CN112509777B - Soft magnetic alloy material and preparation method and application thereof - Google Patents
Soft magnetic alloy material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of magnetic material preparation, and discloses a soft magnetic alloy material, a preparation method and application thereof, wherein the preparation method of the soft magnetic alloy material comprises the following steps: smelting the composite material into molten metal, atomizing to form spherical particles, and cooling to obtain metal spheroidal powder; carrying out thermal reduction treatment to obtain a FeSiAlPBCu material; spraying an oxide and a phosphoric acid solution on the surface of the iron powder, and reducing to obtain alloy particles; mixing the alloy particles with silica sol and phosphate solution, reducing and drying; and mixing the dried alloy particles with a FeSiAlPBCu material, pressure forming, and then carrying out heat treatment to obtain the alloy. The soft magnetic alloy material prepared by the invention has high magnetic flux density, small eddy current in particles and among particles, and reduced power consumption, and the high-temperature bonding layer obtained by surface treatment among the particles can ensure that the material has high temperature resistance, so that the requirements of the prior device on high insulation, high frequency, low power consumption and high reliability can be met.
Description
Technical Field
The invention belongs to the field of magnetic material preparation, and particularly relates to a soft magnetic alloy material and a preparation method and application thereof.
Background
In recent years, the market of public cloud and private cloud is rapidly increased, a large number of data centers are built, higher requirements are put on the performance of a server power supply, the server power supply is gradually developed towards modularization, intellectualization and the like, the main development is focused on the aspects of high power density, high reliability, high intellectualization, remote control, real-time monitoring, redundancy parallel operation and the like, the working environment is deteriorated due to heating of devices, the working environment of the devices needs to be reduced through a large amount of cooling equipment, a large amount of electric power is consumed, and the demand of high-reliability devices capable of working for a long time in a high-temperature environment is more and more urgent.
The soft magnetic alloy material has the characteristics of low power consumption, high magnetic permeability, excellent current superposition, high Curie temperature and the like, is widely applied to the power supply technology of electronic equipment, and plays a key role in the energy conversion from a power supply to a device.
However, resin or semi-inorganic resin is adopted among particles of the soft magnetic alloy material as the powder core material, so that the temperature resistance of the material is poor, the insulation of the alloy material is low, the eddy current among the particles is large, the high-frequency performance is poor, the high-frequency power consumption is high, and along with the rapid growth of a data center, the key is that the material performance is improved, the material power consumption is reduced, and the reliability is improved. In order to overcome the weakness, the alloy powder components need to be optimized, the eddy currents between alloy material particles and in the particles are reduced, the loss is reduced, the heat generation is reduced, and the energy conversion efficiency is improved. Therefore, the component design of the alloy powder plays an important role in reducing the power consumption of the material and improving the reliability of the material, so that the development of a new soft magnetic material technology with high performance, low power consumption and high reliability is necessary.
The prior art discloses a preparation method of an iron-silicon magnetic core, which is characterized in that iron-silicon magnetic powder core powder is subjected to acid treatment and then is subjected to dry pressing forming, so that the powder is easier to form, the product density is improved, and the iron-silicon magnetic core can achieve high magnetic conductivity after being subjected to heat treatment. The invention adds the component of the easily oxidized metal, eliminates the stress by heat treatment after insulating the surface of the FeSiAl material, and bonds by resin. However, the use of resin bonding has not solved the reliability of the magnetic powder core in a high temperature environment for a long time because the long-time high-temperature operation accelerates the deterioration of the material performance due to the problem that the organic matter is decomposed and aged at a certain temperature.
