CN115083718A - Preparation method of iron-based composite magnetic powder core - Google Patents
Preparation method of iron-based composite magnetic powder core Download PDFInfo
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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
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- 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
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- 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 an iron-based composite magnetic powder core, which comprises the steps of carrying out wet grinding pretreatment on flake iron-based alloy powder, first spherical iron-based alloy powder and a silane coupling agent, and then sequentially carrying out screening, first annealing treatment, passivation treatment, insulation coating treatment, mixing with a release agent, pressing, second annealing treatment and insulating paint spraying operation on the surface to prepare the iron-based composite magnetic powder core with high magnetic permeability and low magnetic loss. The preparation method disclosed by the invention is low in production cost, simple in preparation process and has a large-scale popularization and application prospect.
Description
Technical Field
The invention relates to the technical field of soft magnetic materials, in particular to a preparation method of an iron-based composite magnetic powder core.
Background
The metal magnetic powder core is powder made of metal or alloy soft magnetic material, and is a soft magnetic material with good comprehensive performance and formed by pressing through a special process. The magnetic ferrite has some excellent characteristics of metal soft magnetism and ferrite soft magnetism, so that the magnetic conductivity is small, the linearity is good, the saturation magnetic density is high, the working frequency range is wide, and the magnetic ferrite has extremely important significance for the development of electronic products towards the directions of high precision, high sensitivity, large capacity and miniaturization, and is also a key basic material for preparing electronic components.
The soft magnetic powder core applied in the market mainly comprises a metal soft magnetic powder core (iron powder core, ferrosilicon aluminum powder core and ferronickel powder core), an amorphous core, a nanocrystalline core and a ferrite powder core. The alloy soft magnetic material has the characteristics of high magnetic conductivity, high magnetic induction intensity, excellent direct current superposition performance and the like, but the resistivity is low; at high frequencies, eddy current losses increase dramatically with increasing frequency and are unusable. Among alloy-based magnetic powder cores, sendust cores are most commonly used. The sendust core has the advantages of good high-frequency magnetic performance, temperature stability, wide constant magnetic conductivity, low loss, near zero magnetostriction, low cost and the like.
With the shortage of energy sources and the increasingly serious dependence all over the world, the efficiency of energy conversion needs to be improved to reduce energy consumption, so that the magnetic powder core is required to have low loss, high magnetic induction intensity and low cost, and the future development direction of the metal magnetic powder core is required. With the higher and higher working frequency of the magnetic powder core application, the main problem of the products is how to consider the high magnetic permeability and low loss of the magnetic core.
CN100490029A discloses a composite powder for magnetic powder core and a preparation method of the magnetic powder core, wherein two annealed amorphous nanocrystalline magnetic powders are uniformly mixed and subjected to insulation bonding treatment, and the mixture is pressed into a magnetic core and then annealed to obtain the magnetic powder core with comprehensive characteristics. The magnetic powder core prepared by the method is relatively high in price, the preparation flow time is long, and the cost is increased.
CN101118797A discloses a composite powder for magnetic powder core, a magnetic powder core and a preparation method thereof, wherein the composite powder for magnetic powder core is prepared by uniformly mixing 50-96 wt% of iron-based soft magnetic powder and 4-50 wt% of iron-based amorphous soft magnetic powder with high insulating property and different requirements, so as to prepare the magnetic powder core with comprehensive and comprehensive requirements, the loss characteristic is low, and the magnetic conductivity characteristic is improved.
CN105185560A discloses a method for preparing an iron-based metal soft magnetic powder core, which comprises the steps of annealing iron-based flaky metal soft magnetic powder serving as raw material powder, passivating, insulating, coating, drying, pressing into a magnetic powder core, and annealing and painting to obtain a finished magnetic powder core. The magnetic powder core has high density, good mechanical strength, high magnetic permeability, high quality factor and low loss.
However, the magnetic powder core blank obtained by the method has low density, and the magnetic permeability needs to be further improved because of the existence of pores in the internal air gap.
