CN113066627B - Composite magnetic powder core and preparation method thereof - Google Patents
Composite magnetic powder core and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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- 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
- H01F1/20—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 in the form of particles, e.g. powder
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- 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
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- 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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- 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
Abstract
The invention provides a composite magnetic powder core, which comprises superparamagnetic nano particles and metal soft magnetic powder, wherein the superparamagnetic nano particles account for 0.5-5% of the total weight of the superparamagnetic nano particles and the metal soft magnetic powder. The composite magnetic powder core of the invention fills gaps among the micrometer magnetic powder particles by using the superparamagnetic nano particles, thereby obviously weakening the magnetic dilution effect, improving the saturation magnetic induction and the magnetic permeability, and the superparamagnetic nano particles have extremely low coercivity, so that the problem of hysteresis loss rise caused by adding the conventional nano magnetic particles can be overcome. The composite magnetic powder core has lower power loss in the high-frequency field, thereby promoting the high-frequency, miniaturization and low power consumption of the metal magnetic powder core.
Description
Technical Field
The invention relates to the field of materials, in particular to a composite magnetic powder core and a preparation method thereof.
Background
The soft magnetic composite material (Soft magnetic composite, SMC) or metal magnetic powder core is a multiphase heterostructure block material composed of soft magnetic alloy particles and insulating cladding media, has the advantages of soft magnetic alloy and ferrite, is widely used in the fields of electronic power, new energy, communication, automobiles, intelligent manufacturing, household appliances, military industry and the like, and is a key base material for national economy and national defense construction. In recent years, with the rapid development of high-end application fields such as new energy automobiles, high-power charging piles, 5G communication and solar power generation, higher requirements are put on the comprehensive electromagnetic performance of magnetic components such as metal magnetic powder cores.
The preparation of the metal magnetic powder core is based on the powder metallurgy technology and mainly comprises the steps of soft magnetic alloy powder preparation, insulating coating, compression molding and subsequent heat treatment. The magnetic powder core is mainly used as a motor stator/rotor and an inductor, and the power loss directly determines the electric energy conversion efficiency of a motor and a circuit and can be divided into hysteresis loss, eddy current loss and residual loss. Where eddy current loss is proportional to the square of the magnetic field frequency. Therefore, the high frequency requires that a large amount of high-resistivity insulating coating medium is introduced into the magnetic powder core to form a uniform and continuous coating structure, and eddy current is limited in the magnetic powder particles, so that the high-frequency eddy current loss is remarkably reduced. However, due to the introduction of a large amount of non-magnetic insulating coating medium and the lack of a subsequent high-temperature sintering densification process, the density of the magnetic powder core is reduced, a large amount of distributed air gaps exist, and the magnetic indexes such as saturation magnetic induction, magnetic permeability and the like are far lower than those of alloy magnetic powder (magnetic dilution effect). In addition, the non-magnetic medium has strong pinning effect on the magnetic domain movement of the magnetic alloy Jin Cifen, the quasi-static coercivity of the magnetic powder core is obviously improved, and the hysteresis loss of the magnetic powder core is far higher than the eddy current loss in a certain frequency range. According to the research results of Jang et al (Jang P, lee B, choi G.effects of annealing on the magnetic properties of Fe-6.5%Si alloy powder cores[J ]. Journal of Applied Physics,2008, 103:07E743), the hysteresis loss of the Fe-6.5wt% Si magnetic powder core is 2-3 times of the eddy current loss at 100mT/50 kHz. Based on the above, the same company at home and abroad proposes to use magnetic ferrite, magnetic nano particles and the compound of the magnetic nano particles and an organic insulating medium as insulating coating media, and develop corresponding coating technical means.
