Manganese-zinc ferrite with wide temperature range, low power consumption and high direct current superposition characteristic and preparation method thereof
Technical Field
The invention relates to the field of manganese-zinc ferrite materials, in particular to a manganese-zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics and a preparation method thereof.
Background
With the continuous development of electronic transformers, the requirements of light weight, high efficiency and energy conservation of the electronic transformers are becoming more and more obvious. The existing soft magnetic ferrite material is suitable for general switching power supply transformers and LCD backlight power supply current converters, is more particularly used for automobile electronics, but has a direct current Bias (DC-Bias) state when being used in most circuits such as AC-DC, DC-DC converters, inductance transformers and the like. As manufacturers for producing and processing manganese-zinc ferrite cores, higher requirements are put forward, and the direct current superposition characteristics of the cores are required to be improved. However, the power consumption of the original manganese-zinc ferrite with high direct current dropping characteristic meets the requirements at low temperature, the power consumption is obviously improved at high temperature, the power consumption at working temperature is increased, the temperature of equipment is overhigh, the energy consumption is overlarge, the requirement of energy saving is not met, and the service life of the equipment is shortened.
Disclosure of Invention
The invention mainly solves the technical problem of providing a wide-temperature low-power-consumption high-direct-current superposition characteristic manganese-zinc ferrite material and a preparation method thereof, and can solve the defects of the existing magnetic core material.
In order to solve the technical problems, the invention adopts a technical scheme that: the manganese zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics comprises: a host component and a dopant component; the doping component accounts for 1.5-2.5% of the total mass of the main component; the main component comprises the following components in percentage by mass: fe2O365.5-68.9% of ZnO3.5-3.9% of Mn in balance3O4The total amount is 100%; the doping component comprises the following components: CaCO3、SiO2、FeO、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3And Li2CO3。
In a preferred embodiment of the present invention, the doping component comprises the following components by mass: CaCO3:SiO2:FeO:MoO3:Nb2O5:Ta2O5:ZrO2:Co2O3:K2CO3:Li2CO3Is 3-5: 2-3: 0.5-1: 1-2: 1-1.5: 0.5-0.8: 2-2.5: 1-1.5: 1-2: 2 to 3.
In order to solve the technical problem, the invention adopts another technical scheme that: the preparation method of the manganese-zinc ferrite material with wide temperature, low power consumption and high direct current superposition characteristics comprises the following steps:
(1) weighing: weighing the main component and the doped component according to the formula ratio for later use;
(2) primary grinding: the formula amount of CaCO in the main component and the doping component3、SiO2、K2CO3And Li2CO3Adding the mixture into a ball mill, adding deionized water for ball milling treatment to obtain a mixture with the average particle size of 5-8 mu m, and drying;
(3) pre-burning: adding the mixed material subjected to primary grinding and drying in the step (2) into a pre-sintering furnace, and performing pre-sintering treatment to obtain pre-sintered powder;
(4) and (3) secondary grinding: adding FeO and MoO in the doping component into the pre-sintering powder obtained in the step (3)3、Nb2O5、Ta2O5、ZrO2And Co2O3Then adding deionized water for ball milling treatment to obtain a mixture with the average particle size of 0.8-1.0 mu m;
(5) blank preparation: adding the bonding slurry into the mixture obtained by secondary grinding in the step (4), uniformly mixing, and pressing into a required blank sample by using a mold;
(6) sintering and forming: and (5) placing the blank sample obtained in the step (5) into a bell jar furnace, and carrying out heating sintering and cooling treatment under a certain oxygen partial pressure to obtain the manganese-zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics.
In a preferred embodiment of the present invention, in the step (2), the deionized water is added in an amount of CaCO in the host component and the doping component3、SiO2、K2CO3And Li2CO32 times of the total mass, wherein the ball milling treatment time is more than 1.5 h; in the step (4), the addition amount of the deionized water accounts for 2.5-3 times of the total mass of the main component and the doping component; and the ball milling treatment time is more than 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: sintering at the constant temperature of 950-1000 ℃ for 2-3 h in the air atmosphere, introducing nitrogen to ensure that the oxygen partial pressure is 5-8%, cooling to 500 ℃ along with the furnace, controlling the oxygen partial pressure to be 2-3%, and continuously cooling to the room temperature.
In a preferred embodiment of the present invention, in the step (5), the adhesive slurry is PVA slurry with a mass concentration of 6-8%, and the added mass of the PVA slurry accounts for 8-10% of the total mass of the main component and the doping component.
