CN114360884B - Gradient nanocrystalline magnetic powder core with high magnetic induction and low loss as well as preparation method and application thereof - Google Patents
Gradient nanocrystalline magnetic powder core with high magnetic induction and low loss as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core suitable for a high-frequency inductance element, and a preparation method and application thereof. According to the invention, fe-based amorphous alloy powder is subjected to discharge plasma treatment, so that the surface layer of the amorphous powder is subjected to nano crystallization, then a coating agent and a lubricant are added, and then compression molding is carried out, finally sintering treatment is carried out at a temperature higher than the crystallization temperature of the Fe-based amorphous alloy powder, the nano crystals on the surface of the powder continue to grow up, the nano crystals in the powder are subjected to nano crystallization, and the gradient difference of the grain sizes is formed, so that the high-magnetic-induction low-loss gradient nano crystal magnetic powder core with large grains on the outer layer and small grains on the inner layer is obtained. The method is simple, environment-friendly and low in cost, can effectively improve the saturated magnetic induction intensity, the magnetic permeability and the resistivity of the Fe-based magnetic powder core, greatly reduce the magnetic loss, and can be widely applied to medium-high frequency electronic devices in various fields.
Description
Technical Field
The invention belongs to the technical field of soft magnetic material forming, and particularly relates to a high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core, a preparation method and application thereof.
Background
With the continuous updating of modern technology, electrification is more and more widely used in many industries, and miniaturization of electronic devices is gradually becoming trend, such as 3C products, communication electronics, medical appliances, new energy automobiles, aerospace and other fields, and target devices of specific application of the electrification are such as 5G communication devices, 5G communication base stations, inductors, executive components, generators, intelligent temperature control devices, transformers, motors, transformers, chokes, complex dampers and the like. Therefore, there is a need for an inductance element with higher magnetic properties and higher efficiency to satisfy the trend of miniaturization of power devices. In particular, these arrangementsIs required to operate at high frequency above several hundred megahertz (MHz) and has high magnetic induction strength (B) s ) And low magnetic loss (W) m ) The soft magnetic alloy can meet the demands of modularization and high-efficiency integration of electronic devices, so that the soft magnetic material is a key material for high-efficiency operation of next-generation electronic power equipment and electronic devices thereof.
Magnetic powder core soft magnetic composite materials are important to research in the field of magnetic materials in recent years. In general, the preparation of the magnetic powder core soft magnetic composite material comprises the following steps: (1) Preparing soft magnetic alloy powder by using methods such as gas atomization or water atomization, wherein the soft magnetic material generally selects iron-based prealloy components containing silicon, nickel, aluminum or cobalt; (2) coating an insulating layer on the surface of the soft magnetic alloy powder; (3) mixing the insulation-coated soft magnetic powder with a lubricant; (4) Pressing the mixed powder obtained in the step (3) into a shape to prepare a green body; (5) Sintering at the temperature of 350-900 ℃ to obtain the magnetic powder core soft magnetic composite material. The magnetic powder core soft magnetic composite material insulating coating layer is characterized in that: each powder particle coated by the insulating layer has a very small eddy current path inside and it has a high electrical resistivity, which can lead to a substantial reduction of eddy current losses generated by the soft magnetic composite during operation. Thus, the individual soft magnetic powder particles and their insulating coating may be referred to as "functional elements", and the soft magnetic composite is formed by combining a plurality of functional elements.
On the other hand, the nanocrystalline soft magnetic composite material has higher magnetic induction intensity and magnetic conductivity. The nanocrystalline magnetically soft alloy has a unique structural length far lower than the ferromagnetic exchange length, so that the magnetic anisotropy constant is reduced, and the nanocrystalline magnetically soft alloy has excellent soft magnetic performance and can be applied to various occasions. According to definition, the functional element of the nanocrystalline consists of a soft magnetic amorphous matrix and nanocrystalline which is nucleated randomly, and the outside is a coated insulating layer. The internal structure is usually obtained by a two-stage route: firstly, an amorphous structure is obtained through rapid solidification, and then, nanocrystalline is formed through modification treatment and crystallization.
Yoshizawa et al, demonstrated that in Fe-SiAfter addition of small amounts of Cu and Nb to B (Fe-Si-B-Nb-Cu also known as Finemet alloy), sintering at 500 to 600 ℃ for 1 hour can have excellent soft magnetic properties. This is because the introduction of Cu increases the number of nucleation sites, while Nb prevents grain growth while inhibiting boride phase formation, so the microstructure developed consists of an amorphous matrix and alpha-Fe+FeSi nanocrystals (about 10 nm). However, B of Finemet alloy s The value is not yet able to meet some needs of high B s Is required for the inductive device. To develop a high B s Soft magnetic alloys, called Nanoperm alloys, were developed by scholars such as Suzuki, which are the manufacturing basis for Finemet alloys. Also, makino et al developed a nonomet alloy containing nonmetallic Fe-Si-B-P-Cu.
