CN117153515A - Iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof - Google Patents

Iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof Download PDF

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CN117153515A
CN117153515A CN202311096671.8A CN202311096671A CN117153515A CN 117153515 A CN117153515 A CN 117153515A CN 202311096671 A CN202311096671 A CN 202311096671A CN 117153515 A CN117153515 A CN 117153515A
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iron
alloy powder
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soft magnetic
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张岩
高菡
臧博闻
向明亮
霍军涛
王军强
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/008—Amorphous alloys with Fe, Co or Ni as the major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—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 metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/24—Magnetic cores
    • H01F27/255—Magnetic cores made from particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F3/00—Cores, Yokes, or armatures
    • H01F3/08—Cores, Yokes, or armatures made from powder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

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Abstract

The invention discloses an iron-based amorphous soft magnetic alloy powder, which is prepared from the following components in percentage by weight a Si b B c P d Cu e C f Ni g M m The method comprises the steps of smelting alloy raw materials with a+b+c+d+e+f+g+m=100 to obtain a master alloy, and processing the master alloy by an aerosol method to obtain the alloy, wherein M is at least one of transition metal elements Sc, ti, V, cr, mn, co, zr, nb, and the atomic percentage of each element is as follows: a is more than or equal to 74 and less than or equal to 81,0.5, b is more than or equal to 7,8.5, c is more than or equal to 10.5,5, d is more than or equal to 7, e is more than or equal to 0.5 and less than or equal to 0.8, f is more than or equal to 0 and less than or equal to 2, g is more than or equal to 1 and less than or equal to 1.5, and m is more than or equal to 0 and less than or equal to 4. The invention also discloses nanocrystalline soft magnetic alloy powder and nanocrystalline magnetic powder cores prepared from the iron-based amorphous soft magnetic alloy powder. The invention obtains the iron-based amorphous soft magnetic alloy powder with better amorphous forming capability under the condition of a certain high iron content, and the iron-based nanocrystalline soft magnetic alloy powder obtained after crystallization and annealing has the advantages of high saturation magnetic induction intensity, higher magnetic permeability and lower loss.

Description

Iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof.
Background
The iron-based amorphous nanocrystalline alloy is excellent in heat resistance due to its high saturation induction (B s ) Low coercivity (H) c ) High effective permeability (mu) e ) The silicon steel is widely applied in the field of power equipment, and can replace silicon steel in the field of power transmission and conversion, so that the development of miniaturization and energy conservation of devices can be promoted. In the soft magnetic material, the soft magnetic composite material combines the advantages of soft magnetic ferrite and soft magnetic alloy material, has good soft magnetic performance and good insulating performance, and has good three-dimensional isotropy, higher resistivity, higher saturation induction intensity and lower magnetic core loss.
The current method for improving the soft magnetic composite material is concentrated on insulating coating and component regulation, wherein the components of the soft magnetic alloy powder more intuitively determine the soft magnetic performance of the soft magnetic composite material. In addition, the powder obtained by different preparation methods has different microstructures, the powder prepared by a water atomization method and a mechanical ball milling method which are commonly used in the market has low sphericity, is difficult to coat and further can influence the loss of a magnetic powder core, so that the performance of the magnetic powder core is reduced, and the powder prepared by an air atomization method has the advantages of better sphericity, smaller particles and more uniform distribution, is favorable for later coating, and further reduces the loss.
The Fe-Si-B-Nb-Cu nanocrystalline alloy system has better soft magnetism and low H c High mu e But B is the advantage of s Lower, which is detrimental to the development of miniaturization of the device. Fe-Si-B-P-Cu nanocrystalline alloy system having high B s However, the heat treatment process with relatively high heating rate required by the alloy components is difficult to realize in industrial mass production, and the final nanocrystalline alloy powder H c The preparation and the industrialization application of the high-frequency low-loss magnetic powder core are not facilitated. The addition of C element in Fe-Si-B-P-Cu-C nanocrystalline alloy system effectively reduces the necessary heating rate of the heat treatment process, but the preparation of alloy powder with excellent amorphous structure is still difficult to obtain for the gas atomization preparation method with relatively low cooling rate, and the nanocrystalline structure with lower average grain size is still difficult to obtain even through crystallization heat treatment process, so that the preparation of alloy powder with low coercivity is not favored.