In a preferred embodiment of the present invention, in the step (6), the sintering process conditions are: firstly, in the atmosphere, heating from room temperature to 650 ℃ at a heating rate of 1-1.5 ℃/min, then heating from 650 ℃ to 1000 ℃ at a heating rate of 2-3 ℃/min under the condition that the oxygen partial pressure is 0.05%, then adjusting the oxygen partial pressure to 1%, heating from 1000 ℃ to 1150 ℃ at a heating rate of 5-8 ℃/min, then heating from 1150 ℃ to 1350 ℃ at a heating rate of 10 ℃/min, and preserving heat for 3.5-6.5 h; and in the temperature reduction stage, reducing the temperature from 1350 ℃ to 1100 ℃ at the temperature reduction rate of 2-2.5 ℃/min under the oxygen partial pressure of 1-3%, then reducing the temperature from 1100 ℃ to 500 ℃ at the temperature reduction rate of 5-8 ℃/min under the oxygen partial pressure of 0.5-1.5%, and finally returning the temperature to the room temperature at the speed of 2.5-3 ℃/min under the oxygen partial pressure of 0.01-0.05%.
The invention has the beneficial effects that: according to the preparation method of the manganese-zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristic, the ferrite material is endowed with good wide temperature range and high direct current superposition characteristic by adjusting the iron and the zinc in the main components and the proportion of the doped component components, the high temperature loss of the ferrite material is effectively controlled, the crystal grains of the material are refined and uniform by regulating and controlling the processes of pre-sintering, twice ball milling and sintering molding, and the obtained material has high density, high Curie temperature and excellent electromagnetic 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 manganese zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics, which comprises the following components: a host component and a dopant component; the doping component accounts for 1.5% of the total mass of the main component; the main component comprises the following components in percentage by mass: fe2O365.5%、ZnO 3.5%,Mn3O431 percent; the doping component comprises the following components: CaCO3、SiO2、FeO、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3And Li2CO3And the mass ratio of each component in the doping component is as follows: CaCO3:SiO2:FeO:MoO3:Nb2O5:Ta2O5:ZrO2:Co2O3:K2CO3:Li2CO3Is 3: 2: 0.5: 1: 1: 0.5: 2: 1: 1: 2.
the preparation method of the manganese-zinc ferrite material with wide temperature, low power consumption and high direct current superposition characteristics comprises the following steps:
(1) weighing: weighing the main component and the doped component according to the formula ratio for later use;
(2) primary grinding: the formula amount of CaCO in the main component and the doping component3、SiO2、K2CO3And Li2CO3Adding into a ball mill, adding CaCO in the main component and the doping component3、SiO2、K2CO3And Li2CO3Ball-milling deionized water 2 times the total mass for 1.5h to obtain a mixture with the average particle size of 5-8 μm, and then drying in an oven at 100-120 ℃;
(3) pre-burning: adding the mixed material subjected to primary grinding and drying in the step (2) into a pre-sintering furnace, sintering at a constant temperature of 950 ℃ for 3 hours in an air atmosphere, introducing nitrogen to ensure that the oxygen partial pressure is 5%, cooling to 500 ℃ along with the furnace, controlling the oxygen partial pressure to be 2%, and continuously cooling to room temperature to obtain pre-sintered powder;
(4) and (3) secondary grinding: adding FeO and MoO in the doping component into the pre-sintering powder obtained in the step (3)3、Nb2O5、Ta2O5、ZrO2And Co2O3Then adding deionized water which is 2.5 times of the total mass of the main component and the doping component for ball milling treatment for 2 hours to obtain a mixture with the average particle size of 0.8-1.0 mu m;
(5) blank preparation: adding PVA slurry with the mass concentration of 6 percent which accounts for 8 percent of the total mass of the main component and the doping component into the mixture obtained by secondary grinding in the step (4) as bonding slurry, uniformly mixing, and pressing into a required blank sample by using a mould;
(6) sintering and forming: putting the blank sample obtained in the step (5) into a bell jar furnace, firstly heating from room temperature to 650 ℃ at a heating rate of 1 ℃/min in an atmospheric atmosphere, then heating from 650 ℃ to 1000 ℃ at a heating rate of 2 ℃/min under the condition that the oxygen partial pressure is 0.05 percent, then adjusting the oxygen partial pressure to 1 percent, heating from 1000 ℃ to 1150 ℃ at a heating rate of 5 ℃/min, then heating from 1150 ℃ to 1350 ℃ at a heating rate of 10 ℃/min, and preserving heat for 3.5 h; and in the temperature reduction stage, reducing the temperature from 1350 ℃ to 1100 ℃ at the temperature reduction rate of 2 ℃/min under the oxygen partial pressure of 1 percent, then reducing the temperature from 1100 ℃ to 500 ℃ at the temperature reduction rate of 5 ℃/min, and finally reducing the temperature to the room temperature at the speed of 2.5 ℃/min under the oxygen partial pressure of 0.01 percent, so as to obtain the manganese-zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics.
