CN116092807A - Amorphous magnetic powder core and preparation method thereof - Google Patents

Amorphous magnetic powder core and preparation method thereof Download PDF

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Publication number
CN116092807A
CN116092807A CN202211515264.1A CN202211515264A CN116092807A CN 116092807 A CN116092807 A CN 116092807A CN 202211515264 A CN202211515264 A CN 202211515264A CN 116092807 A CN116092807 A CN 116092807A
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powder
treatment
amorphous
core
mass
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王雷杰
於扬栋
陈建宇
卢杨斌
楼凯
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • 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
    • 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
    • H01F1/15341—Preparation processes therefor
    • 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
    • H01F1/34—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 non-metallic substances, e.g. ferrites
    • H01F1/342—Oxides
    • H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
    • 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

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides an amorphous magnetic powder core and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Carrying out embrittlement heat treatment on Fe-based amorphous alloy, crushing, carrying out pre-annealing treatment to obtain amorphous powder, and sieving two parts of amorphous powder with different screens to obtain first powder and second powder; (2) Mixing the first powder and the second powder, and performing magnetron sputtering treatment on the mixed powder by using MgO to obtain precursor powder; (3) The method comprises the steps of carrying out surface modification treatment on nano ferrite powder, mixing and grinding precursor powder and the surface modified nano ferrite powder, adding a binder for granulating, carrying out annealing treatment after pressing treatment, and obtaining the amorphous magnetic powder core.

Description

Amorphous magnetic powder core and preparation method thereof
Technical Field
The invention belongs to the field of magnetic materials, and relates to an amorphous magnetic powder core and a preparation method thereof.
Background
With the development of electronic power technology, the development of electronic devices toward miniaturization, high frequency and large current is a necessary trend. Conventional magnetic powder cores such as iron powder cores, iron silicon aluminum powder cores, iron nickel powder cores and iron nickel molybdenum powder cores have various problems facing new performance requirements. The concrete expression is as follows: the price of the iron silicon powder core is moderate, the direct current superposition performance is excellent, but the high-frequency loss is high; the iron-silicon-aluminum powder core has wide application range, low loss, good frequency performance and excellent cost performance, but the direct current superposition characteristic is not ideal. The iron-nickel powder core has the best direct current bias characteristic, but has higher price and high loss; iron nickel molybdenum has the most excellent performance, but is also the most expensive. The iron-based amorphous magnetic powder core has the characteristics of constant magnetic conductivity, high resistivity, low loss, good temperature stability and the like at high frequency, meets the national energy conservation and emission reduction requirements, is low in cost, is an important development direction of magnetic powder core materials, and gradually becomes a research and application hot spot in recent years.
The most critical process for preparing the soft magnetic composite material is the surface insulation treatment process of the magnetic powder particles, and the process is mainly divided into the following three types: chemical surface treatment process, organic matter coating treatment process and inorganic matter coating treatment. The chemical surface treatment process mainly adopts inorganic acid or inorganic acid salt at present, but the passivation layer prepared by the method is not high-temperature resistant, and the used acid reagent causes a considerable pollution to the environment. The organic matter coating treatment process can only be processed at a lower temperature due to the poor high temperature resistance of the organic matter. The current common and applicable magnetic powder coating method is inorganic coating treatment.
CN104368807a discloses a coating method of powder for metal soft magnetic composite material and a preparation method of a magnet. In the patent, a sol-gel method and a high-temperature heat treatment method are adopted to coat a layer of nano Al 2 O 3 And coating the silane coupling agent and the silicone resin, and drying the coated organic matters to obtain coated powder. The soft magnetic composite material prepared in the patent has high magnetic permeability and lower loss. However, the whole preparation process is complex, has more influencing factors and is unfavorable for controlling the productUniformity, long time consumption and low production efficiency. At the same time, the method involves multi-step chemical reactions and metal solutions, which are easy to pollute the environment.
CN104575913a discloses a method for preparing low-loss amorphous magnetic powder, in which soft magnetic powder is reacted and passivated in a mixed aqueous solution of phosphoric acid, nitric acid and chromic acid, and insulating agents such as mica powder, kaolin, zirconia powder and alumina powder are added for treatment after powder passivation. The magnetic powder core prepared by the patent has low loss and better direct current superposition performance. However, the powder prepared by the patent has more non-magnetic substances on the surface, so that the magnetic permeability of the magnetic powder core is attenuated.