Therefore, the development of the preparation method of the iron-based composite magnetic powder core with high green body density, high magnetic conductivity and low magnetic loss is of great significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of an iron-based composite magnetic powder core, which adopts flake alloy powder and spherical alloy powder to prepare the magnetic powder core, improves the density of a blank body, reduces pores in the magnetic powder core and reduces the loss of the magnetic powder core. The preparation method has the advantages of low production cost, simple preparation process, low equipment requirement and better performance of the prepared magnetic powder core.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an iron-based composite magnetic powder core, comprising the steps of:
(1) wet grinding pretreatment, sieving separation and drying are sequentially carried out on the flake iron-based alloy powder, the first spherical iron-based alloy powder and the silane coupling agent to obtain first powder;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently subjected to first annealing treatment, passivation treatment and insulation coating treatment in sequence, then mixed with an adhesive, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
(3) after the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, sequentially filling the mixture into a die cavity according to the sequence of flaky powder, spherical powder and flaky powder, and pressing the mixture to prepare a magnetic core blank;
(4) and after the magnetic core blank is subjected to second annealing treatment, insulating paint is sprayed on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
According to the preparation method of the iron-based composite magnetic powder core, the flaky iron-based alloy powder, the first spherical iron-based alloy powder and the silane coupling agent are subjected to wet grinding pretreatment, so that the first spherical iron-based alloy powder is flaky, and then the first powder with the average particle size D50 of 20-200 mu m is obtained through sieving, separation and drying, so that the compactness of the prepared iron-based composite magnetic powder core is improved, and meanwhile, the iron-based composite magnetic powder core has higher magnetic conductivity and can keep the performance of lower loss. The silane coupling agent has the effects that after the first annealing treatment, the generated silicon dioxide is decomposed to coat the surfaces of the first powder and the second spherical iron-based alloy powder, so that the powder has better fluidity; furthermore, the powder is prevented from being corroded in the air. And (3) sequentially filling the flaky powder, the spherical powder and the flaky powder into a die cavity in sequence to be pressed into a magnetic core blank, wherein the magnetic core blank is mainly prepared by the reason that the magnetic conductivity of the flaky powder is higher than that of the spherical powder, and the magnetic conductivity of the iron-based composite magnetic powder core obtained to the maximum extent can be greatly improved according to the sequence of the flaky powder, the spherical powder and the flaky powder.
Preferably, the iron-based alloy powder in step (1) includes any one of or a combination of at least two of FeSi, FeNi, FeSiAl, FeNiMo, FeSiAlNi, fesicl or FeSiAlTi, wherein typical but non-limiting combinations include a combination of FeSi and FeNi, a combination of FeSiAl and FeNiMo, a combination of FeSiAlNi and fesicrcr, a combination of FeSiAlTiFeSi, FeNi and FeSiAl or a combination of three of FeNiMo, FeSiAlNi and fesicricrcr.
Preferably, the sheet iron-based alloy powder is sieved through a 50-150 mesh screen before wet grinding pretreatment, such as 50 mesh, 60 mesh, 70 mesh, 80 mesh, 90 mesh or 100 mesh screen, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the first spherical iron-based alloy powder is sieved through a 300-500 mesh screen before wet grinding pretreatment, such as 300 mesh, 350 mesh, 400 mesh, or 500 mesh, but not limited to the recited values, and other values within the range are also applicable.
Preferably, the mass parts of the flaky iron-based alloy powder, the first spherical iron-based alloy powder and the silane coupling agent are 5-20 parts, 80-95 parts and 0.5-5 parts respectively; the amount of the flaky iron-based alloy powder is 5 to 20 parts, for example, 5 parts, 8 parts, 10 parts, 15 parts, or 20 parts, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable; the amount of the spherical iron-based alloy powder is, for example, 80 parts, 83 parts, 85 parts, 90 parts or 95 parts, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable; the silane coupling agent is used in an amount of 0.5 to 5 parts, for example, 0.5 part, 0.7 part, 1.0 part, 1.5 parts, or 2 parts, but the amount is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the solvent used in the wet-milling pretreatment in step (1) comprises alcohol and/or acetone.
Preferably, the wet-milling pretreatment time is 1 to 5 hours, for example, 1 hour, 2 hours, 3 hours, 4 hours, 4.5 hours, or 5 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the rotation frequency of the wet grinding pretreatment is 20 to 30Hz, such as 20Hz, 21Hz, 23Hz, 25Hz, 27Hz, or 30Hz, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the first powder has an average particle size D50 of 20 to 200. mu.m, for example, 20 μm, 30 μm, 50 μm, 80 μm, 90 μm, 100 μm or 200 μm, but is not limited to the values listed, and other values not listed within the range of values are also applicable.
