CN113096949A - Preparation method of compact soft magnetic composite iron core material and soft magnetic composite material - Google Patents

Preparation method of compact soft magnetic composite iron core material and soft magnetic composite material Download PDF

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CN113096949A
CN113096949A CN202110371870.XA CN202110371870A CN113096949A CN 113096949 A CN113096949 A CN 113096949A CN 202110371870 A CN202110371870 A CN 202110371870A CN 113096949 A CN113096949 A CN 113096949A
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iron core
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core material
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CN113096949B (en
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马毅龙
邵斌
李超群
龙芝梅
栗克建
郭东林
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Chongqing University of Science and Technology
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust

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Abstract

The invention discloses a preparation method of a compact soft magnetic composite iron core material and the soft magnetic composite material, comprising the following steps: respectively preparing metal soft magnetic powder, soft magnetic ferrite powder and glass sintering aid powder, mixing the three powders to obtain compound powder, and carrying out vacuum hot pressing treatment on the compound powder to obtain the soft magnetic composite material, wherein the metal soft magnetic powder is at least one of FeCo powder, FeNi powder and FeSiAl powder, and the soft magnetic ferrite powder is nickel-zinc ferrite powder and/or manganese-zinc ferrite powder. The invention has the beneficial effects that: the composite iron core material with high density, high saturation magnetization, high magnetic conductivity and low magnetic loss can be prepared, and the application prospect is good.

Description

Preparation method of compact soft magnetic composite iron core material and soft magnetic composite material
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a preparation method of a compact soft magnetic composite iron core material and a soft magnetic composite material.
Background
Soft magnetic powder cores are widely used in electronic and electrical components such as inductors and current transformers as inductive filters, choke coils, and the like. With the 5G high-frequency era, electronic and electrical devices of communication, computers and new energy automobiles are continuously pursuing miniaturization, high efficiency and high frequency. This requires a higher permeability and lower magnetic losses of the soft magnetic powder core material, especially at high frequencies with high permeability and low losses. Ferrites and metal alloys are the two most important types of soft magnetic materials that make up the soft magnetic powder core. The most important advantage of soft magnetic ferrite is high resistivity, but the saturation magnetization is generally lower than 0.5T, which limits the upper limit of application and does not meet the development trend of miniaturization and high efficiency. The saturation magnetization of metallic soft magnetic materials is as high as 2.2T, but its resistivity is 10-6～10-4Omega m) ratio of soft magnetic ferrite (1-10)5Ω · m) is at least 4 orders of magnitude lower, which is the biggest obstacle to its application in the high frequency domain. At present, various methods attempt to perform insulating coating on metal soft magnet to obtain soft magnet composite materials with high magnetic permeability, high saturation magnetic induction and high resistivity, such as insulating coating by using oxides or organic matters, passivation or oxidation treatment, and the like, however, after coating, the soft magnet performance of the magnet is reduced due to the magnetic dilution effect. To reduce the influence of this magnetic dilution effect, an insulating coating may be performed with soft magnetic ferrite powder. At present, ferrite particles are prepared by a wet chemical method for insulation coating, and mechanical mixing is also used for insulation coating, but the uniform coating and the formation of a compact high-strength block material are still very difficult.
Disclosure of Invention
In view of this, the invention provides a method for preparing a compact soft magnetic composite iron core material, which can be used for preparing a metal soft magnetic/ferrite composite compact iron core material.
The technical scheme is as follows:
the preparation method of the compact soft magnetic composite iron core material is characterized by comprising the following steps of: step one, respectively preparing metal soft magnetic powder, soft magnetic ferrite powder and glass sintering aid powder;
step two, mixing the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder to obtain compound powder;
step three, carrying out vacuum hot pressing treatment on the compound powder to obtain a soft magnetic composite material;
the metal soft magnetic powder is one of FeCo powder, FeNi powder and FeSiAl powder;
the soft magnetic ferrite powder is nickel-zinc ferrite powder or manganese-zinc ferrite powder.
