CN112086257A - Magnetic powder core with high magnetic conductivity and high quality factor and preparation method and application thereof - Google Patents
Magnetic powder core with high magnetic conductivity and high quality factor and preparation method and application thereof Download PDFInfo
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- 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
- H01F1/20—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
- H01F1/24—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 the particles being insulated
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- 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
- H01F1/20—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
- H01F1/24—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 the particles being insulated
- H01F1/26—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 the particles being insulated by macromolecular organic substances
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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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- 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
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Abstract
The invention provides a preparation method of a magnetic powder core with high magnetic conductivity and high quality factor, which mainly comprises the steps of carrying out surface modification on flaky magnetic powder, then carrying out insulation coating by adopting tetraethoxysilane, then carrying out secondary coating by using silicon resin and zinc stearate, pressing the obtained magnetic powder into a magnetic powder core blank, and finally carrying out annealing treatment. The invention selects the flaky magnetic powder as the raw material, the anisotropy of the flaky magnetic powder is better than that of the spherical magnetic powder, the magnetic conductivity of the flaky magnetic powder is higher, and the excellent anisotropy is convenient for the orientation treatment of the magnetic field; although the quality factor is lower, the quality factor is effectively improved after coating, the magnetic field treatment can also generate positive effect on the improvement of the magnetic conductivity, and the quality factor is further improved. And (3) molding the coated magnetic powder by a compression ring, selecting magnetic field heat treatment for orientation treatment, and simultaneously performing heat treatment, so that compared with the existing heat treatment process, no additional process is added, and the magnetic powder core with higher quality factor and higher magnetic conductivity is obtained.
Description
Technical Field
The invention relates to a soft magnetic material, in particular to a preparation method of a magnetic powder core with high magnetic conductivity and high quality factor.
Background
With the rapid development of modern electronic technology, high frequency, light weight and high performance become important development directions of soft magnetic materials. The soft magnetic material mainly comprises: pure iron, ferrite, permalloy, metallic soft magnet, amorphous soft magnet, and the like. In practical application, the soft magnetic powder core material is widely applied to the market of electronic components in an excellent plastic shape, and gradually starts to develop into high frequency so as to adapt to the application scene of continuous high frequency. However, soft magnetic materials at high frequencies generally have low permeability, high dielectric constant, large magnetic and electrical losses, and therefore, improving the above properties is a primary problem for applications of soft magnetic materials. The absorption properties of soft magnetic materials are generally characterized by the dielectric constant and the permeability μ, taneDenotes the electrical loss, tanmRepresenting the magnetic loss, the energy loss tan and the quality factor Q can be represented by the following formula:
＝′-j″，μ＝μ′-jμ′
tan＝tane+tanm＝″/′+μ″/μ′
Q＝μ′/μ″
from the above equation, it can be seen that the energy loss is determined by the electrical and magnetic losses. In terms of magnetic loss alone, the magnetic permeability and the quality factor of the soft magnetic material are improved, and the energy loss of the soft magnetic material is effectively reduced.
The metal magnetic powder cores such as Fe-Si-Al, Fe-Ni-Mo and the like are important materials of soft magnetic materials in the electronic industry because of low loss and low cost and do not contain rare earth elements. The existing preparation method of the magnetic powder core has a great space for improving the characteristics of magnetic conductivity, quality factor and the like, for example, Chinese patent application publication No. CN109285685 discloses a preparation method of a gas atomization sendust magnetic powder core with high magnetic conductivity, and the magnetic conductivity reaches up to 127; chinese patent application publication No. CN108777205 discloses an iron-silicon-aluminum composite magnetic powder core and a preparation method thereof, and the magnetic permeability of the prepared magnetic powder core is up to 140; chinese patent application publication No. CN108987022 discloses a FeSiAl magnetic powder core and a preparation method thereof, and the magnetic powder core prepared by the method has the highest magnetic conductivity of 50 and the highest quality factor of 30. Chinese patent No. CN106205930 discloses a method for preparing an iron-nickel-molybdenum metal magnetic powder core, and the magnetic conductivity reaches up to 200. It can be seen that improving the magnetic powder core permeability and improving the quality factor by various means becomes a hot problem in the present research on soft magnetic materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides the preparation method of the magnetic powder core, which has the advantages of simple process, high magnetic conductivity of the prepared magnetic powder core and high quality factor.