CN102136331a discloses a high-efficiency soft magnetic composite material and a preparation method thereof, in which soft magnetic metal and soft magnetic ferrite powder are mixed uniformly according to a proportion, so that the soft magnetic ferrite powder is coated on the surface of the soft magnetic metal, and then the soft magnetic ferrite powder is sintered and densified by spark plasma sintering to be formed by composite sintering, and finally is subjected to stress-relief annealing heat treatment. The soft magnetic composite material prepared by the patent has the characteristics of high saturation magnetic induction intensity and high resistivity, and has high magnetic permeability, low coercive force, low loss and excellent comprehensive mechanical properties. However, in the patent, the soft magnetic metal particles are directly contacted with the soft magnetic ferrite, so that the metal ions in the outer ferrite insulating layer and the core particles are mutually diffused, the core Fe element is diffused and activated, the loss at high frequency is attenuated, and meanwhile, the production environment required by the discharge plasma sintering equipment used in the patent is high in requirement, and the large-scale production is not facilitated.
Disclosure of Invention
The invention aims to provide an amorphous magnetic powder core and a preparation method thereof. The magnetron sputtering method adopted in the preparation process can effectively control the thickness of the plating layer, has high deposition rate and compact and uniform film formation, and the magnetron sputtering method and the mechanical ball milling method adopted in the whole process are suitable for mass production and are environment-friendly.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an amorphous magnetic powder core, the method comprising the steps of:
(1) Carrying out embrittlement heat treatment on Fe-based amorphous alloy, crushing, carrying out pre-annealing treatment to obtain amorphous powder, and sieving two parts of amorphous powder with different screens to obtain first powder and second powder;
(2) Mixing the first powder and the second powder, and performing magnetron sputtering treatment on the mixed powder by using MgO to obtain precursor powder;
(3) And carrying out surface modification treatment on the nano ferrite powder, mixing and grinding the precursor powder and the surface modified nano ferrite powder, adding a binder for granulating, and carrying out annealing treatment after pressing treatment to obtain the amorphous magnetic powder core.
In the invention, firstly, mgO film is plated on the surface of amorphous powder by magnetron sputtering, and then nano ferrite is coated on the surface of the powder of the core-shell structure of amorphous powder/MgO by a mechanical ball milling method. The ferrite of the outermost layer can provide certain magnetic conductivity compensation while inhibiting eddy current loss due to high resistivity and certain magnetism. The MgO coating layer is used as an intermediate layer to play a role in blocking element diffusion between amorphous powder particles and ferrite particles, improves the soft magnetic performance, improves the resistivity, and further reduces the power loss of the powder.
Preferably, the Fe-based amorphous alloy of step (1) comprises an Fe-Si-B-C amorphous alloy.
Preferably, the crushing is followed by a sieving treatment.
Preferably, the screen mesh number of the screening treatment is 80 to 100 mesh, for example: 80 mesh, 85 mesh, 90 mesh, 95 mesh or 100 mesh, etc.
Preferably, the temperature of the pre-annealing treatment in step (1) is 380 to 430 ℃, for example: 380 ℃, 390 ℃, 400 ℃, 410 ℃, 430 ℃ or the like.
Preferably, the pre-annealing treatment is performed for 1 to 3 hours, for example: 1h, 1.5h, 2h, 2.5h or 3h, etc.
Preferably, the first powder has a mesh number of 100 to 200 mesh, for example: 100 mesh, 120 mesh, 150 mesh, 180 mesh or 200 mesh, etc.
Preferably, the second powder has a mesh number of 200 to 300 mesh, for example: 200 mesh, 220 mesh, 250 mesh, 280 mesh or 300 mesh, etc.
Preferably, the mass ratio of the first powder to the second powder in the step (2) is (30-50): (50-70), for example: 30:70, 35:65, 40:60, 45:55, or 50:70, etc.
Preferably, the magnetron sputtering treatment in the step (2) has a vacuum degree of 1×10 -3 ～5×10 -3 Pa, for example: 1X 10 - 3 Pa、2×10 -3 Pa、3×10 -3 Pa、4×10 -3 Pa or 5X 10 -3 Pa, and the like.
