CN112979302A - Manganese-zinc power ferrite material and preparation method thereof - Google Patents
Manganese-zinc power ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a manganese-zinc power ferrite material and a preparation method thereof, wherein the main component of the ferrite material comprises 73-74 wt% of iron oxide, 3-4 wt% of zinc oxide and the balance of manganese oxide, and the auxiliary components comprise 500-1000ppm of calcium carbonate, 200-500ppm of silicon dioxide, 2000-5000ppm of cobaltosic oxide, 100-200ppm of zirconium oxide, 200-600ppm of niobium pentoxide, 100-200ppm of zirconium oxide, 200-1000ppm of titanium dioxide and 1000-2000ppm of copper calcium titanate; the invention reduces the high-frequency loss of the manganese-zinc power ferrite material by trace additives such as calcium copper titanate and the like, greatly reduces the power loss of the manganese-zinc ferrite material while keeping the performances of magnetic conductivity and saturation magnetic induction intensity not to be deteriorated, and has high saturation magnetic induction intensity.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a manganese-zinc power ferrite material suitable for 5MHz and a preparation method thereof.
Background
Manganese-zinc ferrite is an important soft magnetic material and is mainly used for manufacturing various magnetic components, such as transformer cores, inductors and the like. The Mn-Zn ferrite has higher initial permeability than Ni-Fe ferrite, and lower loss than Fe-based amorphous alloy, Co-based amorphous alloy, Fe-Si-Al and Fe-Si-Cr metal magnetic powder cores. With the development of power electronic technology, the trend of miniaturization, integration and lightness of magnetic components requires that manganese-zinc ferrite materials can adapt to higher use frequency. Domestic and foreign enterprises develop manganese-zinc power ferrite with the use frequency as high as 500-3MHz by improving the process and the formula. For example, N49 for TDK, 7H10, 7H20 for FDK can be applied to 500-1MHz, Ferroxcube to 3F4, 3F46, 3F5 for 1-3MHz, and the like. However, the manganese-zinc ferrite is less researched in a MHz frequency band, and the electromagnetic performance of the manganese-zinc ferrite can be further improved by adjusting the microstructure, the chemical composition and the preparation process.
In the aspects of domestic and foreign patents, manganese zinc ferrite materials suitable for 500-2MHz are respectively disclosed in patents US20170352455A1 and US20190096554A1, and manganese zinc ferrite materials suitable for 3MHz are respectively disclosed in patents CN10755984A and CN 107129292A. Manganese-zinc ferrite materials suitable for 5MHz are disclosed in patents CN108911733A and CN108863338A, respectively, but rare metals indium, gallium or toxic metal cadmium are used.
Disclosure of Invention
Aiming at the defects in the prior art, the primary object of the invention is to provide a manganese-zinc power ferrite material.
The second purpose of the invention is to provide a preparation method of the manganese-zinc power ferrite material.
In order to achieve the above primary object, the solution of the present invention is:
a manganese-zinc power ferrite material comprises a main component and an auxiliary component;
the main components comprise the following components:
iron oxide (Fe)2O3) 73-74wt％，
3-4 wt% of zinc oxide (ZnO),
manganese oxide (MnO) balance;
the accessory components comprise the following components in percentage by weight based on 100 percent of the total mass of the main component:
in order to achieve the second objective, the solution of the invention is:
the preparation method of the manganese-zinc power ferrite material comprises the following steps:
(1) putting the main components into a ball mill for ball milling and mixing, and carrying out primary ball milling for 30-60min to obtain mixed powder;
(2) placing the mixed powder in a muffle furnace for heat preservation and presintering to obtain presintering powder;
(3) grinding the pre-sintered powder, performing secondary ball milling, putting the powder into a grinding machine, and adding auxiliary components and pure water for sanding, wherein the particle size is controlled to be 1-2 mu m;
(4) drying the ground slurry obtained in the step (3), adding polyvinyl alcohol for granulation, and performing compression molding after drying to obtain a molded blank;
(5) and placing the molded blank into a sintering furnace with atmosphere regulation, and sintering in the atmosphere of nitrogen and oxygen.
As a preferred embodiment of the present invention, in the step (1), the main components include 73 to 74 wt% of iron oxide, 3 to 4 wt% of zinc oxide and the balance of manganese oxide.
