved, the loss is reduced, and the excessive use of the two elements can deteriorate the soft magnetic performance and reduce the mechanical strength of the soft magnetic composite material.
3. According to the method for preparing the soft magnetic composite material, the soft magnetic composite material can keep proper compactness 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 pressure is too large, and the magnetic loss and the anti-saturation capacity are poor.
The dried powder slurry is fully ground and screened by a granularity of 50-100 meshes, and the excessive or the too small granularity of the powder can influence the resistivity and magnetostriction noise of a final soft magnetic composite material sample, and is optimal by 50-100 meshes.
By controlling the heat treatment process, the lubricant can be slowly decomposed in the first heating and heat preservation process, so that the magnetic powder core sample is not washed out at a too high decomposition speed; the second heating and heat preserving process can lead the sodium silicate to react completely; the third heating and heat preserving process is favorable for improving the density of the soft magnetic composite material product and completely volatilizing volatile substances.
4. The soft magnetic composite material provided by the invention has the advantages of high resistivity, low magneto loss, low eddy current loss, low noise and the like, meets the use requirement of power frequency, and is suitable for being used in reactors.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 100 meshes; wherein, in atomic percent, the alloy matrix powder comprises 81.2wt% Fe, 4wt% Si, 3wt% Al, 0.8wt% B, 6wt% Ni, 2wt% Nb and 3wt% 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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with a 50-mesh granularity sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10% of PbPdO by mass 2 And 5% by mass of SiO 2 ，PbPdO 2 And SiO 2 Dispersing in water to form nano oxide suspension, and the 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 with 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 conditions of 1000Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and 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) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 400 meshes; wherein, in atomic percent, the alloy matrix powder comprises 80.3wt% Fe, 6wt% Si, 5wt% Al, 0.2wt% B, 8wt% Ni, 0.3wt% Nb and 0.2wt% 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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with 100-mesh granularity to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 15% of PbPdO by mass 2 And SiO with mass fraction of 10% 2 ，PbPdO 2 And SiO 2 Dispersing in water to form nano oxide suspension, and the 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 with 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 conditions of 2000Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and 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) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 200 meshes; wherein, in atomic percent, the alloy matrix powder comprises 80wt% Fe, 3wt% Si, 9wt% Al, 0.5wt% B, 2wt% Ni, 1.5wt% Nb and 4wt% N; n is added in the form of SiN powder.
(2) Adding the suspension of nano oxide and instant sodium silicate powder into the alloy matrix powder obtained in the step (1), uniformly stirring to form slurry, heating at 60 ℃ and keeping the temperature, continuously stirring until the slurry is dried, and fully grinding and dryingSieving with 80 mesh sieve to obtain magnetic powder coated with insulating layer; wherein the nano oxide suspension comprises 13% of PbPdO by mass 2 And 7% by mass of SiO 2 ，PbPdO 2 And SiO 2 Dispersing in water to form nano oxide suspension, and the 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 with 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 conditions of 1500Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and 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) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 500 meshes; wherein, in atomic percent, the alloy matrix powder comprises 81.2wt% Fe, 4wt% Si, 3wt% Al, 0.8wt% B, 6wt% Ni, 2wt% Nb and 3wt% 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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with a 50-mesh granularity sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10% of PbPdO by mass 2 And 5% by mass of SiO 2 ，PbPdO 2 And SiO 2 Dispersing in water to form nano oxide suspension, and the 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 with 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 conditions of 1000Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and cooling to room temperature to obtain the soft magnetic composite material.
Comparative example 1
The comparative example provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 100 meshes; wherein, the alloy matrix powder comprises 81.2wt% Fe, 4wt% Si, 3wt% Al, 0.8wt% B, 6wt% Ni, 2wt% Nb and 3wt% N in atomic percent.
(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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with a 50-mesh granularity sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10% of sodium phosphate by mass and 5% of SiO by mass 2 。
(3) Uniformly mixing the magnetic powder coated by the insulating layer with 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 conditions of 1000Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and cooling to room temperature to obtain the soft magnetic composite material.
Comparative example 2
The comparative example provides a soft magnetic composite material and a preparation method thereof, comprising the following steps,
(1) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 100 meshes; wherein, the alloy matrix powder comprises 81.2wt% Fe, 4wt% Si, 3wt% Al, 0.8wt% B, 6wt% Ni, 2wt% Nb and 3wt% N in atomic percent.
(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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with a 50-mesh granularity sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 5% of SiO by mass 2 ，SiO 2 Dispersing in water to form nano oxide suspension.