In summary, amorphous nanocrystalline powder has a wide application background, but most of the existing soft magnetic alloy powder on the market is prepared by a water atomization method and a mechanical crushing method, and the prepared powder has poor sphericity, is not easy to coat and has uneven particle size; and the existing iron-based amorphous nanocrystalline alloy is lower in B s Or higher H c And the heat treatment mode which is difficult to realize hinders the application scene and the industrialized development of the nanocrystalline magnetic powder core. Therefore, developing nanocrystalline alloy powder with high saturation magnetic induction intensity, high magnetic permeability, high DC bias performance and low loss component has very important industrialization value.
Patent document publication No. CN110541116B discloses an iron-based nanocrystalline magnetically soft alloy with controllable crystallization,the chemical composition of the iron-based nanocrystalline magnetically soft alloy is Fe 84 Si 2 B 13-x Cu 1 P x Wherein x is more than or equal to 1 and less than or equal to 4; after undergoing an amorphous structure, the iron-based nanocrystalline magnetically soft alloy finally has a nanocrystalline structure after heat treatment, and the grain size is 8-12nm; the saturation magnetic induction intensity is 1.57-1.85T. The method has poor amorphous forming ability of alloy component and large amount of B element, which causes the powder obtained by gas atomization method to contain a large amount of Fe-B phase, so that H c Higher.
Patent document publication No. CN115537684A discloses a novel iron-based amorphous nanocrystalline wave-absorbing material and a method for producing the same, which uses a high Fe high C alloy raw material, has poor amorphous forming ability, contains Fe-B phase in powder with diameter below 20 μm obtained by an aerosol method, has a larger average alpha-Fe grain size after crystallization heat treatment, and has a structure which leads to H of alloy powder c Higher, the hysteresis loss after press forming cannot be kept low.
Patent document with publication number CN114045435B discloses an iron-based amorphous nanocrystalline wave absorbing material and a preparation method thereof, wherein the iron-based amorphous nanocrystalline wave absorbing material comprises induction smelting, ultrahigh-pressure water vapor combined atomization, and processes of later mechanical ball milling, crystallization annealing treatment and the like are matched. The amorphous powder obtained by the method has poor sphericity and is unfavorable for the later pressing and insulating coating treatment.
In view of the defects in the prior art, by means of alloy component regulation and improvement of a preparation process, the amorphous nanocrystalline powder with high saturation induction and low loss is developed, and the soft magnetic performance of the powder is improved, so that the key requirement of the current industrialization on the magnetic powder core is particularly important.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention provides iron-based amorphous soft magnetic alloy powder which has high sphericity and smooth surface and is easy for later insulating coating.
An Fe-based amorphous soft magnetic alloy powder is prepared from Fe with molecular formula a Si b B c P d Cu e C f Ni g M m Wherein a+b+c+d+e+f+g+m=100The alloy raw material is smelted to obtain master alloy, and then the master alloy is prepared by an aerosol method, wherein M is at least one of transition metal elements Sc, ti, V, cr, mn, co, zr, nb, and the atomic percentage of each element is as follows: a is more than or equal to 74 and less than or equal to 81,0.5, b is more than or equal to 7,8.5, c is more than or equal to 10.5,5, d is more than or equal to 7, e is more than or equal to 0.5 and less than or equal to 0.8, f is more than or equal to 0 and less than or equal to 2, g is more than or equal to 1 and less than or equal to 1.5, and m is more than or equal to 0 and less than or equal to 4.
The invention adopts the alloy raw materials with high iron content, and prepares the iron-based amorphous soft magnetic alloy powder by an air atomization method, so that the sphericity of the obtained powder is higher, the particle distribution is more uniform, and the invention is beneficial to the later-stage pressing and insulating coating. The alloy component has higher amorphous forming capability, and the alloy powder prepared by the gas atomization method has an excellent initial amorphous structure, and can obtain a uniform nanocrystalline composite structure after crystallization annealing heat treatment. The average grain size of alpha-Fe grains in the structure is lower, so that the alloy powder has higher magnetic permeability and lower coercivity; meanwhile, due to precipitation of a large number of alpha-Fe crystal grains, the magnetic powder has high saturation magnetic induction intensity; smaller powder particle sizes can be obtained by pressure adjustment. Because the alloy system has the intrinsic magnetic characteristics of high saturation induction intensity, high magnetic permeability and low coercivity, the magnetic powder core obtained after compression molding shows lower loss; the magnetic powder core obtained by pressing the powder with smaller particle size has good high-frequency stability.