As a preferred embodiment of the invention, in the step (2), the temperature of the muffle furnace is 900-950 ℃, and the holding time is 1-2 h.
In the step (3), the time of the secondary ball milling is 60-120 min.
In the step (3), the sanding time is 30-60 min.
As a preferred embodiment of the present invention, in the step (3), the subcomponents included 500-1000ppm calcium carbonate, 200-500ppm silica, 2000-5000ppm tricobalt tetroxide, 200-600ppm zirconia, 100-200ppm niobium pentoxide, 200-1000ppm titania and 1000-2000ppm copper calcium titanate.
As a preferred embodiment of the present invention, in the step (4), the content of the polyvinyl alcohol is 10-15 wt%, and the temperature for drying is 150-300 ℃.
As a preferred embodiment of the present invention, in the step (5), the sintering temperature is 1100-1120 ℃, the temperature rising rate is 1-3 ℃/min during the sintering process, the heat preservation time is 3-5h, and the oxygen content in the heat preservation stage is 0.75-1.5%, and more preferably 1-1.25%.
Due to the adoption of the scheme, the invention has the beneficial effects that:
first, the invention is through CaCu3Ti4O12The micro additive reduces the high-frequency loss of the manganese-zinc power ferrite material, greatly reduces the power loss of the manganese-zinc ferrite material at 1-5MHz while keeping the performance of magnetic permeability and saturation magnetic induction intensity not to be deteriorated, and has high saturation magnetic induction intensity.
Secondly, the sintering temperature of the manganese-zinc power ferrite which is conventionally applied to the kHz frequency band is above 1300 ℃, the invention selects low-temperature sintering, and can effectively reduce the grain size, thereby improving the cut-off frequency, reducing the residual loss of the manganese-zinc ferrite in the 5MHz frequency band, and simultaneously avoiding the sharp reduction of other electromagnetic properties.
Detailed Description
The invention provides a manganese-zinc power ferrite material and a preparation method thereof.
< manganese-zinc power ferrite Material >
The manganese-zinc power ferrite material comprises a main component and an auxiliary component, wherein the auxiliary component is a trace additive for improving electromagnetic performance.
(Main component)
Wherein, the main components comprise the following components:
iron oxide (Fe)2O3) 73-74wt％，
3-4 wt% of zinc oxide (ZnO),
manganese oxide (MnO) balance;
(subcomponent)
The accessory components comprise the following components in percentage by weight based on 100 percent of the total mass of the main component:
the invention obtains higher saturation magnetic induction intensity by improving the content of the main component iron oxide, and reduces the content of zinc oxide to reduce the initial permeability, thereby improving the cut-off frequency of the manganese-zinc power ferrite material and further achieving the purpose of reducing the MHz frequency band loss of the manganese-zinc power ferrite material.
The invention creatively adds CaCu3Ti4O12(CCTO)，CaCu3Ti4O12Is a perovskite-like phase, the sintering temperature is about 1100 ℃ generally, and the manganese-zinc ferrite can exist stably when being sintered at a low temperature (1110 ℃). CCTO is therefore present mainly in the grain boundaries as a heterogeneous component in MnZn power ferrite materials, whereas CaCu3Ti4O12As a high-resistance material, the MnZn power ferrite material can play a role in increasing the resistance of a grain boundary, thereby reducing the eddy current loss of the MnZn power ferrite material.
At the same time, CaCu is added3Ti4O12The problem of sharp decrease in permeability while decreasing the loss can be avoided. By adding CaCu3Ti4O12The power loss tested under the conditions of 3MHz, 30mT, 100 ℃ and 5MHz, 20mT, 100 ℃ is respectively reduced by 42% and 32%, and the magnetic permeability and the saturation magnetic induction intensity are respectively reduced by only 4% and 1%.
< preparation method of manganese-zinc power ferrite material >
The preparation method of the manganese-zinc power ferrite material comprises the following steps:
(1) putting the main components into a ball mill for ball milling and mixing, and carrying out primary ball milling for 30-60min to obtain mixed powder;
(2) placing the mixed powder in a muffle furnace for heat preservation and presintering to obtain presintering powder;
(3) grinding the pre-sintered powder, performing secondary ball milling, putting the powder into a grinding machine, and adding auxiliary components and pure water for sanding, wherein the particle size is controlled to be 1-2 mu m;
(4) drying the ground slurry obtained in the step (3), adding polyvinyl alcohol for granulation, and performing compression molding after drying to obtain a molded blank;
(5) and placing the molded blank into a sintering furnace with atmosphere regulation, and sintering in the atmosphere of nitrogen and oxygen.