Preferably, the vibration power of the magnetron sputtering process is 20 to 40W, for example: 20W, 25W, 30W, 35W, 40W, or the like.
Preferably, the sputtering power of the magnetron sputtering process is 150 to 250W, for example: 150W, 180W, 200W, 220W, 250W, etc.
Preferably, the sputtering time of the magnetron sputtering process is 2 to 4 hours, for example: 2h, 2.5h, 3h, 3.5h or 4h, etc.
Preferably, the surface modification treatment of the nano ferrite powder in the step (3) comprises placing the nano ferrite powder in an aqueous solution of polyethylene glycol, stirring for 0.5-1 h (for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h or 1h, etc.), and then performing vacuum drying treatment to obtain the surface modified nano ferrite powder.
Preferably, the nano ferrite powder comprises nickel zinc ferrite powder and/or manganese zinc ferrite powder.
Preferably, the nano ferrite powder has a median particle diameter D50 of 100 to 200nm, for example: 100nm, 120nm, 150nm, 180nm or 200nm, etc.
Preferably, the polyethylene glycol comprises PEG-4000 and/or PEG-6000.
Preferably, the mass of the polyethylene glycol is 0.7-1.2% of the mass of the nano ferrite powder, for example: 0.7%, 0.8%, 0.9%, 1%, 1.1% or 1.2%, etc.
Preferably, the mass of the surface-modified nano ferrite powder in the step (3) is 4 to 10% of the mass of the precursor powder, for example: 4%, 5%, 6%, 8% or 10%, etc.
Preferably, the ball-to-material ratio of the mixed grinding is (6-10): 1, for example: 6:1, 7:1, 8:1, 9:1, or 10:1, etc.
Preferably, the rotational speed of the mixing mill is 100 to 300rpm, for example: 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, etc.
Preferably, the time of the mixed grinding is 5 to 8 hours, for example: 5h, 5.5h, 6h, 7h or 8h, etc.
Preferably, the binder of step (3) comprises any one or a combination of at least two of epoxy resin, phenolic resin or polyurethane resin.
Preferably, the mass of the binder is 0.5 to 2.5% of the total mass of the precursor powder and the surface-modified nano ferrite powder, for example: 0.5%, 1%, 1.5%, 2% or 2.5%, etc.
Preferably, the pressure of the pressing treatment in the step (3) is 20-25T/cm 2 For example: 20T/cm 2 、21T/cm 2 、22T/cm 2 、23T/cm 2 、24T/cm 2 Or 25T/cm 2 Etc.
Preferably, the time of the pressing treatment is 1 to 5 seconds, for example: 1s, 2s, 3s, 4s or 5s, etc.
Preferably, the atmosphere of the annealing treatment includes a nitrogen atmosphere.
Preferably, the annealing treatment is performed at a temperature of 350 to 430 ℃, for example: 350 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃ or 430 ℃ and the like.
Preferably, the annealing treatment is performed for 0.5 to 1 hour, for example: 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, etc.
In a second aspect, the present invention provides an amorphous magnetic powder core, the amorphous magnetic powder core being produced by the method according to the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts a magnetron sputtering method and a mechanical ball milling method to prepare the amorphous powder/MgO/ferrite amorphous composite material with a double-layer core-shell structure, and the prepared magnetic powder core has high magnetic conductivity, low power loss and good direct current superposition performance. The magnetron sputtering method adopted in the preparation process can effectively control the thickness of the plating layer, has high deposition rate and compact and uniform film formation, and the magnetron sputtering method and the mechanical ball milling method adopted in the whole process are suitable for mass production and are environment-friendly.
