CN113517128A - Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material - Google Patents

Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material Download PDF

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Publication number
CN113517128A
CN113517128A CN202110866708.5A CN202110866708A CN113517128A CN 113517128 A CN113517128 A CN 113517128A CN 202110866708 A CN202110866708 A CN 202110866708A CN 113517128 A CN113517128 A CN 113517128A
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China
Prior art keywords
iron
cobalt
resin
coating
powder
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CN202110866708.5A
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Chinese (zh)
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黄昊
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Mingxin Soft Magnetic Technology Jiangsu Co ltd
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Mingxin Soft Magnetic Technology Jiangsu Co ltd
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Priority to CN202110866708.5A priority Critical patent/CN113517128A/en
Publication of CN113517128A publication Critical patent/CN113517128A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/0266Moulding; Pressing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition

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

Abstract

The invention relates to a preparation method of a magnetic material, in particular to a manufacturing method of an iron-cobalt micro-nano composite soft magnetic material. The preparation method of the novel low-loss iron-cobalt soft magnetic composite material comprises the following steps: cleaning iron-cobalt powder with acetone solution, wherein the cobalt content is 35-55%, and the balance is iron; after the materials are dried, the mixed powder is subjected to ultrasonic oscillation or ball milling by a high-energy ball mill to be fully compounded; coating iron-cobalt composite powder with phosphoric acid solution for one time, wherein the concentration of orthophosphoric acid is 0.5-5 wt%; coating the iron-cobalt composite material with a second blending resin, wherein the blending resin is prepared by mixing epoxy resin, phenolic resin, organic silicon resin and the like according to a certain proportion, and the content of the blending resin is 1-1.5 wt%; adding release agent barium stearate for compression molding. The preparation method of the invention realizes the soft magnetic composite material with high resistivity and high magnetic permeability under high frequency and is suitable for being used under high frequency.

Description

Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material
Technical Field
The invention relates to the technical field of soft magnetic material production, in particular to a preparation method of a low-loss iron-cobalt micro-nano composite soft magnetic material.
Background
With the development of electronic technology, the trend of inductance devices is more and more biased toward high frequency, miniaturization, high power and high efficiency, which requires that the soft magnetic core material should have high resistivity, low loss, high saturation magnetic flux density, high dc bias characteristic and low noise. Iron powder is widely used for preparing soft magnetic materials as a material with high magnetic permeability and low cost, but pure iron has relatively serious eddy current loss generated due to low resistivity at high frequency, so that the application range of an inductance element is limited. Therefore, coating iron powder increases the resistivity to reduce the loss, but a nonmagnetic coating agent or the like lowers the permeability of the soft magnetic material. The invention develops and improves the soft magnetic material under the background to prepare the high-permeability soft magnetic material which can be produced in a large scale.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a novel iron-cobalt micro-nano composite material with high magnetic permeability. And compounding the micron-sized iron powder and the nanoscale cobalt powder to prepare the micro-nano composite soft magnetic material with high magnetic conductivity and low loss.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a novel low-loss iron-cobalt micro-nano composite soft magnetic material comprises the following steps:
(1) cleaning the micron-sized iron powder and 35-55 wt% of nano-sized cobalt powder by using acetone to remove grease; the purity of the iron powder used in the invention is about 99.9%, the granularity is 20-50 microns, the purity of the cobalt powder is about 99.9%, and the granularity is 50 nm;
(2) then the material obtained in the step (1) is placed in a vacuum drying oven for drying;
(3) compounding: fully compounding the mixed powder, wherein the compounding mode is ultrasonic vibration for 0.5-10h or full ball milling for 1-100 h;
(4) primary surface coating: performing ultrasonic treatment on the magnetic micro-nano composite particles, an accelerator and an orthophosphoric acid acetone solution at the temperature of 5-80 ℃ for 5-100min, wherein the orthophosphoric acid addition amount of the phosphoric acid solution is 0.5-5 wt%;
(5) drying the solvent in the material obtained in the step (4) in a ventilation drying box at the temperature of 5-80 ℃;
(6) secondary coating of the surface: coating blended resin such as epoxy resin, organic silicon resin and the like and an accelerant on the surface of the iron-cobalt alloy coated with phosphoric acid, wherein the epoxy resin, the organic silicon resin and the like are mixed for 1-50min at 50-300 ℃ according to a certain proportion to form the blended resin, the blended resin is dissolved in an acetone solvent and is mixed with the material in the step (5), and the addition amount of the blended resin is 1-1.5%;
(7) heating the material in the step (6) at 50-300 ℃ for 1-50min for drying and degassing;
(8) preparing a magnetic core: pressing into a phi 13X 4X 2 iron-cobalt product by adopting a cold pressing and hot pressing combined mode.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the invention realizes the soft magnetic composite material with high resistivity and high magnetic permeability under high frequency and is suitable for being used under high frequency.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example one
Taking 100g of iron-cobalt powder, wherein the content of cobalt is 50%, and the balance is Fe, cleaning iron powder and nickel powder for three times by acetone for full degreasing, then placing the iron powder and the nickel powder in an ultrasonic cleaning machine for oscillation for 1 hour, after drying the materials, adding a phosphoric acid solution with the addition of 1 wt% of orthophosphoric acid, after drying an acetone solvent, adding 1 wt% of blending resin and an accelerator for coating, adding a release agent of barium stearate, cold-pressing for 10s under 800MPa, and performing gradient hot-pressing to obtain an iron-nickel product with phi 13X 4X 2.
Example two
Taking 100g of iron-cobalt powder, wherein the content of cobalt is 50%, and the balance is Fe, cleaning iron powder and nickel powder for three times by acetone for full degreasing, then placing the iron powder and the nickel powder for ball milling for 50h in a high-energy ball mill, after drying the materials, adding a phosphoric acid solution with the addition of 1 wt% of orthophosphoric acid, after drying an acetone solvent, adding 1 wt% of blending resin and an accelerator for coating, adding a release agent of barium stearate, cold-pressing for 10s under 800MPa, and performing gradient hot-pressing to obtain an iron-nickel product with phi 13X 4X 2.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (4)