Preferably, the first annealing treatment in step (2) is performed by heating to 550-700 ℃ at a heating rate of 1-5 ℃/min under the protection of nitrogen, keeping the temperature for 1-3 h, and cooling to room temperature, wherein the heating rate is 1-5 ℃/min, such as 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 4.5 ℃/min, or 5 ℃/min, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable; the temperature is raised to 550 to 700 ℃, for example, 550 ℃, 580 ℃, 600 ℃, 650 ℃ or 700 ℃, but the temperature is not limited to the recited values, and other values not recited in the numerical range are also applicable; the heat preservation time is 1 to 3 hours, and may be, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 2.8 hours, 3 hours, etc., but the heat preservation time is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the passivating agent used in the passivating treatment in step (2) includes any one or a combination of at least two of phosphoric acid, boric acid, hydrogen peroxide, and nitric acid, wherein typical but non-limiting combinations include a combination of phosphoric acid and boric acid, a combination of hydrogen peroxide and nitric acid, or a combination of phosphoric acid and hydrogen peroxide.
Preferably, the total mass of the passivating agent is 0.1 to 3 wt% of the total mass of the powder, and may be, for example, 0.1 wt%, 0.5 wt%, 0.8 wt%, 1 wt%, 2 wt%, or 3 wt%, but is not limited to the recited values, and other values not recited within the range of the values are also applicable.
Preferably, the insulating agent used in the insulation coating process includes any one or a combination of at least two of silicates, phosphates, mica powder or kaolin, wherein typical but non-limiting combinations include combinations of silicates and phosphates, combinations of mica powder and kaolin silicates, combinations of phosphates and mica powder or combinations of kaolin, silicates and phosphates, preferably SiO 2 CaO or Al 2 O 3 Any one of or a combination of at least two of, wherein a typical but non-limiting combination includes SiO 2 And CaO, Al 2 O 3 And SiO 2 Combinations of (5) or CaO, Al 2 O 3 And SiO 2 The combination of the three.
Preferably, the amount of the insulating agent added is 0.1 to 5 wt% of the total mass of the powder, and may be, for example, 0.1 wt%, 0.5 wt%, 1 wt%, 2 wt%, 3 wt%, or 5 wt%, but is not limited to the recited values, and other values not recited within this range are also applicable.
Preferably, the insulation coating treatment in the step (2) is dried.
Preferably, the temperature of the drying is 70 to 140 ℃, for example, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 120 ℃ or 140 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the adhesive of step (2) includes an organic adhesive or an inorganic adhesive.
Preferably, the organic binder comprises any one or a combination of at least two of an epoxy resin, a silicone resin, or a phenolic resin, wherein typical but non-limiting combinations include a combination of an epoxy resin and a silicone resin, a combination of a phenolic resin and an epoxy resin, or a combination of a silicone resin, a phenolic resin, and an epoxy resin.
Preferably, the inorganic binder includes phosphate.
The binder is preferably added in an amount of 1 to 5 wt% based on the total mass of the powder, and may be, for example, 1 wt%, 1.5 wt%, 2 wt%, 3 wt%, 4 wt%, or 5 wt%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the mold release agent in step (3) comprises any one or a combination of at least two of zinc stearate, barium stearate, aluminum stearate or talc, wherein typical but non-limiting combinations include a combination of zinc stearate and barium stearate, a combination of aluminum stearate and talc, a combination of barium stearate and aluminum stearate or a combination of talc, zinc stearate and barium stearate.
The release agent is preferably added in an amount of 0.3 to 3 wt% based on the total mass of the granulated flaky powder, and may be, for example, 0.3 wt%, 0.5 wt%, 1 wt%, 2 wt%, or 3 wt%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
The release agent is preferably added in an amount of 0.3 to 3 wt% based on the total mass of the granulated spherical powder, and may be, for example, 0.3 wt%, 0.5 wt%, 1 wt%, 2 wt%, or 3 wt%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the mass ratio of the flaky powder to the spherical powder to the flaky powder sequentially filled in the cavity is (0.5 to 1.5): (5 to 9): 0.5 to 3, and for example, it may be 0.5:5:0.5, 1:6:3, 1:8:1, 1:7:2, or 1.5:9:3, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the pressure of the pressing is 12-20T/cm 2 For example, it may be 12T/cm 2 、15T/cm 2 、16T/cm 2 、18T/cm 2 、19T/cm 2 Or 20T/cm 2 And the like, but are not limited to the recited values, and other values not recited within the numerical range are also applicable.