The technical scheme of the invention is to provide a preparation method of a magnetic powder core with high magnetic permeability and high quality factor, which comprises the following steps:
(1) surface modification: adding the flaky magnetic powder into the uniformly mixed deionized water, ammonia water and an ethanol solution of APTES (3-aminopropyltriethoxysilane), and fully stirring;
(2) insulating and coating: adding TEOS (tetraethyl orthosilicate) into the solution obtained in the step (1), and stirring; after cleaning, drying to obtain silicon dioxide coated flaky magnetic powder;
(3) secondary coating: stirring and mixing the flaky magnetic powder obtained in the step (2) with silicone resin and zinc stearate dissolved in acetone, and then drying to obtain secondary coated magnetic powder;
(4) and (3) pressing and forming: putting the magnetic powder obtained in the step (3) into a mould, and carrying out pressure maintaining for a period of time at a certain pressure for compression molding to obtain an annular magnetic powder core blank;
(5) annealing treatment: and (5) annealing the magnetic powder core blank obtained in the step (4) in an annealing furnace or in the magnetic field of magnetic field heat treatment equipment to obtain a finished product.
Further, in the step (1), the volume ratio of the deionized water, the ammonia water, the APTES and the ethanol is (5-20): 1-4): 0.5-2): 60, and the mass volume ratio of the flaky magnetic powder to the ethanol is (0.5-3): 10.
Further, the sheet magnetic powder in the step (1) is one or a mixture of several of metal sheet magnetic powder of FeSiAl, FeSi and FeNi. The metal sheet magnetic powder is made of FeSiAl, FeSi, FeNi and the like, and is coated with SiO2 by using TEOS (tetraethyl orthosilicate) hydrolytic condensation to obtain the sheet magnetic powder with the inter-sheet insulation.
Furthermore, in the step (2), the volume ratio of TEOS to ethanol is (0.5-3): 6, the stirring time is 5-100 min, and the time is regulated to obtain coating layers with different silicon dioxide coating qualities.
Further, the solvents for cleaning in the step (2) are ethanol and deionized water, and the ethanol and the deionized water are sequentially used for cleaning.
Furthermore, the mass ratio of the silicone resin and the zinc stearate dissolved in the acetone to the magnetic powder in the step (3) is (1-10): 0.1-1): 100, and the volume mass ratio of the acetone to the magnetic powder (mL: g) is (1-3): 1.
Further, in the step (4), the inner diameter of the die is 12.7mm, the outer diameter is 20.3mm, and the height is 60 mm. The mass of the magnetic powder is 2-6 g each time, the pressing pressure is 1200-2000 MPa, and the pressure maintaining time is 0.5-3 min.
Further, in the step (5), the annealing temperature of the annealing furnace is 400-800 ℃, and the annealing time is 1-4 h; the magnetic field heat treatment temperature is 400-800 ℃, the magnetic field size is 0.1-1T, and the annealing time is 1-4 h.
The magnetic powder core prepared by the invention works under the condition that f is 110kHz, the magnetic conductivity is higher than 200, and the quality factor is higher than 100.
The invention has the advantages and beneficial effects that: the magnetic powder is prepared from metal flake magnetic powder, the anisotropy of the flake magnetic powder is superior to that of spherical magnetic powder, the magnetic conductivity of the flake magnetic powder is high, and the excellent anisotropy is convenient for magnetic field orientation treatment; although the quality factor is lower, the quality factor is effectively improved after coating, the magnetic field treatment can also generate positive effect on the improvement of the magnetic conductivity, and the quality factor is further improved. And (3) molding the coated magnetic powder by a compression ring, selecting magnetic field heat treatment for orientation treatment, and simultaneously performing heat treatment, so that compared with the existing heat treatment process, no additional process is added, and the magnetic powder core with higher quality factor and higher magnetic conductivity is obtained.
Drawings
FIG. 1 is a graph showing the change of permeability with frequency at different coating times in example 1.
FIG. 2 is a graph of Q-factor versus frequency for different cladding times in example 1.
FIG. 3 is a graph of permeability versus frequency for heat treatments of different magnetic field strengths as in example 2.
