CN110937887A - High-frequency low-loss MnZn ferrite material and preparation method thereof - Google Patents
High-frequency low-loss MnZn ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of magnetic materials, and discloses a high-frequency low-loss MnZn ferrite material and a preparation method thereof. The high-frequency low-loss MnZn ferrite material comprises a main component and an auxiliary component, wherein the main component comprises 68.5-73.5% of Fe by mass fraction2O32.5-5.5% of ZnO, and the balance of Mn3O4The auxiliary components comprise the following components in percentage by weight based on the total weight of the main components: 200-800ppm CaCO3200-600ppm V2O5100-500ppm ZrO2100-800ppm Nb2O51000-2O3100-500ppm NiO. The MnZn ferrite material of the inventionThe method is matched with and added with a proper amount of main components and auxiliary components, the pre-sintering process of the pre-sintering material is strictly controlled, and the low-temperature sintering process is adopted, so that the cost of the ferrite is reduced on the basis of keeping the performances of high initial permeability, saturated magnetic induction intensity and the like, and meanwhile, lower high-frequency (1MHz) loss is obtained at 100 ℃.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a high-frequency low-loss MnZn ferrite material and a preparation method thereof.
Background
The soft magnetic ferrite is an important component material with the most varieties, the widest application and the largest dosage, and is made into various elements such as transformers, inductors, filters and the like due to the excellent performances such as high magnetic conductivity, high Bs, low high-frequency loss and the like, and is widely applied to communication, televisions, mobile phones, base stations and the like.
With the progress of science and technology, electronic components are gradually becoming smaller, miniaturized, and high-frequency, and lower loss is required. At present, the power consumption of the manganese-zinc ferrite is reduced mainly from the aspects of optimization of a formula, improvement of a preparation method and the like so as to meet industrial requirements.
Disclosure of Invention
The invention aims to further reduce the loss of ferrite materials and provides a high-frequency low-loss MnZn ferrite material and a preparation method thereof.
To achieve the object of the present invention, a high-frequency low-loss MnZn ferrite material of the present invention comprises a main component and an auxiliary component, wherein the main component contains 68.5-73.5% by mass of Fe2O32.5-5.5% of ZnO, and the balance of Mn3O4The auxiliary components comprise the following components in percentage by weight based on the total weight of the main components: 200-800ppm CaCO3200-600ppm V2O5100-500ppm ZrO2100-800ppm Nb2O51000-2O3100-500ppm NiO.
Preferably, the main component contains 69.0-70.0% by mass of Fe2O33.0-4.0% of ZnO, and the balance of Mn3O4The auxiliary components comprise the following components in percentage by weight based on the total weight of the main components: 350-450ppm CaCO3250-350ppm V2O5250 and 350ppm ZrO2、450-550ppm Nb2O51000-2200ppm of Co2O3200-450ppm NiO.
The ferrite is prepared by adding a trace amount of Ni element into MnZn ferrite, and has low loss (less than or equal to 110 kW/m) when T is 100 ℃, f is 1MHz and B is 50mT on the basis of maintaining the performances of high initial permeability, high saturation magnetic flux density and the like3) Performance is in the leading position in the industry.
Further, the invention also provides a high-frequency low-loss MnZn ferrite material and a preparation method thereof, wherein the method comprises the following steps:
(1) carrying out wet ball milling mixing on the main components, namely carrying out primary ball milling, wherein the material: ball: water 1: 6: 1, spraying after ball milling;
(2) pre-burning the primary ball-milling spray material obtained in the step (1), and then cooling;
(3) adding auxiliary components after the step (2) is finished, and performing secondary ball milling to obtain the following materials: ball: the water ratio is the same as that of the primary ball milling, and the mixture is subjected to spray granulation and molding;
(4) and carrying out low-temperature sintering, wherein the sintering temperature of the low-temperature sintering is 900-1100 ℃.
Further, the ball milling medium in the steps (1) and (3) is silicon carbon steel.
Further, the pre-sintering temperature in the step (2) is 700-900 ℃, for example 790-810 DEG C
Further, the air in the step (2) is used as a presintering atmosphere, the temperature rising rate is 1-3 ℃/min, the temperature is raised to the presintering temperature, and then the temperature is preserved for 2-4 h and then the air is cooled.
Further, the granularity of the secondary ball-milled powder in the step (3) is controlled to be 0.8-1.5 mu m, and PVA (polyvinyl alcohol) is added during spray granulation.