Preferably, the second annealing treatment in step (4) is performed at N 2 Or H 2 Raising the temperature to 550-700 ℃ at a temperature raising rate of 1.5-3 ℃/min in the atmosphere, and keeping the temperature for 1-3 h, wherein the temperature raising rate is 1.5-3 ℃/min, for example, 1.5 ℃/min, 1.8 ℃/min, 2 ℃/min, 2.2 ℃/min, 2.5 ℃/min or 3 ℃/min, but the temperature raising rate is not limited to the recited values, and other values not recited in the numerical value range are also applicable; the temperature is raised to 550 to 700 ℃, for example, 550 ℃, 580 ℃, 600 ℃, 650 ℃ or 700 ℃, but the temperature is not limited to the recited values, and other values not recited in the numerical range are also applicable; the heat preservation time is 1 to 3 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 2.8 hours or 3 hours, but the heat preservation time is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) 5-20 parts of flaky iron-based alloy powder, 80-95 parts of first spherical iron-based alloy powder and 0.5-5 parts of silane coupling agent are sequentially subjected to wet grinding pretreatment for 1-5 hours at the rotating speed and frequency of 20-30 Hz, screened, separated and dried to obtain first powder with the average particle size D50 of 20-200 mu m; the iron-based alloy powder comprises one or the combination of at least two of FeSi, FeNi, FeSiAl, FeNiMo, FeSiAlNi, FeSiCr and FeSiAlTi; screening the flaky iron-based alloy powder through a screen of 50-150 meshes before wet grinding pretreatment; screening the spherical iron-based alloy powder through a screen of 300-500 meshes before wet grinding pretreatment; the solvent adopted in the wet grinding pretreatment comprises alcohol and/or acetone;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently subjected to first annealing treatment, passivation treatment and insulation coating treatment in sequence, then mixed with an adhesive, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, under the protection of nitrogen, the temperature is raised to 550-700 ℃ at the heating rate of 1-5 ℃/min, the temperature is kept for 1-3 h, and the temperature is cooled to the room temperature;
the passivating agent adopted by the passivation treatment comprises any one or the combination of at least two of phosphoric acid, boric acid, hydrogen peroxide or nitric acid; the total mass of the passivator is 0.1-3 wt% of the total mass of the powder;
the insulating agent adopted in the insulating coating treatment comprises any one or combination of at least two of silicate, phosphate, mica powder or kaolin, and is preferably SiO 2 CaO or Al 2 O 3 Any one or a combination of at least two of them; the addition amount of the insulating agent is 0.1-5 wt% of the total mass of the powder;
the adhesive comprises an organic adhesive or an inorganic adhesive; the organic adhesive comprises any one of epoxy resin, silicone resin or phenolic resin or a combination of at least two of the epoxy resin, the silicone resin and the phenolic resin; the inorganic binder includes a phosphate; the addition amount of the adhesive is 1-5 wt% of the total mass of the powder;
(3) after the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, sequentially filling the mixture into a die cavity according to the sequence of flaky powder, spherical powder and flaky powder, and pressing the mixture to prepare a magnetic core blank; the release agent comprises any one or the combination of at least two of zinc stearate, barium stearate, aluminum stearate or talcum powder; the addition amount of the release agent is 0.3-3 wt% of the total mass of the granulated flaky powder; the addition amount of the release agent is after granulation0.3-3 wt% of the total mass of the spherical powder; the mass ratio of the flaky powder to the spherical powder to the flaky powder sequentially filled into the die cavity is (0.5-1.5) to (5-9) to (0.5-3); the pressing pressure is 12-20T/cm 2 ；
(4) The magnetic core blank is arranged at N 2 /H 2 And heating to 550-700 ℃ at a heating rate of 1.5-3 ℃/min in the atmosphere, carrying out heat preservation for 1-3 h, carrying out second annealing treatment, and spraying insulating paint on the surface of the iron-based composite magnetic powder core to obtain the iron-based composite magnetic powder core.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method of the iron-based composite magnetic powder core provided by the invention has the advantages of low production cost, simple preparation process and low equipment requirement, and the prepared magnetic powder core has high magnetic conductivity and low magnetic loss and is suitable for large-scale popularization and application.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the following examples are set forth herein. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Example 1
The embodiment provides a preparation method of an iron-based composite magnetic powder core, which comprises the following steps:
(1)5 parts of sheet iron-based alloy powder, 95 parts of first spherical iron-based alloy powder and 0.5 part of silane coupling agent are sequentially subjected to wet grinding pretreatment for 2 hours at the rotating speed and frequency of 20Hz, screened, separated and dried to obtain first powder; the iron-based alloy powder is FeSiAl; screening the flaky iron-based alloy powder through a 50-mesh screen before wet grinding pretreatment; sieving the first spherical iron-based alloy powder through a 300-mesh sieve before wet-grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently sieved by 50 meshes, 70 meshes and 100 meshes, subjected to first annealing treatment, passivation treatment and insulating coating treatment in sequence, mixed with a bonding agent, and sieved by 50 meshes for granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, the temperature is raised to 600 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, the temperature is kept for 50min, and the temperature is cooled to the room temperature;
