CN111116189A - High-frequency high-impedance manganese-zinc ferrite and preparation method thereof - Google Patents
High-frequency high-impedance manganese-zinc ferrite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof, wherein the manganese-zinc ferrite comprises functional components and auxiliary functional components; the functional components, calculated as respective oxides, comprise Fe2O366.5-69.5 mol%, MnO 25.1-27.4 mol%, and the balance of ZnO, wherein the total amount is 100%; the auxiliary functional components account for 3-8% of the total mass of the functional components and comprise a first auxiliary functional component and a second auxiliary functional component, so that the prepared manganese-zinc ferrite has ultrahigh working frequency, higher impedance characteristic performance and excellent performance, and can meet the use requirements of the existing miniaturized and light-weight electronic components.
Description
Technical Field
The invention relates to the field of magnetic materials, in particular to a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof.
Background
With the expansion and material upgrade of the application fields of magnetic materials such as switching power supplies, vehicle-mounted lighting and vehicle-mounted system DC-DC converters, LCD (LED) display inverter transformers, variable frequency air conditioners, solar inverters and the like, the integration level of electronic devices is higher and higher, and in order to ensure stable, reliable and efficient operation of equipment and systems, the innovation of new materials has gradually led the research and development direction of manganese-zinc ferrite magnetic materials, for example, the development of magnetic materials capable of keeping stable transformer performance under wider working frequency. In addition, with the gradual expansion of the application field of magnetic materials, the magnetic materials are required to be adapted to electronic equipment with smaller volume, higher efficiency and energy conservation, and can maintain stable electrical performance under complex climatic conditions and electromagnetic working environments, and the performance of the existing magnetic materials needs to be further improved.
Disclosure of Invention
The invention mainly solves the technical problem of providing a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof, and can prepare a magnetic product which meets the requirements of electronic equipment.
In order to solve the technical problems, the invention adopts a technical scheme that: provided is a high-frequency high-impedance manganese-zinc ferrite comprising: functional components and auxiliary functional components; wherein the functional components are calculated as respective oxides and comprise Fe2O366.5-69.5 mol%, MnO 25.1-27.4 mol%, and the balance of ZnO, wherein the total amount is 100%; the auxiliary functional components account for 3-8% of the total mass of the functional components; the auxiliary functional components include a first auxiliary functional component and a second auxiliary functional component.
In a preferred embodiment of the present invention, the mass ratio of the first auxiliary functional component to the second auxiliary functional component is 3:2 to 1: 0.5.
In a preferred embodiment of the present invention, the first auxiliary functional component comprises CuO, CoO, V2O5And Bi2O3(ii) a The second auxiliary functional component comprises CaCO3、TiO2And SiO2。
In a preferred embodiment of the present invention, the CuO, CoO and V are2O5And Bi2O3The mass ratio of (1): 1:0.5:0.5.
In a preferred embodiment of the invention, the CaCO3、TiO2And SiO2The mass ratio of (A) to (B) is 0.5:0.3: 1.
In order to solve the technical problem, the invention adopts another technical scheme that: the preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(1) weighing: weighing the functional components, the first auxiliary functional components and the second auxiliary functional components according to the formula ratio for later use;
(2) primary mixing: mixing the weighed functional components and the first auxiliary functional components according to the formula amount, then placing the mixture into a vibratory mill to be vibrated and milled until the particle size is below 10 mu m, and then adding the mixture into a ball mill to be sanded, so that the particle size after sanding is controlled to be 0.8-1.0 mu m;
(3) pre-sintering treatment: placing the materials subjected to sanding in the step (2) into a rotary kiln for presintering treatment;
(4) secondary material mixing: adding the materials subjected to the pre-sintering in the step (3) into a ball mill for sanding, controlling the particle size after sanding to be 0.8-1.0 mu m, adding a second auxiliary functional component with the formula amount, and stirring at a high speed to mix uniformly;
(5) spray granulation: adding a binder, a lubricant and deionized water into the mixture obtained after the secondary mixing, stirring and mixing to obtain slurry, and then carrying out spray granulation by using a granulator;
(6) pressing into a blank and sintering: and (4) pressing the granules obtained in the step (5) into magnetic blanks according to the requirement, then orderly placing the magnetic blanks into a sintering furnace, and sintering to obtain the high-frequency high-impedance manganese-zinc ferrite.
