CN107954706B - High-permeability soft magnetic ferrite material and preparation method thereof - Google Patents
High-permeability soft magnetic ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-permeability soft magnetic ferrite material which comprises a main component and auxiliary components, wherein the main component comprises the following components in percentage by weight: 50.8-53.8 mol% of ferric oxide, 25.2-27.2 mol% of manganese oxide and the balance of zinc oxide; the auxiliary component is TiO2、CaCO3、Bi2O3、Co2O3、Li2O、ZrO2、WO3the soft magnetic ferrite material with high magnetic permeability has initial magnetic permeability of more than 7000(25 ℃), initial magnetic permeability change of less than 13% in the range of-55-85 ℃, initial magnetic permeability of more than 6000 in the range of 10 kHz-400 kHz, cutoff frequency of more than 5MHz and hysteresis constant eta of more than 7000BLess than 0.2X 10‑6(-55 ℃ C. to 85 ℃ C., B1. gtoreq.1.5 mT, B2. gtoreq.3 mT), with a hysteresis constant η at 25 ℃ ofBLess than 0.18X 10‑6At a value of/mT. (B1 ═ 1.5mT, B2 ═ 3 mT). The method can be widely applied to communication transformers and network transformers which require small signal transmission distortion and strong high-frequency anti-interference capability.
Description
Technical Field
The invention relates to a soft magnetic ferrite material and a preparation method thereof, in particular to a high-permeability soft magnetic ferrite material and a preparation method thereof.
Background
The manganese zinc ferrite material with high magnetic conductivity is mainly used in the fields of electronic circuit broadband transformers, Integrated Services Digital Networks (ISDN), Local Area Networks (LAN), Wide Area Networks (WAN), background lighting and the like, pulse and coupling transformers, electromagnetic wave resistant filters and the like.
with the development of network technology, xDSL communication technology is widely used, and outdoor facilities of modern communication equipment, such as repeaters, microwave relay stations, submarine cables, equipment under optical cable deionized water, and the like, not only require high temperature resistance, but also require severe cold tolerance and reliable and stable operation of communication equipment, so that the inductance of the material is required to meet the requirement in a wide temperature range from-55 ℃ to +80 ℃ and even to 125 ℃, which requires the material to have very high magnetic permeability from low temperature to high temperatureB*CDF*DTC(ηBis a hysteresis constant, CDF is a core distortion factor, DTC is a transformer distortion factor), and the THD performance is directly proportional to eta on the premise that the shape of the core and the structure of the transformer are not changedBThus, therefore, it isthe smaller the THD requirement, then ηBthe smaller the difference according to etaBthe definition of (eta) B is delta tg delta/(mu e multiplied by delta B), and B is usually (1.5-3mT) in the industry, so that the basic performance in the industry can be less than 0.2 multiplied by 10-6At 25 ℃ but rarely at wide temperatures.
In addition, in the network transformer, in order to achieve the functions of signal coupling, high voltage isolation, impedance matching, electromagnetic interference suppression and the like, the ferrite material is required to have high magnetic permeability, maintain high magnetic permeability in a wide frequency range and have high cut-off frequency, the magnetic permeability of the material with 7000 magnetic permeability commonly used in the industry at present is only less than 50% at the frequency of 400kHz, the magnetic permeability is reduced very fast at high frequency, and the cut-off frequency of the material is basically 2.5MHz, so when the material is applied to the network transformer, the anti-electromagnetic interference capability of the material is general.
for example, patent document CN101183586A of Toyobo corporation discloses a soft magnetic ferrite material with high magnetic permeability and low THD and a preparation method thereof, and a magnetic core prepared by the method has the magnetic permeability of 7000-13000 at normal temperature and simultaneously has etaB<0.2×10-6The material has the characteristics of mT, has better low THD performance, but does not show the characteristic of high magnetic permeability in a wide range; for example, patent document CN101728048B of skaton corporation discloses a wide-temperature low-distortion manganese-zinc ferrite for broadband network transformer and a preparation method thereof, wherein the magnetic core prepared by the use method has the magnetic permeability of 5000-10000 and the relative loss factor<1.5×10-6coefficient of magnetic hysteresis etaB<0.8×10-6/mT(-40℃)、ηB<0.2×10-6/mT(25℃)、ηB<0.2×10-6The material has the advantages of low specific gravity loss and wide-temperature range and low THD (total harmonic distortion) characteristics at 85 ℃. The material has good low-THD performance at wide temperature, but does not show the characteristic of high magnetic permeability in a wide range, and even shows the wide frequency range; for example, patent document CN101863657A of Tombstone corporation discloses a wide temperature range high initial magnetthe Mn-Zn ferrite material with permeability is also widely applied to the communication field, has initial permeability of more than 5000 between minus 60 ℃ and 130 ℃, has the characteristics of wide temperature and high permeability but does not show the low THD characteristic, for example, Tiantong company patent document CN101894650A discloses a wide temperature and high permeability low distortion soft magnetic ferrite which has permeability of 6000 and permeability of more than 5000 between minus 55 ℃ and 85 ℃, and simultaneously has etaB<0.3×10-6At 25 ℃ C, the relative loss factor tan delta/. mu.i<10×10-6Curie temperature is more than 125 ℃, and the material has the characteristics of wide temperature range and high magnetic permeability, but eta of the materialBIs relatively large.