the passivation treatment adopts phosphoric acid with the concentration of 10 percent accounting for 1 weight percent of the total mass of the powder;
the insulation coating treatment adopts kaolin accounting for 0.6 wt% of the total mass of the powder;
the adhesive is epoxy resin accounting for 2.5 wt% of the total mass of the powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then are sequentially placed into a die cavity according to the sequence of flaky powder-spherical powder-flaky powder, wherein the mass ratio of flaky powder-spherical powder-flaky powder is 0.5:9:0.5, and the mixture is pressed into a magnetic core blank; the release agent is zinc stearate accounting for 0.3 wt% of the total mass of the granulated powder; the pressure of the pressing is 12.5T/cm 2 ；
(4) And heating the magnetic core blank to 600 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 1h, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
Example 2
The embodiment provides a preparation method of an iron-based composite magnetic powder core, which comprises the following steps:
(1) sequentially carrying out wet grinding pretreatment on 10 parts of sheet iron-based alloy powder, 90 parts of first spherical iron-based alloy powder and 1 part of silane coupling agent at the rotating speed and frequency of 25Hz for 2 hours, sieving, separating and drying to obtain first powder; the iron-based alloy powder is FeSiAl; screening the flaky iron-based alloy powder through a 50-mesh screen before wet grinding pretreatment; the first spherical iron-based alloy powder is sieved by a 350-mesh sieve before wet grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently sieved by a 50-mesh sieve, a 70-mesh sieve and a 100-mesh sieve, subjected to first annealing treatment, passivation treatment and insulating coating treatment in sequence, mixed with a bonding agent, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, the temperature is raised to 550 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, the temperature is kept for 1.5h, and the temperature is cooled to room temperature;
the passivation treatment adopts phosphoric acid with the concentration of 10 percent accounting for 0.8 weight percent of the total mass of the mixed powder;
the insulation coating treatment adopts kaolin accounting for 0.6 wt% of the total mass of the mixed powder;
the adhesive is epoxy resin accounting for 4 wt% of the total mass of the mixed powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then are sequentially placed into a die cavity according to the sequence of flaky powder-spherical powder-flaky powder, wherein the mass ratio of flaky powder-spherical powder-flaky powder is 1:8:1, and the mixture is pressed into a magnetic core blank; the release agent is zinc stearate accounting for 0.3 wt% of the total mass of the granulated powder; the pressing pressure is 12T/cm 2 ；
(4) And heating the magnetic core blank to 650 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 1.5h, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
Example 3
The embodiment provides a preparation method of an iron-based composite magnetic powder core, which comprises the following steps:
(1) sequentially carrying out wet grinding pretreatment on 20 parts of sheet iron-based alloy powder, 80 parts of first spherical iron-based alloy powder and 2 parts of silane coupling agent at the rotating speed and frequency of 25Hz for 2 hours, sieving, separating and drying to obtain first powder; the iron-based alloy powder is FeSiAl; screening the flaky iron-based alloy powder through a 150-mesh screen before wet grinding pretreatment; sieving the first spherical iron-based alloy powder through a 300-mesh sieve before wet-grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently sieved by a 50-mesh sieve, a 70-mesh sieve and a 100-mesh sieve, subjected to first annealing treatment, passivation treatment and insulating coating treatment in sequence, mixed with a bonding agent, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, wherein the temperature is raised to 600 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, the temperature is kept for 2 hours, and the temperature is cooled to room temperature;
the passivation treatment adopts phosphoric acid with the concentration of 10 percent accounting for 0.6 weight percent of the total mass of the mixed powder;
the insulation coating treatment adopts kaolin accounting for 0.5 wt% of the total mass of the mixed powder;
the adhesive is epoxy resin accounting for 3.5 wt% of the total mass of the mixed powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then are sequentially placed into a die cavity according to the sequence of flaky powder-spherical powder-flaky powder, wherein the mass ratio of flaky powder-spherical powder-flaky powder is 1.5:7:1.5, and the mixture is pressed into a magnetic core blank; the release agent is zinc stearate accounting for 0.3 wt% of the total mass of the granulated powder; the pressing pressure is 14T/cm 2 ；
(4) And heating the magnetic core blank to 650 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 1.5h, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
Example 4
The embodiment provides a preparation method of an iron-based composite magnetic powder core, which comprises the following steps:
(1) sequentially carrying out wet grinding pretreatment on 20 parts of sheet iron-based alloy powder, 80 parts of first spherical iron-based alloy powder and 3 parts of silane coupling agent for 1h at the rotating speed and frequency of 28Hz, sieving, separating and drying to obtain first powder; the iron-based alloy powder is FeSiAl; screening the flaky iron-based alloy powder through a 150-mesh screen before wet grinding pretreatment; sieving the first spherical iron-based alloy powder through a 400-mesh sieve before wet-grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently sieved by a 50-mesh sieve, a 70-mesh sieve and a 100-mesh sieve, subjected to first annealing treatment, passivation treatment and insulating coating treatment in sequence, mixed with a bonding agent, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, the temperature is raised to 550 ℃ at the heating rate of 2.5 ℃/min under the protection of nitrogen, the temperature is kept for 2h, and the temperature is cooled to room temperature;
the passivation treatment adopts phosphoric acid with the concentration of 10 percent accounting for 0.5 weight percent of the total mass of the mixed powder;
the insulation coating treatment adopts kaolin accounting for 0.4 wt% of the total mass of the mixed powder;
the adhesive is epoxy resin accounting for 3 wt% of the total mass of the mixed powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then are sequentially placed into a die cavity according to the sequence of flaky powder-spherical powder-flaky powder, wherein the mass ratio of flaky powder-spherical powder-flaky powder is 2:6:2, and the mixture is pressed into a magnetic core blank; the release agent is zinc stearate accounting for 0.15 wt% of the total mass of the granulated powder; the pressing pressure is 13.5T/cm 2 ；
(4) And heating the magnetic core blank to 650 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 2 hours, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
Example 5
The embodiment provides a preparation method of an iron-based composite magnetic powder core, which comprises the following steps:
(1) sequentially carrying out wet grinding pretreatment on 20 parts of sheet iron-based alloy powder, 80 parts of first spherical iron-based alloy powder and 5 parts of silane coupling agent for 1h at the rotating speed and frequency of 28Hz, sieving, separating and drying to obtain first powder; the iron-based alloy powder is FeSiAl; screening the flaky iron-based alloy powder through a 50-mesh screen before wet grinding pretreatment; the first spherical iron-based alloy powder is sieved by a 350-mesh sieve before wet grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently sieved by a 50-mesh sieve, a 70-mesh sieve and a 100-mesh sieve, subjected to first annealing treatment, passivation treatment and insulating coating treatment in sequence, mixed with a bonding agent, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, the temperature is raised to 650 ℃ at the heating rate of 2.5 ℃/min under the protection of nitrogen, the temperature is kept for 2h, and the temperature is cooled to room temperature;
the passivation treatment adopts phosphoric acid with the concentration of 10 percent accounting for 0.3 weight percent of the total mass of the mixed powder;
the insulation coating treatment adopts kaolin accounting for 0.35 wt% of the total mass of the mixed powder;
the adhesive is silicone resin accounting for 5 wt% of the total mass of the mixed powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then are sequentially placed into a die cavity according to the sequence of flaky powder-spherical powder-flaky powder, wherein the mass ratio of flaky powder-spherical powder-flaky powder is 2:5:3, and the mixture is pressed into a magnetic core blank; the release agent is zinc stearate accounting for 0.3 wt% of the total mass of the granulated powder; the pressing pressure is 13.5T/cm 2 ；
(4) And heating the magnetic core blank to 700 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 2 hours, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
Comparative example 1
The comparative example provides a method for preparing an iron-based composite magnetic powder core, comprising the following steps:
(1) mixing 100 parts of spherical iron-based alloy powder and 3 parts of silane coupling agent sequentially through mechanical stirring for 1 hour, and drying to obtain first powder; the iron-based alloy powder is FeSiAl; screening the spherical iron-based alloy powder through a 300-mesh screen before wet grinding pretreatment; the wet grinding pretreatment adopts 200 parts of alcohol;
(2) the first powder is mixed with an adhesive after being sequentially subjected to first annealing treatment, passivation treatment and insulation coating treatment, and is subjected to sieving granulation treatment to obtain granulated powder;
the first annealing treatment is carried out, the temperature is raised to 650 ℃ at the heating rate of 2.5 ℃/min under the protection of nitrogen, the temperature is kept for 2h, and the temperature is cooled to room temperature;
the passivation treatment adopts 10 percent phosphoric acid which accounts for 1.5 weight percent of the total mass of the mixed powder;
the insulation coating treatment adopts kaolin accounting for 0.35 wt% of the total mass of the mixed powder;
the adhesive is silicone resin accounting for 5 wt% of the total mass of the mixed powder;
(3) mixing the granulated powder with a release agent, and pressing into a magnetic core blank; the release agent is zinc stearate accounting for 0.3 wt% of the total mass of the granulated powder; the pressing pressure is 13T/cm 2 ；
(4) And heating the magnetic core blank to 700 ℃ at the heating rate of 2.2 ℃/min in nitrogen atmosphere, preserving the heat for 2 hours, and spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
The permeability of the iron-based composite magnetic powder core obtained in the above examples and comparative examples at 50kHz and the magnetic loss at 50kHz and 100mT are shown in Table 1.