Although the Nanoperm alloy and the Nanomet alloy improve the saturation magnetic induction strength B s Value of but its magnetic loss W at high frequency operation m Still high, the low-loss requirements of increasingly miniaturized electronic devices in the future cannot be met. On the other hand, although the regulation of the material composition of the nanocrystalline magnetically soft alloy has been studied and reported, the regulation of the gradient size difference of the nanocrystalline has not been reported. Therefore, it is necessary to explore a nano gradient magnetic material with high magnetic induction and low loss so as to expand the industrialized application field.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a preparation method of a high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core, which is characterized in that Fe-based amorphous alloy powder is treated by discharge plasma to crystallize a powder surface layer, then the powder surface layer is pressed after a coating agent and a lubricant are added, finally sintering treatment is carried out at a temperature higher than the crystallization temperature, nanocrystalline grains on the powder surface continue to grow, the amorphous inside the powder starts to crystallize, and the gradient difference of grain sizes is formed, so that the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core with large grains on the outer layer and small grains on the inner layer is obtained.
The method can improve the magnetic permeability U of the original Fe-based micron-sized magnetic powder core i And the magnetic loss during middle and high frequency operation is reduced, the manufacturing process flow is simple, personalized manufacturing can be realized, andcan be produced in batch, and is especially suitable for the application of medium-high frequency electronic devices.
The invention also aims to provide the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss.
The invention also aims to provide the application of the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core in the electronic devices in the middle-high frequency field.
The high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core can be applied to the fields of 3C products, communication electronics, medical appliances, new energy automobiles, aerospace and the like, and target devices of specific application of the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core are such as 5G communication devices, 5G communication base stations, chokes, inductors, executive components, generators, intelligent temperature control devices, transformers, motors, transformers, dampers and the like.
The invention aims at realizing the following technical scheme:
a preparation method of a high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core comprises the following steps:
(1) Performing discharge plasma treatment on Fe-based amorphous alloy powder, wherein the treatment conditions are as follows: the voltage is 130-150V, the current is 1.6-2.2A, the rotating speed is 1000-1500 r/min, the discharge treatment time is 2-4 h each time, the discharge treatment is carried out for 10-30 minutes each time, the next discharge treatment is carried out until the discharge treatment times reach 5-10 times, and the Fe-based alloy powder with nano-crystallized surface is obtained;
(2) Mixing, coating and drying the Fe-based alloy powder with the coating agent, uniformly mixing with the lubricant, and performing compression molding to obtain a high-density magnetic powder core pressed compact;
(3) Sintering and forming the high-density magnetic powder core compact obtained in the step (2) in an inert gas atmosphere, wherein the surface nanocrystalline of the Fe-based alloy powder grows into large-size nanocrystalline, and the internal amorphous nanocrystalline is crystallized into small-size nanocrystalline, so that the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core is obtained.
Preferably, the conditions of the discharge plasma treatment in the step (1) are as follows: the voltage is 135V, the current is 2-2.3A, the rotating speed is 1100-1200 r/min, the discharge treatment time is 2.3-3 h each time, the discharge treatment is carried out for 10-30 minutes each time, and the next discharge treatment is carried out until the discharge treatment times reach 5-10 times.
Preferably, the content of Fe 70-90 at.% of Fe-based amorphous alloy powder element in the step (1) is the balance of two or more elements in the following components: si, co, B, C, P, cu, ni, mo, al, ta, nb and Sn; the particle size of the Fe-based amorphous alloy powder is 20-110 mu m.
More preferably, the Fe-based amorphous alloy powder of step (1) is Fe 83 Si 5 B 8 Cu 4 、Fe 80 Si 10 B 6 Nb 4 And Fe (Fe) 82 Si 7 B 6 P 3 Cu 2 At least one of them.
Preferably, the Fe-based amorphous alloy powder in the step (1) is prepared by raw material batching, rod making, rotary electrode atomization method for preparing alloy powder and sieving.
Preferably, the apparatus for the discharge Plasma treatment in the step (1) is a Plasma-BM-S type discharge Plasma machine.
Preferably, the discharge plasma treatment in the step (1) is performed in a stainless steel ball mill tank, and before the discharge plasma treatment, a high-purity inert gas is used for purifying the atmosphere, and then the inert gas is introduced.
