CN108558385B - Wide-temperature-range high-efficiency soft magnetic ferrite material and magnetic core preparation method and application - Google Patents
Wide-temperature-range high-efficiency soft magnetic ferrite material and magnetic core preparation method and application Download PDFInfo
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Abstract
The invention provides a wide-temperature high-efficiency soft magnetic ferrite material and a magnetic core preparation method and application, wherein a main formula and effective doping are optimized, the wide-temperature high-efficiency soft magnetic ferrite material is developed, a multi-section type balanced atmosphere sintering method is adopted, and the density, the grain size, the porosity and the distribution of the ferrite material in grains and among the grains are controlled, so that the microstructure of the ferrite material is more effectively controlled, and the main characteristic parameters of the material are ensured to be harmonious and uniform; the final product ui can reach 3400, the core loss at 25-120 ℃ is 350mW @100 ℃ is 250mW, the L value stably reaches + 3.5% in the temperature range of-40-85 ℃, and the integral loss level is reduced by 8-13.8% in a wider temperature range; the high-temperature Bs is greatly improved, the inductance stability is excellent under the wide-temperature condition, and the production cost is reduced by more than 20%.
Description
Technical Field
The invention relates to a soft magnetic ferrite material, in particular to a wide-temperature-range high-efficiency soft magnetic ferrite material, a preparation method and application of a magnetic core.
Background
Since the research and development of a soft magnetic ferrite material in 1935 by a Netherlands Phillips laboratory is successful, the history of the soft magnetic ferrite material is over 80 years, and the magnetic property of the ferrite is from the ferrimagnetic property, so that the saturation magnetization Ms of the ferrite is lower than that of metal magnetic property, but the resistivity rho of the ferrite is much higher than that of the metal magnetic property, and the soft magnetic ferrite material has good high-frequency characteristics. In the field of weak current high frequency technology, soft magnetic ferrite has unique advantages. Magnetic cores made of such materials are core components of various inductors, electronic transformers, choke coils, suppressors, filters, and the like. Soft magnetic ferrite materials are listed as "advanced high and new technology industrialization important field guideline (2011) published by the department of national institute of improvement and modification(s), etc., and" advanced high and new technology field directory (2015) published by the national ministry of science and technology "and supported by national emphasis, as basic materials for electronic information technology. The LED power generation system is widely applied to the pillar industry and the emerging industry of computers, household appliances, energy-saving lamps, LEDs, network communication, automobiles, electric vehicles, high-speed rails, wind power, nuclear power generation and the like.
The one-key starting and automatic door device of the automobile is a relatively complex electromechanical integrated system and is an important development direction of high-end automobile intellectualization. With the popularization and application of one-key starting and automatic door systems in high-profile automobiles, the attention and research of soft magnetic manufacturers at home and abroad are gradually aroused. Although research, development and application of automobile one-key starting and automatic door systems have been advanced at home and abroad, the realization of functions under extreme temperature conditions is very difficult, and systematic research and development of soft magnetic ferrite materials and magnetic cores, which are core functional components of the one-key starting and automatic door systems, are not common. The systematic research of the soft magnetic ferrite material and the magnetic core for the automobile product functionalization demand has very important significance for the design and development of high-end automobile products and intelligent automobile products. The high-inductance-stability high-voltage power supply has excellent inductance stability under wide temperature conditions, and is a key technical requirement for ensuring that an automobile starts ignition by one key and starts opening and closing of an automatic door under various climatic conditions.
Disclosure of Invention
In view of the above, the invention provides a wide-temperature-range high-efficiency soft magnetic ferrite material, a magnetic core preparation method and an application.
The technical scheme of the invention is realized as follows:
in one aspect, the present invention provides a wide-temperature high-efficiency soft magnetic ferrite material, which comprises a main component and an additive component,
the proportions of the main components are respectively as follows:
Fe2O3 70～72mol％
MnO 20～22mol％
ZnO 7～9mol％
the proportion of each main component is 100mol percent;
relative to the total amount of the main components, the weight percentages of the additive components are respectively as follows:
on the basis of the technical scheme, preferably, the nano SiO2The particle size of (A) is in the range of 50 to 200 nm.
On the other hand, the invention provides a preparation method of the wide-temperature high-efficiency soft magnetic ferrite magnetic core, which comprises the following steps,
s1, mixing the main components and the additive components, and performing ball milling, granulation and presintering to obtain a manganese-zinc ferrite material;
and S2, carrying out compression molding, sintering and grinding on the manganese-zinc ferrite material obtained in the step S1 to obtain a final product.