TABLE 1
| Magnetic permeability | Loss (W/cm) 3 ) | |
| Example 1 | 118 | 89 |
| Example 2 | 120 | 91 |
| Example 3 | 122 | 93 |
| Example 4 | 143 | 92 |
| Example 5 | 151 | 93 |
| Comparative example 1 | 115 | 95 |
In conclusion, the preparation method of the iron-based composite magnetic powder core provided by the invention has the advantages that the iron-based composite magnetic powder core prepared by wet grinding pretreatment of the flake iron-based alloy powder, the spherical iron-based alloy powder and the silane coupling agent has high magnetic conductivity and relatively low magnetic loss, is good in comprehensive performance, and has the prospect of large-scale popularization and application.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the iron-based composite magnetic powder core is characterized by comprising the following steps:
(1) wet grinding pretreatment, sieving separation and drying are sequentially carried out on the flake iron-based alloy powder, the first spherical iron-based alloy powder and the silane coupling agent to obtain first powder;
(2) the first powder and the second spherical iron-based alloy powder are respectively and independently subjected to first annealing treatment, passivation treatment and insulation coating treatment in sequence, then mixed with an adhesive, and subjected to sieving granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
(3) the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, and then sequentially filled into a die cavity according to the sequence of the flaky powder, the spherical powder and the flaky powder to be pressed into a magnetic core blank;
(4) and after the magnetic core blank is subjected to second annealing treatment, spraying insulating paint on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core.
2. The production method according to claim 1, wherein the iron-based alloy powder in the step (1) includes any one or a combination of at least two of FeSi, FeNi, FeSiAl, FeNiMo, FeSiAlNi, fesiccr, and FeSiAlTi;
preferably, the flaky iron-based alloy powder is sieved by a sieve with 50-150 meshes before wet grinding pretreatment;
preferably, the first spherical iron-based alloy powder is sieved by a sieve with 300-500 meshes before wet grinding pretreatment;
preferably, the mass parts of the flaky iron-based alloy powder, the first spherical iron-based alloy powder and the silane coupling agent are 5-20 parts, 80-95 parts and 0.5-5 parts respectively.
3. The method according to claim 1 or 2, wherein the solvent used in the wet-milling pretreatment of step (1) comprises alcohol and/or acetone;
preferably, the time of the wet grinding pretreatment is 1-5 h;
preferably, the rotating speed frequency of the wet grinding pretreatment is 20-30 Hz;
preferably, the average particle size D50 of the first powder is 20-200 μm.
4. The preparation method according to any one of claims 1 to 3, wherein the first annealing treatment in the step (2) is performed by raising the temperature to 550 to 700 ℃ at a temperature raising rate of 1 to 5 ℃/min under the protection of nitrogen, maintaining the temperature for 1 to 3 hours, and cooling to room temperature.
5. The preparation method according to any one of claims 1 to 4, wherein a passivating agent used in the passivating treatment in the step (2) comprises any one or a combination of at least two of phosphoric acid, boric acid, hydrogen peroxide or nitric acid;
preferably, the total mass of the passivator is 0.1-3 wt% of the total mass of the powder;
preferably, the insulating agent used in the insulating coating treatment includes any one or a combination of at least two of silicates, phosphates, mica powder or kaolin, and is preferably SiO 2 CaO or Al 2 O 3 Any one or a combination of at least two of;
preferably, the addition amount of the insulating agent is 0.1-5 wt% of the total mass of the powder.
6. The manufacturing method according to any one of claims 1 to 5, wherein the insulating coating treatment in the step (2) is followed by drying;
preferably, the drying temperature is 70-140 ℃.
7. The method according to any one of claims 1 to 6, wherein the adhesive in the step (2) comprises an organic adhesive or an inorganic adhesive;
preferably, the organic adhesive comprises any one of epoxy resin, silicone resin or phenolic resin or a combination of at least two of the epoxy resin, the silicone resin or the phenolic resin;
preferably, the inorganic binder includes phosphate;
preferably, the addition amount of the adhesive is 1-5 wt% of the total mass of the powder.