1. A preparation method of a high-performance iron-cobalt micro-nano composite soft magnetic material is characterized by comprising the following steps:
(1) taking iron-cobalt powder, cleaning and mixing with acetone according to a certain proportion;
(2) compounding: drying the material obtained in the step (1), and then performing ultrasonic oscillation for 0.5-10h or performing ball milling for 1-100h by using a high-energy ball mill;
(3) and (3) phosphoric acid coating: performing primary phosphoric acid coating on the material obtained in the step (2);
(4) coating by using blended resin: adding blending resin and an accelerant into the material obtained in the step (3) and performing ultrasonic oscillation on the material subjected to primary coating to perform secondary coating;
(5) and (3) pressing and forming: and (4) adding a release agent barium stearate into the material obtained in the step (4), and performing cold pressing and hot pressing combined with cold pressing of 50-1000MPa and gradient hot pressing and compression molding to obtain the material.
2. The preparation method of claim 1, wherein the cobalt powder is added in an amount of 50-80 wt% in the iron-cobalt powder.
3. The method for preparing according to claim 1 or 2, characterized in that it comprises the following steps:
(1) cleaning the micron-sized iron powder and 35-55 wt% of nano-sized cobalt powder by using acetone to remove grease; the purity of the iron powder used in the invention is about 99.9%, the granularity is 20-50 microns, the purity of the cobalt powder is about 99.9%, and the granularity is 50 nm;
(2) then the material obtained in the step (1) is placed in a vacuum drying oven for drying;
(3) compounding: fully compounding the mixed powder, wherein the compounding mode is ultrasonic vibration for 0.5-10h or full ball milling for 1-100 h;
(4) primary surface coating: performing ultrasonic treatment on the magnetic micro-nano composite particles, an accelerator and an orthophosphoric acid acetone solution at the temperature of 5-80 ℃ for 5-100min, wherein the orthophosphoric acid addition amount of the phosphoric acid solution is 0.5-5 wt%;
(5) drying the solvent in the material obtained in the step (4) in a ventilation drying box at the temperature of 5-80 ℃;
(6) secondary coating of the surface: adopting epoxy resin, organic silicon resin and other blending resin and an accelerant to complete ultrasonic oscillation with the primary coating material so as to coat the mixture on the surface of the iron-cobalt alloy coated with phosphoric acid;
(7) heating the material in the step (6) at 5-300 ℃ for 5-100min for drying and degassing;
(8) preparing a magnetic core: pressing into a phi 13X 4X 2 iron-cobalt product by adopting a cold pressing and hot pressing combined mode.
4. The preparation method according to claim 3, characterized in that the epoxy resin and the organic silicon resin are mixed for 5-100min at 5-500 ℃ according to a certain proportion to form a blended resin, the blended resin is dissolved in an acetone solvent and mixed with the primary coating material, and the addition amount of the blended resin is 1-1.5%.
CN202110866708.5A 2021-07-29 2021-07-29 Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material Withdrawn CN113517128A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110866708.5A CN113517128A (en) 2021-07-29 2021-07-29 Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110866708.5A CN113517128A (en) 2021-07-29 2021-07-29 Preparation method of novel low-loss iron-cobalt micro-nano composite soft magnetic material

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CN113517128A true CN113517128A (en) 2021-10-19

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Application publication date: 20211019