CN111138179A - Broadband high-impedance manganese-zinc ferrite material and preparation method thereof - Google Patents
Broadband high-impedance manganese-zinc ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a broadband high-impedance manganese-zinc ferrite material which comprises a main component and an auxiliary component, wherein the main component comprises Fe2O3ZnO and Mn3O4(in MnO); the auxiliary component is selected from SiO2、CaCO3、Nb2O5、Co2O3、TiO2At least one of (1). The manganese-zinc ferrite material has direct current resistivity of more than 3000 omega-m, Curie temperature of more than 210 ℃, normal-temperature saturation magnetic induction intensity of more than 440mT, initial magnetic conductivity of more than 650, and high impedance characteristic in a wide frequency range of 0.01 MHz-700 MHz.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a manganese zinc ferrite material which has the characteristics of high direct current resistivity, high Curie temperature and high saturation magnetic induction density and has high impedance in a wide frequency range and a manufacturing method thereof.
Background
With the reduction of signal delay and the increase of signal frequency, the problem of electromagnetic interference of electronic products is more and more emphasized, and an effective way to solve or reduce electromagnetic pollution and improve the capability of electronic equipment to resist electromagnetic interference is to adopt an electromagnetic compatibility design in which a large amount of materials for resisting electromagnetic interference (EMI) are required.
Commonly used EMI resistant materials are MnZn ferrite and NiZn ferrite materials, which have relatively low resistivity compared to NiZn ferrite but if Fe is in the main formulation2O3The mol percentage content is not more than 50 percent, so that Fe can be inhibited2+Ions are generated, so that the resistivity is improved, and the use frequency is greatly improved.
In the MnZn ferrite material with impedance characteristics related to the prior art, generally, a main formula adopts ZnO with a high proportion, so that although the low-frequency impedance is favorably improved, the Curie temperature is reduced, or components such as CuO, NiO and the like are added in the main formula, the use frequency is improved, but the low-frequency impedance is low, and the cost is high. For example, the invention patent of chinese publication No. CN101857426A provides a broadband high-impedance MnZn ferrite material, which adopts a lean iron formula, in which the ZnO proportion in the main formula is 16 mol% to 21 mol%, and a higher ZnO proportion is beneficial to improving low-frequency impedance, but the curie temperature is only 115 ℃, and cannot be used in working environments with high temperature requirements, such as 5G communication, automotive electronics, and the like. The invention patent of China with the publication number of CN104261812A provides an EMI resistant ferrite material, which adopts a lean iron formula, has the resistivity of only 100 omega M, and has excellent impedance characteristic only in the frequency range of 1-100M. The invention patent of China with the publication number of CN101805173A provides a MnZn ferrite material with a lean iron formula, which adopts the lean iron formula, and ZrO must be added as an auxiliary component2And SnO2The resistivity is only 50 omega m, the low loss characteristic is opposite to the high impedance direction. In summary, the disclosed iron-deficient MnZn ferrite material has the main formula which improves the low-frequency impedance by high proportion of ZnO, or improves the use frequency by adding components such as CuO, NiO and the like as auxiliary components, but can cause low Curie temperature, low-frequency impedance and high cost.
Therefore, the ferrite material composition and the preparation method in the prior art are difficult to obtain the MnZn ferrite material which has high direct current resistivity, high Curie temperature, high saturation magnetic induction density and high impedance characteristic in a wide frequency range in a coordinated mode, so that the use requirement in the specific field is difficult to meet.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
a broadband high-impedance MnZn-Mn-Zn ferrite material comprises a main component and an auxiliary component, wherein the main component comprises Fe2O3ZnO and Mn3O4(ii) a And the auxiliary component is selected from SiO2、CaCO3、Nb2O5、Co2O3、TiO2At least one of (1). The direct current resistivity of the material is more than 3000 omega.m, the Curie temperature is more than 210 ℃, the normal temperature saturation magnetic induction intensity is more than 440mT, the initial magnetic conductivity is more than 650, and the material also has the broadband range of 0.01 MHz-700 MHz and has high impedance characteristic, wherein 1MHz
Impedances of 25MHz, 100MHz and 500MHz are greater than 3 Ω, 35 Ω, 125 Ω and 1000 Ω, respectively.
Further, the main component comprises 46.0-50.0 mol% of Fe calculated by respective oxides2O3And 4.0-8.9 mol% ZnO, the balance being Mn3O4(in MnO). Fe in the main formula of the invention2O3The mol percentage content is not more than 50 percent, and the Fe is effectively inhibited2+Ion generation, reducing Fe2+～Fe3+The resistivity of the material is improved by the electron transfer between the two, so that the use frequency of the material is greatly improved. The ZnO mole percentage content in the main formula is lower, so that the characteristics of high Curie temperature and high saturation magnetic induction intensity are obtained.