Further, the adding amount of PVA in the step (3) is 8-10% of the mass of the mixture obtained by secondary ball milling.
Further, the step (3) is formed into a pressed magnetic ring.
Further, the size of the magnetic ring is phi 12.5mm phi 7.5mm 7 mm.
Further, the sintering device in the step (4) is a bell jar furnace capable of strictly controlling the atmosphere.
Preferably, the sintering temperature of the low-temperature sintering in the step (4) is 980-1020 ℃.
Further, in the step (4), the low-temperature sintering is carried out by heating to the sintering temperature at the speed of 1-3 ℃/min, keeping the temperature for 2-6 h under the oxygen partial pressure of 0.05-3%, then cooling to 20-25 ℃ at the speed of 1-4 ℃/min, and the oxygen content in the cooling stage is 0-1.5%.
The preparation method adopts a solid phase method process, the grain size of the sintered sample is 0.8-1.5 mu m, the sintered sample has high initial permeability, high saturation magnetic flux density and high Curie temperature, the loss of the existing soft magnetic ferrite when the frequency is 1MHz is reduced, and the cost is reduced by adopting low-temperature sintering.
The high-frequency low-loss MnZn ferrite material of the invention achieves the following technical properties, indexes and parameters:
(1) initial permeability
μi≥900(T＝25℃，B<0.25mT)；
(2) Magnetic loss
Pcv≤110kW/m3(T＝100℃，f＝1MHz，B＝50mT)；
(3) Saturation magnetic induction
Bs≥540mT(25℃，H＝1194A/m)；
Bs≥450mT(100℃，H＝1194A/m)；
Compared with the prior art, the MnZn ferrite material disclosed by the invention is matched with and added with a proper amount of main components and auxiliary components, the pre-sintering process of the pre-sintering material is strictly controlled, the low-temperature sintering process is adopted, the cost of the ferrite is reduced on the basis of keeping the performances of high initial permeability, saturated magnetic induction strength and the like, and meanwhile, the low high-frequency (1MHz) loss is obtained at 100 ℃, and the MnZn ferrite material is in the leading level of the industry.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Is prepared from Fe2O369.5 percent of ZnO, 3.5 percent of ZnO and the balance of Mn3O4Mixing the three main raw materials by primary ball milling, presintering at 700 ℃ to prepare a presintering material, and adding an auxiliary component CaCO3Is 400ppm, V2O5300ppm, ZrO2300ppm, Co2O32000ppm, Nb2O5500ppm NiO and 400ppm NiO, performing secondary ball milling, mixing uniformly, performing spray granulation (adding PVA), pressing into a magnetic ring with the size of phi 12.5mm phi 7.5mm phi 7mm, and preparing the magnetic ring according to the methodThe preparation method (wherein the pre-sintering heating rate is 2 ℃/min, the PVA addition amount during spray granulation is 9% of the mixture mass after the secondary ball milling, the temperature is raised to 1000 ℃ at the speed of 2 ℃/min in the sintering process, the heat preservation time is set to 4h, the oxygen content in the heat preservation stage is set to 1.8%, the temperature is reduced to 25 ℃ at the speed of 2.5 ℃/min, and the oxygen content in the temperature reduction stage is 1.0%), after sintering in a bell jar furnace with strictly controlled atmosphere, the performance is tested, and the results are shown in Table 1.
Example 2
The pre-sintering temperature was increased to 750 ℃, the other components and the preparation method thereof were the same as in example 1, and the results of the performance test are shown in table 1.
Example 3
The pre-sintering temperature was raised to 800 ℃, the other components and the preparation method thereof were the same as in example 1, and the results of the performance test are shown in table 1.
Example 4
The pre-sintering temperature was raised to 850 ℃, the other components and the preparation method thereof were the same as in example 1, and the results of the performance test are shown in table 1.
Example 5
The pre-sintering temperature was increased to 900 ℃, the other components and the preparation method thereof were the same as in example 1, and the results of the performance test are shown in table 1.
TABLE 1 initial permeability μ i, saturation induction Bs, magnetic loss Pcv of the samples of examples 1-5
It can be seen from the results of examples 1-5 that the ferrite material prepared according to the formulation of the present invention has already undergone a solid phase reaction from above 700 ℃, and all of them have incomplete reaction with the increase of the pre-sintering temperature, and have a certain influence on the performance of the material, and the ferrite material with relatively good performance can be obtained by keeping the reaction at 800 ℃.