Preferably, in order to make the iron-based amorphous soft magnetic alloy powder have high saturation induction, the ferromagnetic element should be kept at a high value, i.e., 77.ltoreq.a+g.ltoreq.81.5.
Preferably, in order to make the prepared iron-based amorphous soft magnetic alloy powder have higher amorphous forming capability, the content of the metalloid element is also kept larger, namely 11.5-15.5.
The atomic percentage of Fe is related to the saturation magnetic induction, the alloy powder with high Fe content is favorable for obtaining high saturation magnetic induction, and the atomic percentage of Fe in the iron-based amorphous soft magnetic alloy powder is more than or equal to 74 and less than or equal to 81. By regulating and controlling the content of Fe, the alloy is enabled to separate out alpha-Fe crystal grains with higher content after the heat treatment process, and the separation of Fe-B nonmagnetic phase crystal grains is inhibited, the saturation magnetic induction intensity of the powder is improved, and excellent soft magnetic performance is obtained.
The Si element can widen the annealing interval, so that the initial crystallization peak moves towards a higher temperature direction, the thermal stability of the alloy is enhanced, the addition of B, P and C elements can improve the amorphous forming capability of the powder matrix, alpha-Fe grains are more completely separated out during the heat treatment, but the addition of excessive B element can narrow the annealing interval between the two crystallization peaks, so as to obtain an ideal nanocrystalline structure, the atomic percentage of Si in the iron-based amorphous soft magnetic alloy powder is more than or equal to 0.5 and less than or equal to 7, the atomic percentage of B is more than or equal to 8.5 and less than or equal to 10.5, the atomic percentage of P is more than or equal to 5 and less than or equal to d and less than or equal to 7, and the atomic percentage of C is more than or equal to 0 and less than or equal to 2.
In the iron-based nanocrystalline alloy with high iron content, cu promotes the precipitation of alpha-Fe crystal grains, can refine the crystal grains and promote the uniformity of particle dispersion, and the addition of Cu can reduce the coercive force of alloy powder, wherein the atomic content percentage of Cu in the iron-based amorphous soft magnetic alloy powder is more than or equal to 0.5 and less than or equal to 0.8.
The Ni element can improve amorphous forming ability and improve high-temperature soft magnetic property stability of the iron-based alloy. The element M in the alloy is at least one of transition metal elements Sc, ti, V, cr, mn, co, zr, nb, but because of the excessively high cost, the atom percentage content of Ni in the iron-based amorphous soft magnetic alloy powder is more than or equal to 1 and less than or equal to 1.5, and the atom percentage content of M is more than or equal to 0 and less than or equal to 4.
Preferably, the middle diameter D of the iron-based amorphous soft magnetic alloy powder 50 17-18 μm.
Preferably, the atomization gas pressure of the gas atomization method is 8-10 MPa, and too small pressure can reduce the cooling rate of the sprayed melt, further cause the deterioration of the initial amorphous structure of the alloy powder, and cause the precipitation of crystal grains with larger grain sizes and even the precipitation of crystal phases other than alpha-Fe crystal grains.
Preferably, the nozzle angle adopted by the gas atomization method is 30-45 degrees, and the aperture of the quartz tube is 0.8-1.0 mm. Too large a pore size will result in a median diameter D of the alloy powder particles resulting from the spraying 50 Too large, is unfavorable for the refinement of powder; at the same time, too large powder particlesThe cooling time of the pellets is long, and it is difficult to obtain an excellent initial amorphous structure.
The invention also provides a nanocrystalline magnetic powder core, which is prepared by mixing the iron-based amorphous soft magnetic alloy powder with an epoxy resin adhesive and pressing the mixture by a cold pressing method; and then carrying out heat treatment on the amorphous magnetic powder core in a vacuum state. The nanocrystalline magnetic powder core has high saturation magnetic induction intensity, low loss and excellent soft magnetic performance.
