CN108538533B - Preparation method of soft magnetic composite material by interface diffusion - Google Patents

Preparation method of soft magnetic composite material by interface diffusion Download PDF

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CN108538533B
CN108538533B CN201810595194.2A CN201810595194A CN108538533B CN 108538533 B CN108538533 B CN 108538533B CN 201810595194 A CN201810595194 A CN 201810595194A CN 108538533 B CN108538533 B CN 108538533B
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soft magnetic
powder
magnet
composite material
low
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CN108538533A (en
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彭晓领
李静
杨艳婷
徐靖才
金红晓
金顶峰
洪波
王新庆
葛洪良
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China University of Metrology
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China Jiliang University
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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
    • H01F41/0253—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
    • H01F41/0266—Moulding; Pressing
    • 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
    • H01F1/14708—Fe-Ni based alloys
    • H01F1/14733—Fe-Ni based alloys in the form of particles
    • H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
    • 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
    • H01F1/14766—Fe-Si based alloys
    • 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
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust

Abstract

The invention relates to an interface diffusion preparation method of a soft magnetic composite material. The soft magnetic composite material takes Fe, Fe-Si, Fe-Ni-Mo and Fe-Si-Al powder as raw materials; will be provided withMixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder; filling the passivation powder into a forming die, and pressing to form a magnetic ring; by using B2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3And coating the surface of the magnetic ring with low-melting-point compounds such as CuO, low-melting-point glass powder and the like, performing vacuum annealing at 400-1000 ℃ for 1-48 h to enable the low-melting-point compounds to diffuse into the magnetic ring through a particle interface, improving the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material. The invention has the advantages that: an insulating medium is not required to be added before the magnetic ring is pressed and formed, so that the uneven distribution of the insulating medium in the pressing process is avoided; the insulating layer obtained by the penetration and diffusion at the internal interface of the magnet through vacuum annealing is very thin, so that the problem that the magnetic permeability of the magnet is greatly reduced due to the insulating layer in the traditional process is solved.