Preferably, the content of the glass sintering aid powder in the compound powder is 0.2-5% by mass, the content of the soft magnetic ferrite powder is 0.5-10% by mass, and the balance is the metal soft magnetic powder.
Preferably, the specific process in the second step is to perform ball milling on the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder, add tetraethoxysilane and absolute ethyl alcohol as a protective medium, perform vacuum drying, and further perform grinding in an inert atmosphere to obtain the compound powder.
Preferably, in the second step, the amount of the tetraethoxysilane is 0.5 to 2.5 wt.% of the total mass of the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder.
Preferably, in the second step, the ball-material ratio is 10:1, the ball milling rotation speed is 100-.
Preferably, in the third step, the compound powder is loaded into a pressing mold, and the pressing mold is placed into a hot pressing furnace for vacuum hot pressing;
the hot pressing treatment is carried out in two sections: firstly, the temperature is maintained for 1-5min under the conditions of 600-650 ℃ and 300-500MPa, then the temperature is reduced to 450-550 ℃ and the temperature is maintained for 5-10min under the conditions of 30-50 MPa.
Preferably, in the first step, the metallic soft magnetic powder with the particle size of 10-100 μm is taken and flattened for later use, and the flattening treatment is wet ball milling.
Preferably, in the first step, the ball-to-material ratio of the wet ball milling is 5:1-20:1, the ball milling rotation speed is 50-400rpm, the ball milling time is 4-40h, and the ball milling medium is selected from absolute ethyl alcohol, isopropanol, glycerol or n-heptane.
Preferably, the glass sintering aid powder is 48.7Li selected from the following components2O-36.4B2O3-14.9SiO2(LBS)、20Li2O-30ZnO-50B2O3(LZB)、30Li2O-10MgO-60B2O3(LMB)、52.45Li2O-31.06B2O3-11.99SiO2-2.25CaO-2.25Al2O3(LBSCA)。
The second purpose of the present invention is to provide a soft magnetic composite material. The technical scheme is as follows:
the soft magnetic composite material is characterized by being prepared by adopting the preparation method.
Drawings
FIG. 1 is a powder particle morphology of the soft metal powder after ball milling treatment in example 1;
FIG. 2 is a static hysteresis chart of a sample prepared in example 1;
FIG. 3 is the morphology of the powder particles of the soft metal powder after ball milling treatment in example 3;
FIG. 4 is a static hysteresis chart of a sample prepared in example 3.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
A preparation method of a compact soft magnetic composite iron core material comprises the following steps:
step one, respectively preparing metal soft magnetic powder, soft magnetic ferrite powder and glass sintering aid powder;
the metal soft magnetic powder is one of FeCo powder, FeNi powder and FeSiAl powder. Flattening treatment is carried out on the atomized metal soft magnetic powder with the particle size of 10-100 mu m, for example, wet ball milling can be adopted, the ball-material ratio of the wet ball milling is 5:1-20:1, the ball milling rotating speed is 50-400rpm, the ball milling time is 4-40h, and the ball milling medium is selected from absolute ethyl alcohol, isopropanol, glycerol or n-heptane.
The soft magnetic ferrite powder is nickel-zinc ferrite powder or nano-particles or micro-particles of manganese-zinc ferrite powder.
The preparation process of the nickel-zinc ferrite powder comprises the following steps: adding a proper amount of FeCl into deionized water according to the atomic ratio of metal elements in the nickel-zinc ferrite compound3·6H2O、ZnCl2·6H2O、NiCl2·6H2O, and a dispersant, and stirred for 30min to dissolve it. The dispersant may be polyethylene glycol in an amount of 3 wt.% of the total mass of the metal compound. Then adding alkali solution with certain concentration as precipitant into the mixed solution at the speed of 4ml/min while stirring to maintain the pH value of the solution at 9.5-10, wherein the alkali solution can be NaOH solution. After the reaction is completed, the mixture is placed for 8 to 10 hours, washed by deionized water and dried in a drying oven for 24 hours. And then, grinding the sample, and carrying out sintering treatment in a tube furnace at the temperature of 600-800 ℃, and keeping the temperature for 1-2h to obtain the nickel-zinc ferrite powder.
