CN112694323A - Wide-temperature-range high-Bs manganese-zinc ferrite magnetic material and preparation method thereof - Google Patents

Wide-temperature-range high-Bs manganese-zinc ferrite magnetic material and preparation method thereof Download PDF

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CN112694323A
CN112694323A CN202011601516.3A CN202011601516A CN112694323A CN 112694323 A CN112694323 A CN 112694323A CN 202011601516 A CN202011601516 A CN 202011601516A CN 112694323 A CN112694323 A CN 112694323A
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temperature
sintering
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manganese
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王孚亮
陈明
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Yixin Electronic Material Co ltd
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Yixin Electronic Material Co ltd
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Abstract

The invention belongs to the technical field of manganese-zinc ferrite magnetic materials, and particularly relates to a wide-temperature high-Bs manganese-zinc ferrite magnetic material and a preparation method thereof. The material comprises main material components and additive components, wherein the main material components comprise the following components in percentage by mass: 62-70% Fe2O325-30% of MnO and 3-7% of ZnO, wherein the additive components comprise the following components in percentage by mass of the total mass of the main material components: 0.03-0.07% SnO2、0.30‑0.40％Co2O3、0.08‑0.15％TiO2、0.02‑0.04％Nb2O5、0.20‑0.35％NiO、0.02‑0.05％V2O5. The manganese-zinc-iron sample material is obtained by primary sanding, primary spray granulation, pre-sintering, secondary sanding, secondary spray granulation, compression molding and sintering, and simultaneously, the manganese-zinc-iron sample material is ensuredThe wide temperature range and high Bs performance of the material are improved, and the comprehensive performance of the material is improved.

Description

Wide-temperature-range high-Bs manganese-zinc ferrite magnetic material and preparation method thereof
Technical Field
The invention belongs to the technical field of manganese-zinc ferrite magnetic materials, and particularly relates to a wide-temperature high-Bs manganese-zinc ferrite magnetic material and a preparation method thereof.
Background
The manganese-zinc ferrite is Mn0.5Zn0.5Fe2O4The soft magnetic ferrite with the spinel structure is used as a very important basic functional material in the electronic industry and the information industry, has the magnetic properties of high saturation magnetic induction intensity, high initial permeability, low loss, low coercive force and the like, and can be used in clean energy, LED illumination, aerospace, mixed power and the likeThe method has important application in the fields of hybrid power, electric automobiles and the like, and is inseparable from the production and life of people. In order to meet the requirements of different fields on manganese zinc ferrite materials, the requirements of the industry on various properties of the ferrite are gradually improved. Because the manganese-zinc ferrite material is widely applied and the temperature difference between different application environments is large, the manganese-zinc ferrite magnetic ring is required to have a good wide temperature characteristic; in some electronic devices where a large direct current flows, the high saturation magnetic flux density (Bs) of the manganese-zinc-ferrite material is required in order to ensure that the inductance of the magnetic core is not too greatly affected after the large direct current flows.
However, at present, the existing soft magnetic ferrite cannot guarantee the saturation magnetic flux density under the condition of guaranteeing wide temperature, cannot guarantee the curie temperature and the stability of magnetic performance within a wide temperature range under the condition of guaranteeing the saturation magnetic flux density, and is limited in the application range of manganese-zinc-iron. For example, the invention patent with the patent number "CN 102693802A" discloses a wide temperature MnZn power ferrite material and a preparation method thereof, which consists of main components and auxiliary components, wherein the main components and the content are calculated by oxides as follows: fe2O352.1-52.6 mol%, ZnO 9-11.5 mol%, and MnO in balance; the auxiliary components calculated by the total weight of the main component raw materials are as follows: CaCO3、ZrO2、Nb2O5、SiO2And Co2O3And Co2O3The feedstock must be greater than 0.35 wt%. Although the material has lower loss in the temperature range of 25-140 ℃, the saturation magnetic flux density is also lower, and the performance requirements of the material cannot be met in most cases. Therefore, it is necessary to develop a manganese zinc ferrite magnetic material that satisfies both a wide temperature range and a high saturation magnetic flux density.