Further, the auxiliary component is added in an amount ranging from SiO based on the total weight of the main component2：0.002－0.012wt％、CaCO3：0.01－0.10wt％、Nb2O5：0.01－0.05wt％、Co2O3：0.01－1.20wt％、TiO2: 0.01-0.30 wt%. Of the auxiliary components of the invention, CaCO3Has effects of optimizing grain boundary, refining crystal grain, and improving material loss, wherein Ca2+Segregation to grain boundariesSo that the crystal grains are uniform and the crystal boundary is obvious. During sintering of ferrites, CaCO3With SiO2Reaction takes place, Ca2+And Si4+Diffusing to the grain boundary to form CaSiO with the thickness of 1-10 nm on the grain boundary layer3The insulating layer improves the resistivity of the material and plays a role in improving the broadband impedance characteristic; nb2O5The material exists in a crystal boundary, plays a role in preventing the growth of crystal grains, and has a fine and uniform microstructure due to the inhibition effect of the growth of the crystal grains, so that the crystal grains become uniform and compact, the porosity is reduced, the resistance of domain wall displacement and magnetization vector rotation is reduced, the initial magnetic conductivity of the material is not reduced or increased, and the improvement of the impedance of a broadband is facilitated; co2O3And TiO2The magnetic permeability temperature characteristic is improved, the contribution of the magnetic permeability temperature characteristic to the K1 value is improved, the initial magnetic permeability at normal temperature is improved, and the impedance characteristic in a wide frequency range is improved. Addition of Co2O3Can generate CoFe with high K1 positive value2O4Due to Co2+Has a large K1 value and comprehensively utilizes Fe2+And Co2+For the compensation effect of K1, K1 value has a plurality of compensation points, and the corresponding permeability temperature curve is flatter in a wider temperature range, so that good wide-temperature characteristics can be obtained. Ti4+Tends to occupy B site and forces part of magnetic ion Fe3+Transfer from the B position to the A position, resulting in Fe in the B position3+/Fe2+The probability of inter-electron transition is reduced, and the resistivity of the material is improved.
The invention also provides a manufacturing method of the broadband high-impedance MnZn manganese zinc ferrite material, which comprises the following steps of:
1) mixing Fe2O3、Mn3O4And ZnO are evenly mixed and dried according to the proportion;
2) presintering the powder obtained in the step 1) at the temperature of 800-950 ℃ for 2-3 hours, and then naturally cooling;
3) adding the at least one auxiliary component into the powder obtained in the step 2) according to the proportion, and then adding deionized water accounting for 40-60 wt% of the total weight of the main components and a dispersing agent accounting for 0.5-3 wt% of the total weight of the main components for ball milling;
4) adding 5-8 wt% of aqueous solution of organic binder into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
5) pressing the granular material obtained in the step 4) into a green body sample;
6) sintering the green body sample obtained in the step 5) at the sintering temperature of 1260-1380 ℃, preserving the heat for 4-8 hours at the sintering temperature, then cooling slowly and cooling to 180 ℃, and discharging. Wherein the oxygen partial pressure of the heat preservation section is 2-10%, and the equilibrium oxygen partial pressure is adopted in the temperature reduction process.
In the method provided by the invention, the dispersant used in step 3) can be a dispersant commonly used in the art, for example, the dispersant can be selected from polypropionic acid, gluconic acid, citric acid and the like; the ball milling time is 20-30 minutes, and the particle size of the powder after ball milling is less than 1.3 m.
In the method provided by the invention, the organic binder in the step 4) is polyvinyl alcohol.
In the method provided by the invention, the green compact prepared by pressing in the step 5) has the density of 3.0 +/-0.2 g/cm 3.
In the method provided by the invention, in the step 6), air sintering is adopted when the temperature is raised from normal temperature to high temperature, and a small amount of nitrogen is adopted for protection and temperature reduction in the temperature reduction section. The equilibrium oxygen partial pressure of the cooling section is calculated according to a formula, wherein a takes a value of 7-10, b takes a value of 13000-.
The sintering process of the preparation method adopts air sintering, and the cooling section adopts a method of reducing temperature by a small amount of nitrogen protection, thereby preparing the broadband high-impedance MnZn ferrite material with the direct current resistivity of more than 3000 omega.m, the Curie temperature of more than 210 ℃, the normal-temperature saturation magnetic induction intensity of more than 440mT, the initial permeability of more than 650 and the broadband high-impedance characteristic in the broadband range of 0.01MHz to 700MHz, wherein the impedance of 1MHz, 25MHz, 100MHz and 500MHz is respectively more than 3 omega, 35 omega, 125 omega and 1000 omega.