It is seen that compatibility with wide-temperature range high magnetic permeability and low THD characteristics is not yet established, and it is possible to improve frequency characteristics and cut-off frequency.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a high-permeability soft magnetic ferrite material with wide frequency, wide temperature range and low harmonic distortion.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a high-permeability soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component comprises the following components in percentage by weight: 50.8-53.8 mol% of ferric oxide, 25.2-27.2 mol% of manganese oxide and the balance of zinc oxide; the auxiliary component is TiO2、CaCO3、Bi2O3、Co2O3、Li2O、ZrO2、WO3At least five of them.
In the high-permeability soft magnetic ferrite material of the invention, multi-Fe is adopted2O3And less ZnO formula according to μ i ∞ Ms2/(2K1+3λsSigma), reducing magnetocrystalline anisotropy constant K1 and saturation magnetostriction coefficient lambdas, increasing saturation magnetization intensity Ms, reducing internal and external stress of the material, forming an accurate and uniform microstructure, and obtaining ferrite with high initial permeability.
According to the Snooker formula, the cutoff frequency fr is gamma.Ms/[ 3 pi.1 ], and Ms can be improved by increasing fr.
In addition, the introduced trace auxiliary components enter the interior of the crystal grains and the crystal boundary respectively, so that solid phase reaction can be promoted, the sintering temperature can be reduced, and the crystal grains can be controlled to grow in a certain size range (the size of the crystal grains is about 9-15 mu m).
Preferably, the mass ratio of each component of the auxiliary component to the total amount of the main component is: TiO 22400～600ppm、CaCO30～50ppm、Bi2O30～200ppm、Co2O3300～500ppm、Li2O 0～100ppm、ZrO20～400ppm、WO3200～400ppm。
Meanwhile, the invention also provides a preparation method of the high-permeability soft magnetic ferrite material, which comprises the following steps:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 0.9-1.2 mu m;
(2) presintering the slurry A obtained in the step (1) for 3-5 hours at the temperature of 850-950 ℃ to obtain powder A;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 0.9-1.1 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 2.8-3.2 g/cm3；
(5) And (4) sintering and forming the green body obtained in the step (4), wherein the sintering process is divided into three stages of heating, heat preservation and cooling, so that the high-permeability soft magnetic ferrite material is obtained.
Preferably, in the step (1), the weight ratio of the ball grinding material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: and 3, ball milling for 80-100 min.
More preferably, in the step (1), the diameter of the steel ball is 7 mm.
Preferably, in the powder A in the step (2), the synthesis degree of the spinel is 10-25%.
More preferably, in the powder a in the step (2), the degree of synthesis of spinel is 15%.
Preferably, in the step (3), the weight ratio of the ball milling material B to the deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: and 5, ball milling for 60-80 min.
More preferably, in the step (3), the diameter of the steel ball is 5 mm.
Preferably, in the step (3), the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 10, in the polyvinyl alcohol solution, the mass percent of polyvinyl alcohol is 8%.
Preferably, in the step (4), the adding amount of the zinc stearate is 2 per mill of the mass of the powder B.
Preferably, in the step (5), the sintering process is: heating in the air for 6-8 hours to increase the temperature from 25 ℃ to 1300-1365 ℃; the heat preservation stage is as follows: preserving the heat for 8 to 11 hours at the temperature of 1300 to 1365 ℃; the cooling stage is as follows: in an equilibrium atmosphere, the temperature is reduced from 1300 ℃ to 1365 ℃ to 25 ℃.