The prior art also discloses a soft magnetic alloy material, a preparation method thereof and an electronic device, wherein the preparation method of the low-power consumption soft magnetic alloy material comprises the following steps: (1) preparing a metal material into spherical powder, wherein the metal material comprises the following components: 82-94 wt% of Fe, 3-6 wt% of Si, 1.5-4.5 wt% of Al, 0.35-2.0 wt% of Cr, 0.5-2.0 wt% of P, 0.5-2.0 wt% of B, 0.05-0.5 wt% of Co, 0.05-0.5 wt% of Cu and 0.05-0.5 wt% of C; (2) and carrying out heat treatment on the spherical powder at the temperature of 300-500 ℃ in a protective atmosphere to form crystallized particles. The material prepared by the method has the advantages of high magnetic conductivity, high saturation magnetic flux, low power consumption and the like. According to the invention, the Cr oxide layer is formed in the high-temperature treatment process by adding the Cr element, so that the working stability of the material in a high-temperature environment is improved, but the addition of the Cr element can cause the increase of the power consumption of the material, so that the reliability of the device working at high temperature can be provided, but the power consumption is greatly increased, and the better comprehensive performance cannot be achieved.
Disclosure of Invention
The invention aims to provide a preparation method and application of a soft magnetic alloy material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a low-power consumption soft magnetic alloy material comprises the following steps:
(1) smelting Fe, Si, Al, P, B and Cu into molten metal, atomizing to form spherical particles, and cooling at 10 deg.C6-107Cooling at K/s to obtain metal spheroidal powder;
(2) carrying out thermal reduction treatment on the metal spherical powder to obtain a FeSiAlPBCu material;
(3) spraying an oxide and a phosphoric acid solution on the surface of the iron powder, and reducing to obtain eutectic protective layer alloy particles containing phosphate on the surface;
(4) mixing the eutectic protective layer alloy particles with silica sol and phosphate solution, reducing and drying;
(5) and (4) mixing the eutectic protective layer alloy particles treated in the step (4) with a FeSiAlPBCu material, forming, and then carrying out heat treatment to obtain the soft magnetic alloy material.
Preferably, in the step (1), the iron, silicon, aluminum, phosphorus, boron and copper are smelted in the form of composite materials; the composite material comprises the following components in percentage by mass: 87.5 to 93.8wt% of Fe, 4 to 6wt% of Si, 1.0 to 2.5wt% of Al, 0.6 to 2.0wt% of P, 0.5 to 1.5wt% of B, and 0.1 to 0.5wt% of Cu.
More preferably, the composite material consists of the following components in percentage by mass: 90-93.8 wt% of Fe, 4-6 wt% of Si, 1.0-2 wt% of Al, 0.6-2.0 wt% of P, 0.5-1.5 wt% of B, and 0.1-0.3 wt% of Cu.
Preferably, in the step (1), an atomizing tower is used for atomizing, and the pressure of the atomizing tower is negative pressure; the atmosphere of the atomization tower is at least one of nitrogen, argon and helium.
Preferably, the specific operation of the step (1) is to smelt a composite material with iron, silicon, aluminum, phosphorus, boron and copper as components to form molten metal, form spherical particles in an atomization tower through high-speed inert gas by feeding the molten metal into the atomization tower through negative pressure, and reduce the temperature at a rate of 106-107Cooling at K/s to form metal spheroidal powder; the granularity of the spheroidal powder is 6-20 mu m, and the sphericity S is 0.95>S>0.8。
Preferably, in the step (2), the temperature of the thermal reduction treatment is 500 ℃ to 700 ℃ and the time is 0.5 to 2 hours.
Preferably, in the step (3), the particle size of the iron powder is 0.5 to 2 μm.
Preferably, step (3) further comprises pickling and washing the iron powder with water before spraying the oxide and phosphoric acid solution; the acid solution used in the acid washing process is at least one of phosphoric acid or sulfuric acid and hydrochloric acid.
More preferably, the mass concentration of the acid solution is 10 to 30%.
The alloy material obtained by atomization contains Si, and Si can form a certain segregation structure on the surface of alloy particles under certain atmosphere treatment, so that silicate is formed with oxide at high temperature.
Preferably, in the step (3), the oxide is one of manganese oxide, magnesium oxide, zinc oxide or sodium oxide.
Preferably, in the step (3), the temperature of the reduction treatment is 800-1000 ℃ and the time is 0.5-2 hours.
Preferably, in the step (4), the phosphate is one of manganese dihydrogen phosphate, zinc phosphate or iron phosphate.
Preferably, in the step (4), the temperature of the reduction treatment is 300 ℃ to 500 ℃ and the time is 0.2 to 1.5 hours.