Preferably, the epoxy resin is W-6D epoxy resin, and the mass fraction of the W-6D epoxy resin in the amorphous magnetic powder core is 2-3 wt%.
Preferably, the heat treatment temperature is 400-500 ℃ and the time is 45-90 min. The amorphous magnetic powder core is subjected to heat treatment to form a nanocrystalline structure, so that the soft magnetic performance of the amorphous magnetic powder core can be further improved, and the magnetic loss is reduced.
The invention also provides application of the nanocrystalline magnetic powder core in the field of integrally formed inductors. The nanocrystalline magnetic powder core has high saturation magnetic induction intensity, excellent soft magnetic performance and low loss, and can meet the development requirements of magnetic elements on high frequency, high efficiency and miniaturization. The material has wide application prospect in the fields of power transformers and high-frequency devices, and is a core base material for improving the electric energy transmission efficiency.
The invention also discloses an iron-based nanocrystalline magnetically soft alloy powder, which is prepared by heat treatment of the iron-based amorphous magnetically soft alloy powder in a vacuum state. The iron-based nanocrystalline magnetically soft alloy powder has uniform particle size distribution and excellent soft magnetic performance.
Preferably, the heat treatment temperature is 400-500 ℃ and the time is 45-90 min.
Preferably, the saturation induction intensity B of the iron-based nanocrystalline magnetically soft alloy powder s 170-185 emu/g.
Preferably, the alpha-Fe average grain size of the iron-based nanocrystalline magnetically soft alloy powder is 25-27 nm.
The iron-based nanocrystalline magnetically soft alloy powder can also be used for preparing nanocrystalline magnetic powder cores, and nanocrystalline magnetic powder cores prepared by using the iron-based nanocrystalline magnetically soft alloy powder are beneficial to miniaturization and high frequency of devices, and can be applied to the aspects of inductors, transformers, switching power supplies and the like.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The invention adopts the gas atomization method to prepare the iron-based amorphous soft magnetic alloy powder, the sphericity of the obtained powder is higher, the particle distribution is more uniform, and the invention is beneficial to the later-stage pressing and insulating coating.
(2) The alloy composition has better amorphous forming capability, the iron-based amorphous soft magnetic alloy powder prepared by an air atomization method of the alloy has an excellent initial amorphous structure, a good nanocrystalline structure can be obtained after crystallization annealing heat treatment, and the average grain size of the nanocrystalline structure is lower, so that the iron-based amorphous soft magnetic alloy powder has high saturation magnetic induction and excellent soft magnetic property; the magnetic powder core after compression molding has the characteristics of high frequency and low loss, and meanwhile, the magnetic permeability of the magnetic powder core has good high-frequency stability.
(3) The invention has simple production process, low cost and mature process and is suitable for large-scale production.
Drawings
Fig. 1 is a scanning electron microscope image of the iron-based amorphous soft magnetic alloy powder in example 1.
Fig. 2 is an X-ray diffraction pattern of the iron-based amorphous soft magnetic alloy powder and the heat-treated nanocrystalline soft magnetic alloy powder in example 1.
Fig. 3 is a differential heat scanning calorimetric curve of the iron-based amorphous soft magnetic alloy powder and the nanocrystalline soft magnetic alloy powder after heat treatment in example 1.
Fig. 4 is a graph showing the magnetometer curves of vibration samples of the iron-based amorphous soft magnetic alloy powder and the nanocrystalline soft magnetic alloy powder after heat treatment in example 1.
Detailed Description
In order to further illustrate the technical aspects of the present invention, preferred embodiments of the present invention are described below with reference to examples, but it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, and are not limiting of the present invention.