The preparation method of the manganese-zinc ferrite controls the synthesis rate of the pre-sintered powder spinel to be 10-25% when the powder is pre-sintered. Not only the problems of easy deformation and powder plasticity in the magnetic core sintering process are relieved, but also the electromagnetic property of the final magnetic core is improved; when the sintering in the step (5) is carried out, the heat preservation temperature is not more than 1365 ℃, the heat preservation time is 8-11 hours, the magnetic core can be fully reacted by adopting the low-temperature long-time sintering, the sizes of internal crystal grains are uniform, the generation of impurity phases is reduced, and meanwhile, the Fe in the ferrite is used as the equilibrium oxygen partial pressure phase diagram of the Mn-Zn ferrite of Morineav in the cooling section2+Determining the oxidation degree and the oxygen content of each temperature point by content (controlling the material peak point), drawing a basic temperature curve and a balanced atmosphere curve, and controlling the peak position of the material at low temperature to ensure that the low-temperature THD performance of the material reachesAnd (5) greatly improving.
More preferably, in the step (5), the oxygen content in the temperature rising stage is 1-21%, and the temperature reduction rate in the temperature reduction stage is 5-8 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
the soft magnetic ferrite material with high magnetic conductivity has excellent performances of wide frequency, wide temperature range, high magnetic conductivity, wide temperature range and low harmonic distortion, has the initial magnetic conductivity of more than 7000(25 ℃), the initial magnetic conductivity change of less than 13% in the range of-55-85 ℃, the initial magnetic conductivity of more than 6000 in the range of 10 kHz-400 kHz, the cut-off frequency of more than 5MHz, and the hysteresis constant eta of the materialBLess than 0.2X 10-6-mT (-55 ℃ to 85 ℃, B1 ═ 1.5mT, B2 ═ 3mT), where the hysteresis constant η at 25 ℃ [ [ eta ] ]BLess than 0.18X 10-6The material is characterized by being/mT (B1 is 1.5mT, B2 is 3mT), can be widely applied to communication transformers and network transformers which require small signal transmission distortion and strong high-frequency anti-interference capacity, and is a breakthrough of the current communication and network application materials.
Drawings
FIG. 1 is an SEM image of the inner grains of a sample ring obtained in example 2;
FIG. 2 is an SEM image of the inner grains of a sample ring obtained in the comparative example.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The 7 embodiments and the comparative components and the contents of the soft magnetic ferrite material with high magnetic permeability are shown in table 1:
TABLE 1 high-permeability soft magnetic ferrite materials with various compositions and contents
Example 1
The preparation method of the high-permeability soft magnetic ferrite material in the embodiment 1 of the invention comprises the following steps:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 0.9 mu m; wherein, the weight ratio of the ball milling material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: 3, ball milling time is 80min, and the diameter of the steel ball is 7 mm;
(2) presintering the slurry A obtained in the step (1) for 5 hours at the temperature of 850 ℃ to obtain powder A; in the powder A, the synthesis degree of spinel is 10%, and the weight ratio of the ball milling material B to deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: 5, ball milling time is 60min, and the diameter of the steel ball is 5 mm;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 0.9 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B, wherein the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 10, in the polyvinyl alcohol solution, the mass percent of polyvinyl alcohol is 8%;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 2.8g/cm3The addition amount of the zinc stearate is 2 per mill of the mass of the powder B;
(5) sintering the green body obtained in the step (4) on a specific curve: a temperature rising stage: heating at 25-1300 deg.c in air for 6 hr; and (3) a heat preservation stage: keeping the temperature at 1300 ℃ and 1 percent of oxygen content for 8 hours; and (3) cooling: and (3) cooling at 1300-25 ℃ in a balanced atmosphere at the rate of 5 ℃/min to obtain the high-permeability soft magnetic ferrite material.
Example 2
The preparation method of the high-permeability soft magnetic ferrite material in embodiment 2 of the invention comprises the following steps:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 1.2 mu m; wherein, the weight ratio of the ball milling material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: 3, ball milling time is 100min, and the diameter of the steel ball is 7 mm;
(2) presintering the slurry A obtained in the step (1) for 3 hours at the temperature of 950 ℃ to obtain powder A; in the powder A, the synthesis degree of spinel is 25%, and the weight ratio of the ball milling material B to deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: 5, ball milling time is 80min, and the diameter of the steel ball is 5 mm;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 1.1 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B, wherein the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 10, in the polyvinyl alcohol solution, the mass percent of polyvinyl alcohol is 8%;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 3.2g/cm3The addition amount of the zinc stearate is 2 per mill of the mass of the powder B;
(5) sintering the green body obtained in the step (4) on a specific curve: a temperature rising stage: heating in air at 25-1365 deg.c for 8 hr; and (3) a heat preservation stage: the temperature is 1365 ℃, the oxygen content is 21 percent, and the temperature is kept for 11 hours; and (3) cooling: and cooling at the temperature of 1365-25 ℃ in a balanced atmosphere at the speed of 8 ℃/min to obtain the high-permeability soft magnetic ferrite material.