Preferably, the Fe-based alloy powder with nano-crystallized surface in the step (1) is obtained, and a nano-crystal film with the thickness of 50-500 nm is obtained on the surface.
Preferably, the coating agent in the step (2) is organic silicon resin, and the coating agent and the organic solvent are mixed according to the volume ratio of 75-85: 25-15, and then mixing with surface nano-crystallized Fe-based alloy powder, wherein the mass ratio of the surface nano-crystallized Fe-based alloy powder to the coating agent solution is 10:1, a step of; the organic solvent is a ketone organic solvent, more preferably at least one of butanone and acetone.
Preferably, the Fe-based alloy powder with nano-crystallized surface in the step (2) is mixed and coated with a coating agent for 25-55 min; the drying temperature is 50-80 ℃ and the drying time is 20-40 min.
Preferably, the lubricant in the step (2) is zinc stearate, and the lubricant accounts for 0.1-0.5% of the total mass of the Fe-based alloy powder with the nano-crystallized surface and the coating agent.
Preferably, the time of mixing with the lubricant in the step (2) is 10-30 min.
Preferably, the pressure of the compression molding in the step (2) is 1.5-3 GPa, and the compression time is 5-60 s.
Preferably, the temperature of the sintering treatment in the step (3) is higher than the crystallization temperature of the Fe-based amorphous alloy powder, and the time is 10 min-1 h; more preferably 30 to 35 minutes.
Preferably, the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core obtained in the step (3) can be subjected to paint spraying treatment, wherein the paint spraying material is epoxy resin or polyester mixture, and the paint spraying thickness is 80-260 mu m; more preferably 80 to 150. Mu.m.
The paint spraying treatment of the obtained high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core aims at preventing the soft magnetic property of the magnetic powder core from being deteriorated due to oxidation and corrosion of oxygen, water and the like.
The gradient nanocrystalline magnetic powder core with high magnetic induction and low loss is prepared by the method.
The gradient nanocrystalline magnetic powder core with high magnetic induction and low loss is applied to electronic devices in the field of medium and high frequency (more than 30 MHz).
Preferably, the medium-high frequency (greater than 30 MHz) field is 3C products, communication electronics, medical devices, new energy automobiles and aerospace field; more preferred electronic devices are 5G communication devices, 5G communication base stations, chokes, inductors, performance components, generators, intelligent temperature control devices, transformers, motors, transformers, and dampers.
In the method, in the discharge treatment process of the discharge plasma in the step (1), high-frequency alternating current can generate high voltage between the iron core electrode rod and the stainless steel grinding groove, and the high voltage can break down the gas in the discharge chamber (between the discharge barrier and the grinding groove), so as to generate cold discharge plasma; in the discharging process, the instantaneous high temperature causes a layer of nano crystal film to be generated on the surface of Fe-based amorphous powder, the thickness is about 50-500 nm, and thus the soft magnetic gradient alloy powder with the nano surface and the amorphous structure inside is obtained. Meanwhile, partial closed pores in the Fe-based amorphous powder can be opened and most of satellite powder adhered on the surface of the powder can be removed in the plasma treatment process, so that the density of the pressed powder is improved. In the sintering process of the step (3), fe-based amorphous powder starts to crystallize, and as the plasma treatment in the step (1) causes the surface of the powder to crystallize, crystal grains on the surface of the powder continue to grow up, and crystallization starts to occur in the powder in the sintering process, so that gradient difference of crystal grain sizes is formed, specifically, the surface nanocrystalline grows to be nearly 100nm, the internal amorphous phase is crystallized to be about 10nm, and the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss of the large crystal grains on the outer layer and the small crystal grains on the inner layer is obtained.
Compared with the prior art, the invention has the following advantages:
the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core prepared by the method provided by the invention has the advantage that the unique gradient nano structure enables the magnetic performance of the Fe-based magnetic powder core to be improved. Compared with the Fe-based magnetic powder core which is not subjected to the nano crystallization treatment on the powder surface in the step (1), the magnetic conductivity and the saturation magnetic induction of the Fe-based magnetic powder core are improved by 8-15%, and in addition, the magnetic loss of the Fe-based magnetic powder core can be reduced by 6-10%. The invention has simple process of plasma discharge surface crystallization treatment, environmental protection and low cost, and can improve the comprehensive performance of the composite magnetic powder core.
Drawings
FIG. 1 is a schematic cross-sectional view of an amorphous alloy powder according to step (2) of the embodiment of the present application.