The preparation of the manganese-zinc ferrite powder is the same as that of the nickel-zinc ferrite powder, and the specific process comprises the following steps: adding a proper amount of FeCl into deionized water according to the atomic ratio of metal elements in the manganese-zinc ferrite compound3·6H2O、ZnCl2·6H2O、MnCl2·4H2O, and 3 wt.% of polyethylene glycol, stirring for 30min, and adding a NaOH solution with a concentration of 4ml/min into the mixed solution while stirring to maintain the pH of the solution at 9.5-10. After the reaction is completed, the mixture is placed for 8 to 10 hours, washed by deionized water and dried in a drying oven for 24 hours. And then, grinding the sample, and sintering in a tube furnace at the temperature of 1100-1200 ℃, and keeping the temperature for 1-2h to obtain the manganese-zinc ferrite powder.
The glass sintering aid powder is selected from 48.7Li2O-36.4B2O3-14.9SiO2(LBS glass frit), 20Li2O-30ZnO-50B2O3(LZB glass powder), 30Li2O-10MgO-60B2O3(LMB glass frit), 52.45Li2O-31.06B2O3-11.99SiO2-2.25CaO-2.25Al2O3(LBSCA glass powder), and the proportion of each component compound in the four glass powders is molar ratio.
According to the composition of the above four glass powders, the starting material is selected from Li2CO3、SiO2、H3BO3，ZnO、(MgCO3)4Mg(OH)2·5H2O、CaO、Al2O3. The process for preparing the glass powder by adopting the melting method comprises the following steps: weighing the raw materials according to the atomic ratio of the component compounds of the four glass powders respectively, and performing ball milling treatment by using a ball mill for 4-6h by using absolute ethyl alcohol as a protective solvent. And then, drying the ball-milled slurry, heating to 900-950 ℃, preserving the heat for 1h, and then performing water quenching. And drying the obtained glass fragments, and grinding, wet ball milling for 20-40h and drying to obtain the glass powder for the test.
Step two, mixing the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder to obtain compound powder;
the content of the glass sintering aid powder in the mixed powder is 0.2-5% by mass, the content of the soft magnetic ferrite powder is 0.5-10% by mass, and the balance is the metal soft magnetic powder.
The mixing process is as follows: firstly, taking metal soft magnetic powder, glass sintering aid powder and soft magnetic ferrite powder according to the mass ratio for ball milling, wherein the ball-material ratio is 10:1, the ball milling rotation speed is 100-150rpm, and the ball milling time is 6-10 h; simultaneously adding tetraethoxysilane, wherein absolute ethyl alcohol is taken as a protective medium, and the dosage of the tetraethoxysilane is 0.5-2.5 wt.% of the total mass of the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder; then vacuum drying is carried out; and adding zinc stearate into the glove box, further grinding the mixture in an inert atmosphere, and pulverizing the dried and agglomerated mixed powder to obtain the compound powder, wherein the addition amount of the zinc stearate is 0.3 to 1 wt.% of the total mass of the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder.
Step three, filling the compound powder into a pressing mold, putting the pressing mold into a hot pressing furnace for vacuum hot pressing treatment, wherein the hot pressing treatment is carried out in two sections: the temperature is maintained for 1-5min under the conditions of 650 ℃ at 600-. And (3) after sintering, carrying out heat treatment on the sample at the temperature of 400-550 ℃ in an inert atmosphere, and preserving the heat for 1-4h to further remove the internal stress to obtain the soft magnetic composite material.
The detailed preparation processes of several typical soft magnetic composite iron core materials are as in examples 1-3.