Disclosure of Invention
In order to solve the problem that the existing manganese-zinc-magnetic ferrite material cannot simultaneously ensure the wide-temperature property and the high-Bs property, the invention provides a wide-temperature high-Bs manganese-zinc-ferrite magnetic material, which simultaneously ensures the wide-temperature property and the high-Bs property of the material and improves the comprehensive property of the material.
The invention provides a manganese zinc ferrite with wide temperature range and high BsThe magnetic material comprises a main material component and an additive component, wherein the main material component comprises the following components in percentage by mass: 62-70% Fe2O325-30% of MnO and 3-7% of ZnO, wherein the additive components comprise the following components in percentage by mass of the total mass of the main material components: 0.03-0.07% SnO2、0.30-0.40％Co2O3、0.08-0.15％TiO2、0.02-0.04％Nb2O5、0.20-0.35％NiO、0.02-0.05％V2O5。
Further, the main material components comprise the following components in percentage by mass: 67% Fe2O328% MnO and 5% ZnO, wherein the components of the additive component comprise the following components in percentage by total mass of the main material component: 0.05% SnO2、0.35％Co2O3、0.13％TiO2、0.03％Nb2O5、0.30％NiO、0.03％V2O5。
The preparation method of the wide-temperature high-Bs manganese-zinc ferrite magnetic material comprises the following steps:
(1) mixing the main ingredients to obtain a mixed material, and performing primary spray granulation after primary sanding on the mixed material;
(2) presintering after primary spray granulation, and adding an additive component into the presintering material;
(3) after pre-sintering, sequentially carrying out secondary sanding and secondary spray granulation;
(4) and carrying out profiling and sintering processes after secondary spray granulation to obtain the manganese-zinc-iron sample material.
Further, in the step (1), the average particle diameter of the particles after primary sanding is 1.5-2.5 μm.
Further, in the step (2), the burn-in step: and (3) placing the pre-sintering material in a high-temperature electric furnace for pre-sintering, adopting a programmed heating process to raise the temperature to 550-650 ℃ at the speed of 10 ℃/min, preserving the heat for 1-2h, and then lowering the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the pre-sintering. With the rise of the presintering temperature, the saturation magnetization of the powder is gradually increased, the coercive force and the relative residual magnetization are firstly increased and then decreased, the invention adopts the temperature programming, the temperature of 600-700 ℃ is set as the optimal temperature, and the saturation magnetization of the powder is ensured.
Further, in the step (3), the average particle diameter of the particles after secondary sanding is 0.6-0.8 μm.
Further, in the step (3), after secondary sanding, PVA liquid is added into the slurry for component correction, and secondary spray granulation is performed after stirring for 1.5h, wherein the concentration of the PVA liquid is 10-12%, and the addition amount is 7-9% of the total mass of the main material components.
Further, in the step (4), the sintering process: and (3) feeding the material subjected to secondary spray granulation into a sintering furnace for sintering, adopting a program to heat up at the oxygen partial pressure of 6-10%, increasing the temperature to 550-600 ℃ at the speed of 10 ℃/min and preserving the heat for 1-2h, then increasing the temperature to 1000-1200 ℃ at the speed of 12 ℃/min and preserving the heat for 0.5-3.5h, finally cooling to 550-650 ℃ at the speed of 8 ℃/min and preserving the heat for 1-2h, and finally cooling the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the sintering process. The grain size can be increased by properly increasing the temperature rise speed, so that the initial permeability is improved, and the power consumption is reduced, but if the temperature rise speed is too high, the pores are increased, the uniformity of the grains is poor, the power consumption is increased, and the temperature rise speed of 10 ℃/min and 12 ℃/min is the optimal temperature rise speed.