Based on the above technical solution, preferably, in step S1, in the step S1, pure water, a dispersant, a binder and an antifoaming agent are added in the ball milling process, the particle size distribution is controlled to be 100 to 300 μm, and the weight percentage of water is controlled to be 0.15 to 0.25%.
In addition to the above technical solutions, in the step S1, it is preferable that a PVA solution of 7 wt% to 10 wt% is added during the granulation in the step S1, and spray drying is adopted.
Based on the above technical solution, preferably, in the step S1, in the step S1, the pre-firing temperature is 950 to 1050 ℃, and the pre-firing time is 30 to 90 min.
On the basis of the above technical solution, preferably, in the step S2, the sintering process in the step S2 includes,
s2-1, heating from room temperature to 900 ℃ in an atmospheric atmosphere at a heating rate of 0.5-2.0 ℃/min;
s2-2, adjusting the oxygen partial pressure to 0.4-0.5%, and heating up from 900 ℃ to 1200 ℃ at a heating rate of 1.0-3.0 ℃/min;
s2-3, adjusting the oxygen partial pressure to 5-7%, heating up from 1200 ℃ to 1350-1370 ℃ at a heating rate of 3-10 ℃/min, and preserving heat for 4.2-7 h;
s2-4, cooling under the condition of balanced oxygen partial pressure to obtain a sintered density of 4.75-5 kg/m3The magnetic core of (2).
Preferably, in the step S2, in the step S2-4, the temperature is reduced to 900 ℃ from the highest sintering temperature, the temperature reduction rate is 2.5-5 ℃/min, and the oxygen partial pressure is controlled to be 0.02% -0.5%; then, the temperature is reduced from 900 ℃ to room temperature at a rate of 1.5-4 ℃/min, and the oxygen partial pressure is controlled to be 0-0.005%.
On the basis of the technical scheme, preferably, the grain size of a final product is 3-5 mu m, the initial magnetic conductivity ui reaches more than 3300, and the power loss is 290-310 kW/m under the values of 80-120 ℃, 100kHz and 200mT Bs3The Bs at 100 ℃ are above 410 mT.
In a third aspect, the wide-temperature high-efficiency soft magnetic ferrite material of the first aspect of the invention is applied to the fields of automobile one-key starting and magnetic cores of automatic door devices.
Compared with the prior art, the wide-temperature-range high-efficiency soft magnetic ferrite material and the preparation method and application of the magnetic core have the following beneficial effects:
(1) the main formula and effective doping are optimized, the wide-temperature-range high-efficiency soft magnetic ferrite material is developed, the grain size of the final product is 3-5 mu m, the initial magnetic conductivity ui reaches more than 3400, and the power loss is 290-310 kW/m at 80-120 ℃, 100kHz and 200mT Bs (magnetic resonance power efficiency)3Bs at 100 ℃ is above 430 mT;
(2) the density, the grain size and the porosity of the ferrite material and the distribution of the ferrite material in and among grains are controlled by adopting a multi-section type balanced atmosphere sintering method, so that the microstructure of the soft magnetic ferrite is more effectively controlled, and the main characteristic parameters of the material are ensured to be harmonious and uniform;
(3) the final product ui can reach 3400, the core loss at 25-120 ℃ is 350mW @100 ℃ is 250mW, the L value stably reaches + 3.5% in the temperature range of-40-85 ℃, and the integral loss level is reduced by 8-13.8% in a wider temperature range; the high-temperature Bs is greatly improved, the inductance stability is excellent under the wide-temperature condition, and the production cost is reduced by more than 20%.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The soft magnetic ferrite material of the present embodiment includes a main component and an additive component, wherein,
the proportions of the main components are respectively as follows:
Fe2O3 70mol％
MnO 22mol％
ZnO 8mol％
relative to the total amount of the main components, the weight ratio of each additive component is respectively as follows:
nanometer SiO with particle size range of 50-100 nm2 100PPM。
The preparation steps of the soft magnetic ferrite magnetic core with high Bs value and low power loss are as follows:
first, the main components and the additive components are weighed and mixed uniformly.
And secondly, adding pure water, a dispersing agent, an adhesive and a defoaming agent into the mixed material, and performing ball milling, wherein the particle size distribution is controlled to be 100-300 mu m, and the weight percentage of water is 0.15%.
Then, a 7 wt% PVA solution was added to the powder obtained by the ball-milling, and granulated by spray drying.