Comparative example 1
The amount of NiO added to the auxiliary components in example 3 was reduced to 0ppm, and the other components and other production methods were the same as in example 3, and the results of the performance test were shown in Table 2.
Comparative example 2
The amount of NiO added as an auxiliary component in example 3 was reduced to 100ppm, and other components and other production methods were the same as in example 3, and the results of the performance test were shown in Table 2.
Comparative example 3
The amount of NiO added as an auxiliary component in example 3 was reduced to 200ppm, and other components and other production methods were the same as in example 3, and the results of the performance test were shown in Table 2.
Comparative example 4
The amount of NiO added to the auxiliary components in example 3 was increased to 600ppm, and the other components and other preparation methods were the same as in example 3, and the results of the performance test were shown in Table 2.
TABLE 2 initial permeability μ i, saturation induction, magnetic loss Pcv of the samples of comparative examples 1 to 4
Addition of NiO can cause Ni to react2+Ions (radius of 0.072nm, atomic weight of 58.7) enter MnZn ferrite with face-centered cubic structure to replace Mn2+Ions (with radius of 0.08nm and atomic weight of 54.94) reduce the lattice constant of MnZn ferrite, increase molecular weight, reduce crystal grains, reduce porosity and improve compactness of MnZn material by matching with proper sintering process, and reduce the magnetocrystalline anisotropy constant K of MnZn ferrite after Ni substitution1And a magnetostriction coefficient lambdas, the saturation magnetic induction Bs is increased, and the magnetic conductivity is improved. However, when Ni reaches a critical value, it overcompensates for the magnetostriction coefficient λ s of the ferrite, but increases it, resulting in magnetic conductanceThe rate drops instead.
Comparative example 5
The amount of PVA added during spray granulation in example 3 was changed to 5% by mass of the mixture after the secondary ball milling, the other preparation methods were the same as in example 3, and the results of the performance test are shown in table 3.
Comparative example 6
The amount of PVA added during spray granulation in example 3 was changed to 15% of the mass of the mixture after the secondary ball milling, the other preparation methods were the same as in example 3, and the results of the performance tests are shown in table 3.
TABLE 3 initial permeability μ i, saturation induction, magnetic loss Pcv of the samples of comparative examples 5 to 6
It is known from the combination of example 3 and comparative examples 5-6 that the ferrite material has poor performance at 5% PVA because the powder is not completely bonded and the delamination phenomenon occurs during the molding process due to the small amount of binder, while the ferrite material has poor performance at 15% PVA because the binder is too much and the binder is not completely removed during the sintering process.
Comparative example 7
Co in the auxiliary component of example 32O3The amount of (2) was reduced to 500ppm, the other components were prepared in the same manner as in example 3, and the results of the performance test are shown in Table 4.
Comparative example 8
Co in the auxiliary component of example 32O3The amount of (2) was reduced to 1000ppm, the other components were prepared in the same manner as in example 3, and the results of the performance test are shown in Table 4.
Comparative example 9
Co in the auxiliary component of example 32O3The amount of (2) was increased to 3000ppm, the other components were prepared in the same manner as in example 3, and the results of the performance test are shown in Table 4.
TABLE 4 initial permeability μ i, saturation induction, magnetic loss Pcv of the samples of comparative examples 7 to 9
Co2O3Of (5) Co2+Negative magnetocrystalline anisotropy constant K for ferrites1The compensation is carried out, the temperature characteristic of magnetic conductivity can be improved, the magnetization resistance of the material is effectively reduced, and the initial magnetic conductivity and high-frequency power consumption of the ferrite material are further improved when Co is used2O3When the amount of (A) is too large or too small, the overall properties of the material are deteriorated due to the magnetocrystalline anisotropy constant K1The value is not equal to 0, only adding proper amount of Co2O3So that the material has better performance.
As is clear from the combination of example 3 and comparative examples 7 to 9, Co2O3When the amount of (B) is 2000ppm, the MnZn ferrite can obtain a good performance.
Comparative example 10
The holding temperature in the sintering process of example 3 was set to 800 ℃, the composition and other preparation methods were the same as in example 3, and the performance test results are shown in table 5.
Comparative example 11
The holding temperature in the sintering process of example 3 was set to 900 ℃, the composition and other preparation methods were the same as in example 3, and the performance test results are shown in table 5.
Comparative example 12
The holding temperature in the sintering process of example 3 was set to 1100 ℃, the composition and other preparation methods were the same as in example 3, and the results of the performance tests are shown in table 5.