Example 1
Step one, taking metal soft magnetic powder FeCo atomized powder, wherein the mass ratio of two elements in the FeCo atomized powder is 1:1, and the particle size of the powder is 30-50 mu m; the flattening treatment process comprises the steps of putting 10g of FeCo powder into a ball mill, adding absolute ethyl alcohol and grinding balls, wherein the ball-material ratio is 10:1, the ball milling rotation speed is 200rpm, and the time is 20 hours for later use. Fig. 1 shows the morphology of the powder particles after ball milling.
According to Mn0.6Zn0.4Fe2O4Adding a proper amount of FeCl into deionized water according to the atomic ratio of metal elements Mn, Zn and Fe in the compound3·6H2O、ZnCl2·6H2O、MnCl2·4H2O and 3 wt.% of polyethylene glycol, stirring for 30-60min, and adding NaOH precipitant with a concentration of 4ml/min while stirring to maintain the pH of the solution at 9.5-10. After the reaction is completed, the mixture is placed for 10 hours, washed by deionized water and then dried in a drying oven for 24 hours at the temperature of 80 ℃. The sample was then ground for 10min and placed in a tube furnace for sintering. And (3) during sintering, adopting argon protection, keeping the temperature at 1150 ℃ for 2 h. Cooling to obtain manganese-zinc ferrite powder for later use.
LBSCA glass powder is prepared by adopting a melting method. The initial raw material is Li2CO3、H3BO3、SiO2、CaO、Al2O3. Weighing 5g of raw materials according to the proportion of component compounds of the LBS CA glass powder, performing ball milling treatment in a ball mill, adding a proper amount of absolute ethyl alcohol as a protective solvent, and performing ball milling for 4 hours. And then, drying the ball-milled slurry, heating to 950 ℃, preserving the heat for 1h, and then performing water quenching. Drying the obtained glass fragments, grinding, sieving with 100 mesh sieve, collecting powder, placing into a ball mill, adding appropriate amount of anhydrous ethanol and grinding balls at a ball-to-material ratio of 10:1, and making into ballThe milling speed is 350rpm, and the milling time is 20 h. And then collecting a sample, and drying to obtain glass sintering aid powder for later use.
And step two, mixing the FeCo metal soft magnetic powder subjected to the flakiness treatment with LBSCA and manganese zinc ferrite powder, wherein the mass ratio of the LBSCA is 2%, and the mass ratio of the manganese zinc ferrite powder is 6%. Weighing 8g of mixed powder, putting the mixed powder into a rolling ball mill, continuously ball-milling, and simultaneously adding 2% by mass of tetraethoxysilane and a proper amount of absolute ethyl alcohol, wherein the ball-material ratio is 10:1, the ball-milling rotating speed is 150rpm, and the ball-milling time is 6 hours. And then taking out a sample, carrying out vacuum drying, adding zinc stearate, wherein the addition amount of the zinc stearate is 0.3 percent of the total mass of the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder, further grinding in a glove box, and then filling in an alloy die.
Step three, putting the mould into a hot pressing furnace for vacuum hot pressing treatment, wherein the sintering temperature is 650 ℃, the heat preservation time is 2min, and the pressure is 300 MPa; then the temperature is reduced to 450 ℃, the temperature is preserved for 5min, and the pressure is 30 MPa. And cooling the mold, and demolding to obtain the compact soft magnetic composite block. The sample was then heat treated in a nitrogen atmosphere and held at 450 ℃ for 2h to further remove internal stresses.
The density of the sample measured by the Archimedes method was 7.95g/cm3The saturation magnetization of the sample measured by the vibrating sample magnetometer was 179.8emu/g, and the static hysteresis loop is shown in FIG. 2. The permeability of the sample was measured by a soft magnetic material dynamic measuring device and found to have a good frequency stability of 56 at 1 kHz.
Example 2
Step one, taking metal soft magnetic powder FeCo atomized powder, wherein the mass ratio of two elements in the FeCo atomized powder is 1:1, and the particle size of the powder is 30-50 mu m; the flattening treatment process comprises the steps of putting 10g of FeCo powder into a ball mill, adding absolute ethyl alcohol and a grinding ball, wherein the ball-material ratio is 15:1, the ball milling rotation speed is 150rpm, and the time is 8h for later use.