The invention has the beneficial effects that:
the wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the invention is simultaneously added with a plurality of elements for composite doping, and a proper proportion is selected, so that the wide-temperature property and the high-Bs property of the material are ensured, and the comprehensive performance of the material is improved. Adding SnO2The uniformity of crystal grains can be improved, the porosity and eddy current loss are reduced, and the initial magnetic conductivity and the initial resistivity are improved; adding Co2O3And TiO2Can improve Bs and its temperature characteristic of the material, and raise the initial magnetic conductivity; nb2O5The complete growth of crystal grains can be promoted, the uniformity of the crystal grains is ensured, and the Bs performance is improved; NiO can block the growth of crystal grains, refine the crystal grains and improve the saturation magnetization; v2O5The doping can change solid phase sintering into liquid phase sintering, so that the saturation magnetic induction intensity is increased.
According to the preparation method of the wide-temperature high-Bs manganese-zinc ferrite magnetic material, provided by the invention, twice sanding and twice spray granulation are adopted, so that the slurry is mixed more uniformly and fully, the full completion of solid-phase reaction in the pre-sintering process is facilitated, the time of twice sanding and twice spray granulation is reduced, the energy consumption is reduced, and the preparation method is simple and practical to operate and has good applicability.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The manganese-zinc ferrite magnetic material with wide temperature and high Bs provided by the embodiment comprises main material components and additive components, wherein the main material components comprise the following components in percentage by mass: 65% Fe2O328 percent of MnO and 7 percent of ZnO, and the components of the additive components comprise the following components in percentage by mass of the total mass of the main material components: 0.03% SnO2、0.30％Co2O3、0.08％TiO2、0.02％Nb2O5、0.2％NiO、0.02％V2O5。
The preparation method of the wide-temperature high-Bs manganese-zinc ferrite magnetic material comprises the following steps:
(1) mixing the main ingredients to obtain a mixed material, and performing primary spray granulation on the mixed material after primary sanding, wherein the average particle size of particles after primary sanding is 1.5 mu m;
(2) presintering after primary spray granulation, adding an additive component into the presintering material, putting the presintering material into a high-temperature electric furnace for presintering, raising the temperature to 550 ℃ at the speed of 10 ℃/min by adopting a program, preserving the temperature for 1.5h, and then reducing the temperature in a sintering furnace to room temperature at the temperature reduction speed of 5 ℃/min to finish the presintering;
(3) pre-burning, performing secondary sanding, wherein the average particle size of particles after secondary sanding is 0.6 mu m, adding PVA liquid into the slurry after secondary sanding for component correction, stirring for 1.5h, and performing secondary spray granulation, wherein the concentration of the PVA liquid is 10%, the addition amount is 7% of the total mass of the main material components, and performing secondary spray granulation after PVA component correction;
(4) carrying out compression molding and sintering processes after secondary spray granulation, wherein the sintering process comprises the following steps: and (3) feeding the material subjected to secondary spray granulation into a sintering furnace for sintering, heating to 550 ℃ at the speed of 10 ℃/min by adopting a program under the oxygen partial pressure of 6%, preserving heat for 1.5h, then heating to 1000 ℃ at the speed of 12 ℃/min, preserving heat for 2h, finally cooling to 550 ℃ at the speed of 8 ℃/min, preserving heat for 2h, and finally cooling the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the sintering process to obtain the manganese-zinc-iron sample material.