Example 2
The invention discloses a manganese zinc ferrite material with wide temperature range, low power consumption and high direct current superposition characteristics, which comprises the following components: a host component and a dopant component; the doping component accounts for 2.5% of the total mass of the main component; the main component comprises the following components in percentage by mass: fe2O368.9%、ZnO 3.9%,Mn3O427.2 percent; the doping component comprises the following components: CaCO3、SiO2、FeO、MoO3、Nb2O5、Ta2O5、ZrO2、Co2O3、K2CO3And Li2CO3And the mass ratio of each component in the doping component is as follows: CaCO3:SiO2:FeO:MoO3:Nb2O5:Ta2O5:ZrO2:Co2O3:K2CO3:Li2CO3Is 5: 3: 1: 2: 1.5: 0.8: 2.5: 1.5: 2: 3.
the preparation method of the manganese-zinc ferrite material with wide temperature, low power consumption and high direct current superposition characteristics comprises the following steps:
(1) weighing: weighing the main component and the doped component according to the formula ratio for later use;
(2) primary grinding: the formula amount of CaCO in the main component and the doping component3、SiO2、K2CO3And Li2CO3Adding into a ball mill, adding CaCO in the main component and the doping component3、SiO2、K2CO3And Li2CO3Ball-milling deionized water 2 times of the total mass for 1.8 to obtain a mixture with the average particle size of 5-8 mu m, and then drying in an oven at 100-120 ℃;
(3) pre-burning: adding the mixed material subjected to primary grinding and drying in the step (2) into a pre-sintering furnace, sintering at the constant temperature of 1000 ℃ for 2 hours in the air atmosphere, introducing nitrogen to ensure that the oxygen partial pressure is 8%, cooling to 500 ℃ along with the furnace, controlling the oxygen partial pressure to be 3%, and continuously cooling to room temperature to obtain pre-sintered powder;
(4) and (3) secondary grinding: adding FeO and MoO in the doping component into the pre-sintering powder obtained in the step (3)3、Nb2O5、Ta2O5、ZrO2And Co2O3Then adding deionized water which is 3 times of the total mass of the main component and the doping component to perform ball milling treatment for 2.5 to obtain a mixture with the average particle size of 0.8-1.0 mu m;
(5) blank preparation: adding PVA slurry with the mass concentration of 8 percent which accounts for 10 percent of the total mass of the main component and the doping component into the mixture obtained by secondary grinding in the step (4) as bonding slurry, uniformly mixing, and pressing into a required blank sample by using a mould;
(6) sintering and forming: putting the blank sample obtained in the step (5) into a bell jar furnace, firstly heating from room temperature to 650 ℃ at a heating rate of 1.5 ℃/min in an atmospheric atmosphere, then heating from 650 ℃ to 1000 ℃ at a heating rate of 3 ℃/min under the condition that the oxygen partial pressure is 0.05 percent, then adjusting the oxygen partial pressure to 1 percent, heating from 1000 ℃ to 1150 ℃ at a heating rate of 8 ℃/min, then heating from 1150 ℃ to 1350 ℃ at a heating rate of 10 ℃/min, and preserving heat for 6.5 h; and in the temperature reduction stage, reducing the temperature from 1350 ℃ to 1100 ℃ at the temperature reduction rate of 2.5 ℃/min under the oxygen partial pressure of 3 percent, then reducing the temperature from 1100 ℃ to 500 ℃ at the temperature reduction rate of 8 ℃/min under the oxygen partial pressure of 1.5 percent, and finally reducing the temperature to room temperature at the oxygen partial pressure of 0.05 percent and the rate of 3 ℃/min to obtain the manganese-zinc ferrite material with wide temperature, low power consumption and high direct current superposition characteristics.
The manganese-zinc ferrite obtained by the method has the density of 4.95g/cm through testing3An initial permeability at 25 ℃ of 3100 or more; 100KHZ, 200mT, power loss lower than 420KW/m at 25 deg.C3(ii) a 100KHZ, 200mT, power loss lower than 330KW/m at 100 deg.C3(ii) a The Curie temperature is more than or equal to 235 ℃; 1194A/m, the saturation magnetic flux density at 25 ℃ is higher than 510mT, 1194A/m, the saturation magnetic flux density at 100 ℃ is higher than 440 mT; under the conditions of 1KHZ, 0.3V, normal temperature and current application of 6A, a 4284A inductance bridge tester is used for detecting, the inductance of the inductor is 2.5-3.8 mH, and the superposed inductance is 38-42 muH.
The manganese-zinc ferrite material obtained by the invention has good wide-temperature high-direct-current superposition characteristics and effectively controlled high-temperature loss through the adjustment of iron and zinc in the main components and the proportion of the doped component components, the crystal grains of the material are refined and uniform through the regulation and control of the processes of pre-sintering, twice ball milling and sintering molding, the density of the obtained material is high, the Curie temperature is high, and the electromagnetic performance is excellent.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.