In a preferred embodiment of the present invention, in the steps (2) and (4), the sanding process conditions are as follows: the materials by weight ratio: ball: water =1: 6.5-7: 0.5-1, and the sanding time is 1-2 h.
In a preferred embodiment of the present invention, in the step (3), the process conditions of the pre-firing treatment are as follows: raising the temperature from room temperature to 600-650 ℃ at a heating rate of 10-15 ℃/min, then continuously raising the temperature to 850-900 ℃ at a heating rate of 5-10 ℃/min, then keeping the temperature for 2-2.5 h at constant temperature, and then lowering the temperature to room temperature at a speed of 20-30 ℃/min.
In a preferred embodiment of the invention, in the step (5), the mass ratio of the binder, the lubricant and the deionized water is 3:0.5: 15-5: 1: 30.
In a preferred embodiment of the present invention, in the step (6), the sintering process conditions are: firstly, injecting nitrogen into the sintering furnace, adjusting the oxygen partial pressure in the sintering furnace to be 10-15%, raising the temperature from room temperature to 1000-1100 ℃ at the temperature raising rate of 3-5 ℃/min under the oxygen partial pressure, keeping the temperature at constant temperature for 30-60 min, then adjusting the filling amount of the nitrogen, adjusting the oxygen partial pressure in the sintering furnace to be the equilibrium oxygen partial pressure, continuously raising the temperature to 1360-1380 ℃ at the speed of 5-8 ℃/min under the oxygen partial pressure, and keeping the temperature at constant temperature for 5-6 h.
The invention has the beneficial effects that: according to the high-frequency high-impedance manganese-zinc ferrite and the preparation method thereof, the design of the iron-rich functional component and two auxiliary functional components is matched with the design of a special pre-sintering process and a sintering process, so that the prepared manganese-zinc ferrite has higher working frequency and excellent impedance performance.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
The embodiment of the invention comprises the following steps:
example 1
The invention discloses a high-frequency high-impedance manganese-zinc ferrite, which comprises the following components: functional components and auxiliary functional components; the auxiliary functional components account for 3 percent of the total mass of the functional components.
Wherein the functional components are calculated as respective oxides and comprise Fe2O366.5mol percent, MnO 27.4mol percent and the balance of ZnO, wherein the total amount is 100 percent. The functional component adopts high-purity raw materials, and the purity of each raw material is kept above 99.5 wt% so as to ensure the performance of the manganese-zinc ferrite.