Wherein, in the step (1), the main components comprise 73-74 wt% of ferric oxide, 3-4 wt% of zinc oxide and the balance of manganese oxide.
In the step (2), the temperature of the muffle furnace is 900-.
In the step (3), the time of the secondary ball milling is 60-120 min.
In the step (3), the sanding time is 30-60 min.
In the step (3), the secondary components include 500-1000ppm calcium carbonate, 200-500ppm silica, 2000-5000ppm tricobalt tetroxide, 200-600ppm zirconia, 100-200ppm niobium pentoxide, 200-1000ppm titania and 1000-2000ppm copper calcium titanate.
In the step (4), the content of the polyvinyl alcohol is 10-15 wt%, and the drying temperature is 150-300 ℃.
In the step (5), the sintering temperature is 1100-1120 ℃, the heating rate is 1-3 ℃/min during the sintering process, the heat preservation time is 3-5h, and the oxygen content in the heat preservation stage is 0.75-1.5%, preferably 1-1.25%.
The present invention will be further described with reference to the following examples.
Example 1:
the preparation method of the manganese-zinc power ferrite material comprises the following steps:
(1) 73.34 wt% of Fe2O33.30 wt% of ZnO and the balance of MnO are put into a ball mill for ball milling and mixing, and the ball milling is carried out for 30min once to obtain mixed powder;
(2) placing the mixed powder in a muffle furnace at 900 ℃ and preserving heat for 1h for pre-sintering to obtain pre-sintered powder;
(3) grinding the pre-sintered powder, performing secondary ball milling for 60min, putting into a grinding machine, and adding the auxiliary components (shown in table 1) and pure water for sanding, wherein the particle size is controlled to be 1 mu m;
(4) drying the ground slurry obtained in the step (3), adding 15 wt% of polyvinyl alcohol (PVA) for granulation, drying at 250 ℃, and then performing compression molding to obtain a molded blank;
(5) placing the formed blank into a sintering furnace with atmosphere regulation, and performing reaction on the blank in a reaction furnace N2And O2Is sintered in the atmosphere of (2). The sintering heat preservation temperature is 1100 ℃, the temperature rise rate is 2 ℃/min during the sintering process, the heat preservation time is 4h, the oxygen content in the heat preservation stage is 1.25 percent, and finally the manganese-zinc power ferrite magnetic ring with the outer diameter of 14mm, the inner diameter of 9mm and the height of 5mm is obtained.
The initial permeability, saturation magnetic induction and power loss of the prepared manganese-zinc ferrite magnetic ring were tested, and the test results are listed in table 2. Wherein:
the initial permeability test conditions were: 25 ℃ and 10 kHz.
The saturated magnetic induction intensity test conditions are as follows: 50Hz, 1194A/m, 25 ℃ and 100 ℃.
The power loss test conditions were: 1MHz-50mT, 3MHz-30mT, 5MHz-20 mT.
Example 2:
the preparation process and the main components are the same as example 1, the content of the modified additives (the auxiliary components) is shown in Table 1, the test conditions are the same as example 1, and the test results are shown in Table 2.
Comparative example 1:
the preparation process and the main components are the same as example 1, the content of the modified additives is shown in Table 1, the test conditions are the same as example 1, and the test results are shown in Table 2.
Comparative example 2:
the preparation process and the main components are the same as example 2, the content of the modified additives is shown in Table 1, the test conditions are the same as example 1, and the test results are shown in Table 2.
TABLE 1 sample numbers, corresponding specific main component ratios and additive amounts
TABLE 2 respective sample numbers and corresponding test results
As is clear from the test results of example 1 and example 2 in Table 2, by adding an appropriate amount of CaCu3Ti4O12The power loss of the manganese-zinc ferrite at 1-5MHz can be greatly reduced, and the magnetic permeability and the saturation magnetic induction intensity can not be deteriorated. CaCu3Ti4O12The loss was the lowest at 2000ppm addition, and from the test results of comparative example 2, CaCu3Ti4O12When added in excess, power losses increase again.