Fig. 2 is a schematic diagram of the sintering process to produce gradient nanocrystals according to step (4) of the present embodiment.
FIG. 3 is a schematic diagram of the gradient nanocrystals obtained in step (4) of the present application.
Fig. 4 shows the magnetic permeability of the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss in the step (5) paint spraying treatment of example 1.
Fig. 5 shows the saturation induction of the gradient nanocrystalline magnetic powder core with high induction and low loss in the step (5) paint spraying treatment of example 1.
Fig. 6 shows the magnetic loss of the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss in the step (5) paint spraying treatment of example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The specific conditions are not noted in the examples of the present invention, and are carried out according to conventional conditions or conditions suggested by the manufacturer. The raw materials, reagents, etc. used, which are not noted to the manufacturer, are conventional products commercially available.
Example 1
(1) Pulverizing: fe by designing pure iron, pure silicon, pure boron and pure copper 83 Si 5 B 8 Cu 4 Preparing materials in atomic percentage, preparing bars, preparing alloy powder by a rotary electrode gas atomization method, screening the powder to obtain Fe with the particle size of 20-110 mu m 83 Si 5 B 8 Cu 4 Spherical amorphous powder.
(2) Crystallizing the powder surface: fe obtained in the step (1) 83 Si 5 B 8 Cu 4 Placing spherical amorphous powder into stainless steel ball mill tank, and using pressure of 2×10 5 And purifying the atmosphere in the grinding tank for 3 times by Pa high-purity argon, and then introducing argon. The powder was treated using a Plasma-BM-S type discharge Plasma machine with a voltage set at 135V, a current controlled at 2A, a motor speed of 1100r/min, and a discharge treatment time of 2.5 hours each time. And carrying out the next time after the discharge treatment is finished for 10 minutes until the discharge treatment times reach 8 times. In the discharge process, high-frequency alternating current can generate high voltage between the iron core electrode rod and the stainless steel grinding groove, and the high voltage can break down gas in a discharge chamber (between a discharge barrier and the grinding groove), so that cold discharge plasma is generated. In the discharge process, the instantaneous high temperature causes Fe 83 Si 5 B 8 Cu 4 The spherical amorphous powder produced a nanocrystalline film on its surface, with a thickness of about 150nm. Meanwhile, fe can also be added in the plasma treatment process 83 Si 5 B 8 Cu 4 The partial closed-cell hollow powder in the spherical amorphous powder is opened and most of satellite powder adhered on the surface of the powder is removed, so that the density of the pressed powder is improved.
(3) Powder coating and compression molding: the organic silicon resin (MQ silicon resin) and acetone are mixed according to the mass ratio of 85:15, and then adding Fe which is subjected to plasma surface crystallization treatment in the step (2) 83 Si 5 B 8 Cu 4 And (3) spherical amorphous powder is stirred for 30min to finish coating, wherein the mass ratio of the amorphous powder to the organic silicon resin acetone mixed solution is 10:1. And (5) putting the coated powder into a drying oven at 65 ℃ for drying treatment for 30min. And then uniformly mixing the dried coated powder with zinc stearate, wherein the zinc stearate accounts for 0.4% of the total mass of the amorphous powder and the organic silicon resin. Finally cold pressing is carried out, the molding pressure is 2GPa, the pressing time is 20s, and Fe is molded 83 Si 5 B 8 Cu 4 A magnetic powder core.
(4) Sintering to generate gradient nanocrystalline: fe obtained in the step (3) 83 Si 5 B 8 Cu 4 And sintering the magnetic powder core in an argon atmosphere. Fe (Fe) 83 Si 5 B 8 Cu 4 The crystallization temperature of the alloy component is 490 ℃, so that the sintering temperature is 490 ℃ and the sintering time is 30min. Fe during sintering 83 Si 5 B 8 Cu 4 The amorphous powder starts to crystallize, and the surface of the powder is crystallized by the plasma treatment in the step 2, so that grains on the surface of the powder start to grow first and the inside starts to crystallize in the sintering process, and the gradient nanometer magnetic powder core with high magnetic induction and low loss is obtained due to the difference of grain sizes.
(5) And (3) paint spraying treatment: in order to prevent the soft magnetic property of the magnetic powder core from being deteriorated due to oxidation and corrosion of oxygen, water and the like, the gradient nano magnetic powder core with high magnetic induction and low loss obtained in the step (4) needs to be subjected to paint spraying treatment, and the paint spraying material is selected from epoxy resin E-44, and the paint spraying thickness is about 110 mu m.