FIG. 4 is a graph of the figure of merit as a function of frequency for heat treatments of different magnetic field strengths in example 2.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
Taking 24g of commercially available sheet-shaped sendust as a raw material, putting the commercially available sheet-shaped sendust into a mixed solution of 240mL of ethanol, 8mL of ammonia water, 40mL of deionized water and 4mL of APTES, stirring for 10min, adding 40mL of TEOS, stirring for 30min to obtain sheet-shaped sendust magnetic powder coated with silicon dioxide, washing the sheet-shaped sendust magnetic powder for several times by using ethanol and deionized water, and ventilating and drying the sheet-shaped sendust magnetic powder in a fume hood for 12 h. And (3) taking 10g of the obtained magnetic powder, and stirring 0.2g of silicon resin and 0.03g of zinc stearate in 10mL of acetone until the acetone is volatilized, so that the magnetic powder, the silicon resin and the zinc stearate are uniformly mixed, and the magnetic powder is coated for the second time. Drying in a forced air drying oven at 60 deg.C for 1h to obtain raw material for compression ring. Taking 2g of the above raw materials, placing in a compression molding mold with inner diameter of 12.7mm, outer diameter of 20.3mm and height of 60mm, pressing under 1800MPa, and maintaining pressure for 1min to obtain annular magnetic powder core blank. And (3) annealing the obtained blank in an annealing furnace at the high temperature of 700 ℃ for 4 hours under the protection of argon to obtain the finished magnetic powder core.
Example 2
Example 2 differs from example 1 only in that the stirring time after the addition of TEOS is 60min, as in example 1.
Example 3
Example 3 differs from example 1 only in that the stirring time after the addition of TEOS is 80min, as in example 1.
The magnetic powder cores obtained in examples 1 to 3 were subjected to performance tests, and the results are shown in fig. 1, 2 and table 1.
TABLE 1 magnetic powder core permeability μ' and quality factor Q at 110kHz
FIGS. 1 and 2 show that the TEOS is added and then the reaction time is 30min, 60min and 80min for coating, and the SiO is not coated2The magnetic powder of (2) and the variation curve of the magnetic permeability and the quality factor of the obtained magnetic powder core along with the frequency. Table 1 records the specific permeability and quality factor Q at 110 kHz. According to table 1 in conjunction with fig. 1 and 2, it is shown that uncoated magnetic flakes have a high magnetic permeability themselves, but at 110kHz the quality factor is only 65.1, with a maximum value of the quality factor around 40 kHz. After TEOS is used as a silicon source for coating, the quality factor of the magnetic powder can reach more than 100, the quality factor is highest when the coating time is 60min, and reaches the highest value near 110kHz, which shows that the quality factor is improved and the application frequency is improved by coating the magnetic powder. But as the cladding reaction time increases and the permeability decreases, the excess cladding time permeability will be below 200.
Example 4
Taking 24g of commercially available sheet-shaped sendust as a raw material, putting the commercially available sheet-shaped sendust into a mixed solution of 240mL of ethanol, 8mL of ammonia water, 40mL of deionized water and 4mL of APTES, stirring for 10min, adding 40mL of TEOS, stirring for 30min to obtain sheet-shaped sendust magnetic powder coated with silicon dioxide, washing the sheet-shaped sendust magnetic powder for several times by using ethanol and deionized water, and ventilating and drying the sheet-shaped sendust magnetic powder in a fume hood for 12 h. 10g of the obtained magnetic powder is taken, and 0.2g of silicon resin and 0.03g of zinc stearate are stirred in 10mL of acetone until the acetone is volatilized, and the three are uniformly mixed. Drying in a forced air drying oven at 60 deg.C for 1h to obtain raw material for compression ring. Taking 2g of the above raw materials, placing in a compression molding mold with inner diameter of 12.7mm, outer diameter of 20.3mm and height of 60mm, pressing under 1800MPa, and maintaining pressure for 1min to obtain annular magnetic powder core blank. And (3) annealing the obtained blank in a magnetic field heat treatment furnace at the high temperature of 700 ℃ for 4h under the vacuum protection and the magnetic field intensity of 0.4T to obtain the finished magnetic powder core.
Example 5
Example 5 differs from example 4 only in that the magnetic field strength was 0.5T during the magnetic field heat treatment, and the rest is the same as example 4.
Example 6
Example 6 differs from example 4 only in that the magnetic field strength was 0.6T during the magnetic field heat treatment, and the rest is the same as example 4.