Preferably, in the step (5), the mass ratio of the reduced iron powder to the FeSiAlPBCu material is (1-10): 100.
Preferably, in the step (5), the pressure used for the pressure forming is 1600-.
Preferably, in the step (5), the temperature of the heat treatment is 600 ℃ to 800 ℃ for 0.5 to 2 hours.
The soft magnetic alloy material is prepared by the preparation method, the magnetic permeability of the soft magnetic alloy material is 74-95, and the magnetic flux density is 970-1310 mT.
The soft magnetic alloy material is applied to the field of semiconductors.
The principle is as follows: smelting a composite material into molten metal, forming spherical particles under negative pressure and inert gas, quickly dropping the spherical particles into cooling water to be cooled into spheroidal powder, and carrying out reduction treatment to obtain a FeSiAlPBCu material; reacting iron powder with an acid solution, cleaning, spraying oxides on the surface, carrying out thermal reduction treatment to form an insulating eutectic layer of 20-100nm between the particle surfaces, mixing the insulating eutectic layer with silica sol and phosphate solution under a protective atmosphere, drying in a reducing atmosphere at the temperature of 300-500 ℃, and forming reduced iron powder of a stress-relief layer on the surface of the eutectic layer; mixing the FeSiAlPBCu material with the reduced iron powder, pressure forming and heat treatment to obtain the soft alloy material.
The invention has the advantages that:
(1) the soft magnetic alloy material prepared by the invention has high magnetic flux density, small eddy current in particles and among particles, and reduced power consumption, and the high-temperature bonding layer obtained by surface treatment among the particles can ensure that the material has high temperature resistance, so that the requirements of the prior device on high insulation, high frequency, low power consumption and high reliability can be met.
(2) According to the invention, through controlling the material components and the process, an oxide layer of about 20-100nm is formed between the melted particles, so that the insulation resistance between the particles is high and the eddy current is small, and a certain high-resistance grain boundary is formed between the grains in the particles, so that the eddy current in the material is small, and the eddy current between the particles is further reduced through the high-insulation reduced Fe coating, and the material has high magnetic conductivity and saturation magnetic flux, certain magnetic conductivity, high saturation magnetic flux density and low power consumption.
(3) Compared with the prior art, the preparation method has the obvious advantages that: the manufactured iron-silicon magnetic core has the magnetic permeability of 74-97, and has low iron loss and higher magnetic flux density; the process steps are simple, and the cost of raw and auxiliary materials is low.
Drawings
FIG. 1 is a graph comparing the reliability of materials prepared in examples 1-4 and comparative examples 1-2.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below with reference to the examples to further illustrate the features and advantages of the invention, and any changes or modifications that do not depart from the gist of the invention will be understood by those skilled in the art to which the invention pertains, the scope of which is defined by the scope of the appended claims.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like which are not indicated for manufacturers are all conventional products which can be obtained by commercial purchase.
Example 1
A preparation method of a soft magnetic alloy material comprises the following steps:
(1) smelting 87.5wt% of Fe, 6wt% of Si, 2.5wt% of Al, 2.0wt% of P, 1.5wt% of B and 0.5wt% of Cu in a vacuum furnace to form molten metal, enabling the molten metal to enter an atomizing tower through negative pressure to form spherical particles under high-speed nitrogen gas, quickly falling into cooling water, and cooling to form metal quasi-spherical powder, wherein the particle size of the spherical powder is 20 mu m, and the sphericity S is 0.83;
(2) treating the powder at 700 ℃ for 0.5 hour in a hydrogen atmosphere;
(3) ultrasonically cleaning 2 mu m of reduced iron powder and a solution with sulfuric acid concentration of 10% for 10 minutes, cleaning with pure water, and drying, and then spraying magnesium oxide and phosphoric acid solution on the surface, wherein the content of magnesium oxide is 2wt%, and the content of phosphoric acid is 5 wt%. Treating the powder for 0.5 hour at 1000 ℃ in an ammonia atmosphere to obtain eutectic protective layer alloy particles with phosphate on the surface;
(4) mixing the eutectic protective layer alloy particles treated in the step (3) with silica sol and phosphate solution in a nitrogen atmosphere, wherein the silica sol concentration is 40 wt%, the addition proportion is 3wt% of the weight of the mixed solution, the hydrochloric acid solution concentration is 40 wt%, the addition proportion is 20 wt%, and drying is carried out in a hydrogen atmosphere at 500 ℃;
(5) mixing the eutectic protective layer alloy particles treated in the step (4) with a FeSiAlPBCu material according to a mixing ratio of 1:100, and molding under the pressure of 1600 plus 2500MPa, wherein the size of a pressed magnetic ring is Outer Diameter (OD) Inner Diameter (ID) Thickness (TH) =12.0mm 8.0mm 3.0 mm; and (3) sintering the pressed magnetic ring by using an atmosphere box furnace, wherein the sintering atmosphere adopts hydrogen, the sintering temperature is controlled at 700 ℃, the heat preservation time is 0.5h, and the sintered magnetic ring is cooled to the room temperature along with the furnace to obtain the soft magnetic alloy material of the embodiment 1.