Example 1
The alloy composition in this embodiment is Fe 80.5 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1 . The preparation method of the iron-based amorphous soft magnetic alloy powder, the iron-based nanocrystalline soft magnetic alloy powder and the nanocrystalline magnetic powder core comprises the following steps:
s1, proportioning: fe, si, B, fe with purity of not less than 99% 3 P, cu, C and Ni alloy raw materials are Fe according to atomic percent 80.5 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1 Weighing to prepare alloy raw materials;
s2, smelting master alloy: placing the alloy raw materials prepared in the step S1 into an induction smelting furnace, vacuumizing to less than 1.0Pa, smelting the alloy in an argon atmosphere with the purity of 99%, preserving heat for 10min after smelting, and repeatedly smelting each alloy ingot for three times to ensure the component uniformity of the alloy to form master alloy;
s3, preparing iron-based amorphous soft magnetic alloy powder: and (2) placing the master alloy prepared in the step (S2) into an air atomizing device, wherein a nozzle is 1.0mm, and the angle of the nozzle is 30-45 degrees. Heating and melting the master alloy to a gushing state, and preserving heat at the temperature for 10s after complete melting, wherein the pressure of the adopted atomized gas is more than or equal to 8MPa, so as to obtain the iron-based amorphous soft magnetic alloy powder in an extremely cold state;
s4, preparing an amorphous magnetic powder core: the iron-based amorphous soft magnetic alloy powder prepared in the step S3 is doped with 2wt.% of epoxy resin and dissolved in acetone, the iron-based amorphous soft magnetic alloy powder is coated under ultrasonic vibration, and is pressed into an amorphous magnetic powder core with the inner diameter of 8mm, the outer diameter of 13mm and the thickness of 2mm under the pressure of 1.8GPa by adopting a cold pressing method;
s5, heat treatment: sealing the iron-based amorphous soft magnetic alloy powder prepared in the step S3 and the amorphous magnetic powder core prepared in the step S4 in a vacuum state (less than or equal to 5 multiplied by 10) -3 Pa), placing the powder into a vacuum tube furnace at a certain temperature for heat treatment, and preserving heat for 60min, wherein the heat treatment temperature of the iron-based amorphous soft magnetic alloy powder is 420-500 ℃, and the heat treatment temperature of the amorphous magnetic powder core is 420-500 ℃ to obtain the iron-based nanometerCrystalline magnetically soft alloy powder and nanocrystalline magnetic powder cores.
The iron-based amorphous soft magnetic alloy powder obtained by the method and the iron-based nanocrystalline soft magnetic alloy powder obtained by heat treatment and nanocrystalline magnetic powder core are detected as follows:
sieving the iron-based amorphous soft magnetic alloy powder obtained in the step S3 to obtain a median diameter D 50 The surface morphology of the iron-based amorphous soft magnetic alloy powder is shown in figure 1 by using a scanning electron microscope SEM to observe the alloy powder with the particle size of 17-18 mu m, and the powder prepared by an air atomization method is good in sphericity and uniform in particle distribution as can be seen from figure 1.
And (3) performing microstructure analysis on the iron-based amorphous soft magnetic alloy powder obtained in the step S3 by adopting X-ray diffraction (XRD). FIG. 2 shows that XRD patterns of the iron-based amorphous soft magnetic alloy powder prepared in the step S3 are steamed bread peaks, and no crystals are precipitated; XRD pattern of nanocrystalline soft magnetic alloy powder obtained after heat treatment in step S5 shows that at temperature T a Heat treatment at 420 ℃ for 60min, wherein the heat treatment has obvious sharp diffraction peaks near 2θ=45°, 65 ° and 85 °, i.e. alpha-Fe crystal grains are precipitated, and the average grain size of the alpha-Fe crystal grains is 27nm; with increasing temperature, at temperature T a Under the conditions of 500 ℃ and 60min of heat preservation, fe-B phase is separated out.
The heat performance analysis is carried out on the iron-based amorphous soft magnetic alloy powder in the step S3 and the nanocrystalline soft magnetic alloy powder after the heat treatment in the step S5 by adopting a Differential Scanning Calorimetry (DSC), the obtained DSC curve is shown in the figure 3, and the temperature T of the iron-based amorphous soft magnetic alloy powder is known from the figure 3 a Heat treatment at 420 ℃ for 60min, and complete alpha-Fe grain precipitation; with increasing temperature, at temperature T a Under the conditions of 500 ℃ and 60min of heat preservation, the Fe-B phase is completely separated out.