The auxiliary functional components comprise a first auxiliary functional component and a second auxiliary functional component, and the first auxiliary function componentThe mass ratio of the components to the second auxiliary functional component is 3: 2. Specifically, the first auxiliary functional component comprises the following components in a mass ratio of 1: 1:0.5:0.5 of CuO, CoO, V2O5And Bi2O3(ii) a The second auxiliary functional component comprises CaCO with the mass ratio of 0.5:0.3:13、TiO2And SiO2。
The preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(1) weighing: weighing the formula amount of Fe2O3Oxides of MnO and ZnO; CuO, CoO, V2O5And Bi2O3And CaCO3、TiO2And SiO2And is ready for use;
(2) primary mixing: according to the formula amount, weighing the Fe2O3Oxides of MnO and ZnO with 1: CuO, CoO and V in a mass ratio of 1:0.5:0.52O5And Bi2O3Mixing, placing the mixture into a vibromill, vibromilling the mixture at the vibromill frequency of 30-50 Hz until the particle size is below 10 mu m, and adding the mixture into a ball mill according to the weight ratio: ball: water =1:6.5: sanding for 1-2 h according to the proportion of 0.5, and controlling the grain diameter after sanding to be 0.8-1.0 mu m;
(3) pre-sintering treatment: placing the material subjected to sanding in the step (2) into a rotary kiln, raising the temperature from room temperature to 650 ℃ at a heating rate of 10 ℃/min, then continuing raising the temperature to 900 ℃ at a heating rate of 5 ℃/min, then keeping the temperature for 2h at a constant temperature, and then lowering the temperature to room temperature at a speed of 20 ℃/min to finish pre-sintering treatment;
(4) secondary material mixing: adding the materials subjected to the pre-sintering in the step (3) into a ball mill, and mixing the materials in a weight ratio: ball: sanding for 1-2 h according to the ratio of water =1:6.5:0.5 to control the particle size after sanding to be 0.8-1.0 μm, then adding a second auxiliary functional component with the formula amount, and stirring and mixing uniformly at a high speed of 800 r/min;
(5) spray granulation: adding a binder, a lubricant and deionized water in a mass ratio of 3:0.5:15 into the mixture obtained after the secondary mixing, stirring and mixing to obtain slurry, and then carrying out spray granulation by using a granulator; wherein the binder is PVA, and the lubricant is zinc stearate;
(6) pressing into a blank and sintering: pressing the granules obtained in the step (5) into magnetic blanks according to the requirement, then placing the magnetic blanks into a sintering furnace in order, enabling the placing amount of the magnetic blanks to be smaller than 1/2 of the internal volume of the sintering furnace, and sintering to obtain the high-frequency high-impedance manganese-zinc ferrite, wherein the sintering process conditions are as follows: firstly, injecting nitrogen into a sintering furnace, adjusting the oxygen partial pressure in the sintering furnace to be 10%, raising the temperature from room temperature to 1000 ℃ at the heating rate of 3 ℃/min under the oxygen partial pressure, keeping the temperature for 60min at a constant temperature, then adjusting the filling amount of the nitrogen, adjusting the oxygen partial pressure in the sintering furnace to be the equilibrium oxygen partial pressure, continuously raising the temperature to 1360 ℃ at the rate of 5 ℃/min under the oxygen partial pressure, and keeping the temperature for 6h at the constant temperature.
The high-frequency high-impedance wave-absorbing filtering manganese-zinc ferrite prepared by the embodiment has the following properties by tests: the initial permeability is 6300 (1.0 kHz, 0.3V, 23 +/-3 ℃);
the working temperature range is 0 +/-2-100 +/-2 ℃;
density 4.85g/cm3；
Curie temperature 158 ℃;
1MHz, T25-15-12 standard magnetic ring test 2TS Z is larger than 125 Ω;
and 2TS Z is larger than 125 omega by the test of a standard magnetic ring of 5MHz and T25-15-12.
Example 2
The invention discloses a high-frequency high-impedance manganese-zinc ferrite, which comprises the following components: functional components and auxiliary functional components; the auxiliary functional components account for 3-8% of the total mass of the functional components.
Wherein the functional components are calculated as respective oxides and comprise Fe2O369.5mol%, MnO 25.1 mol%, and the balance ZnO, the total amount being 100%. The functional component adopts high-purity raw materials, and the purity of each raw material is kept above 99.5 wt% so as to ensure the performance of the manganese-zinc ferrite.