Example 2
The manganese-zinc ferrite magnetic material with wide temperature and high Bs provided by the embodiment comprises main material components and additive components, wherein the main material components comprise the following components in percentage by mass: 68% Fe2O329% MnO and 3% ZnO, wherein the additive components comprise the following components in percentage by mass of the total mass of the main material components: 0.07% SnO2、0.40％Co2O3、0.15％TiO2、0.04％Nb2O5、0.35％NiO、0.05％V2O5。
The preparation method of the wide-temperature high-Bs manganese-zinc ferrite magnetic material comprises the following steps:
(1) mixing the main ingredients to obtain a mixed material, and performing primary spray granulation on the mixed material after primary sanding, wherein the average particle size of particles after primary sanding is 2.2 mu m;
(2) presintering after primary spray granulation, adding an additive component into the presintering material, putting the presintering material into a high-temperature electric furnace for presintering, raising the temperature to 650 ℃ at the speed of 10 ℃/min by adopting a program, preserving the temperature for 1h, and then reducing the temperature in a sintering furnace to room temperature at the temperature reduction speed of 5 ℃/min to finish the presintering;
(3) pre-burning, performing secondary sanding, wherein the average particle size of particles after secondary sanding is 0.8 mu m, adding PVA liquid into the slurry after secondary sanding for component correction, stirring for 1.5h, and performing secondary spray granulation, wherein the concentration of the PVA liquid is 10%, the addition amount is 9% of the total mass of the main material components, and performing secondary spray granulation after PVA component correction;
(4) carrying out compression molding and sintering processes after secondary spray granulation, wherein the sintering process comprises the following steps: and (3) feeding the material subjected to secondary spray granulation into a sintering furnace for sintering, heating to 600 ℃ at the speed of 10 ℃/min by adopting a program under the oxygen partial pressure of 10%, preserving heat for 1h, then heating to 1200 ℃ at the speed of 12 ℃/min, preserving heat for 2.5h, finally cooling to 650 ℃ at the speed of 8 ℃/min, preserving heat for 1h, and finally cooling the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the sintering process to obtain the manganese-zinc-iron sample material.
Example 3
The manganese-zinc ferrite magnetic material with wide temperature and high Bs provided by the embodiment comprises main material components and additive components, wherein the main material components comprise the following components in percentage by mass: 67% Fe2O328 percent of MnO and 5 percent of ZnO, and the components of the additive components comprise the following components in percentage by total mass of the main material components: 0.05% SnO2、0.35％Co2O3、0.13％TiO2、0.03％Nb2O5、0.30％NiO、0.03％V2O5。
The preparation method of the wide-temperature high-Bs manganese-zinc ferrite magnetic material comprises the following steps:
(1) mixing the main ingredients to obtain a mixed material, and performing primary spray granulation on the mixed material after primary sanding, wherein the average particle size of particles after primary sanding is 1.8 mu m;
(2) presintering after primary spray granulation, adding an additive component into the presintering material, putting the presintering material into a high-temperature electric furnace for presintering, raising the temperature to 500 ℃ at the speed of 10 ℃/min by adopting a program, preserving the temperature for 1.5h, and then reducing the temperature in a sintering furnace to room temperature at the temperature reduction speed of 5 ℃/min to finish the presintering;
(3) pre-burning, performing secondary sanding, wherein the average particle size of particles after secondary sanding is 0.7 mu m, adding PVA liquid into the slurry after secondary sanding for component correction, stirring for 1.5h, and performing secondary spray granulation, wherein the concentration of the PVA liquid is 10%, the addition amount is 8% of the total mass of the main material components, and performing secondary spray granulation after PVA component correction;
(4) carrying out compression molding and sintering processes after secondary spray granulation, wherein the sintering process comprises the following steps: and (3) feeding the material subjected to secondary spray granulation into a sintering furnace for sintering, heating to 580 ℃ at the speed of 10 ℃/min by adopting a program under the oxygen partial pressure of 8%, preserving heat for 1.5h, heating to 1100 ℃ at the speed of 12 ℃/min, preserving heat for 2h, cooling to 600 ℃ at the speed of 8 ℃/min, preserving heat for 1.5h, and cooling the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the sintering process to obtain the ferromanganese-zinc sample material.
Comparative example 1
The wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the comparative example does not add SnO in the added components2The other components and the preparation method are the same as those in example 3.
Comparative example 2
The wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the comparative example does not add Co in the additive components2O3And TiO2The other components and the preparation method are the same as those in example 3.
Comparative example 3
The wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the comparative example does not add Nb in the additive components2O5The other components and the preparation method are the same as those in example 3.
Comparative example 4
The wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the comparative example does not add NiO in the added components, and other components and the preparation method are the same as those in the example 3.
Comparative example 5
The wide-temperature high-Bs manganese-zinc ferrite magnetic material provided by the comparative example does not add V in the added components2O5The other components and the preparation method are the same as those in example 3.