The magnetic powder cores obtained in examples 4 to 6 were subjected to the performance test, and the results are shown in FIGS. 3, 4 and Table 2
Magnetic powder core permeability real part μ' and quality factor Q at table 2.110 kHz
| Magnetic field intensity | 0 (no magnetic field) | Example 4(0.4T) | Example 5(0.5T) | Example 6(0.6T) |
| Magnetic permeability mu' | 238.4 | 235.5 | 272.1 | 249.2 |
| Quality factor Q | 101.7 | 104.8 | 109.2 | 106.4 |
Fig. 3 and 4 show the change curves of the magnetic permeability and the quality factor of the magnetic powder core with frequency after the magnetic field heat treatment and the magnetic field-free heat treatment under different magnetic field strengths of 0.4T, 0.5T and 0.6T respectively. Table 2 records the specific permeability and quality factor Q at 110 kHz. Table 2 in conjunction with fig. 3 and 4 shows that the permeability reached up to 272.1 and the quality factor reached up to 109.2 in the 0.5T field heat treatment. This indicates that proper magnetic field heat treatment can improve the magnetic permeability of the magnetic powder core and improve the quality factor of the magnetic powder core.
Materials, reagents and experimental equipment related to the embodiment of the invention are all commercial products conforming to the field of soft magnetic materials unless specified otherwise.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, modifications and decorations can be made without departing from the core technology of the present invention, and these modifications and decorations shall also fall within the protection scope of the present invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (10)
1. The preparation method of the magnetic powder core with high magnetic permeability and high quality factor is characterized by comprising the following steps:
(1) surface modification: adding the flaky magnetic powder into the uniformly mixed deionized water, ammonia water and 3-aminopropyltriethoxy ethanol solution, and fully stirring;
(2) insulating and coating: adding tetraethoxysilane into the solution obtained in the step (1), and stirring; after cleaning, drying to obtain silicon dioxide coated flaky magnetic powder;
(3) secondary coating: stirring and mixing the flaky magnetic powder obtained in the step (2) with silicone resin and zinc stearate dissolved in acetone, and then drying to obtain secondary coated magnetic powder;
(4) and (3) pressing and forming: putting the magnetic powder obtained in the step (3) into a mold, maintaining the pressure, and performing compression molding to obtain an annular magnetic powder core blank;
(5) annealing treatment: and (5) annealing the magnetic powder core blank obtained in the step (4) in an annealing furnace or in the magnetic field of magnetic field heat treatment equipment to obtain a finished product.
2. The method for preparing the magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein in the step (1), the volume ratio of deionized water to ammonia water to 3-aminopropyltriethoxy to ethanol is (5-20) to (1-4) to (0.5-2) to 60, and the mass volume ratio of the flaky magnetic powder to ethanol is (0.5-3) to 10.
3. The method for preparing a magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the flake magnetic powder in the step (1) is one or a mixture of several of FeSiAl, FeSi and FeNi.
4. The method for preparing the magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the volume ratio of the ethyl orthosilicate to the ethanol in the step (2) is (0.5-3): 6, and the stirring time is 5-100 min.
5. The method for preparing a magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the cleaning solvent in the step (2) is ethanol and deionized water.
6. The method for preparing the magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the mass ratio of the silicone resin dissolved in the acetone, the zinc stearate and the magnetic powder in the step (3) is (1-10): 0.1-1): 100, and the volume mass ratio of the acetone to the magnetic powder (mL: g) is (1-3): 1.
7. The method for preparing magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the step (4) is that the inner diameter of the die is 12.7mm, the outer diameter is 20.3mm, and the height is 60 mm; the mass of the magnetic powder is 2-6 g each time, the pressing pressure is 1200-2000 MPa, and the pressure maintaining time is 0.5-3 min.
8. The method for preparing the magnetic powder core with high magnetic permeability and high quality factor according to claim 1, wherein the annealing temperature of the annealing furnace in the step (5) is 400-800 ℃, and the annealing time is 1-4 h; the temperature of the magnetic field heat treatment is 400-800 ℃, the magnetic field size is 0.1-1T, and the annealing time is 1-4 h.
9. A magnetic powder core, characterized in that it is produced by the method of any one of claims 1 to 8.
10. Use of a magnetic powder core according to claim 9, characterized in that the magnetic powder core has a magnetic permeability of more than 200, a quality factor of more than 100 and an operating frequency of f-110 kHz.
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| CN113066629A (en) * | 2021-03-26 | 2021-07-02 | 福建尚辉润德新材料科技有限公司 | Insulating coating method of metal soft magnetic composite material and metal soft magnetic composite material |
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| CN113066629A (en) * | 2021-03-26 | 2021-07-02 | 福建尚辉润德新材料科技有限公司 | Insulating coating method of metal soft magnetic composite material and metal soft magnetic composite material |
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