According to the theory of the composite material, a certain amount of nano-scale soft magnetic particles are added into the micro-scale soft magnetic powder particles in a compounding way to prepare the micro/nano composite magnetic powder core, so that the volume fraction of a non-magnetic phase and a distributed air gap can be reduced, and the magnetic conductivity and the saturation induction intensity can be obviously improved. Compared with the micron particles, the nanometer magnetic particles have better filling property, can be filled into gaps of the micron particles, and have obvious effect of improving the magnetic performance of the magnetic powder core. However, since the nanoscale magnetic particles have a higher coercivity, hysteresis losses of conventional micro/nano composite magnetic powder cores are greatly increased, resulting in a higher level of overall power consumption of the magnetic powder cores.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a composite magnetic powder core and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the composite magnetic powder core comprises superparamagnetic nano particles and metal soft magnetic powder, wherein the superparamagnetic nano particles account for 0.5% -5% of the total weight of the superparamagnetic nano particles and the metal soft magnetic powder.
The composite magnetic powder core is prepared by mixing superparamagnetic nano particles and micron-sized metal soft magnetic powder. The composite magnetic powder core fills gaps among the micrometer magnetic powder particles by using the superparamagnetic nanoparticles, so that the magnetic dilution effect is obviously weakened, the saturation magnetic induction and the magnetic permeability are improved, the superparamagnetic nanoparticles have extremely low coercivity, and the problem of hysteresis loss rise caused by adding the conventional nanometer magnetic particles can be solved. The composite magnetic powder core has lower power loss in the high-frequency field, thereby promoting the high-frequency, miniaturization and low power consumption of the metal magnetic powder core.
Preferably, the superparamagnetic nanoparticle is Fe 3 O 4 、Ni 0.5 Zn 0.5 Fe 2 O 4 、Zn 0.25 Fe 2.75 O 4 Or MnFe 2 O 4 The metal soft magnetic powder is at least one of pure Fe, fe-Si, fe-Ni, fe-Si-Al, fe-Ni-Mo, fe-Si-Al-Ni, fe-Si-B and Fe-Si-B-Cu-Nb amorphous nanocrystalline magnetic powder.
The inventor finds that the composite magnetic powder core prepared by matching the superparamagnetic nano particles and the metal soft magnetic powder is more beneficial to improving magnetic permeability and reducing hysteresis loss.
Preferably, the particle size distribution of the metal soft magnetic powder satisfies 15 μm.ltoreq.D50.ltoreq.75μm.
Preferably, the superparamagnetic nanoparticles have a particle size of less than 25nm.
The inventor finds that in the composite magnetic powder core, the critical dimension of the superparamagnetic nano-particles is between a few nanometers and tens of nanometers and is smaller than 25 nanometers, and the superparamagnetic nano-particles are matched with the metal soft magnetic powder with the particle size distribution, so that the magnetic permeability can be further improved, and the hysteresis loss can be reduced.
Preferably, the composite magnetic powder core is prepared by the following method: mixing the superparamagnetic nano particles and the metal soft magnetic powder after surface modification, dispersing the mixture in a resin solution for powder insulation coating, and drying to obtain insulated coated mixed magnetic powder; pressing the mixed magnetic powder to obtain blank, and annealing at 380-580 deg.C.
The superparamagnetic nano particles in the composite magnetic powder core are subjected to surface modification, so that the magnetic loss is reduced.
The invention also provides a preparation method of any one of the composite magnetic powder cores, which comprises the following steps:
(1) Carrying out surface modification on the superparamagnetic nano particles, wherein the surface modifier for surface modification is a silane surface modifier;
(2) Mixing the superparamagnetic nano particles and the metal soft magnetic powder after surface modification, dispersing the mixture in a resin solution for powder insulation coating, and drying to obtain insulated coated mixed magnetic powder;
(3) Pressing the mixed magnetic powder to obtain blank, and annealing at 380-580 deg.C.
The surface modification treatment of the superparamagnetic nanoparticles prevents the superparamagnetic nanoparticles from agglomerating and losing the superparamagnetic effect, and can enhance the binding force of the superparamagnetic nanoparticles and organic insulating coating media such as silicone resin.
Preferably, in the step (1), the silane-based surface modifier is APTS (3-aminopropyl triethoxysilane), KH550 (γ -aminopropyl triethoxysilane), or KH560 (γ - (2, 3-glycidoxy) propyl trimethoxysilane); and carrying out surface modification on the superparamagnetic nanoparticles by using an ethanol solution of the silane surface modifier, wherein the mass concentration of the ethanol solution of the silane surface modifier is 0.8-1.2%.