And then presintering at 950 ℃ in air atmosphere for 30min to obtain the manganese-zinc ferrite material.
And finally, carrying out compression molding on the manganese-zinc ferrite material obtained by pre-sintering, and then sintering under the following conditions to obtain a final product:
s2-1, in the atmosphere, raising the temperature from room temperature to 900 ℃ at the temperature raising rate of 0.5 ℃/min;
s2-2, adjusting the oxygen partial pressure to 0.4%, and heating from 900 ℃ to 1200 ℃ at the heating rate of 1.0 ℃/min;
s2-3, adjusting the oxygen partial pressure to 5%, heating up from 1200 ℃ to 1350 ℃ at the heating rate of 3 ℃/min, and preserving heat for 4.2 h;
s2-4, firstly, reducing the temperature from the highest sintering temperature to 900 ℃, wherein the temperature reduction rate is 2.5 ℃/min, and the oxygen partial pressure is controlled to be 0.02-0.5%; then, the temperature is reduced from 900 ℃ to room temperature at the rate of 1.5 ℃/min, the oxygen partial pressure is controlled to be 0-0.005 percent, and the sintered density is 4.75kg/m3The magnetic core of (2).
Example 2
The soft magnetic ferrite material of the present embodiment includes a main component and an additive component, wherein,
the proportions of the main components are respectively as follows:
Fe2O3 71mol％
MnO 21mol％
ZnO 8mol％
relative to the total amount of the main components, the weight ratio of each additive component is respectively as follows:
nanometer SiO with particle size range of 50-100 nm2 200PPM。
The preparation steps of the soft magnetic ferrite magnetic core with high Bs value and low power loss are as follows:
first, the main components and the additive components are weighed and mixed uniformly.
And secondly, adding pure water, a dispersing agent, an adhesive and a defoaming agent into the mixed material, and performing ball milling, wherein the particle size distribution is controlled to be 100-300 mu m, and the weight percentage of water is 0.2%.
Then, 8 wt% of PVA solution was added to the powder obtained by the ball milling, and spray drying was used for granulation.
And then presintering at 1000 ℃ for 60min in an air atmosphere to obtain the manganese-zinc ferrite material.
And finally, carrying out compression molding on the manganese-zinc ferrite material obtained by pre-sintering, and then sintering under the following conditions to obtain a final product:
s2-1, in the atmosphere, raising the temperature from room temperature to 900 ℃ at the temperature raising rate of 1.5 ℃/min;
s2-2, adjusting the oxygen partial pressure to 0.4-0.5%, and heating up from 900 ℃ to 1200 ℃ at the heating rate of 2 ℃/min;
s2-3, adjusting the oxygen partial pressure to 5-7%, heating from 1200 ℃ to 1368 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 5.5 h;
s2-4, firstly, reducing the temperature from the highest sintering temperature to 900 ℃, wherein the temperature reduction rate is 3.5 ℃/min, and the oxygen partial pressure is controlled to be 0.02-0.5%; then, the temperature is reduced from 900 ℃ to room temperature at a rate of 3 ℃/min, the oxygen partial pressure is controlled to be 0-0.005%, and the sintered density is 4.85kg/m3The magnetic core of (2).
Example 3
The soft magnetic ferrite material of the present embodiment includes a main component and an additive component, wherein,
the proportions of the main components are respectively as follows:
Fe2O3 72mol％
MnO 21mol％
ZnO 7mol％
relative to the total amount of the main components, the weight ratio of each additive component is respectively as follows:
nanometer SiO with particle size range of 50-100 nm2 500PPM。
The preparation steps of the soft magnetic ferrite magnetic core with high Bs value and low power loss are as follows:
first, the main components and the additive components are weighed and mixed uniformly.
And secondly, adding pure water, a dispersing agent, an adhesive and a defoaming agent into the mixed material, and performing ball milling, wherein the particle size distribution is controlled to be 100-300 mu m, and the weight percentage of water is 0.25%.
Then, 10 wt% of PVA solution was added to the powder obtained by the ball milling, and spray drying was used for granulation.
And then presintering at 1050 ℃ in an air atmosphere for 90min to obtain the manganese-zinc ferrite material.