Example 3
The preparation method of the high-permeability soft magnetic ferrite material in embodiment 3 of the invention comprises the following steps:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 1.1 mu m; wherein, the weight ratio of the ball milling material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: 3, ball milling time is 90min, and the diameter of the steel ball is 7 mm;
(2) presintering the slurry A obtained in the step (1) for 4 hours at the temperature of 900 ℃ to obtain powder A; in the powder A, the synthesis degree of spinel is 20%, and the weight ratio of the ball milling material B to deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: 5, ball milling time is 70min, and the diameter of the steel ball is 5 mm;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 1 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B, wherein the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 10, in the polyvinyl alcohol solution, the mass percent of polyvinyl alcohol is 8%;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 3g/cm3The addition amount of the zinc stearate is 2 per mill of the mass of the powder B;
(5) sintering the green body obtained in the step (4) on a specific curve: a temperature rising stage: heating at 25-1320 deg.c in air for 6 hr; and (3) a heat preservation stage: keeping the temperature at 1320 ℃ for 9 hours, wherein the oxygen content is 1 percent; and (3) cooling: and cooling at 1320-25 ℃ in a balanced atmosphere at the rate of 5 ℃/min to obtain the high-permeability soft magnetic ferrite material.
Example 4
The preparation method of the high-permeability soft magnetic ferrite material in the embodiment 4 of the invention is the same as the embodiment 3.
Example 5
The preparation method of the high-permeability soft magnetic ferrite material in the embodiment 5 of the invention is the same as the embodiment 3.
Example 6
The preparation method of the high-permeability soft magnetic ferrite material in the embodiment 6 of the invention is the same as the embodiment 3.
Example 7
The preparation method of the high-permeability soft magnetic ferrite material in the embodiment 7 of the invention is the same as the embodiment 3.
Example 8
The preparation method of the high-permeability soft magnetic ferrite material comprises the following steps:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 1.4 mu m; wherein, the weight ratio of the ball milling material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: 3, ball milling time is 90min, and the diameter of the steel ball is 7 mm;
(2) presintering the slurry A obtained in the step (1) for 4 hours at the temperature of 820 ℃ to obtain powder A; in the powder A, the synthesis degree of spinel is 30%, and the weight ratio of the ball grinding material B to deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: 5, ball milling time is 70min, and the diameter of the steel ball is 5 mm;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 1 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B, wherein the weight ratio of the polyvinyl alcohol solution to the slurry B is 1: 10, in the polyvinyl alcohol solution, the mass percent of polyvinyl alcohol is 8%;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 3g/cm3The addition amount of the zinc stearate is 2 per mill of the mass of the powder B;
(5) sintering the green body obtained in the step (4) on a specific curve: a temperature rising stage: heating at 25-1370 deg.c in air for 6 hr; and (3) a heat preservation stage: 1370 ℃, 4 percent of oxygen content and preserving heat for 4 hours; and (3) cooling: 1370-25 ℃, and cooling in a balanced atmosphere at the speed of 5 ℃/min to obtain the high-permeability soft magnetic ferrite material.