The high-magnetic-induction low-loss nano-gradient Fe prepared by adopting the method 83 Si 5 B 8 Cu 4 Magnetic powder core, unique gradient nano structure to make Fe 83 Si 5 B 8 Cu 4 The nano magnetic performance of the magnetic powder core is improved. And Fe which has not been subjected to the surface crystallization treatment of the powder in the step (2) 83 Si 5 B 8 Cu 4 Compared with the magnetic powder core (only performing the steps (1), (3) to (5)), the magnetic permeability of the magnetic powder core is improved from 210H/m to 230H/m (shown in fig. 4), the magnetic permeability of the magnetic powder core is improved by 9%, the saturation induction intensity of the magnetic powder core is improved from 166 emu/g to 186emu/g, the saturation induction intensity of the magnetic powder core is improved by 11% (shown in fig. 5), and the magnetic loss of the magnetic powder core is reduced by 6.1% (shown in fig. 6). Therefore, the comprehensive demand characteristics of the composite magnetic powder core obtained through the surface crystallization treatment of the plasma discharge are improved.
Example 2
(1) Pulverizing: pure iron, pure silicon, pure boron and pure niobium are mixed according to Fe 80 Si 10 B 6 Nb 4 Preparing alloy powder by a designed atomic percentage batching and rod making method through a rotary electrode gas atomization method, and screening the powder to obtain Fe with the particle size of 20-110 mu m 80 Si 10 B 6 Nb 4 Spherical amorphous powder.
(2) Crystallizing the powder surface: fe obtained in the step (1) 80 Si 10 B 6 Nb 4 Placing spherical amorphous powder into stainless steel ball mill tank, and using pressure of 2×10 5 And purifying the atmosphere in the grinding tank for 3 times by Pa high-purity argon, and then introducing argon. The powder is processed by using a Plasma-BM-S type discharge Plasma machine, the voltage is set to be 135V, the current is controlled to be 2.1A, the motor rotating speed is 1200r/min, and the discharge processing time is 3h each time. And carrying out the next time after the discharge treatment is finished for 10 minutes until the discharge treatment times reach 7 times. In the discharge process, high-frequency alternating current can generate high voltage between the iron core electrode rod and the stainless steel grinding groove, and the high voltage can break down gas in a discharge chamber (between a discharge barrier and the grinding groove), so that cold discharge plasma is generated. In the discharge process, the instantaneous high temperature causes Fe 80 Si 10 B 6 Nb 4 The spherical amorphous powder produced a nanocrystalline film on its surface, with a thickness of about 150nm.Meanwhile, fe can also be added in the plasma treatment process 80 Si 10 B 6 Nb 4 The partial closed-cell hollow powder in the spherical amorphous powder is opened and most of satellite powder adhered on the surface of the powder is removed, so that the density of the pressed powder is improved.
(3) Powder coating and compression molding: the preparation method comprises the following steps of (1) mixing organic silicon resin (MQ silicon resin) and butanone according to a mass ratio of 80:20, and then adding Fe which is subjected to plasma surface crystallization treatment in the step (2) 83 Si 5 B 8 Cu 4 And (3) spherical amorphous powder is stirred for 35min to finish coating, wherein the mass ratio of the amorphous powder to the organic silicon resin acetone mixed solution is 10:1. And (5) putting the coated powder into a drying oven at 65 ℃ for drying treatment for 35min. And then uniformly mixing the dried coated powder with zinc stearate, wherein the zinc stearate accounts for 0.5% of the total mass of the amorphous powder and the organic silicon resin. Finally cold pressing to form Fe with the forming pressure of 2.2GPa and the pressing time of 25s 80 Si 10 B 6 Nb 4 A magnetic powder core.
(4) Sintering to generate gradient nanocrystalline: fe obtained in the step (3) 80 Si 10 B 6 Nb 4 And sintering the magnetic powder core in an argon atmosphere. Fe (Fe) 80 Si 10 B 6 Nb 4 The crystallization temperature of the alloy component is 440 ℃, so that the sintering temperature is 440 ℃ and the sintering time is 35min. Fe during sintering 80 Si 10 B 6 Nb 4 The amorphous powder starts to crystallize, and the surface of the powder is crystallized by the plasma treatment in the step 2, so that grains on the surface of the powder start to grow first and the inside starts to crystallize in the sintering process, and the gradient nanometer magnetic powder core with high magnetic induction and low loss is obtained due to the difference of grain sizes.