(2) The relative magnetic permeability of the amorphous magnetic powder core prepared by the method can reach more than 90, and the power loss can reach 426.7kW/m 3 In the following, the DC superposition characteristic is kept at about 68-69% under the magnetic field intensity of 100Oe, and the amorphous powder/MgO/ferrite has excellent magnetic permeability, lower power loss and good DC superposition characteristic.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides an amorphous magnetic powder core, and the preparation method of the amorphous magnetic powder core comprises the following steps:
(1) Carrying out crushing and screening after embrittlement heat treatment of Fe-Si-B-C amorphous alloy to obtain powder below 100 meshes, and carrying out N-phase sintering 2 Pre-annealing for 2 hours at 400 ℃ in the atmosphere, and screening the pre-annealed powder to obtain first powder with 100-200 meshes and second powder with 200-300 meshes;
(2) Uniformly mixing the first powder and the second powder according to the mass ratio of 3:7, placing the uniformly mixed powder into a sputtering chamber of a powder magnetron sputtering instrument, simultaneously installing a required MgO target on a magnetron sputtering target frame, closing the sputtering chamber, and vacuumizing the sputtering chamber to ensure that the background vacuum degree of the sputtering chamber is 2 multiplied by 10 -3 Pa. Introducing argon gas to make the internal air pressure reach one atmosphere, regulating the vibration power to 30W, regulating the sputtering power to 200W, sputtering for 3h, and opening the cabin door of the sputtering chamber to obtain amorphous powder/MgO corePrecursor powder of the shell structure;
(3) Uniformly mixing 150nm manganese zinc ferrite powder with PEG-6000 water solution with the mass of 0.8% of ferrite, stirring for 1h, drying to obtain surface modified nano ferrite powder, putting the amorphous powder/MgO core-shell powder and the surface modified nano ferrite powder with the mass of 8% of the amorphous powder/MgO core-shell powder into a ball pot for ball milling at the speed of 200r/min for 6h, wherein zirconia balls are adopted as ball milling media in the ball milling process, the ball material ratio is 8:1, obtaining the amorphous powder/MgO/ferrite double-layer core-shell soft magnetic amorphous composite material after ball milling, and uniformly mixing the amorphous powder/MgO/ferrite double-layer core-shell soft magnetic amorphous composite material with epoxy resin with the mass of 1% of the powder for ball milling. And placing the granulated powder into a mold at 21T/cm 2 Pressure maintaining for 3s, putting the pressed magnetic rings with the outer diameter of 20mm and the inner diameter of 10mm into N 2 Annealing at 400 ℃ for 1h in the atmosphere.
Example 2
This example differs from example 1 only in that the mass of PEG-6000 in step (3) is 1.2% of the mass of ferrite, and other conditions and parameters are exactly the same as in example 1.
Example 3
The present example differs from example 1 only in that the sputtering power of the powder magnetron sputtering apparatus was 250W, the sputtering time was 4h, and other conditions and parameters were identical to those of example 1.
Example 4
The present example differs from example 1 only in that the first powder and the second powder are uniformly mixed in a mass ratio of 4:6, and other conditions and parameters are exactly the same as those of example 1.
Example 5
This example differs from example 1 only in that the amorphous powder/MgO core-shell powder and the surface-modified nano ferrite powder having a mass of 12wt% of the amorphous powder/MgO core-shell powder in step (3) were put into a spherical tank for ball milling, and the other conditions and parameters were exactly the same as in example 1.
Example 6
The difference between this example and example 1 is that in step (3), the amorphous powder/MgO/ferrite double-layer core-shell structure soft magnetic amorphous composite material and 3% of the powder mass of the epoxy resin are uniformly mixed and granulated, and the other conditions and parameters are identical to those of example 1.
Example 7
This example differs from example 1 only in that the mass of polyethylene glycol in step (3) is 0.3% of the mass of the nano ferrite powder, and other conditions and parameters are exactly the same as in example 1.
Comparative example 1
The comparative example is different from example 1 only in that the amorphous powder is not subjected to magnetron sputtering as MgO target material, and is directly ball-milled with surface modified manganese zinc ferrite to prepare the magnetic powder core of amorphous powder/ferrite core-shell structure, and other conditions and parameters are identical to those of example 1.
Comparative example 2
The comparative example is different from example 1 only in that the amorphous powder/MgO powder was not ball-milled with the surface-modified manganese zinc ferrite, and the magnetic powder core of amorphous powder/MgO core-shell structure was directly prepared, and other conditions and parameters were exactly the same as example 1.
Comparative example 3
This comparative example differs from example 1 only in that only the first powder was used, and other conditions and parameters were exactly the same as example 1.