The invention has the beneficial effects that:
fe in the main formula of the invention2O3The mol percentage content does not exceed 50 percent, and the formulation is lowThe proportion of ZnO in mol percent and reasonable auxiliary components, thereby obtaining the MnZn ferrite with excellent comprehensive properties such as high Curie temperature, high saturation magnetic induction density characteristic and the like. The manganese-zinc ferrite material obtained by the composition and the preparation method has the characteristics of high direct current resistivity, high Curie temperature and high saturation magnetic induction intensity, and has high impedance in a wide frequency range. In addition, the broadband high-impedance MnZn ferrite material does not contain a high proportion of noble metals, is expensive, avoids the use of a raw material NiO with a higher price, has the characteristics of low cost and simple process, and can meet the good running of 5G communication, automobile electronics, EMI resistance and other electronic products, thereby better meeting the market demand.
Drawings
Fig. 1 is a graph of the impedance frequency of the present invention.
Detailed Description
Examples 1 to 4 and comparative example 1 are based on Fe2O3、Mn3O4And ZnO as a main component, and ferrite materials obtained by adding different amounts of the main components, mixing the materials in a ball mill for 0.5 hour, taking out and drying the materials. The obtained powder was preburnt at 900 ℃ for 2.5 hours in a box-type resistance furnace. And then putting the pre-sintered powder into a ball mill, and adding auxiliary components into the obtained powder based on the total weight of the main components: 0.008 wt% SiO20.02 wt% of CaCO30.30 wt% of Co2O3(ii) a Then adding deionized water accounting for 50 wt% of the total weight of the main components and a dispersing agent accounting for 1.5 wt% of the total weight of the main components, and performing ball milling. Ball milling the powder to average particle size of 1.0 +/-0.2 micron; based on the total weight of the powder after ball milling, 7 wt% of polyvinyl alcohol solution is added to the powder, mixed uniformly and granulated, and the granules are pressed into annular samples of OR 25X 8-15 mm. And finally, preserving the heat for 5 hours at 1350 ℃ in a bell jar furnace controlled by a computer program, then slowly cooling and cooling to 180 ℃ and discharging. Wherein the oxygen partial pressure of the heat preservation section is 5.0 percent, and the balanced oxygen partial pressure is adopted in the temperature reduction process.
TABLE 1
Note: indicates that the main component range is out of the preferred range of the present invention.
The data of the results of measuring electromagnetic physical properties of examples 1 to 4 and comparative example 1 are shown in Table 2 below.
TABLE 2
As can be seen from table 2: examples 1-4, which are consistent with the preferred ranges of the present invention, have higher curie temperatures, all above 210 ℃, initial permeability of greater than 650, resistivity of greater than 3000 Ω · m, and broadband high impedance characteristics. Comparative example 1, Fe in ferrite Material of conventional Main component2O3、
The ZnO content is beyond the limited range of the invention, the prepared material can not obtain the excellent broadband impedance characteristic of the invention, the resistivity of the material is only 6 omega m, the impedance falls to 2 omega at 25MHz, and the impedance characteristic does not exist at higher frequency; at the same time, the material of comparative example 1 also did not have a high curie temperature.
It can also be seen from fig. 1: the MnZn ferrite material has high impedance characteristic in a wide frequency range of 0.01 MHz-700 MHz, and can ensure the normal operation of devices in the wide frequency range.
Examples 5 to 11 and comparative examples 2 to 4 were carried out while fixing the main component at 47.8 mol% of Fe2O346.7 mol% Mn3O4 in terms of MnO and 5.5 mol% ZnO, to the powder obtained, auxiliary components were added, based on the total weight of the main component, see Table 3 below.
TABLE 3
Note: indicates that the auxiliary ingredient ranges are beyond the preferred ranges of the present invention.
The data of the results of measuring electromagnetic physical properties of examples 5 to 11 and comparative examples 2 to 4 are shown in Table 4 below.
TABLE 4
As can be seen from table 4: the auxiliary components of examples 5-11 are in the preferred range of the present invention, and have initial permeability of more than 650, resistivity of more than 3000 Ω · m, and broadband high-impedance characteristics. Comparative examples 2 to 4 show that the added auxiliary components out of the range of the present invention cause discontinuous grain growth and abnormal change in grain structure, and that the obtained material has low magnetic permeability and normal temperature saturation magnetic induction, poor low frequency impedance characteristics, and low comprehensive properties.