Magnetic property analysis is carried out on the iron-based amorphous soft magnetic alloy powder prepared in the step S3 and the nanocrystalline soft magnetic alloy powder subjected to heat treatment in the step S5 by adopting a Vibrating Sample Magnetometer (VSM), and the obtained VSM curve is shown as figure 4, and the B of the iron-based amorphous soft magnetic alloy powder s B of nano-crystalline soft magnetic alloy powder after 420 ℃ heat treatment at 171.48emu/g s 180.02emu/g from VSM graphIt appears that the soft magnetic powder exhibits typical soft magnetic properties.
The iron-based nanocrystalline magnetically soft alloy powder prepared in this example had an average grain size of α -Fe (D), and a saturation induction density (B s ) Coercivity (H) c ) And the density (ρ) of the nanocrystalline magnetic powder core are shown in table 1.
Example 2
The alloy composition in this example is: fe (Fe) 80.5 Si 0.5 B 8.5 P 7 Cu 0.5 C 2 Ni 1 The method for preparing the iron-based amorphous soft magnetic alloy powder, the nanocrystalline soft magnetic alloy powder and the nanocrystalline magnetic powder core from the alloy raw materials according to the above proportions is the same as in example 1.
The iron-based nanocrystalline magnetically soft alloy powder prepared in this example had an average grain size of α -Fe (D), and a saturation induction density (B s ) Coercivity (H) c ) And the density (ρ) of the nanocrystalline magnetic powder core are shown in table 1.
Example 3
In the embodiment, the alloy component is Fe 80 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1.5 The method for preparing the iron-based amorphous soft magnetic alloy powder, the nanocrystalline soft magnetic alloy powder and the nanocrystalline magnetic powder core from the alloy raw materials according to the above proportions is the same as in example 1.
The iron-based nanocrystalline magnetically soft alloy powder prepared in this example had an average grain size of α -Fe (D), and a saturation induction density (B s ) Coercivity (H) c ) And the density (ρ) of the nanocrystalline magnetic powder core are shown in table 1.
Example 4
The alloy composition in this embodiment is: fe (Fe) 78.5 Si 0.5 B 8.5 P 7 Cu 0.5 C 2 Ni 1 Co 2 The method for preparing the iron-based amorphous soft magnetic alloy powder, the nanocrystalline soft magnetic alloy powder and the nanocrystalline magnetic powder core from the alloy raw materials according to the above proportions is the same as in example 1.
The iron-based nanocrystalline magnetically soft alloy powder prepared in this example had an average grain size of α -Fe (D), and a saturation induction density (B s ) Coercivity (H) c ) And the density (ρ) of the nanocrystalline magnetic powder core are shown in table 1.
Example 5
The alloy composition in this embodiment is: fe (Fe) 76.5 Si 0.5 B 8.5 P 7 Cu 0.5 C 2 Ni 1 Co 4 The method for preparing the iron-based amorphous soft magnetic alloy powder, the nanocrystalline soft magnetic alloy powder and the nanocrystalline magnetic powder core from the alloy raw materials according to the above proportions is the same as in example 1.
The nanocrystalline soft magnetic alloy powder prepared in this example had an average grain size of α -Fe (D), and a saturation induction density (B s ) Coercivity (H) c ) And the density (ρ) of the nanocrystalline magnetic powder core are shown in table 1.
Comparative example 1
Preparation of alloy component Fe 81.5 Si 0.5 B 4.5 P 11 Cu 0.5 C 2 The amorphous forming capability of the powder prepared by the gas atomization is poor, and an amorphous powder precursor cannot be obtained, so that the average alpha-Fe grain size is overlarge after crystallization heat treatment, and the powder obtained by the gas atomization method contains a large amount of Fe-B phase, so that the H of the iron-based nanocrystalline magnetically soft alloy powder is caused c The results of the alloy performance test of this comparative example are shown in Table 1.
Comparative example 2
Preparation example 1 alloy composition Fe 80.5 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1 The atomization gas pressure of the gas atomization method is 6MPa, and high cooling speed cannot be obtained due to the fact that the atomization pressure is too low, the amorphous degree of the solidified alloy powder is low, and H of the alloy powder after nano crystallization heat treatment is caused c The alloy performance test results of this comparative example are shown in table 1, which are higher and the powder particle size is larger, which is unfavorable for the preparation of the high-frequency low-loss magnetic powder core.
