CN112086257B - 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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- 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
- H01F1/20—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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- 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
- H01F1/20—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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- 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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- 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
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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 adopting tetraethoxysilane to carry out insulating coating, then carrying out secondary coating by using silicone 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 superior to that of the spherical magnetic powder, the permeability of the flaky magnetic powder is higher, and the excellent anisotropy is convenient for the magnetic field orientation treatment; although the quality factor is lower, the quality factor is effectively improved after coating, and magnetic field treatment can also have positive effect on improving magnetic permeability and further improve the quality factor. And forming the coated magnetic powder compression ring, performing orientation treatment by selecting magnetic field heat treatment, and performing heat treatment simultaneously, so that compared with the existing heat treatment process, the magnetic powder core with higher quality factor and magnetic conductivity is obtained without adding additional working procedures.
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 are important development directions of soft magnetic materials. The soft magnetic material mainly comprises: pure iron, ferrite, permalloy, metallic soft magnetic, amorphous soft magnetic, etc. In practical application, soft magnetic powder core materials are widely applied to the market of electronic components in excellent plastic shapes, and gradually start to develop to high frequency so as to adapt to the application scene of continuous high frequency. However, soft magnetic materials at high frequencies typically have a relatively low permeability and a relatively high dielectric constantGreater magnetic and electrical losses, and therefore improving the above performance becomes a primary problem for soft magnetic materials for use. The absorption characteristics of soft magnetic materials are generally characterized by dielectric constant ε and permeability μ, tan δ e Representing electrical loss, tan delta m Representing the magnetic loss, its energy loss tan delta and quality factor Q can be represented by the following formula:
ε=ε′-jε″,μ=μ′-jμ′
tanδ=tanδ e +tanδ m =ε″/ε′+μ″/μ′
Q=μ′/μ″
as can be seen from the above equation, the energy loss is determined by the electrical loss and the magnetic loss. In terms of magnetic loss alone, improving the magnetic permeability and the quality factor of the soft magnetic material effectively reduces the energy loss.
The magnetic powder core of Fe-Si-Al, fe-Ni-Mo and other metals is an important material for soft magnetic material in electronic industry because of low loss and low cost and no rare earth element. The existing magnetic powder core preparation method has great improvement space for the characteristics of magnetic conductivity, quality factor and the like, for example, chinese patent application publication No. CN109285685 discloses a preparation method of a high-magnetic-conductivity aerosolised sendust magnetic powder core, and the magnetic conductivity is up to 127; chinese patent application publication No. CN108777205 discloses a sendust 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 permeability of the prepared magnetic powder core is 50 at most and the quality factor is 30. Chinese patent publication No. CN106205930 discloses a method for preparing iron-nickel-molybdenum metal magnetic powder core, whose magnetic permeability is up to 200. It can be seen that the improvement of magnetic powder core permeability and the improvement of quality factor by various ways becomes a hot spot problem in the current 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 simple process, high magnetic conductivity and high quality factor of the prepared magnetic powder core.
The technical scheme of the invention is to provide a preparation method of a magnetic powder core with high magnetic conductivity and high quality factor, which comprises the following steps:
(1) Surface modification: adding the flaky magnetic powder into deionized water, ammonia water and an ethanol solution of APTES (3-aminopropyl triethoxysilane) which are uniformly mixed, and stirring fully;
(2) Insulating coating: adding TEOS (tetraethyl orthosilicate) into the solution obtained in the step (1), and stirring; after cleaning, drying to obtain flaky magnetic powder coated with silicon dioxide;
(3) And (3) secondary coating: stirring and mixing the flaky magnetic powder obtained in the step (2) with silicon resin dissolved in acetone and zinc stearate, and then drying to obtain secondary coated magnetic powder;
(4) And (5) press forming: placing the magnetic powder obtained in the step (3) into a die, and pressing and forming for a period of time under a certain pressure maintaining to obtain an annular magnetic powder core blank;
(5) Annealing: and (3) placing the magnetic powder core blank obtained in the step (4) into an annealing furnace for annealing, or annealing under the magnetic field of magnetic field heat treatment equipment to obtain a finished product.
Further, in the step (1), the volume ratio of deionized water, ammonia water, APTES and ethanol is (5-20): 1-4): 0.5-2): 60, and the mass volume ratio of flaky magnetic powder and ethanol is (g: mL) 0.5-3): 10.
Further, the sheet magnetic powder in the step (1) is one metal sheet magnetic powder or a mixture of several metal sheet magnetic powders in FeSiAl, feSi, feNi. The metal sheet magnetic powder is FeSiAl, feSi, feNi, which is prepared by hydrolyzing and condensing TEOS (tetraethyl orthosilicate) and coating SiO2 to obtain sheet magnetic powder with inter-sheet insulation.