Description

Preparation method of soft magnetic composite material by interface diffusion
Technical Field
The invention relates to an interface diffusion preparation method of a soft magnetic composite material, belonging to the field of preparation of magnetic materials.
Background
Soft magnetic material, meaning that when magnetization occurs at Hc no greater than 1000A/m, such material is called soft magnet. Typical soft magnetic materials can achieve maximum magnetization with a minimum external magnetic field. Soft magnetic materials (soft magnetic materials) are magnetic materials with low coercivity and high magnetic permeability. Soft magnetic materials are easy to magnetize and demagnetize, and are widely used in electrical and electronic equipment.
The soft magnetic material mainly includes metal soft magnetic and ferrite soft magnetic. The metallic soft magnet has the advantage of high saturation magnetization, but low resistivity, and therefore high frequency eddy current loss. The soft magnetic ferrite has low saturation magnetic flux density, low magnetic conductivity, low Curie temperature, low medium-high frequency loss and low cost. The first three disadvantages are its drawbacks, limiting its range of use, and improvements are being attempted now (early 21 st century). The latter two low are its advantages, facilitating the entry into the high frequency market, and are now (in the beginning of the 21 st century) being expanded in an effort.
The soft magnetic composite material is a soft magnetic material formed by mixing and pressing ferromagnetic powder particles and an insulating medium. Compared with the traditional metal soft magnetic alloy and ferrite material, the material has a plurality of unique advantages: the magnetic metal particles are dispersed in a non-conductor object, so that the high-frequency eddy current loss can be reduced, and the application frequency is improved; the powder core can be processed by adopting a hot pressing method, and the magnet with a complex shape can also be manufactured by injection molding by utilizing the existing plastic engineering technology (in the beginning of the 21 st century); the method has the advantages of low density, light weight, high production efficiency, low cost, good product repeatability and consistency and the like. The disadvantage is that the permeability is generally low because the magnetic particles are separated by the non-magnetic body, the magnetic circuit is interrupted.
The key point of the research and production of the soft magnetic composite material is that the metal magnetic powder is coated by an insulating medium in an insulating way, so that the resistivity of a matrix is improved, and the high-frequency loss is reduced. The existing process is to mix an insulating medium and metal magnetic powder and then press the mixture to form the product. However, the coating interface between the insulating medium and the metal magnetic powder is easy to be separated in the pressing process to form uneven coating, so that the eddy current loss is high.
Aiming at the problems of the soft magnetic composite material, the method adopts the technical methods of metal magnetic powder compression molding, insulating medium magnet surface coating and vacuum annealing to enable the insulating medium to generate interface diffusion, and improves the resistivity of the magnet.
Disclosure of Invention
The invention aims to provide an interface diffusion preparation method of a soft magnetic composite material.
The preparation method comprises the following specific steps:
1) raw material preparation
The adopted soft magnetic alloy powder is as follows: fe. Fe-Si, Fe-Ni-Mo, Fe-Si-Al;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
Coating the surface of the magnetic ring with a low-melting-point compound, diffusing the low-melting-point compound into the magnetic ring through a particle interface by adopting a vacuum annealing process, increasing the resistivity of the magnet, and cooling the furnace to room temperature to obtain a soft magnetic composite material;
the low-melting-point compound comprises: b is2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3CuO and low melting glass frit;
the vacuum annealing temperature is 400-1000 ℃, and the annealing time is 1-48 h.
The invention has the advantages that:
1. an insulating medium is not required to be added before the magnetic ring is pressed and formed, so that the uneven distribution of the insulating medium in the pressing process is avoided;
2. the insulating layer obtained by the penetration and diffusion at the internal interface of the magnet through vacuum annealing is very thin, so that the problem that the magnetic permeability of the magnet is greatly reduced due to the insulating layer in the traditional process is solved.
Detailed Description
The present invention will be described in detail with reference to the following examples in order to better understand the objects, features and advantages of the present invention. While the invention is described in conjunction with the specific embodiments, it is not intended that the invention be limited to the specific embodiments described. On the contrary, alternatives, modifications and equivalents may be made to the embodiments as may be included within the scope of the invention as defined by the appended claims. The process parameters not specifically mentioned can be carried out according to conventional techniques.
Example 1:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
Using Sb2O3Coating the surface of the magnetic ring, and performing vacuum annealing at 600 ℃ for 24h to ensure that Sb is2O3And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 2:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe-Si;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
By using Bi2O3Coating the surface of the magnetic ring, and annealing in vacuum at 700 ℃ for 12h to ensure that Bi is contained2O3And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 3:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe-Ni;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
By using Na2CO3Coating the surface of the magnetic ring, and annealing at 800 deg.C for 8h to obtain Na2CO3And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 4:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe-Ni-Mo;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
And coating the surface of the magnetic ring with CuO, and annealing at 1000 ℃ for 1h in vacuum to diffuse the CuO into the magnetic ring through a particle interface, so as to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 5:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe-Si-Al;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
By using Mn2O3Coating the surface of the magnetic ring, and annealing for 6h at 900 ℃ in vacuum to ensure that Mn is contained2O3And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 6:
1) raw material preparation
The adopted soft magnetic alloy powder is amorphous alloy;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
By using B2O3Coating the surface of the magnetic ring, and performing vacuum annealing at 400 ℃ for 48h to ensure that B2O3And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 7:
1) raw material preparation
The adopted soft magnetic alloy powder is nanocrystalline alloy;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
By using V2O5Coating the surface of the magnetic ring, and performing vacuum annealing at 500 ℃ for 36h to ensure that V is2O5And diffusing the particles into the magnetic ring through the particle interface to improve the resistivity of the magnet, and cooling the magnet to room temperature to obtain the soft magnetic composite material.
Example 8:
1) raw material preparation
The adopted soft magnetic alloy powder is Fe;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
And coating the surface of the magnetic ring with low-melting-point glass powder, performing vacuum annealing at 650 ℃ for 16h to ensure that the low-melting-point glass powder is diffused into the magnetic ring through a particle interface, increasing the resistivity of the magnet, and cooling the furnace to room temperature to obtain the soft magnetic composite material.

Claims (1)

1. The preparation method of the soft magnetic composite material by interface diffusion is characterized by comprising the following specific steps:
1) raw material preparation
The adopted soft magnetic alloy powder is as follows: fe. Fe-Si, Fe-Ni-Mo, Fe-Si-Al;
2) passivation of soft magnetic alloy powders
Mixing the passivating agent and the soft magnetic alloy powder, stirring and drying to obtain passivating powder;
3) press forming
Filling the passivation powder into a forming die, and pressing to form a magnetic ring;
4) surface coating and interface diffusion
Coating the surface of the magnetic ring with a low-melting-point compound, diffusing the low-melting-point compound into the magnetic ring through a particle interface by adopting a vacuum annealing process, increasing the resistivity of the magnet, and cooling the furnace to room temperature to obtain a soft magnetic composite material;
the low-melting-point compound comprises: b is2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3CuO and low melting glass frit;
the vacuum annealing temperature is 400-1000 ℃, and the annealing time is 1-48 h.
CN201810595194.2A 2018-06-11 2018-06-11 Preparation method of soft magnetic composite material by interface diffusion Active CN108538533B (en)

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CN1043056C (en) * 1994-05-13 1999-04-21 新日本制铁株式会社 Anneal isolating objects with good reactivity and used for silica steel sheet
JP4265358B2 (en) * 2003-10-03 2009-05-20 パナソニック株式会社 Manufacturing method of composite sintered magnetic material
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CN104036901B (en) * 2014-05-28 2016-08-24 浙江大学 A kind of high magnetic conductivity and low loss soft magnetic metal composite and preparation method thereof
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