According to the compound Ni0.6Zn0.4Fe2O4Adding a proper amount of FeCl into deionized water according to the atomic ratio of Ni, Zn and Fe3·6H2O、ZnCl2·6H2O、NiCl2·6H2O, and 3 wt.% polyethylene glycol, stirring for 60min, and adding NaOH precipitant at a rate of 4ml/min while stirring to maintain the pH of the solution at 9.5-10. After the reaction is completed, the mixture is placed for 10 hours, then is repeatedly washed by deionized water for three times, and is dried in a drying oven for 24 hours at the drying temperature of 80 ℃. The sample was then ground for 10min and placed in a tube furnace for sintering. And (3) during sintering, adopting argon protection, keeping the temperature at 800 ℃ for 1 h. Cooling to obtain nickel-zinc ferrite powder for later use.
Preparation of 48.7Li by melting method2O-36.4B2O3-14.9SiO2(LBS) glass powder, the proportion of each component is atomic ratio. The initial raw material is Li2CO3、H3BO3、SiO2. Weighing 5g of raw materials according to a corresponding proportion, carrying out ball milling treatment in a ball mill, adding a proper amount of absolute ethyl alcohol as a protective solvent, adding 30g of grinding balls, and carrying out ball milling for 6 hours at a ball milling rotation speed of 350 rpm. And then, drying the ball-milled slurry, heating to 900 ℃, preserving the heat for 1h, and then performing water quenching. Drying the obtained glass fragments, grinding, sieving by a 100-mesh sieve, collecting powder, putting into a ball mill, and adding a proper amount of absolute ethyl alcohol and grinding balls, wherein the ball-material ratio is 10:1, the rotating speed is 350rpm, and the ball milling time is 30 hours. And then collecting a sample, and drying to obtain glass sintering aid powder for later use.
And step two, mixing the FeCo metal soft magnetic powder subjected to the flakiness treatment with LBS and nickel-zinc ferrite powder, wherein the LBS accounts for 4% by mass, and the nickel-zinc ferrite powder accounts for 8% by mass. Weighing 8g of mixed powder, putting the mixed powder into a rolling ball mill, continuously ball-milling, and simultaneously adding 1.5% of tetraethoxysilane and a proper amount of absolute ethyl alcohol in a ball-material ratio of 10:1, wherein the ball-milling rotating speed is 150rpm, and the ball-milling time is 6 hours. And then taking out a sample, carrying out vacuum drying, adding zinc stearate, wherein the addition amount of the zinc stearate is 0.5 percent of the total mass of the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder, further grinding in a glove box, and then filling in an alloy die.
Step three, putting the mould into a hot pressing furnace for vacuum hot pressing treatment, wherein the sintering temperature is 600 ℃, the heat preservation time is 1min, and the pressure is 500 MPa; then the temperature is reduced to 450 ℃, the temperature is preserved for 10min, and the pressure is 30 MPa. And cooling the mold, and demolding to obtain the compact soft magnetic composite block. The sample was then heat treated under nitrogen, held at 500 ℃ for 1h and furnace cooled.
The density was found to be 7.72g/cm3The saturation magnetization is 170.3emu/g, and the magnetic permeability has better frequency stability along with the increase of frequency.
Example 3
Step one, taking Fe85Si9.5Al5.5 atomized powder as metal soft magnetic powder, wherein the proportion of each element in FeSiAl is mass ratio, and the particle size of the powder is 10-50 mu m. The Fe85Si9.5Al5.5 powder is subjected to flattening treatment, namely wet ball milling, the ball-feed ratio is 12:1, the rotating speed is 50rpm, the time is 40h, and the ball milling medium is absolute ethyl alcohol. The morphology of the Fe85Si9.5Al5.5 powder after the flattening treatment is shown in figure 3.