Further, in the step (2), the volume ratio of TEOS to ethanol is (0.5-3): 6, the stirring time is 5-100 min, and coating layers with different silicon dioxide coating quality can be obtained by regulating and controlling the time.
Further, in the step (2), the cleaning solvent is ethanol and deionized water, and the cleaning solvent is sequentially cleaned by ethanol and deionized water.
Further, the mass ratio of the silicon resin dissolved with 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 and 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 60mm. The mass of the pressed 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 hours; 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 at f=110 kHz, the magnetic permeability is higher than 200, and the quality factor is higher than 100.
The invention has the advantages and beneficial effects that: the invention selects the metal flaky magnetic powder as the raw material, the anisotropy of the flaky magnetic powder is better than that of the spherical magnetic powder, the permeability of the flaky magnetic powder is higher, and the excellent anisotropy is convenient for the magnetic field orientation treatment; although the quality factor is lower, the quality factor is effectively improved after coating, and magnetic field treatment can also have positive effect on improving magnetic permeability and further improve the quality factor. And forming the coated magnetic powder compression ring, performing orientation treatment by selecting magnetic field heat treatment, and performing heat treatment simultaneously, so that compared with the existing heat treatment process, the magnetic powder core with higher quality factor and magnetic conductivity is obtained without adding additional working procedures.
Drawings
FIG. 1 is a graph showing the magnetic permeability versus frequency at various coating times in example 1.
Fig. 2 is a graph showing the change of quality factor with frequency at different coating times in example 1.
FIG. 3 is a graph showing the magnetic permeability versus frequency for different magnetic field strength heat treatments in example 2.
FIG. 4 is a graph showing the variation of quality factor with frequency for different magnetic field strength heat treatments in example 2.
Detailed Description
The invention is further described in connection with the following detailed description.
Example 1
Taking 24g of commercially available flaky iron-silicon-aluminum as a raw material, putting the 24g of the commercially available flaky iron-silicon-aluminum into a mixed solution of 240mL of ethanol, 8mL of ammonia water, 40mL of deionized water and 4mL of APTES which are uniformly mixed, stirring for 10min, adding 40mL of TEOS, stirring for 30min to obtain flaky iron-silicon-aluminum magnetic powder coated with silicon dioxide, washing the flaky iron-silicon-aluminum magnetic powder with ethanol and deionized water for several times, and carrying out ventilation drying in a fume hood for 12h. Mixing 10g of the obtained magnetic powder with 0.2g of silicone resin and 0.03g of zinc stearate in 10mL of acetone until the acetone volatilizes, and uniformly mixing the magnetic powder, the silicone resin and the zinc stearate, wherein the magnetic powder is coated for the second time. Drying in a forced air drying oven at 60deg.C for 1 hr to obtain raw materials for compression ring. Taking 2g of the raw materials, placing the raw materials into a compression molding die with the inner diameter of 12.7mm, the outer diameter of 20.3mm and the height of 60mm, pressing the raw materials under 1800MPa, and maintaining the pressure for 1min to obtain the annular magnetic powder core blank. And (3) annealing the blank in an annealing furnace at a high temperature of 700 ℃ under the protection of argon for 4 hours 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 was 60min, the remainder being the same as example 1.
Example 3
Example 3 differs from example 1 only in that the stirring time after the addition of TEOS was 80min, the remainder being the same as 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, respectively, that after TEOS addition, the coating reaction times were 30min, 60min and 80min, respectively, and that the uncoated SiO was coated 2 The magnetic powder of (2) and the magnetic permeability and quality factor of the obtained magnetic powder core are changed along with the frequency. Table 1 records the specific permeability and quality factor Q at 110kHz. According to Table 1 and in combination with FIGS. 1 and 2, an uncoated film is shownThe magnetic flake powder has high magnetic permeability, but the quality factor is only 65.1 at 110kHz, and the maximum value of the quality factor is about 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 at the coating time of 60min and reaches the highest value near 110kHz, which shows that the magnetic powder coating improves the quality factor and the application frequency. However, as the coating reaction time increases, the permeability decreases and the excess coating time permeability will be less than 200.
Example 4
Taking 24g of commercially available flaky iron-silicon-aluminum as a raw material, putting the 24g of the commercially available flaky iron-silicon-aluminum into a mixed solution of 240mL of ethanol, 8mL of ammonia water, 40mL of deionized water and 4mL of APTES which are uniformly mixed, stirring for 10min, adding 40mL of TEOS, stirring for 30min again, obtaining flaky iron-silicon-aluminum magnetic powder coated with silicon dioxide, washing the flaky iron-silicon-aluminum magnetic powder with ethanol and deionized water for several times, and ventilating and drying the flaky iron-silicon-aluminum magnetic powder in a fume hood for 12h. Mixing 10g of the obtained magnetic powder with 0.2g of silicone resin and 0.03g of zinc stearate in 10mL of acetone, stirring until the acetone volatilizes, and uniformly mixing the above three materials. Drying in a forced air drying oven at 60deg.C for 1 hr to obtain raw materials for compression ring. Taking 2g of the raw materials, placing the raw materials into a compression molding die with the inner diameter of 12.7mm, the outer diameter of 20.3mm and the height of 60mm, pressing the raw materials under 1800MPa, and maintaining the pressure for 1min to obtain the annular magnetic powder core blank. And (3) annealing the obtained blank in a magnetic field heat treatment furnace for 4 hours at the high temperature of 700 ℃ and the magnetic field strength of 0.4T under vacuum protection to obtain the finished magnetic powder core.