Example 9
In this embodiment, the performances of the soft magnetic ferrite materials with high magnetic permeability prepared in examples 1 to 7 and comparative example are analyzed, and the specific performances are shown in table 2:
TABLE 2 Performance data of the high permeability soft magnetic ferrite materials prepared in examples 1 to 7 and comparative example
As can be seen from the data in Table 2, the soft magnetic ferrite material with high magnetic permeability has excellent performance of wide frequency, wide temperature, high magnetic permeability, wide temperature and low harmonic distortion, has the initial magnetic permeability of more than 7000(25 ℃), initial magnetic permeability change of less than 13% in the range of-55-85 ℃, initial magnetic permeability of more than 6000 in the range of 10 kHz-400 kHz, cutoff frequency of more than 5MHz and material hysteresis constant eta of the materialBLess than 0.2X 10-6-mT (-55 ℃ to 85 ℃, B1 ═ 1.5mT, B2 ═ 3mT), where the hysteresis constant η at 25 ℃ [ [ eta ] ]BLess than 0.18X 10-6/mT(B1＝1.5mT，B2＝3mT)。
the particle size of slurry A in step 1) in the comparative example, the synthesis degree of spinel in step 2) and the temperature of raising, keeping and lowering the temperature in step 5) are different from those in example 2, the synthesis rate of spinel in the comparative example reaches 30%, the sintering is also different, although the main components are the same and the initial permeability is equivalent in the test performance, the initial permeability change rate, the cut-off frequency and the hysteresis constant η are the sameBAre inferior to those of examples 1 to 7. The internal microscopic grain structures of the two samples were observed to be different (FIGS. 1 and 2 are SEM images of the internal grains of the sample rings obtained in example 2 and comparative example). As can be seen from FIGS. 1 and 2, the grains of the sample ring obtained in example 2 were uniformly dense, and the average grain size was 9 to 15 μm, and the average grain size of the sample ring obtained in comparative example 1 was 15 to 20 μm.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A high-permeability soft magnetic ferrite material is characterized by comprising a main component and an auxiliary component, wherein the main component comprises the following components in percentage by weight: 50.8-53.8 mol% of ferric oxide, 25.2-27.2 mol% of manganese oxide and the balance of zinc oxide; the auxiliary component is TiO2、CaCO3、Bi2O3、Co2O3、Li2O、ZrO2、WO3at least five of the soft magnetic ferrite materials with high magnetic permeability have the following properties that the initial magnetic permeability is more than 7000 at 25 ℃, the initial magnetic permeability change is less than 13 percent within the range of-55 to 85 ℃, the initial magnetic permeability is more than 6000 within the range of 10kHz to 400kHz, the cut-off frequency is more than 5MHz, and the hysteresis constant η is more than 1.5mT at-55 to 85 ℃, B1 and B2 are 3mTBLess than 0.2X 10-6a hysteresis constant of η at 25 ℃ under the conditions of B1-1.5 mT and B2-3 mTBLess than 0.18X 10-6/mT。
2. The soft magnetic ferrite material with high magnetic permeability as claimed in claim 1, wherein the mass ratio of each component of the auxiliary component to the total amount of the main component is: TiO 22400～600ppm、CaCO30～50ppm、Bi2O30～200ppm、Co2O3300～500ppm、Li2O 0～100ppm、ZrO20～400ppm、WO3200～400ppm。
3. A method for preparing a high permeability soft magnetic ferrite material according to any one of claims 1 to 2, characterized by comprising the steps of:
(1) mixing the main components to obtain a ball grinding material A, and adding deionized water into the ball grinding material A for ball milling to obtain slurry A with the average particle size of 0.9-1.2 mu m;
(2) presintering the slurry A obtained in the step (1) for 3-5 hours at the temperature of 850-950 ℃ to obtain powder A; in the powder A, the synthesis degree of spinel is 10-25%;
(3) mixing the powder A obtained in the step (2) and the auxiliary components to obtain a ball grinding material B, adding deionized water into the ball grinding material B for ball grinding to obtain slurry B with the average particle size of 0.9-1.1 mu m, adding a polyvinyl alcohol solution into the slurry B, and stirring to obtain powder B;
(4) adding zinc stearate into the powder B obtained in the step (3), and then performing compression molding to obtain a green body, wherein the density of the green body is 2.8-3.2 g/cm3；
(5) Sintering and molding the green body obtained in the step (4), wherein the sintering process is divided into three stages of heating, heat preservation and cooling, so as to obtain the high-permeability soft magnetic ferrite material; the temperature rising stage comprises the following steps: heating in the air for 6-8 hours to increase the temperature from 25 ℃ to 1300-1365 ℃; the heat preservation stage is as follows: preserving the heat for 8-11 hours at the temperature of 1300-1365 ℃; the cooling stage is as follows: in an equilibrium atmosphere, reducing the temperature from 1300-1365 ℃ to 25 ℃; the oxygen content in the temperature rising stage is 1-21%, and the temperature reduction rate in the temperature reduction stage is 5-8 ℃/min.
4. The method for preparing a high-permeability soft magnetic ferrite material according to claim 3, wherein in the step (1), the weight ratio of the ball grinding material A to the deionized water is 1: 1.1, the weight ratio of the ball milling material A to the steel balls is 1: and 3, ball milling for 80-100 min.
5. The method for preparing a high-permeability soft magnetic ferrite material according to claim 3, wherein in the step (3), the weight ratio of the ball milling material B to the deionized water is 1: 1, the weight ratio of the ball milling material A to the steel balls is 1: and 5, ball milling for 60-80 min.
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| CN110577400A (en) * | 2019-09-30 | 2019-12-17 | 山东春光磁电科技有限公司 | Preparation method of manganese zinc ferrite with high magnetic conductivity |
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