The auxiliary functional components comprise a first auxiliary functional component and a second auxiliary functional component, and the first auxiliary functional component and the second auxiliary functional componentThe mass ratio of the second auxiliary functional components is 1: 0.5. Specifically, the first auxiliary functional component comprises the following components in a mass ratio of 1: 1:0.5:0.5 of CuO, CoO, V2O5And Bi2O3(ii) a The second auxiliary functional component comprises CaCO with the mass ratio of 0.5:0.3:13、TiO2And SiO2。
The preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(1) weighing: weighing the formula amount of Fe2O3Oxides of MnO and ZnO; CuO, CoO, V2O5And Bi2O3And CaCO3、TiO2And SiO2And is ready for use;
(2) primary mixing: according to the formula amount, weighing the Fe2O3Oxides of MnO and ZnO with 1: CuO, CoO and V in a mass ratio of 1:0.5:0.52O5And Bi2O3Mixing, placing the mixture into a vibromill, vibromilling the mixture at the vibromill frequency of 30-50 Hz until the particle size is below 10 mu m, and adding the mixture into a ball mill according to the weight ratio: ball: sanding for 1-2 h at the ratio of water =1:7: 1, and controlling the grain diameter after sanding to be 0.8-1.0 μm;
(3) pre-sintering treatment: placing the material subjected to sanding in the step (2) into a rotary kiln, raising the temperature from room temperature to 650 ℃ at a temperature rise rate of 15 ℃/min, then continuing raising the temperature to 850 ℃ at a temperature rise rate of 10 ℃/min, then keeping the temperature for 2.5h at constant temperature, and then lowering the temperature to room temperature at a rate of 30 ℃/min to finish pre-sintering treatment;
(4) secondary material mixing: adding the materials subjected to the pre-sintering in the step (3) into a ball mill, and mixing the materials in a weight ratio: ball: sanding for 1-2 h according to the ratio of water =1:7: 1 to control the particle size after sanding to be 0.8-1.0 μm, then adding a second auxiliary functional component with the formula amount, and stirring and mixing uniformly at a high speed of 800 r/min;
(5) spray granulation: adding a binder, a lubricant and deionized water in a mass ratio of 5: 1:30 into the mixture obtained after the secondary mixing, stirring and mixing to obtain slurry, and then carrying out spray granulation by using a granulator; wherein the binder is PVA, and the lubricant is zinc stearate;
(6) pressing into a blank and sintering: and (4) pressing the granules obtained in the step (5) into magnetic blanks according to the requirement, then orderly placing the magnetic blanks into a sintering furnace, and sintering to obtain the high-frequency high-impedance manganese-zinc ferrite. The sintering process conditions are as follows: firstly, injecting nitrogen into the sintering furnace, adjusting the oxygen partial pressure in the sintering furnace to be 15%, raising the temperature from room temperature to 1100 ℃ at the temperature raising rate of 5 ℃/min under the oxygen partial pressure, keeping the temperature for 30min at a constant temperature, then adjusting the filling amount of the nitrogen, adjusting the oxygen partial pressure in the sintering furnace to be the equilibrium oxygen partial pressure, continuously raising the temperature to 1380 ℃ at the temperature raising rate of 8 ℃/min under the oxygen partial pressure, and keeping the temperature for 5h at the constant temperature.
The high-frequency high-impedance wave-absorbing filtering manganese-zinc ferrite prepared by the embodiment has the following properties by tests: the initial permeability is 6100 (1.0 kHz, 0.3V, 23 +/-3 ℃);
the working temperature range is 0 +/-2-100 +/-2 ℃;
density 4.82g/cm3；
A Curie temperature of 163 ℃;
1MHz, T25-15-12 standard magnetic ring test 2TS Z is larger than 128 omega;
and 2TS Z is larger than 132 omega by the test of a standard magnetic ring of T25-15-12 at 5 MHz.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high-frequency high-impedance manganese-zinc ferrite, comprising: functional components and auxiliary functional components; wherein the functional components are calculated as respective oxides and comprise Fe2O366.5-69.5 mol%, MnO 25.1-27.4 mol%, and the balance of ZnO, wherein the total amount is 100%; the auxiliary functional components account for 3-8% of the total mass of the functional components; the auxiliary functional component comprises a first auxiliaryA sexual functional component and a second auxiliary functional component.