(5) And (3) paint spraying treatment: in order to prevent the soft magnetic property of the magnetic powder core from being deteriorated due to oxidation and corrosion of oxygen, water and the like, the gradient nano magnetic powder core with high magnetic induction and low loss obtained in the step (4) needs to be subjected to paint spraying treatment, and the paint spraying material is selected from epoxy resin type E-44, and the paint spraying thickness is about 130 mu m.
The nano-gradient Fe with high magnetic induction and low loss prepared by adopting the scheme 80 Si 10 B 6 Nb 4 Magnetic powder core, unique gradient nano structure to make Fe 80 Si 10 B 6 Nb 4 The nano magnetic performance of the magnetic powder core is improved. And Fe which has not been subjected to the surface crystallization treatment of the powder in the step (2) 80 Si 10 B 6 Nb 4 Compared with the magnetic powder core (only steps (1), (3) to (5)) the magnetic powder core has the magnetic conductivity improved from 215H/m to 240H/m by 11%, the saturation magnetic induction intensity improved from 160 emu/g to 179emu/g by 10%, and the magnetic loss reduced by 7.2%. Therefore, the comprehensive demand characteristics of the composite magnetic powder core obtained through the surface crystallization treatment of the plasma discharge are improved.
Example 3
(1) Pulverizing: pure iron, pure silicon, pure boron, pure copper, iron-phosphorus alloy are mixed according to Fe 82 Si 7 B 6 P 3 Cu 2 Preparing alloy powder by a designed atomic percentage batching and rod making method through a rotary electrode gas atomization method, and screening the powder to obtain Fe with the particle size of 20-110 mu m 82 Si 7 B 6 P 3 Cu 2 Spherical amorphous powder.
(2) Crystallizing the powder surface: fe obtained in the step (1) 82 Si 7 B 6 P 3 Cu 2 Placing spherical amorphous powder into stainless steel ball mill tank, and using pressure of 2×10 5 And purifying the atmosphere in the grinding tank for 3 times by Pa high-purity argon, and then introducing argon. The powder is processed by using a Plasma-BM-S type discharge Plasma machine, the voltage is set to be 135V, the current is controlled to be 2.3A, the motor rotating speed is 1000r/min, and the discharge processing time is 2.3h each time. And carrying out the next time after the discharge treatment is finished for 10 minutes until the discharge treatment times reach 9 times. In the discharge process, high-frequency alternating current can generate high voltage between the iron core electrode rod and the stainless steel grinding groove, and the high voltage can break down gas in a discharge chamber (between a discharge barrier and the grinding groove), so that cold discharge plasma is generated. In the discharge process, the instantaneous high temperature causes Fe 82 Si 7 B 6 P 3 Cu 2 The spherical amorphous powder produced a nanocrystalline film on its surface, with a thickness of about 180nm. Meanwhile, fe can also be added in the plasma treatment process 82 Si 7 B 6 P 3 Cu 2 The partial closed-cell hollow powder in the spherical amorphous powder is opened and most of satellite powder adhered on the surface of the powder is removed, so that the density of the pressed powder is improved.
(3) Powder coating and compression molding: the organic silicon resin (MQ silicon resin) and acetone are mixed according to the mass ratio of 82:18, uniformly mixing to obtain an organic silicon resin acetone mixed solution, and then adding Fe subjected to plasma surface crystallization treatment in the step (2) 83 Si 5 B 8 Cu 4 And (3) spherical amorphous powder is stirred for 28min to finish coating, wherein the mass ratio of the amorphous powder to the organic silicon resin acetone mixed solution is 10:1. And (5) putting the coated powder into a drying oven at 60 ℃ for drying treatment for 40min. And then uniformly mixing the dried coated powder with zinc stearate, wherein the zinc stearate accounts for 0.4% of the total mass of the amorphous powder and the organic silicon resin. Finally cold pressing is carried out, the molding pressure is 2.3GPa, the pressing time is 15s, and Fe is molded 82 Si 7 B 6 P 3 Cu 2 A magnetic powder core.
(4) Sintering to generate gradient nanocrystalline: fe obtained in the step (3) 82 Si 7 B 6 P 3 Cu 2 And sintering the magnetic powder core in an argon atmosphere. Fe (Fe) 82 Si 7 B 6 P 3 Cu 2 The crystallization temperature of the alloy component is 452 ℃, so that the sintering temperature is 452 ℃ and the sintering time is 40min. Fe during sintering 82 Si 7 B 6 P 3 Cu 2 The amorphous powder starts to crystallize, and the surface of the powder is crystallized by the plasma treatment in the step 2, so that grains on the surface of the powder start to grow first and the inside starts to crystallize in the sintering process, and the gradient nanometer magnetic powder core with high magnetic induction and low loss is obtained due to the difference of grain sizes.