Example 2
A preparation method of a soft magnetic alloy material comprises the following steps:
(1) smelting 93.8wt% of Fe, 4wt% of Si, 1.0wt% of Al, 0.6wt% of P, 0.5wt% of B and 0.1wt% of Cu in a vacuum furnace to form molten metal, enabling the molten metal to enter an atomizing tower through negative pressure to form spherical particles under high-speed nitrogen gas, quickly falling into cooling water, and cooling to form metal quasi-spherical powder, wherein the granularity of the spherical powder is 6 mu m, and the sphericity S is 0.94;
(2) treating the powder at 500 ℃ for 0.5 hour in a hydrogen atmosphere;
(3) carrying out ultrasonic cleaning on 0.5 mu m of reduced iron powder and a solution with sulfuric acid concentration of 10% for 5 minutes, cleaning with pure water, drying, and spraying magnesium oxide and a phosphoric acid solution on the surface, wherein the content of magnesium oxide is 2wt%, and the content of phosphoric acid is 5 wt%. Treating the powder for 2 hours at 800 ℃ in hydrogen atmosphere to obtain eutectic protective layer alloy particles with phosphate on the surface;
(4) mixing the eutectic protective layer alloy particles treated in the step (3) with silica sol and phosphate solution in an argon atmosphere, wherein the silica sol concentration is 40 wt%, the addition proportion is 3wt% of the weight of the mixed solution, the hydrochloric acid solution concentration is 40 wt%, the addition proportion is 20 wt%, and drying is carried out in a hydrogen atmosphere at 300 ℃;
(5) mixing the dried reduced iron powder with a FeSiAlPBCu material according to a mixing ratio of 10:100, and molding under the pressure of 1600 plus 2500MPa, wherein the size of a pressed magnetic ring is that the Outer Diameter (OD) is the Inner Diameter (ID) is the Thickness (TH) =12.0mm is 8.0mm is 3.0 mm; and (3) sintering the pressed magnetic ring by using an atmosphere box furnace, wherein the sintering atmosphere adopts hydrogen, the sintering temperature is controlled at 700 ℃, the heat preservation time is 0.5h, and the sintered magnetic ring is cooled to the room temperature along with the furnace to obtain the soft magnetic alloy material of the embodiment 2.