2. The high-frequency high-impedance manganese-zinc ferrite according to claim 1, wherein the mass ratio of the first auxiliary functional component to the second auxiliary functional component is 3:2 to 1: 0.5.
3. The high frequency high impedance manganese-zinc-ferrite of claim 2, wherein said first auxiliary functional component comprises CuO, CoO, V2O5And Bi2O3(ii) a The second auxiliary functional component comprises CaCO3、TiO2And SiO2。
4. The high frequency high impedance manganese-zinc-ferrite of claim 3, wherein said CuO, CoO, V2O5And Bi2O3The mass ratio of (1): 1:0.5:0.5.
5. The Mn-Zn ferrite composition according to claim 3, wherein the CaCO is used as a starting material3、TiO2And SiO2The mass ratio of (A) to (B) is 0.5:0.3: 1.
6. A preparation method of high-frequency high-impedance manganese-zinc ferrite is characterized by comprising the following steps:
(1) weighing: weighing the functional components, the first auxiliary functional components and the second auxiliary functional components according to the formula ratio for later use;
(2) primary mixing: mixing the weighed functional components and the first auxiliary functional components according to the formula amount, then placing the mixture into a vibratory mill to be vibrated and milled until the particle size is below 10 mu m, and then adding the mixture into a ball mill to be sanded, so that the particle size after sanding is controlled to be 0.8-1.0 mu m;
(3) pre-sintering treatment: placing the materials subjected to sanding in the step (2) into a rotary kiln for presintering treatment;
(4) secondary material mixing: adding the materials subjected to the pre-sintering in the step (3) into a ball mill for sanding, controlling the particle size after sanding to be 0.8-1.0 mu m, adding a second auxiliary functional component with the formula amount, and stirring at a high speed to mix uniformly;
(5) spray granulation: adding a binder, a lubricant and deionized water into the mixture obtained after the secondary mixing, stirring and mixing to obtain slurry, and then carrying out spray granulation by using a granulator;
(6) pressing into a blank and sintering: and (4) pressing the granules obtained in the step (5) into magnetic blanks according to the requirement, then orderly placing the magnetic blanks into a sintering furnace, and sintering to obtain the high-frequency high-impedance manganese-zinc ferrite.
7. The preparation method of high-frequency high-impedance manganese-zinc ferrite according to claim 6, wherein in the steps (2) and (4), the sanding process conditions are as follows: the materials by weight ratio: ball: water =1: 6.5-7: 0.5-1, and the sanding time is 1-2 h.
8. The method for preparing high-frequency high-impedance manganese-zinc ferrite according to claim 6, wherein in the step (3), the process conditions of the pre-sintering treatment are as follows: raising the temperature from room temperature to 600-650 ℃ at a heating rate of 10-15 ℃/min, then continuously raising the temperature to 850-900 ℃ at a heating rate of 5-10 ℃/min, then keeping the temperature for 2-2.5 h at constant temperature, and then lowering the temperature to room temperature at a speed of 20-30 ℃/min.
9. The preparation method of the high-frequency high-impedance manganese-zinc ferrite according to claim 6, wherein in the step (5), the mass ratio of the binder to the lubricant to the deionized water is 3:0.5: 15-5: 1: 30.
10. The method for preparing high-frequency high-impedance manganese-zinc ferrite according to claim 6, wherein in the step (6), the sintering process conditions are as follows: firstly, injecting nitrogen into the sintering furnace, adjusting the oxygen partial pressure in the sintering furnace to be 10-15%, raising the temperature from room temperature to 1000-1100 ℃ at the temperature raising rate of 3-5 ℃/min under the oxygen partial pressure, keeping the temperature at constant temperature for 30-60 min, then adjusting the filling amount of the nitrogen, adjusting the oxygen partial pressure in the sintering furnace to be the equilibrium oxygen partial pressure, continuously raising the temperature to 1360-1380 ℃ at the speed of 5-8 ℃/min under the oxygen partial pressure, and keeping the temperature at constant temperature for 5-6 h.
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