As can be seen from tables 2 and 4, the MnZn ferrite in the content range of the main component and the auxiliary component of the present invention has a DC resistivity of more than 3000 Ω & m, a Curie temperature of more than 210 ℃, a saturation induction at room temperature of more than 440mT, and an initial permeability of more than 650, and also has a high impedance characteristic in a wide frequency range of 0.01MHz to 700MHz, wherein the impedances of 1MHz, 25MHz, 100MHz and 500MHz are more than 3 Ω, 35 Ω, 125 Ω and 1000 Ω, respectively. In the comparative example, the main component or the auxiliary component of the ferrite material which is out of the limited range of the present invention has a significant change in the dc resistivity, the normal temperature saturation magnetic induction, the initial permeability and the impedance characteristic, and the result of the electromagnetic physical property detection is out of the range of the design index of the present invention.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (8)
1. The broadband high-impedance manganese-zinc ferrite material is characterized by comprising a main component and an auxiliary component, wherein the main component comprises Fe2O3ZnO and Mn3O4(in MnO); the auxiliary component is selected from SiO2、CaCO3、Nb2O5、Co2O3、TiO2At least one of; the direct current resistivity of the material is more than 3000 omega.m, the Curie temperature is more than 210 ℃, the normal temperature saturation magnetic induction intensity is more than 440mT, the initial magnetic conductivity is more than 650, and the material also has the broadband range of 0.01 MHz-700 MHz and has high impedance characteristic, wherein the impedance of 1MHz, 25MHz, 100MHz and 500MHz is respectively more than 3 omega, 35 omega, 125 omega and 1000 omega.
2. The broadband high-impedance manganese-zinc ferrite material according to claim 1, wherein said main component comprises 46.0-50.0 mol% of Fe calculated as the respective oxides2O3And 4.0-8.9 mol% ZnO, the balance being Mn3O4。
3. The broadband high impedance manganese-zinc ferrite material of claim 1, wherein the auxiliary component is added in an amount ranging from SiO based on the total weight of the main component2The method comprises the following steps: 0.002-0.012 wt% of CaCO3: 0.01 to 0.10 wt%, Nb2O5The method comprises the following steps: 0.01-0.05 wt% of Co2O3The method comprises the following steps: 0.01-1.20 wt% of TiO2The method comprises the following steps: 0.01-0.30 wt%.
4. A method for preparing the broadband high-impedance manganese zinc ferrite material according to any one of claims 1 to 3, comprising the following steps:
1) mixing Fe2O3、Mn3O4And ZnO are evenly mixed and dried according to the proportion;
2) presintering the powder obtained in the step 1) at the temperature of 800-950 ℃ for 2-3 hours, and cooling;
3) adding the auxiliary components into the powder obtained in the step 2) according to the proportion, and then adding deionized water accounting for 40-60 wt% of the total weight of the main components and a dispersing agent accounting for 0.5-3 wt% of the total weight of the main components for ball milling;
4) adding 5-8 wt% of aqueous solution of organic binder into the powder obtained in the step 3), and uniformly mixing and granulating to obtain granules;
5) pressing the granular material obtained in the step 4) into a green body sample;
6) sintering the green body sample obtained in the step 5) at a sintering temperature of 1260-1380 ℃, preserving heat for 4-8 hours at the sintering temperature, then slowly cooling and cooling to 180 ℃, and discharging, wherein the oxygen partial pressure at the heat preservation section is 2-10%, and the balanced oxygen partial pressure is adopted in the cooling process.
5. The method for preparing the broadband high-impedance manganese-zinc ferrite material according to claim 4, wherein the dispersant used in the step 3) is a mixture of a poly propionic acid, gluconic acid, citric acid; the ball milling time is 20-30 minutes, and the particle size of the powder after ball milling is less than 1.3 mu m.
6. The method for preparing the broadband high-impedance manganese-zinc ferrite material according to claim 4, wherein the organic binder in step 4) is polyvinyl alcohol.
7. The method for preparing the broadband high-impedance manganese-zinc ferrite material according to claim 4, wherein the green density pressed in step 5) is 3.0 ± 0.2g/cm3。
8. The method for preparing the broadband high-impedance Mn-Zn ferrite material of claim 4, wherein in the step 6), air sintering is adopted from normal temperature to high temperature, a small amount of nitrogen is adopted for protection and temperature reduction in the temperature reduction section, and the equilibrium oxygen partial pressure in the temperature reduction section is according to the formula lg (P (O)2) a-b/T, wherein a takes a value of 7-10, b takes 13000 and 18000, and T is absolute temperature.
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| CN113072370A (en) * | 2021-03-25 | 2021-07-06 | 南通众兴磁业有限公司 | Manganese-zinc ferrite magnetic core and preparation method thereof |
| CN116813320A (en) * | 2023-06-08 | 2023-09-29 | 浙江工业大学 | MnZn ferrite for MHz frequency |
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