(3) Uniformly mixing the magnetic powder coated by the insulating layer with 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 conditions of 1000Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and 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) Grading the granularity of the alloy matrix powder by adopting an aerosol method, and then fully and uniformly mixing, wherein the granularity of the alloy matrix powder after grading is 100 meshes; wherein, the alloy matrix powder comprises 81.2wt% Fe, 4wt% Si, 3wt% Al, 0.8wt% B, 6wt% Ni, 2wt% Nb and 3wt% N in atomic percent.
(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 ℃ and keeping the temperature, continuously stirring until the slurry is dried, fully grinding the dried slurry, and sieving with a 50-mesh granularity sieve to obtain magnetic powder coated by an insulating layer; wherein the nano oxide suspension comprises 10% of PbPdO by mass 2 And 5% by mass of SiO 2 Excess insulating agent and sodium silicate will be removed from the insulating layerThe coated magnetic powder falls off.
(3) Uniformly mixing the magnetic powder coated by the insulating layer with 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 conditions of 2500Mpa and room temperature, then putting the annular powder core sample into a high-purity nitrogen environment, and heating to 150 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; then heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 10min; and then heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, and cooling to room temperature to obtain the soft magnetic composite material.
Test examples
The test examples provide performance tests and results of the soft magnetic composite materials prepared in examples 1 to 4 and comparative examples 1 to 3, the test methods are 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 bulk resistance of the soft magnetic composite material was measured using an insulation resistance meter, and then the bulk resistivity was calculated.
The method for testing the anti-saturation capacity of the soft magnetic composite material comprises the following steps: the change of inductance along with the external current is tested by using a direct current bias measurement system, then the inductance is converted into magnetic permeability, and the current is converted into a magnetic field, so that the change of the magnetic permeability along with the external magnetic field can be obtained;
when testing the noise of the soft magnetic composite material, preparing the material into an iron core for reactor preparation according to the 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 directly tests the soft magnetic composite material by using a soft magnetic alternating current B-H loop recorder.
Table 1 results of properties 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 magneto loss, low eddy current loss, low noise and the like, and can meet the working requirements of power frequency (50-100 Hz). In addition, the comparative example 1 uses sodium phosphate to replace oxide containing lead and palladium, which shows that the material obtained by adopting the sodium phosphate process in the prior art has low relative magnetic conductivity 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 removal of the oxide containing lead-palladium has low conductivity and high loss.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (8)
1. A method for preparing a soft magnetic composite material is characterized by comprising the following steps,
(1) Grading the granularity of 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 the slurry 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) Carrying out hydraulic forming and heat treatment on the magnetic powder coated by the insulating layer to obtain the soft magnetic composite material;
wherein the mass concentration of the oxide containing lead and palladium in the nano oxide suspension is 10-15%;
the alloy matrix powder includes Fe, si, al, B, ni, nb, N;
fe, si, al, B, ni, nb, N atomic percent, based on 100 percent of the total atomic percent of the alloy matrix powder, is represented by a, b, c, d, e, f and g, respectively; b is more than or equal to 3.0 and less than or equal to 7.0,2, c is more than or equal to 10,0.1, d is more than or equal to 0.9,2 and less than or equal to e is more than or equal to 10,0.1 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;
the pressure of the hydraulic forming is 1000-2000MPa;
the specific steps of the heat treatment comprise heating to 140-160 ℃ at a heating rate of 8-12 ℃/min, and preserving heat for 8-12min; heating to 480-520 ℃ at a heating rate of 8-12 ℃/min, and preserving heat for 8-12min; then heating to 650-750deg.C at a heating rate of 8-12 deg.C/min, and maintaining for 30-50min.
2. The method of claim 1, wherein the alloy matrix powder has a particle size of 100-400 mesh.
3. The method according to claim 1 or 2, wherein the nano-oxide suspension further comprises silica;
the mass concentration of the silicon dioxide in the nano oxide suspension is 5-10%.
4. A method according to claim 1 or 2, wherein the feedstock 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.
5. The method of claim 1, wherein the hydroforming is at a pressure of 1500MPa.
6. The method according to claim 1 or 2, wherein in step (2), the insulating layer coated magnetic powder is obtained after sieving with a 50-100 mesh particle size.
7. A soft magnetic composite material prepared by the method of any one of claims 1-6.
8. A reactor comprising the soft magnetic composite material prepared by the method of any one of claims 1 to 6 or the soft magnetic composite material of claim 7.
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