Example 3
A preparation method of a soft magnetic alloy material comprises the following steps:
(1) smelting 91.0wt% of Fe, 5wt% of Si, 1.8wt% of Al, 0.8wt% of P, 1.1wt% of B and 0.3wt% of Cu in a vacuum furnace to form molten metal, enabling the molten metal to enter an atomizing tower through negative pressure to form spherical particles under high-speed nitrogen gas, quickly falling into cooling water, and cooling to form metal quasi-spherical powder, wherein the particle size of the spherical powder is 10 mu m, and the sphericity S is 0.91;
(2) treating the powder at 600 ℃ for 1 hour in a hydrogen atmosphere;
(3) carrying out ultrasonic cleaning on 0.5 mu m of reduced iron powder and a solution with the sulfuric acid concentration of 20% for 7 minutes, cleaning with pure water, drying, and spraying magnesium oxide and a phosphoric acid solution on the surface, wherein the magnesium oxide content is 2wt%, and the phosphoric acid content is 5 wt%. Treating the powder for 1 hour at 900 ℃ in hydrogen atmosphere to obtain eutectic protective layer alloy particles with phosphate on the surface;
(4) mixing the eutectic protective layer alloy particles treated in the step (3) with silica sol and phosphate solution in an argon atmosphere, wherein the silica sol concentration is 40 wt%, the addition proportion is 3wt% of the weight of the mixed solution, the hydrochloric acid solution concentration is 40 wt%, the addition proportion is 20 wt%, and drying is carried out in a hydrogen atmosphere at 300 ℃;
(5) mixing the dried reduced iron powder with a FeSiAlPBCu material according to a mixing ratio of 10:100, and molding under the pressure of 1600 plus 2500MPa, wherein the size of a pressed magnetic ring is that the Outer Diameter (OD) is the Inner Diameter (ID) is the Thickness (TH) =12.0mm is 8.0mm is 3.0 mm; and (3) sintering the pressed magnetic ring by using an atmosphere box furnace, wherein the sintering atmosphere adopts hydrogen, the sintering temperature is controlled at 700 ℃, the heat preservation time is 0.5h, and the sintered magnetic ring is cooled to the room temperature along with the furnace to obtain the soft magnetic alloy material of the embodiment 3.
Example 4
A preparation method of a soft magnetic alloy material comprises the following steps:
(1) smelting 91.5wt% of Fe, 4.5wt% of Si, 1.7wt% of Al, 1.2wt% of P, 0.9wt% of B and 0.2wt% of Cu in a vacuum furnace to form molten metal, enabling the molten metal to enter an atomizing tower through negative pressure to form spherical particles under high-speed nitrogen gas, quickly falling into cooling water to be cooled to form metal quasi-spherical powder, wherein the particle size of the spherical powder is 15 mu m, and the sphericity S is 0.88;
(2) treating the powder at 650 ℃ for 1.5 hours in a hydrogen atmosphere;
(3) carrying out ultrasonic cleaning on 1.5 mu m of reduced iron powder and a solution with the sulfuric acid concentration of 25% for 10 minutes, cleaning with pure water, drying, and spraying magnesium oxide and a phosphoric acid solution on the surface, wherein the magnesium oxide content is 5wt%, and the phosphoric acid content is 5 wt%. Treating the powder for 1.5 hours at 850 ℃ in a hydrogen atmosphere to obtain eutectic protective layer alloy particles with phosphate on the surfaces;
(4) mixing the eutectic protective layer alloy particles treated in the step (3) with silica sol and phosphate solution in an argon atmosphere, wherein the silica sol concentration is 40 wt%, the addition proportion is 3wt% of the weight of the mixed solution, the hydrochloric acid solution concentration is 40 wt%, the addition proportion is 20 wt%, and drying is carried out in a hydrogen atmosphere at 300 ℃;
(5) mixing the dried reduced iron powder with a FeSiAlPBCu material according to a mixing ratio of 10:100, and molding under the pressure of 1600 plus 2500MPa, wherein the size of a pressed magnetic ring is that the Outer Diameter (OD) is the Inner Diameter (ID) is the Thickness (TH) =12.0mm is 8.0mm is 3.0 mm; and (3) sintering the pressed magnetic ring by using an atmosphere box furnace, wherein the sintering atmosphere adopts hydrogen, the sintering temperature is controlled at 700 ℃, the heat preservation time is 0.5h, and the sintered magnetic ring is cooled to the room temperature along with the furnace to obtain the soft magnetic alloy material of the embodiment 4.