Comparative example 3
Preparation example 1 alloy composition Fe 80.5 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1 Is prepared by adjusting the gas atomization methodThe nozzle angle of (2) is 60 DEG, and the effective cooling speed is not high due to the excessive angle, so that the alloy powder with excellent amorphous degree cannot be obtained, and H of the iron-based nanocrystalline magnetically soft alloy powder is caused c The alloy performance test results of this comparative example are shown in table 1, which are high, and at the same time, it is difficult to obtain smaller particle size, which is disadvantageous for the preparation of the high frequency low loss magnetic powder core.
Comparative example 4
Preparation example 1 alloy composition Fe 80.5 Si 0.5 B 10.5 P 5 Cu 0.5 C 2 Ni 1 After 2wt.% of epoxy resin is doped into the powder prepared by gas atomization, the magnetic powder core is pressed under the pressure of 1.1GPa by adopting a cold pressing method, compared with the powder prepared by the method in example 1, the density is reduced, the loss is increased, the magnetic permeability is reduced, the soft magnetic performance is obviously reduced, and the performance test result of the alloy of the comparative example is shown in table 1.
TABLE 1 alpha-Fe average grain size (D), saturation induction intensity (B) of iron-based nanocrystalline magnetically soft alloy powders prepared in examples 1 to 5 s ) Coercivity (H) c ) Density of nanocrystalline magnetic powder core

Claims (10)

1. An iron-based amorphous soft magnetic alloy powder is characterized by comprising a molecular formula of Fe a Si b B c P d Cu e C f Ni g M m The method comprises the steps of smelting alloy raw materials with a+b+c+d+e+f+g+m=100 to obtain a master alloy, and processing the master alloy by an aerosol method to obtain the alloy, wherein M is at least one of transition metal elements Sc, ti, V, cr, mn, co, zr, nb, and the atomic percentage of each element is as follows: a is more than or equal to 74 and less than or equal to 81,0.5, b is more than or equal to 7,8.5, c is more than or equal to 10.5,5, d is more than or equal to 7, e is more than or equal to 0.5 and less than or equal to 0.8, f is more than or equal to 0 and less than or equal to 2, g is more than or equal to 1 and less than or equal to 1.5, and m is more than or equal to 0 and less than or equal to 4.
2. The iron-based amorphous soft magnetic alloy powder according to claim 1, wherein the percentage of elements in the alloy raw material satisfies 77.ltoreq.a+g.ltoreq.81.5, 11.5.ltoreq.c+d.ltoreq.15.5.
3. The iron-based amorphous soft magnetic alloy powder according to claim 1, wherein the median diameter of the iron-based amorphous soft magnetic alloy powder is 17 to 18 μm.
4. The iron-based amorphous soft magnetic alloy powder according to claim 1, wherein the atomization gas pressure of the gas atomization method is 8-10 MPa, the nozzle angle is 30-45 degrees, and the aperture of the quartz tube is 0.8-1.0 mm.
5. A nanocrystalline magnetic powder core, which is prepared by mixing the iron-based amorphous soft magnetic alloy powder according to any one of claims 1-4 with an epoxy resin binder and pressing the mixture by a cold pressing method; and then carrying out heat treatment on the amorphous magnetic powder core in a vacuum state.
6. A nanocrystalline magnetic powder core according to claim 5, wherein the heat treatment temperature is 400-500 ℃ for 45-90 min.
7. Use of a nanocrystalline magnetic powder core according to claim 5 or 6 in the field of integrally formed inductors.
8. An iron-based nanocrystalline magnetically soft alloy powder prepared by heat-treating the iron-based amorphous magnetically soft alloy powder according to any one of claims 1 to 4 in a vacuum state.
9. The iron-based nanocrystalline magnetically soft alloy powder according to claim 8, wherein the heat treatment temperature is 400 to 500 ℃ for 45 to 90min.
10. The iron-based nanocrystalline magnetically soft alloy powder according to claim 8 or 9, wherein the saturation induction of the iron-based nanocrystalline magnetically soft alloy powder is 170-185 emu/g, and the α -Fe average grain size of the iron-based nanocrystalline magnetically soft alloy powder is 25-27 nm.
CN202311096671.8A 2023-08-29 2023-08-29 Iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof Pending CN117153515A (en)

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