Performance test:
amorphous magnetic powder cores prepared in examples 1 to 7 and comparative examples 1 to 3 were tested for real part μ' of permeability at 100kHz with a copper wire of 0.4mm diameter uniformly wound thereon for 30+5 turns by using an agilent E4991a analyzer. The test conditions were 100kHz,100mT,25℃for power loss, and a copper wire of 0.4mm diameter was uniformly wound thereon for 30 turns. The test conditions are 100kHz,1V and 25 ℃, the direct current superposition performance of the magnetic ring under the magnetic field intensity of 100Oe is calculated, and the test results are shown in Table 1:
TABLE 1
Relative permeability μ' Power loss (kW/m) 3 ) DC superposition characteristics (100 Oe)
Example 1 93.6 421.8 68.3％
Example 2 92.1 426.7 68.7％
Example 3 90.3 412.9 69.1％
Example 4 97.8 458.4 62.9％
Example 5 88.2 404.3 65.7％
Example 6 89.5 436.4 67.4％
Example 7 81.6 506.4 66.8％
Comparative example 1 88.1 490.8 62.7％
Comparative example 2 80.6 541.2 70.1％
Comparative example 3 81.2 609.7 66.2％
As can be seen from Table 1, according to examples 1 to 3, the relative permeability of the amorphous magnetic powder core prepared by the method of the invention can reach more than 90, and the power loss can reach 426.7kW/m 3 In the following, the DC superposition characteristic is kept at about 68-69% under the magnetic field intensity of 100Oe, and the amorphous powder/MgO/ferrite has excellent magnetic permeability, lower power loss and good DC superposition characteristic.
As can be obtained by comparing the embodiment 1 with the embodiment 4, in the preparation process of the amorphous magnetic powder core, the mass ratio of the first powder to the second powder can influence the performance of the amorphous magnetic powder core, the mass ratio of the first powder to the second powder is controlled to be (30-50): (50-70), the performance of the amorphous magnetic powder core is better, and if the magnetic permeability is beyond the range, although the magnetic permeability can be slightly improved, the power loss is obviously improved, so that the direct current superposition characteristic is reduced.
The comparison of the embodiment 1 and the embodiment 5 shows that the quality ratio of the surface modified nano ferrite powder to the precursor powder can influence the performance of the amorphous magnetic powder core, the quality of the surface modified nano ferrite powder is controlled to be 4-10% of the quality of the precursor powder, the performance of the amorphous magnetic powder core is good, and if the addition amount of the surface modified nano ferrite powder is too high, the magnetic conductivity of the material is obviously reduced.
As can be seen from the comparison of the embodiment 1 and the embodiment 6, the effect of the addition amount of the binder on the preparation of the amorphous magnetic powder core is very obvious, the total mass of the precursor powder and the surface-modified nano ferrite powder needs to be controlled to be 0.5-2.5%, and if the addition amount is too high, the binder can be decomposed during high-temperature annealing, so that the cavities in the magnetic ring are increased, and the magnetic performance is deteriorated.
As compared with example 1 and example 7, less PEG-6000 is used to modify the nano ferrite surface, so the nano ferrite has high surface activation energy, and agglomeration easily occurs in the ball milling process, so that a ferrite layer is not formed effectively on the surface of amorphous powder/MgO particles, and the magnetic permeability and the power loss are deteriorated.
As can be seen from the comparison of example 1 and comparative example 1, the lack of MgO in the intermediate coating between the amorphous powder and the ferrite does not effectively block the mutual expansion of metal ions in the outer ferrite and the core particle, resulting in a decrease in resistivity and deterioration in both permeability and power loss.
Comparison of example 1 and comparative example 2, without the ferrite of the outermost layer, resulted in a lack of effective permeability compensation for the powder, and thus a decrease in permeability. Meanwhile, mgO of the middle coating is relatively thin, and the resistivity cannot be effectively increased, so that the power loss is also attenuated.
As can be seen from the comparison of example 1 and comparative example 3, the present invention, which uses two kinds of powder having particle diameters, prepares an amorphous magnetic powder core, and can increase the overall packing density by filling the second powder having a smaller particle diameter into the gaps of the first powder having a larger particle diameter. Comparative example 3 the magnetic core has a reduced permeability due to the smaller packing density caused by the first powder alone, and the core has a larger eddy current loss due to the larger particle size and is more easily magnetized to saturation in the magnetic field.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.