The manganese-zinc-ferrite magnetic materials prepared in the above examples 1 to 3 and comparative examples 1 to 5 were subjected to performance tests, and the results of the tests are shown in table 1.
TABLE 1-Performance test results of manganese Zinc ferrite magnetic materials
Figure BDA0002869513730000071
As can be seen from table 1, compared with comparative examples 1 to 5, the manganese zinc ferrite magnetic materials of examples 1 to 3 have excellent and stable magnetic properties such as high magnetic permeability, wide temperature, high Bs, strong coercive force, etc., which indicates that the wide temperature property and high Bs property of the materials can be ensured and the comprehensive properties of the materials can be improved by compounding and doping several elements according to the mixture ratio in the invention.
Although the present invention has been described in detail by way of preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (8)

1. The wide-temperature high-Bs manganese-zinc ferrite magnetic material is characterized by comprising main material components and additive components, wherein the main material components comprise the following components in percentage by mass: 62-70% Fe2O325-30% of MnO and 3-7% of ZnO, wherein the additive components comprise the following components in percentage by mass of the total mass of the main material components: 0.03-0.07% SnO2、0.30-0.40％Co2O3、0.08-0.15％TiO2、0.02-0.04％Nb2O5、0.20-0.35％NiO、0.02-0.05％V2O5。
2. The Mn-Zn ferrite magnetic material with wide temperature range and high Bs as claimed in claim 1The environment-friendly and environment-friendly plastic is characterized in that the main material components comprise the following components in percentage by mass: 67% Fe2O328% MnO and 5% ZnO, wherein the components of the additive component comprise the following components in percentage by total mass of the main material component: 0.05% SnO2、0.35％Co2O3、0.13％TiO2、0.03％Nb2O5、0.30％NiO、0.03％V2O5。
3. The method for preparing a wide-temperature high-Bs manganese-zinc ferrite magnetic material as claimed in claim 1, comprising the steps of:
(1) mixing the main ingredients to obtain a mixed material, and performing primary spray granulation after primary sanding on the mixed material;
(2) presintering after primary spray granulation, and adding an additive component into the presintering material;
(3) after pre-sintering, sequentially carrying out secondary sanding and secondary spray granulation;
(4) and carrying out profiling and sintering processes after secondary spray granulation to obtain the manganese-zinc-iron sample material.
4. The method as claimed in claim 3, wherein in step (1), the average particle size of the particles after primary sanding is 1.5-2.5 μm.
5. The method for preparing a wide-temperature high-Bs manganese-zinc ferrite magnetic material as claimed in claim 3, wherein in said step (2), said pre-sintering step: and (3) placing the pre-sintering material in a high-temperature electric furnace for pre-sintering, adopting a programmed heating process to raise the temperature to 550-650 ℃ at the speed of 10 ℃/min, preserving the heat for 1-2h, and then lowering the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the pre-sintering.
6. The method as claimed in claim 3, wherein in step (3), the average particle size of the grains after secondary sanding is 0.6-0.8 μm.
7. The method for preparing a Mn-Zn ferrite magnetic material with wide temperature range and high Bs according to claim 3, wherein in the step (3), PVA solution is added into the slurry after secondary sanding for component correction, and secondary spray granulation is performed after stirring for 1.5h, wherein the concentration of the PVA solution is 10-12%, and the addition amount is 7-9% of the total mass of the main material components.
8. The method as claimed in claim 3, wherein in the step (4), the sintering process comprises: and (3) feeding the material subjected to secondary spray granulation into a sintering furnace for sintering, adopting a program to heat up at the oxygen partial pressure of 6-10%, increasing the temperature to 550-600 ℃ at the speed of 10 ℃/min and preserving the heat for 1-2h, then increasing the temperature to 1000-1200 ℃ at the speed of 12 ℃/min and preserving the heat for 0.5-3.5h, finally cooling to 550-650 ℃ at the speed of 8 ℃/min and preserving the heat for 1-2h, and finally cooling the temperature in the sintering furnace to room temperature at the cooling speed of 5 ℃/min to finish the sintering process.
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