And finally, carrying out compression molding on the manganese-zinc ferrite material obtained by pre-sintering, and then sintering under the following conditions to obtain a final product:
s2-1, in the atmosphere, raising the temperature from room temperature to 900 ℃ at the temperature raising rate of 2.0 ℃/min;
s2-2, adjusting the oxygen partial pressure to be 0.4-0.5%, and heating up from 900 ℃ to 1200 ℃ at a heating rate of 3.0 ℃/min;
s2-3, adjusting the oxygen partial pressure to 7%, heating up from 1200 ℃ to 1370 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 7 h;
s2-4, firstly, reducing the temperature from the highest sintering temperature to 900 ℃, wherein the temperature reduction rate is 5 ℃/min, and the oxygen partial pressure is controlled to be 0.02-0.5%; then, the temperature is reduced from 900 ℃ to room temperature at a rate of 4 ℃/min, the oxygen partial pressure is controlled to be 0-0.005%, and the sintered density is 4.90kg/m3The magnetic core of (2).
The core obtained in example 2 was tested and the following results were obtained:
as can be seen, the grain size of the final product is 3-4 μm, the initial permeability ui reaches above 3400, and the power loss at 80-120 ℃, 100kHz and 200mT Bs is 290-310 kW/m3The Bs at 100 ℃ are above 430 mT.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A wide-temperature-range high-efficiency soft magnetic ferrite material is characterized in that: the ferrite powder comprises a main component and an additive component, wherein,
the proportions of the main components are respectively as follows:
Fe2O3 70～72 mol%
MnO 20～22mol%
ZnO 7～9mol%
the proportion of each main component is 100mol percent;
relative to the total amount of the main components, the weight percentages of the additive components are respectively as follows:
CaCO3 100～1000PPM
SnO2 100～500PPM
Nb2O5 50～100PPM
TiO2 100～500PPM
Co3O4 50～100PPM
nano SiO2 100～500PPM。
2. The wide temperature range high efficiency soft magnetic ferrite material of claim 1, wherein: the nano SiO2The particle size of (A) is in the range of 50 to 100 nm.
3. The method for preparing a magnetic core from the wide temperature range high efficiency soft magnetic ferrite material as claimed in claim 1, wherein: comprises the following steps of (a) carrying out,
s1, mixing the main components and the additive components, and performing ball milling, granulation and presintering to obtain a manganese-zinc ferrite material;
and S2, carrying out compression molding, sintering and grinding on the manganese-zinc ferrite material obtained in the step S1 to obtain a final product.
4. The method of claim 3, wherein: in the step S1, in the step S1, pure water, a dispersant, a binder and a defoaming agent are added in the ball milling process, the particle size distribution is controlled to be 100 to 300 μm, and the weight percentage of the water is 0.15 to 0.25%.
5. The method of claim 3, wherein: in the step S1, a PVA solution of 7 wt% to 10 wt% is added during granulation, and spray drying is adopted.
6. The method of claim 3, wherein: in the step S1, the pre-sintering temperature is 950-1050 ℃, and the pre-sintering time is 30-90 min.
7. The method of claim 3, wherein: the grain size of the final product is 3-5 μm, the initial permeability ui reaches above 3400, and the power loss at 80-120 ℃, 100kHz and 200mT Bs is 290-310 kW/m3The Bs at 100 ℃ are above 430 mT.
8. The wide temperature range high efficiency soft magnetic ferrite material according to claim 1, for use in the field of automobile one-key starting and automatic door device magnetic cores.
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| CN110304913B (en) * | 2019-07-04 | 2021-11-26 | 湖北文理学院 | High-frequency ultralow-loss manganese-zinc soft magnetic ferrite material and preparation method thereof |
| CN110330327B (en) * | 2019-07-04 | 2021-11-26 | 湖北文理学院 | High TcHigh-frequency ultra-low loss soft magnetic ferrite material and preparation method thereof |
| CN112456996B (en) * | 2020-12-07 | 2023-02-03 | 越峰电子(广州)有限公司 | Manganese-zinc ferrite material with high Bs, wide temperature range and low loss power, and preparation method and application thereof |
| CN112592169A (en) * | 2020-12-15 | 2021-04-02 | 山东凯通电子有限公司 | Wide-temperature-range high-frequency low-loss high-permeability manganese-zinc ferrite for LED and preparation method thereof |
| CN113135749B (en) * | 2021-04-21 | 2021-12-24 | 湖北华磁电子科技有限公司 | Wide-temperature-range high-efficiency soft magnetic ferrite material and preparation method thereof |
| CN114685154B (en) * | 2022-04-27 | 2022-12-02 | 湖北华磁电子科技有限公司 | High-frequency wide-temperature ultralow-loss ferrite material and preparation process thereof |
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