Preferably, in the step (2), the weight ratio of the total weight of the superparamagnetic nanoparticles and the metal soft magnetic powder after surface modification to the resin solution is (1-5): 100; the resin solution is a silicone acetone solution.
Preferably, in the step (3), the annealing time is 2 to 4 hours.
Preferably, in the step (3), the density after the pressing is 6.4-6.7 g/cm 2 。
The invention has the beneficial effects that: the invention provides a composite magnetic powder core and a preparation method thereof. The composite magnetic powder core of the invention fills gaps among the micrometer magnetic powder particles by using the superparamagnetic nano particles, thereby obviously weakening the magnetic dilution effect, improving the saturation magnetic induction and the magnetic permeability, and the superparamagnetic nano particles have extremely low coercivity, so that the problem of hysteresis loss rise caused by adding the conventional nano magnetic particles can be overcome. The composite magnetic powder core has lower power loss in the high-frequency field, thereby promoting the high-frequency, miniaturization and low power consumption of the metal magnetic powder core.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
As a composite magnetic powder core of the embodiment of the invention, the composite magnetic powder core comprises superparamagnetic nanoparticles and soft magnetic alloy magnetic powder, wherein the superparamagnetic nanoparticles account for 2% of the total weight of the superparamagnetic nanoparticles and the soft magnetic alloy magnetic powder;
the superparamagnetic nanoparticle is Fe 3 O 4 The average particle size of the superparamagnetic nano particles is 10nm;
the metal soft magnetic powder is Fe93.5Si6.5 (wt%) magnetic powder, and the particle size distribution of the soft magnetic alloy magnetic powder meets d50=30.2 μm.
The preparation method of the composite magnetic powder core of the embodiment comprises the following steps:
(1) Adding the superparamagnetic nano particles into a surface modifier solution, stirring and performing ultrasonic dispersion, then washing with absolute ethyl alcohol, and drying to obtain surface modified superparamagnetic nano particles; the surface modifier solution is ethanol solution of KH560, and the mass concentration of the surface modifier solution is 1%; the weight ratio of the superparamagnetic nanoparticles to the surface modifier solution is 1:100;
(2) Uniformly mixing the surface modified superparamagnetic nano particles with soft magnetic alloy magnetic powder according to the mass ratio to obtain mixed powder; adding the mixed powder into a silicone acetone solution, uniformly mixing the mixed powder and the silicone acetone solution according to the mass ratio of 3:100, and drying to obtain mixed magnetic powder;
(3) Pressing the mixed magnetic powder into a magnetic powder with the density of 6.4-6.7 g/cm 3 The green compacts were annealed at 500℃for 3 hours and cooled to room temperature with a furnace.
Example 2
As a composite magnetic powder core according to an embodiment of the present invention, the only difference between this embodiment and embodiment 1 is:
the superparamagnetic nanoparticle is Zn 0.25 Fe 2.75 O 4 The average particle diameter of the superparamagnetic nano particles is 6nm;
the metal soft magnetic powder is Fe17Ni80.5Mo2.5 (wt%) magnetic powder, and the particle size distribution of the soft magnetic alloy magnetic powder meets D50=48.6 μm.
Example 3
As a composite magnetic powder core according to an embodiment of the present invention, the only difference between this embodiment and embodiment 1 is:
the superparamagnetic nano particle is Ni 0.5 Zn 0.5 Fe 2 O 4 The average particle size of the superparamagnetic nano particles is 10nm;
the metal soft magnetic powder is Fe85Si9.6Al5.4 (wt%) magnetic powder, and the particle size distribution of the soft magnetic alloy magnetic powder meets D50=35.6 μm.
Example 4
As a composite magnetic powder core according to an embodiment of the present invention, the only difference between this embodiment and embodiment 1 is:
the superparamagnetic nanoparticle is Zn 0.25 Fe 2.75 O 4 The average particle diameter of the superparamagnetic nano particles is 6nm;
the metal soft magnetic powder is Fe50Ni50 (wt%) magnetic powder, and the particle size distribution of the soft magnetic alloy magnetic powder meets d50=40.5 μm.