8. The preparation method according to any one of claims 1 to 7, wherein the release agent in the step (3) comprises any one or a combination of at least two of zinc stearate, barium stearate, aluminum stearate or talc;
preferably, the addition amount of the release agent is 0.3-3 wt% of the total mass of the granulated flaky powder;
preferably, the addition amount of the release agent is 0.3-3 wt% of the total mass of the granulated spherical powder;
preferably, the mass ratio of the flaky powder to the spherical powder to the flaky powder sequentially filled in the die cavity is (0.5-1.5) to (5-9) to (0.5-3);
preferably, the pressure of the pressing is 12-20T/cm 2 。
9. The method according to any one of claims 1 to 8, wherein the second annealing treatment in step (4) is performed in the presence of N 2 Or H 2 Heating to 550-700 ℃ at a heating rate of 1.5-3 ℃/min in the atmosphere, and preserving heat for 1-3 h.
10. The method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) 5-20 parts of flaky iron-based alloy powder, 80-95 parts of first spherical iron-based alloy powder and 0.5-5 parts of silane coupling agent are sequentially subjected to wet grinding pretreatment for 1-5 hours at the rotating speed and frequency of 20-30 Hz, screened, separated and dried to obtain first powder with the average particle size D50 of 20-200 mu m; the iron-based alloy powder comprises one or the combination of at least two of FeSi, FeNi, FeSiAl, FeNiMo, FeSiAlNi, FeSiCr and FeSiAlTi; screening the flaky iron-based alloy powder through a screen of 50-150 meshes before wet grinding pretreatment; screening the first spherical iron-based alloy powder through a screen of 300-500 meshes before wet grinding pretreatment; the solvent adopted in the wet grinding pretreatment comprises alcohol and/or acetone;
(2) the first powder and the second spherical iron-based alloy powder are respectively independently subjected to first annealing treatment, passivation treatment and insulation coating treatment in sequence, then mixed with a bonding agent, and subjected to sieve granulation treatment to respectively obtain granulated flaky powder and granulated spherical powder;
the first annealing treatment is carried out, under the protection of nitrogen, the temperature is raised to 550-700 ℃ at the heating rate of 1-5 ℃/min, the temperature is kept for 1-3 h, and the temperature is cooled to the room temperature;
the passivating agent adopted in the passivation treatment comprises any one or a combination of at least two of phosphoric acid, boric acid, hydrogen peroxide or nitric acid; the total mass of the passivator is 0.1-3 wt% of the total mass of the powder;
the insulating agent adopted in the insulating coating treatment comprises any one or combination of at least two of silicates, phosphates, mica powder or kaolin, and is preferably SiO 2 CaO or Al 2 O 3 Any one or a combination of at least two of; the addition amount of the insulating agent is 0.1-5 wt% of the total mass of the powder;
the adhesive comprises an organic adhesive or an inorganic adhesive; the organic adhesive comprises any one or a combination of at least two of epoxy resin, silicone resin or phenolic resin; the inorganic binder includes a phosphate; the addition amount of the adhesive is 1-5 wt% of the total mass of the powder;
(3) after the granulated flaky powder and the granulated spherical powder are respectively and independently mixed with a release agent, sequentially filling the mixture into a die cavity according to the sequence of flaky powder, spherical powder and flaky powder, and pressing the mixture to prepare a magnetic core blank; the release agent comprises any one or the combination of at least two of zinc stearate, barium stearate, aluminum stearate or talcum powder; the addition amount of the release agent is 0.3-3 wt% of the total mass of the granulated flaky powder; the addition amount of the release agent is 0.3-3 wt% of the total mass of the granulated spherical powder; the mass ratio of the flaky powder to the spherical powder to the flaky powder sequentially filled into the die cavity is (0.5-1.5) to (5-9) to (0.5-3); the pressing pressure is 12-20T/cm 2 ；
(4) After the magnetic core blank is subjected to second annealing treatment, insulating paint is sprayed on the surface of the magnetic core blank to obtain the iron-based composite magnetic powder core; the second annealing treatment is carried out at N 2 Or H 2 Heating to 550-700 ℃ at a heating rate of 1.5-3 ℃/min in the atmosphere, and preserving heat for 1-3 h.
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| CN116705493B (en) * | 2023-08-08 | 2023-10-27 | 通友智能装备(江苏)有限公司 | Preparation method of organic coating resin of soft magnetic composite material |
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