(5) And (3) paint spraying treatment: in order to prevent the soft magnetic property of the magnetic powder core from being deteriorated due to oxidation and corrosion of oxygen, water and the like, the gradient nano magnetic powder core with high magnetic induction and low loss obtained in the step (4) needs to be subjected to paint spraying treatment, and the paint spraying material is selected from epoxy resin E-44, and the paint spraying thickness is about 115 mu m.
The nano-gradient Fe with high magnetic induction and low loss prepared by adopting the scheme 82 Si 7 B 6 P 3 Cu 2 Magnetic powder core, unique gradient nano structure to make Fe 82 Si 7 B 6 P 3 Cu 2 The nano magnetic performance of the magnetic powder core is improved. And Fe which has not been subjected to the surface crystallization treatment of the powder in the step (2) 82 Si 7 B 6 P 3 Cu 2 Compared with the magnetic powder core (only steps (1), (3) - (5)) in which the magnetic permeability is improved from 224H/m to 245H/m by 9%, the saturation magnetic induction intensity is improved from 157emu/g to 179emu/g by 12%, and the magnetic loss is reduced by 8.1%. Therefore, the comprehensive demand characteristics of the composite magnetic powder core obtained through the surface crystallization treatment of the plasma discharge are improved.
Comparative example 1
The comparative example only changed the parameters of the plasma ball milling treatment in the step (2) to make Fe 83 Si 5 B 8 Cu 4 The amorphous alloy powder surface was not crystallized and its composition and other experimental parameters were the same as in example 1.
(1) Pulverizing: fe by designing pure iron, pure silicon, pure boron and pure copper 83 Si 5 B 8 Cu 4 Preparing materials in atomic percentage, preparing bars, preparing alloy powder by a rotary electrode gas atomization method, screening the powder to obtain Fe with the particle size of 20-110 mu m 83 Si 5 B 8 Cu 4 Spherical amorphous powder.
(2) Crystallizing the powder surface: fe obtained in the step (1) 82 Si 7 B 6 P 3 Cu 2 Placing spherical amorphous powder into stainless steel ball mill tank, and using pressure of 2×10 5 And purifying the atmosphere in the grinding tank for 3 times by Pa high-purity argon, and then introducing argon. The powder was treated by using a Plasma-BM-S type discharge Plasma machine, the voltage was set to 130V, the current was controlled to 1.7A, the motor speed was 1000r/min, and the discharge treatment time was 2 hours each time.And carrying out the next time after the discharge treatment is finished for 10 minutes until the discharge treatment times reach 9 times.
(3) Powder coating and compression molding: the organic silicon resin (MQ silicon resin) and acetone are mixed according to the mass ratio of 85:15, and then adding Fe which is subjected to plasma surface crystallization treatment in the step (2) 83 Si 5 B 8 Cu 4 And (3) spherical amorphous powder is stirred for 30min to finish coating, wherein the mass ratio of the amorphous powder to the organic silicon resin acetone mixed solution is 10:1. And (5) putting the coated powder into a drying oven at 65 ℃ for drying treatment for 30min. And then uniformly mixing the dried coated powder with zinc stearate, wherein the zinc stearate accounts for 0.4% of the total mass of the amorphous powder and the organic silicon resin. Finally cold pressing is carried out, the molding pressure is 2GPa, the pressing time is 20s, and Fe is molded 83 Si 5 B 8 Cu 4 A magnetic powder core.
(4) Sintering treatment to generate nanocrystalline: fe obtained in the step (3) 83 Si 5 B 8 Cu 4 And sintering the magnetic powder core in an argon atmosphere. Fe (Fe) 83 Si 5 B 8 Cu 4 The crystallization temperature of the alloy component is 490 ℃, so that the sintering temperature is 490 ℃ and the sintering time is 30min. Fe during sintering 83 Si 5 B 8 Cu 4 The amorphous powder forms nanocrystals.
(5) And (3) paint spraying treatment: in order to prevent the soft magnetic property of the magnetic powder core from being deteriorated due to oxidation and corrosion of oxygen, water and the like, the gradient nano magnetic powder core with high magnetic induction and low loss obtained in the step (4) needs to be subjected to paint spraying treatment, and the paint spraying material is selected from epoxy resin E-44, and the paint spraying thickness is about 110 mu m.