Example 5
Example 5 differs from example 4 only in that the magnetic field strength during the magnetic field heat treatment was 0.5T, and the rest was the same as example 4.
Example 6
Example 6 differs from example 4 only in that the magnetic field strength during the magnetic field heat treatment was 0.6T, and the rest was the same as example 4.
The magnetic powder cores obtained in examples 4 to 6 were subjected to performance tests, and the results are shown in FIGS. 3, 4 and Table 2
Table 2.110 magnetic powder core permeability real part μ' and quality factor Q
Magnetic field strength | 0 (no magnetic field) | Example 4 (0.4T) | Example 5 (0.5T) | Example 6 (0.6T) |
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 magnetic permeability and quality factor curves of the magnetic powder core with frequency after the heat treatment of the magnetic field and the heat treatment without the magnetic field at different magnetic field strengths of 0.4T, 0.5T and 0.6T, respectively. Table 2 records the specific permeability and quality factor Q at 110kHz. Table 2 shows that at 0.5T magnetic field heat treatment, the permeability is up to 272.1 and the quality factor is up to 109.2. This shows that proper magnetic field heat treatment can improve the quality factor of the magnetic powder core while improving the magnetic permeability of the magnetic powder core.
The 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 otherwise specified.
While the invention has been described with respect to the preferred embodiments, it will be understood by those skilled in the art that modifications and variations may be made without departing from the spirit and scope of the invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (7)
1. The preparation method of the magnetic powder core with high magnetic conductivity and high quality factor is characterized by comprising the following steps:
(1) Surface modification: adding sheet-shaped magnetic powder into evenly mixed deionized water, ammonia water and 3-aminopropyl triethoxy ethanol solution, and stirring thoroughly, wherein the sheet-shaped magnetic powder is one metal sheet-shaped magnetic powder or a mixture of a plurality of metal sheet-shaped magnetic powders in FeSiAl, feSi, feNi;
(2) Insulating coating: adding ethyl orthosilicate into the solution obtained in the step (1), and stirring; after cleaning, drying to obtain flaky magnetic powder coated with silicon dioxide, wherein the stirring time is 5-100 min;
(3) And (3) secondary coating: stirring and mixing the flaky magnetic powder obtained in the step (2), silicon resin dissolved in acetone and zinc stearate, wherein the mass ratio of the silicon resin dissolved in acetone, the zinc stearate and the magnetic powder is (1-10): 0.1-1): 100, the volume mass ratio of the acetone and the magnetic powder is (1-3): 1, and then drying to obtain the secondarily coated magnetic powder;
(4) And (5) press forming: placing the magnetic powder obtained in the step (3) into a die, maintaining the pressure, and performing compression molding to obtain an annular magnetic powder core blank;
(5) Annealing: and (3) annealing the magnetic powder core blank obtained in the step (4) under the magnetic field of magnetic field heat treatment equipment to obtain a finished product, wherein 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.
2. 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 deionized water, ammonia water and 3-aminopropyl triethoxy to ethanol in the step (1) is (5-20) of ammonia water and 3-aminopropyl triethoxy to ethanol= (1-4) of (0.5-2) of 60, and the mass volume ratio (g: mL) of the flaky magnetic powder to ethanol is (0.5-3) of 10.
3. The method of manufacturing a high permeability high quality factor magnetic powder core according to claim 1, wherein the volume ratio of ethyl orthosilicate to ethanol in step (2) is (0.5-3): 6.
4. The method of manufacturing a high permeability high quality factor magnetic powder core according to claim 1, wherein the cleaning solvent in step (2) is ethanol and deionized water.
5. A method for producing a high permeability high quality factor magnetic powder core according to claim 1, wherein the mold in step (4) has an inner diameter of 12.7mm, an outer diameter of 20.3mm, and a height of 60mm; the mass of the pressed 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.
6. A magnetic powder core, characterized in that it is manufactured by the manufacturing method of a magnetic powder core with high magnetic permeability and high quality factor according to any one of claims 1 to 5.
7. Use of a magnetic powder core according to claim 6, characterized in that the magnetic powder core has a permeability higher than 200, a quality factor higher than 100 and an operating frequency f = 110kHz.
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