Comparative example 1
A preparation method of a low-power consumption soft magnetic alloy material comprises the following steps:
(1) selecting 200g of FeSiAl gas atomization powder with the D50=10 mu m, wherein the mass percentage of Fe is 90.5%, the mass percentage of Si is 5.5%, the mass percentage of Al is 4%, adding glue of epoxy resin with the proportion of 2wt% of the mass of the powder, mixing the glue and the glue in a stirring tank for 10min, placing the slurry in air for air drying, placing the slurry in an oven for further drying after drying, and selecting the temperature as 100 ℃;
(2) after the powder is completely dried, it is crushed and sieved with a 60-300 mesh screen.
Comparative example 2
A preparation method of a low-power consumption soft magnetic alloy material comprises the following steps:
(1) selecting 200g of FeNi gas atomization powder with the D50=10 mu m, wherein the mass of Fe accounts for 50%, the mass of Ni accounts for 50%, treating and drying the powder by phosphoric acid with the concentration of 0.2wt%, adding glue of epoxy resin with the proportion of 2wt% of the powder, mixing the glue and the glue in a stirring tank for 10min, placing the slurry in air for air drying, and placing the slurry in an oven for further drying after drying, wherein the temperature is 100 ℃;
(2) after the powder is completely dried, it is crushed and sieved with a 60-300 mesh screen.
Comparative example 3
A preparation method of a soft magnetic alloy material comprises the following steps:
s1, mixing coarse-particle powder with the particle size of more than 30 μm of the Fe alloy material and fine-particle powder with the particle size of less than 15 μm;
s2, reacting the mixed powder with 1-1.5 wt% of phosphate or nitrate solution, and drying after the reaction is finished to obtain dry powder;
s3, mixing the dry powder with water, water-soluble resin, a silicon-containing aqueous solution, a dispersant and a defoaming agent for pulping to prepare slurry, and spray-drying the slurry to form secondary particle powder; wherein the addition amount of the water-soluble resin is 0.1 to 1wt% and the addition amount of the aqueous solution containing silicon is 0.05 to 0.2wt% based on the mass of the Fe-based alloy material; s4, pressing and forming the secondary particle powder under the pressure of 1200-2000 MPa; s5, tempering the pressed product at 700-800 ℃ for 60-120 minutes in a protective gas atmosphere to obtain the soft magnetic alloy material.
Carrying out compression molding on the untreated powder materials treated in the examples 1-4 and the untreated powder materials treated in the comparative examples 1-2 by using a powder molding press, wherein the pressure is 1600-2500MPa, and the size of a compression magnetic ring is Outer Diameter (OD) × Inner Diameter (ID) × Thickness (TH) =12.0mm × 8.0mm × 3.0 mm; and sintering the pressed magnetic ring by using an atmosphere box furnace, wherein the sintering atmosphere adopts hydrogen, the sintering temperature is controlled at 700 ℃, the heat preservation time is 0.5h, and the sintered magnetic ring is cooled to room temperature along with the furnace.
And (3) evaluating the performance of the sintered magnetic ring, wherein the number of winding turns N is 13Ts, and testing the initial permeability mu of a sample of the magnetic ring by using a 3260B type LAL testeri(1V/1 MHz) and the inductance value under the superposed current; and testing the performance change conditions of the magnetic ring after high-temperature loads of 100H, 500H, 1000H, 1500H and 2000H are respectively carried out, wherein the load current is 5A, and the storage temperature is 180 ℃.
TABLE 1 comparison of the Power consumption of the examples and comparative examples
The materials obtained by comparing examples 1 to 4 and comparative examples 1 to 2 are significantly reduced in power consumption and significantly lower in the rate of deterioration of the material in a high-temperature environment than comparative examples 1 to 2, which indicates that the effect component control and the process treatment are important for low power consumption and high reliability.
Fig. 1 is a graph showing a comparison of reliability (high temperature load) of the materials prepared in examples 1 to 4 and comparative examples 1 to 2, and from fig. 1, it can be seen that the power consumption data at high temperature, compared to comparative examples 1 to 2, shows that the power consumption of the materials of examples 1 to 4 of the present invention is stable at high temperature and does not suddenly increase due to high temperature.
The soft alloy materials obtained in examples 1 to 4 and comparative examples 1 to 2 were subjected to performance tests to obtain data of magnetic permeability, power consumption, magnetic flux density, etc. as shown in table 2.