According to the compound Mn0.6Zn0.4Fe2O4Adding a proper amount of FeCl into deionized water according to the atomic ratio of Mn, Zn and Fe3·6H2O、ZnCl2·6H2O、MnCl2·4H2O and 3 wt.% of polyethylene glycol, stirring for 30-60min, and adding NaOH precipitant with a concentration of 4ml/min while stirring to maintain the pH of the solution at 9.5-10. After the reaction is completed, the mixture is placed for 10 hours, washed by deionized water and then dried in a drying oven for 24 hours at the temperature of 80 ℃. The sample was then ground for 10min and placed in a tube furnace for sintering. And (3) during sintering, adopting argon protection, keeping the temperature at 1150 ℃ for 2 h. Cooling to obtain manganese-zinc ferrite powder.
52.45Li preparation by melting method2O-31.06B2O3-11.99SiO2-2.25CaO-2.25Al2O3(LBSCA) glass powder, the proportion of each component is atomic ratio. The initial raw material is Li2CO3、H3BO3、SiO2、CaO、Al2O3. Weighing 5g of raw materials according to the corresponding proportion of the four kinds of glass, carrying out ball milling treatment in a ball mill,adding a proper amount of absolute ethyl alcohol as a protective solvent, and ball-milling for 4 hours. And then, drying the ball-milled slurry, heating to 950 ℃, preserving the heat for 1h, and then performing water quenching. Drying the obtained glass fragments, grinding, sieving by a 100-mesh sieve, collecting powder, putting into a ball mill, and adding a proper amount of absolute ethyl alcohol and grinding balls, wherein the ball-material ratio is 10:1, the rotating speed is 350rpm, and the ball milling time is 20 hours. And then collecting a sample, and drying to obtain glass sintering aid powder for later use.
And step two, mixing the FeSiAl metal soft magnetic powder subjected to the flakiness treatment with LBSCA and manganese zinc ferrite powder, wherein the LBSCA accounts for 2.5% by mass, and the manganese zinc ferrite powder accounts for 5% by mass. Weighing 8g of mixed powder, putting the mixed powder into a rolling ball mill, continuously ball-milling, and simultaneously adding 2% by mass of tetraethoxysilane and a proper amount of absolute ethyl alcohol, wherein the ball-material ratio is 10:1, the ball-milling rotating speed is 150rpm, and the ball-milling time is 6 hours. And then taking out a sample, carrying out vacuum drying, adding zinc stearate, wherein the addition amount of the zinc stearate is 0.5 percent of the total mass of the metal soft magnetic powder, the glass sintering aid powder and the soft magnetic ferrite powder, further grinding in a glove box, and then filling in an alloy die.
Step three, putting the mould into a hot pressing furnace for vacuum hot pressing treatment, wherein the sintering temperature is 650 ℃, the heat preservation time is 1min, and the pressure is 500 MPa; then the temperature is reduced to 450 ℃, the temperature is preserved for 10min, and the pressure is 30 MPa. And cooling the mold, and demolding to obtain the compact soft magnetic composite block. And then, carrying out heat treatment on the sample in a nitrogen atmosphere, keeping the temperature at 500 ℃ for 1h, and cooling along with the furnace.
The density was found to be 6.05g/cm3The saturation magnetization was 78.2emu/g, and the static hysteresis chart is shown in FIG. 4. The sample was measured to have a permeability of 84.6(100kHz) and a magnetic loss of 51.6W/kg (f 100kHz, Bm 100 mT).
Comparative example 1
The materials and process as in example 2 were used except that a magnet was prepared using only the flaking-treated FeCo metal soft magnetic powder and nickel zinc ferrite powder without adding the glass sintering aid LBS. The magnet density of the prepared sample is about 6.5g/cm through detection3And is easily pulverized and broken, which cannot be accurately achievedThe magnetic properties were determined.