Therefore, the invention greatly reduces the power loss of the manganese-zinc ferrite material at 1-5MHz while keeping the performance of magnetic conductivity and saturation magnetic induction intensity not to be deteriorated through the main components and process control, the selection, the matching and the dosage control of the novel additive, and the material also has high saturation magnetic induction intensity, has excellent technical improvement effect and can meet the requirement of rapid development of electronic technology.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (10)
1. A manganese-zinc power ferrite material is characterized in that: it comprises main component and auxiliary component;
the main components comprise the following components:
73-74 wt% of ferric oxide,
3 to 4 weight percent of zinc oxide,
the balance of manganese oxide;
the accessory components comprise the following components in percentage by weight based on 100 wt% of the total mass of the main component:
2. a method for preparing a manganese-zinc power ferrite material according to claim 1, characterized in that: which comprises the following steps:
(1) mixing the main components, and performing ball milling for 30-60min to obtain mixed powder;
(2) placing the mixed powder in a muffle furnace for heat preservation and presintering to obtain presintering powder;
(3) performing secondary ball milling on the pre-sintered powder, adding auxiliary components and deionized water, and sanding, wherein the particle size is controlled to be 1-2 mu m;
(4) adding polyvinyl alcohol into the ground slurry obtained in the step (3) for granulation, drying and then performing compression molding to obtain a molded blank;
(5) and sintering the molded blank in the atmosphere of nitrogen and oxygen.
3. The method of claim 2, wherein: in the step (1), the main components comprise 73-74 wt% of ferric oxide, 3-4 wt% of zinc oxide and the balance of manganese oxide.
4. The method of claim 2, wherein: in the step (2), the heat preservation temperature of the muffle furnace is 900-.
5. The method of claim 2, wherein: in the step (3), the time of the secondary ball milling is 60-120 min.
6. The method of claim 2, wherein: in the step (3), the sanding time is 30-60 min.
7. The method of claim 2, wherein: in the step (3), the secondary components comprise 500-1000ppm calcium carbonate, 200-500ppm silicon dioxide, 2000-5000ppm cobaltosic oxide, 200-600ppm zirconium oxide, 100-200ppm niobium pentoxide, 200-1000ppm titanium dioxide and 1000-2000ppm copper calcium titanate.
8. The method of claim 2, wherein: in the step (4), the content of the polyvinyl alcohol is 10-15 wt%, and the drying temperature is 150-300 ℃.
9. The method of claim 2, wherein: in the step (5), the sintering heat preservation temperature is 1100-.
10. The method of claim 9, wherein: in the sintering process, the oxygen content in the heat preservation stage is 1-1.25%.
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| CN202110474706.1A Pending CN112979302A (en) | 2021-04-29 | 2021-04-29 | Manganese-zinc power ferrite material and preparation method thereof |
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| CN113998999A (en) * | 2022-01-04 | 2022-02-01 | 天通控股股份有限公司 | Manufacturing method of wide-temperature low-loss high-Bs manganese-zinc ferrite material |
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| CN103693952A (en) * | 2013-12-04 | 2014-04-02 | 江门安磁电子有限公司 | Preparation method of ultra-low-loss MnZn power ferrite material |
| CN110517840A (en) * | 2019-08-12 | 2019-11-29 | 无锡斯贝尔磁性材料有限公司 | A kind of high frequency wide-temperature low-loss MnZn ferrite material and preparation method thereof |
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| CN103693952A (en) * | 2013-12-04 | 2014-04-02 | 江门安磁电子有限公司 | Preparation method of ultra-low-loss MnZn power ferrite material |
| CN110517840A (en) * | 2019-08-12 | 2019-11-29 | 无锡斯贝尔磁性材料有限公司 | A kind of high frequency wide-temperature low-loss MnZn ferrite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113998999A (en) * | 2022-01-04 | 2022-02-01 | 天通控股股份有限公司 | Manufacturing method of wide-temperature low-loss high-Bs manganese-zinc ferrite material |
| CN113998999B (en) * | 2022-01-04 | 2022-04-01 | 天通控股股份有限公司 | Manufacturing method of wide-temperature low-loss high-Bs manganese-zinc ferrite material |
| WO2023130731A1 (en) * | 2022-01-04 | 2023-07-13 | 天通控股股份有限公司 | Method for manufacturing wide-temperature low-loss high-bs manganese-zinc ferrite material |
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