TABLE 2
It can be seen that the soft magnetic alloy materials prepared in embodiments 1-4 of the present invention have the advantages of low power consumption, high magnetic flux density, and high magnetic permeability. The soft magnetic alloy materials of the comparative examples 1 to 3 have high power consumption, low magnetic flux density and low magnetic conductivity, which shows that the performance of the soft magnetic alloy material prepared by the invention is improved.
While the present invention has been described in detail with respect to a soft magnetic alloy material and methods of making and using the same, it is to be understood that the principles and embodiments of the present invention have been described herein with reference to specific examples which are intended to facilitate an understanding of the principles of the present invention and their core concepts, including the best mode, and to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any incorporated methods. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention. The scope of the invention is defined by the claims and may include other embodiments that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims.
Claims (8)
1. The preparation method of the soft magnetic alloy material is characterized by comprising the following steps of:
(1) smelting Fe, Si, Al, P, B and Cu into molten metal, atomizing to form spherical particles, and cooling at 10 deg.C6-107Cooling at K/s to obtain metal spheroidal powder；
(2) Carrying out thermal reduction treatment on the metal spherical powder to obtain a FeSiAlPBCu material;
(3) spraying an oxide and a phosphoric acid solution on the surface of the iron powder, and reducing to obtain eutectic protective layer alloy particles containing phosphate on the surface;
(4) mixing the eutectic protective layer alloy particles with silica sol and phosphate solution, reducing and drying;
(5) mixing the eutectic protective layer alloy particles treated in the step (4) with a FeSiAlPBCu material, forming, and then carrying out heat treatment to obtain the soft magnetic alloy material;
in the step (1), smelting the iron, the silicon, the aluminum, the phosphorus, the boron and the copper in a composite material mode; the composite material comprises the following components in percentage by mass: 87.5 to 93.8wt% of Fe, 4 to 6wt% of Si, 1.0 to 2.5wt% of Al, 0.6 to 2.0wt% of P, 0.5 to 1.5wt% of B, 0.1 to 0.5wt% of Cu;
in the step (3), the oxide is one of manganese oxide, magnesium oxide, zinc oxide or sodium oxide.
2. The production method according to claim 1, wherein in the step (1), the atomization is performed by using an atomization tower; the pressure of the atomizing tower is negative pressure; the atmosphere of the atomization tower is at least one of nitrogen, argon and helium.
3. The preparation method according to claim 1, characterized in that the step (1) is specifically operated by smelting a composite material containing iron, silicon, aluminum, phosphorus, boron and copper as components to form molten metal, feeding the molten metal into an atomizing tower through negative pressure, forming spherical particles through high-speed inert gas in the atomizing tower, and quickly falling into cooling water to be cooled to form metal spheroidal powder; the granularity of the spheroidal powder is 6-20 mu m, and the sphericity S is 0.95> S > 0.8.
4. The method according to claim 1, wherein the step (3) further comprises pickling and washing the iron powder with water before spraying the oxide and phosphoric acid solution; the acid solution used in the acid washing process is at least one of phosphoric acid or sulfuric acid and hydrochloric acid.
5. The method according to claim 1, wherein in the step (4), the phosphate is one of manganese dihydrogen phosphate, zinc phosphate or iron phosphate.
6. The production method according to claim 1, wherein in the step (2), the temperature of the thermal reduction treatment is 500 ℃ to 700 ℃ for 0.5 to 2 hours; in the step (3), the temperature of the reduction treatment is 800-1000 ℃, and the time is 0.5-2 hours; in the step (4), the temperature of the reduction treatment is 300-500 ℃, and the time is 0.2-1.5 hours; in the step (5), the pressure used in the molding process is 1600-; the temperature of the heat treatment is 600-800 ℃, and the time is 0.5-2 hours.
7. A soft magnetic alloy material, characterized in that, the soft magnetic alloy material is prepared by the preparation method of any one of claims 1 to 6, and the magnetic permeability of the soft magnetic alloy material is 74 to 97, and the magnetic flux density is 970- & 1310 mT.
8. Use of a soft magnetic alloy material according to claim 7 in the field of semiconductors.
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