Comparative example 13
The holding temperature in the sintering process of example 3 was set to 1200 ℃, the composition and other preparation methods were the same as in example 3, and the performance test results are shown in table 5.
TABLE 5 initial permeability μ i, saturation induction, magnetic loss Pcv of the samples of comparative examples 10 to 13
The sintering temperature is an important factor directly influencing the microstructure and the magnetic performance, when sintering at low temperature, under-burning condition is generated, the grain size is greatly different, and air holes are dispersed in the grain boundary and the grain interior, so that the performance such as initial permeability, saturation magnetic induction intensity, loss and the like is reduced.
It can be seen from the combination of example 3 and comparative examples 10-13 that, for the ferrite material of the formulation of the present invention, example 3 is a preferred technical solution, and the performance of the material will be reduced to some extent by changing the sintering temperature.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (10)
1. A high-frequency low-loss MnZn ferrite material, comprising a main component and an auxiliary component, wherein the main component contains 68.5 to 73.5% by mass of Fe2O32.5-5.5% of ZnO, and the balance of Mn3O4The auxiliary components comprise the following components in percentage by weight based on the total weight of the main components: 200-800ppm CaCO3200-600ppm V2O5100-500ppm ZrO2100-800ppm Nb2O51000-2O3100-500ppm NiO.
2. According to the claimsThe high-frequency low-loss MnZn ferrite material according to claim 1, wherein the main component contains 69.0 to 70.0% by mass of Fe2O33.0-4.0% of ZnO, and the balance of Mn3O4The auxiliary components comprise the following components in percentage by weight based on the total weight of the main components: 350-450ppm CaCO3250-350ppm V2O5250 and 350ppm ZrO2450 and 550ppm Nb2O51000-2200ppm of Co2O3200-450ppm NiO.
3. A method for preparing a high frequency low loss MnZn ferrite material according to any of claims 1 to 2, characterized in that it comprises the steps of:
(1) carrying out wet ball milling mixing on the main components, namely carrying out primary ball milling, wherein the material: ball: water 1: 6: 1, spraying after ball milling;
(2) pre-burning the primary ball-milling spray material obtained in the step (1), and then cooling;
(3) adding auxiliary components after the step (2) is finished, and performing secondary ball milling to obtain the following materials: ball: the water ratio is the same as that of the primary ball milling, and the mixture is subjected to spray granulation and molding;
(4) and carrying out low-temperature sintering, wherein the sintering temperature of the low-temperature sintering is 900-1100 ℃.
4. The method for preparing a high-frequency low-loss MnZn ferrite material according to claim 3, wherein the ball milling media in the steps (1) and (3) is silicon carbon steel.
5. The preparation method of the high-frequency low-loss MnZn ferrite material according to claim 3, wherein the pre-sintering temperature in the step (2) is 700-900 ℃, for example 790-810 ℃.
6. The preparation method of the high-frequency low-loss MnZn ferrite material according to claim 3, wherein the air in the step (2) is used as a pre-sintering atmosphere, the temperature rising rate is 1-3 ℃/min, the temperature is kept for 2-4 h after the temperature is raised to the pre-sintering temperature, and then cooling is carried out.
7. The preparation method of the high-frequency low-loss MnZn ferrite material according to claim 3, wherein in the step (3), the grain size of the secondary ball-milled powder is controlled to be 0.8-1.5 μm, and PVA is added during spray granulation; preferably, the adding amount of the PVA in the step (3) is 8-10% of the mass of the mixture obtained by the secondary ball milling.
8. The method for preparing a high-frequency low-loss MnZn ferrite material according to claim 3, wherein the step (3) is performed by molding and pressing into a magnetic ring; preferably, the size of the magnetic ring is Φ 12.5mm Φ 7.5mm 7 mm.
9. The method for preparing a high-frequency low-loss MnZn ferrite material according to claim 3, wherein the sintering equipment in the step (4) is a bell jar furnace capable of strictly controlling the atmosphere; preferably, the sintering temperature of the low-temperature sintering in the step (4) is 980-1020 ℃.
10. The preparation method of the high-frequency low-loss MnZn ferrite material according to claim 3, wherein the low-temperature sintering in the step (4) is carried out by raising the temperature to the sintering temperature at a rate of 1-3 ℃/min, keeping the temperature for 2-6 h at an oxygen partial pressure of 0.05-3%, and then reducing the temperature to 20-25 ℃ at a rate of 1-4 ℃/min, wherein the oxygen content in the temperature reduction stage is 0-1.5%.
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