Fe prepared by the method 83 Si 5 B 8 Cu 4 A magnetic powder core with a permeability of 214H/m and a saturation induction of 169 emu/g, compared with the nano-gradient Fe of example 1 83 Si 5 B 8 Cu 4 The magnetic powder core has a magnetic permeability reduced by 7%, a saturation induction strength reduced by 9.2%, and a magnetic loss increased by 6.2%. It can be seen that the difference in grain structure results in the preparation ofFe 83 Si 5 B 8 Cu 4 The magnetic property of the magnetic powder core is reduced.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss is characterized by comprising the following steps:
(1) Performing discharge plasma treatment on Fe-based amorphous alloy powder, wherein the treatment conditions are as follows: the voltage is 135V, the current is 2-2.3A, the rotating speed is 1100-1200 r/min, the discharge treatment time is 2.3-3 h each time, the discharge treatment is carried out for 10-30 minutes each time, the next discharge treatment is carried out until the discharge treatment times reach 5-10 times, and the Fe-based alloy powder with nano-crystallized surface is obtained;
the discharge plasma treatment in the step (1) is carried out in a stainless steel ball mill tank;
(2) Uniformly mixing the Fe-based alloy powder subjected to surface nano crystallization in the step (1) with a coating agent, coating and drying, uniformly mixing with a lubricant, and performing compression molding to obtain a high-density magnetic powder core compact;
(3) Sintering and forming the high-density magnetic powder core compact obtained in the step (2) in an inert gas atmosphere, wherein the nanocrystalline on the surface of the Fe-based alloy powder grows into large-size nanocrystalline, and the amorphous inside of the Fe-based alloy powder is crystallized into small-size nanocrystalline, so that the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss is obtained.
2. The method for preparing the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss according to claim 1, wherein the content of Fe-based amorphous alloy powder elements in the step (1) is between 70 and 90 at%, and the balance is composed of two or more elements of the following components: si, co, B, C, P, cu, ni, mo, al, ta, nb and Sn; the grain diameter of the Fe-based amorphous alloy powder is 20-110 mu m;
the sintering treatment temperature in the step (3) is higher than the crystallization temperature of Fe-based amorphous alloy powder, and the time is 10 min-1 h.
3. The method for preparing a gradient nanocrystalline magnetic powder core with high magnetic induction and low loss according to claim 1, wherein the Fe-based amorphous alloy powder in step (1) is Fe 83 Si 5 B 8 Cu 4 、Fe 80 Si 10 B 6 Nb 4 And Fe (Fe) 82 Si 7 B 6 P 3 Cu 2 At least one of (a) and (b);
the sintering treatment time in the step (3) is 30-35 min.
4. The method for preparing a gradient nanocrystalline magnetic powder core with high magnetic induction and low loss according to claim 1, wherein the thickness of the surface crystal film of the surface nanocrystalline Fe-based alloy powder in step (1) is 50-500-nm.
5. The method for preparing the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss according to claim 1, wherein the step (1) is to use high-purity inert gas to purify the atmosphere before discharging plasma treatment, and then to introduce the inert gas;
the coating agent in the step (2) is organic silicon resin, and the volume ratio of the coating agent to the organic solvent is 75-85: 25-15, and then mixing with surface nano-crystallized Fe-based alloy powder, wherein the mass ratio of the surface nano-crystallized Fe-based alloy powder to the coating agent solution is 10:1, a step of;
the lubricant in the step (2) is zinc stearate, and the lubricant accounts for 0.1-0.5% of the total mass of the Fe-based alloy powder with nano-crystallized surface and the coating agent;
the pressure of the compression molding in the step (2) is 1.5-3 GPa.
6. The method for preparing the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core according to claim 1, wherein the high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core obtained in the step (3) is subjected to paint spraying treatment, the paint spraying material is epoxy resin or polyester mixture, and the paint spraying thickness is 80-260 μm.
7. The high-magnetic-induction low-loss gradient nanocrystalline magnetic powder core prepared by the method of any one of claims 1 to 6.
8. The application of the gradient nanocrystalline magnetic powder core with high magnetic induction and low loss in the electronic device in the middle-high frequency field of claim 7.
9. The use of a high magnetic induction low loss gradient nanocrystalline magnetic powder core according to claim 8 in mid-to-high frequency domain electronics, wherein the mid-to-high frequency domain is 3C product domain, communication electronics domain, medical device domain, new energy automotive domain, and aerospace domain.
10. The use of a high magnetic induction low loss gradient nanocrystalline magnetic powder core according to claim 9 in medium and high frequency domain electronics, wherein the medium and high frequency domain electronics are 5G communication base stations, 5G communication devices, inductors, executive components, generators, intelligent temperature control devices, transformers, motors, transformers, chokes and dampers.
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