The method of the invention has the following advantages: (1) the glass sintering aid is used, has the effects that the glass sintering aid is in a liquid state in the sintering process due to low melting point, plays a role in lubrication, contributes to densification and uniform distribution of mixed powder, increases the density, can also increase the resistance and is favorable for improving the mechanical strength; (2) in the first step, the metal soft magnetic powder is subjected to flattening treatment, so that the resistivity of the powder can be improved, and the high-frequency performance is improved; (3) in the process of ball milling of the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder, the tetraethoxysilane is added, so that the raw material powder can be coated, and the raw material powder is uniformly mixed and sintered to cover the surface of the powder, thereby playing a role in improving the resistivity.
Compared with the prior art, the invention has the beneficial effects that: the composite iron core material with high density, high saturation magnetization, high magnetic conductivity and low magnetic loss can be prepared, and the application prospect is good.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.

Claims (10)

1. A preparation method of a compact soft magnetic composite iron core material is characterized by comprising the following steps: step one, respectively preparing metal soft magnetic powder, soft magnetic ferrite powder and glass sintering aid powder;
step two, mixing the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder to obtain compound powder;
step three, carrying out vacuum hot pressing treatment on the compound powder to obtain a soft magnetic composite material;
the metal soft magnetic powder is one of FeCo powder, FeNi powder and FeSiAl powder;
the soft magnetic ferrite powder is nickel-zinc ferrite powder or manganese-zinc ferrite powder.
2. The method for preparing a dense soft magnetic composite iron core material according to claim 1, wherein: the content of the glass sintering aid powder in the mixed powder is 0.2-5% by mass, the content of the soft magnetic ferrite powder is 0.5-10% by mass, and the balance is the metal soft magnetic powder.
3. The method for preparing a dense soft magnetic composite iron core material according to claim 2, wherein: and the specific process of the second step is that the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder are subjected to ball milling, simultaneously ethyl orthosilicate and absolute ethyl alcohol are added as protective media, then the mixture is subjected to vacuum drying, and further grinding is carried out under inert atmosphere, so that the compound powder is obtained.
4. The method for preparing a dense soft magnetic composite iron core material according to claim 3, wherein: in the second step, the dosage of the tetraethoxysilane is 0.5-2.5 wt% of the total mass of the metal soft magnetic powder, the soft magnetic ferrite powder and the glass sintering aid powder.
5. The method for preparing a dense soft magnetic composite iron core material according to claim 3, wherein: in the second step, the ball-material ratio is 10:1, the ball milling rotation speed is 100-.
6. The method for preparing a dense soft magnetic composite iron core material according to claim 1, wherein: in the third step, the compound powder is filled into a pressing mold, and the pressing mold is placed into a hot pressing furnace for vacuum hot pressing treatment;
the hot pressing treatment is carried out in two sections: firstly, the temperature is maintained for 1-5min under the conditions of 600-650 ℃ and 300-500MPa, then the temperature is reduced to 450-550 ℃ and the temperature is maintained for 5-10min under the conditions of 30-50 MPa.
7. The method for preparing a dense soft magnetic composite iron core material according to claim 1, wherein: in the first step, the metal soft magnetic powder with the particle size of 10-100 microns is taken and flattened for later use, and the flattening treatment is wet ball milling.
8. The method for preparing a dense soft magnetic composite core material according to claim 7, wherein: in the first step, the ball-material ratio of the wet ball milling is 5:1-20:1, the ball milling rotation speed is 50-400rpm, the ball milling time is 4-40h, and the ball milling medium is selected from absolute ethyl alcohol, isopropanol, glycerol or n-heptane.
9. The method for preparing a dense soft magnetic composite iron core material according to claim 1, wherein: the glass sintering aid powder is selected from 48.7Li2O-36.4B2O3-14.9SiO2(LBS)、20Li2O-30ZnO-50B2O3(LZB)、30Li2O-10MgO-60B2O3(LMB)、52.45Li2O-31.06B2O3-11.99SiO2-2.25CaO-2.25Al2O3(LBSCA)。
10. A soft magnetic composite material, characterized by being prepared by the preparation method of any one of claims 1 to 9.
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