Claims (10)

1. A method for preparing an amorphous magnetic powder core, comprising the steps of:
(1) Carrying out embrittlement heat treatment on Fe-based amorphous alloy, crushing, carrying out pre-annealing treatment to obtain amorphous powder, and sieving two parts of amorphous powder with different screens to obtain first powder and second powder;
(2) Mixing the first powder and the second powder, and performing magnetron sputtering treatment on the mixed powder by using MgO to obtain precursor powder;
(3) And carrying out surface modification treatment on the nano ferrite powder, mixing and grinding the precursor powder and the surface modified nano ferrite powder, adding a binder for granulating, and carrying out annealing treatment after pressing treatment to obtain the amorphous magnetic powder core.
The screening mesh number of the first powder in the step (1) is 100-200 meshes, and the screening mesh number of the second powder is 200-300 meshes.
2. The method of manufacturing according to claim 1, wherein the Fe-based amorphous alloy of step (1) comprises an Fe-Si-B-C amorphous alloy;
preferably, the crushing is followed by sieving;
preferably, the number of the screen meshes of the screening treatment is 80-100 meshes.
3. The method of claim 1 or 2, wherein the pre-annealing treatment in step (1) is performed at a temperature of 380 to 430 ℃;
preferably, the pre-annealing treatment time is 1-3 hours;
preferably, the first powder has a mesh number of 100 to 200 mesh;
preferably, the second powder has a mesh number of 200 to 300 mesh.
4. The method according to any one of claims 1 to 3, wherein the mass ratio of the first powder to the second powder in the step (2) is (30 to 50): 50 to 70.
5. The method according to any one of claims 1 to 4, wherein the magnetron sputtering treatment in step (2) has a vacuum degree of 1X 10 -3 ～5×10 -3 Pa；
Preferably, the vibration power of the magnetron sputtering treatment is 20-40W;
preferably, the sputtering power of the magnetron sputtering treatment is 150-250W;
preferably, the sputtering time of the magnetron sputtering treatment is 2-4 h.
6. The method according to any one of claims 1 to 5, wherein the surface modification treatment of the nano ferrite powder in the step (3) comprises placing the nano ferrite powder in an aqueous solution of polyethylene glycol, stirring for 0.5 to 1 hour, and then vacuum drying to obtain the surface modified nano ferrite powder;
preferably, the nano ferrite powder comprises nickel zinc ferrite powder and/or manganese zinc ferrite powder;
preferably, the median particle diameter D50 of the nano ferrite powder is 100-200 nm;
preferably, the polyethylene glycol comprises PEG-4000 and/or PEG-6000;
preferably, the mass of the polyethylene glycol is 0.7-1.2% of the mass of the nano ferrite powder.
7. The method of any one of claims 1-6, wherein the mass of the surface-modified nano ferrite powder of step (3) is 4-10% of the mass of the precursor powder;
preferably, the ball-to-material ratio of the mixed grinding is (6-10): 1;
preferably, the rotation speed of the mixed grinding is 100-300 rpm;
preferably, the time of the mixed grinding is 5-8 hours.
8. The method of any one of claims 1-7, wherein the binder of step (3) comprises any one or a combination of at least two of an epoxy resin, a phenolic resin, or a polyurethane resin;
preferably, the mass of the binder is 0.5 to 2.5% of the total mass of the precursor powder and the surface-modified nano ferrite powder.
9. The process according to any one of claims 1 to 8, wherein the pressure of the pressing treatment in step (3) is 20 to 25T/cm 2 ；
Preferably, the time of the pressing treatment is 1 to 5 seconds;
preferably, the atmosphere of the annealing treatment includes a nitrogen atmosphere;
preferably, the temperature of the annealing treatment is 350-430 ℃;
preferably, the annealing treatment is performed for 0.5 to 1 hour.
10. An amorphous magnetic powder core, characterized in that the amorphous magnetic powder core is produced by the method according to any one of claims 1-9.
CN202211515264.1A 2022-11-29 2022-11-29 Amorphous magnetic powder core and preparation method thereof Pending CN116092807A (en)

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