Example 5
As a composite magnetic powder core according to an embodiment of the present invention, the only difference between this embodiment and embodiment 1 is:
the superparamagnetic nanoparticle is Zn 0.25 Fe 2.75 O 4 The average particle diameter of the superparamagnetic nano particles is 6nm;
the soft magnetic alloy magnetic powder is Fe90.5Si6B3.5 (wt%) magnetic powder, and the particle size distribution of the metal soft magnetic powder meets D50=10.5 μm.
Comparative example 1
As a composite magnetic powder core of comparative example 1 of the present invention, the only difference between this comparative example and example 1 is: the preparation method does not carry out surface modification on the superparamagnetic nano particles.
Comparative example 2
As a composite magnetic powder core of comparative example 2 of the present invention, the only difference between this comparative example and example 1 is: superparamagnetic nanoparticle Fe of the examples were replaced with nano iron powder particles having an average particle size of 50nm 3 O 4 。
Effect experiment
The composite magnetic powder cores of examples 1-5 and comparative examples 1-2 were tested for permeability and loss under test conditions of 50khz @100mt. The results are shown in Table 1.
As can be seen from table 1, the composite magnetic powder core fills the gaps between the particles of the micron magnetic powder by using the superparamagnetic nanoparticles, so that the magnetic dilution effect is obviously weakened, the saturation magnetic induction and the magnetic permeability are improved, and the loss is reduced.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. The composite magnetic powder core is characterized by comprising superparamagnetic nanoparticles and metal soft magnetic powder, wherein the superparamagnetic nanoparticles account for 0.5% -5% of the total weight of the superparamagnetic nanoparticles and the metal soft magnetic powder;
the superparamagnetic nano particles are subjected to surface modification treatment, and the surface modifying agent is a silane surface modifying agent;
the superparamagnetic nano particle is Ni 0.5 Zn 0.5 Fe 2 O 4 、Zn 0.25 Fe 2.75 O 4 Or MnFe 2 O 4 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the superparamagnetic nano particles is 6nm-10nm;
the metal soft magnetic powder is at least one of Fe-Ni, fe-Si-Al, fe-Ni-Mo, fe-Si-Al-Ni, fe-Si-B and Fe-Si-B-Cu-Nb amorphous nanocrystalline magnetic powder; the particle size distribution of the metal soft magnetic powder meets the requirement that D50 is less than or equal to 15 mu m and less than or equal to 75 mu m;
the composite magnetic powder core is prepared by the following method:
mixing the superparamagnetic nano particles and the metal soft magnetic powder after surface modification, dispersing the mixture in a resin solution for powder insulation coating, and drying to obtain insulated coated mixed magnetic powder; pressing the mixed magnetic powder to obtain blank, and annealing at 380-580 deg.C.
2. A method of preparing a composite magnetic powder core according to claim 1, comprising the steps of:
(1) Carrying out surface modification on the superparamagnetic nano particles, wherein the surface modifier for surface modification is a silane surface modifier;
(2) Mixing the superparamagnetic nano particles and the metal soft magnetic powder after surface modification, dispersing the mixture in a resin solution for powder insulation coating, and drying to obtain insulated coated mixed magnetic powder;
(3) Pressing the mixed magnetic powder to obtain blank, and annealing at 380-580 deg.C.
3. A method of preparing a composite magnetic powder core according to claim 2, wherein in step (1), the silane surface modifier is APTS, KH550 or KH560; and carrying out surface modification on the superparamagnetic nanoparticles by using an ethanol solution of the silane surface modifier, wherein the mass concentration of the ethanol solution of the silane surface modifier is 0.8-1.2%.
4. A method for producing a composite magnetic powder core according to claim 2, wherein in the step (2), the weight ratio of the total weight of the surface-modified superparamagnetic nanoparticles and the metal soft magnetic powder to the resin solution is (1 to 5): 100; the resin solution is a silicone acetone solution.
5. A method of producing a composite magnetic powder core according to claim 2, wherein in step (3), the annealing time is 2 to 4 hours.
6. A method for producing a composite magnetic powder core according to claim 2, wherein in the step (3), the density of the pressed compact is 6.4 to 6.7g/cm 2 。
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