CN113024235A - Variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite and preparation method thereof - Google Patents

Variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite and preparation method thereof Download PDF

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CN113024235A
CN113024235A CN202110142699.5A CN202110142699A CN113024235A CN 113024235 A CN113024235 A CN 113024235A CN 202110142699 A CN202110142699 A CN 202110142699A CN 113024235 A CN113024235 A CN 113024235A
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temperature
power ferrite
wide
mol
sintering
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王伟
王继森
丁武慧
丁四海
张红安
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Zhejiang Gauss Magnetic Co ltd
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Zhejiang Gauss Magnetic Co ltd
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Abstract

The invention is suitable for the technical field of soft magnetism, and provides a frequency-conversion wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite and a preparation method thereof, wherein the MnZn power ferrite consists of a main component and an auxiliary component; the main components and the contents thereof are calculated by oxides as follows: fe2O3: 52.00-54.00 mol%, ZnO: 9.00-12.0 mol%, MnO: 35.5 to 38.5 mol% and 0.3 to 0.6 wt% of Co2O3(ii) a The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.05～0.10wt％、SiO2：0.008～0.03wt％、Sb2O3：0.03～0.10wt％、Ta2O5：0.01～0.08wt％、V2O5：0.005～0.02wt％、In2O3：0.01～0.08wt％、Nb2O5: more than four of 0.01 to 0.06 wt%. The MnZn ferrite material prepared by the invention has high frequency band and wide frequency bandThe MnZn power ferrite has the characteristics of low loss at low temperature, and a great deal of research is carried out on the sintering process, and the sintering temperature, the heat preservation time, the sintering oxygen content and the temperature rise and fall curve are improved, so that the process production has the characteristics of low cost and stable process, and the MnZn power ferrite with medium-high frequency conversion, wide temperature and low loss can be manufactured.

Description

Variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite and preparation method thereof
Technical Field
The invention belongs to the technical field of soft magnetism, relates to MnZn ferrite and a preparation method thereof, and particularly relates to frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite and a preparation method thereof.
Background
With the development of communication technology, especially the coming of commercial application of 5G communication technology, the demand and the increasing day by day for high-performance soft magnetic ferrite, as a low-loss soft magnetic MnZn power ferrite widely applied to various communication and electronic fields, the requirement on power materials is higher and higher, and the requirements are not limited to low loss, especially wide temperature and medium-high frequency loss characteristics, and the traditional PC95 has been difficult to meet the requirements of electronic products such as switching power transformers, especially automotive electronics, 5G communication switching power transformers, especially the loss requirement at the frequency of 150 to 300 KHz. The high-frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite is researched and developed on the basis of a wide-temperature low-loss material, so that the MnZn power ferrite has lower loss in a wider frequency and temperature range and a gentle loss curve change, when the MnZn power ferrite is applied to the field of 5G communication power supplies, the energy efficiency ratio is remarkably improved particularly when 5G base stations and 4G base stations are built for generations, other characteristics of the material are further improved, the requirements of the market on the comprehensive characteristics of the material are met, and the MnZn power ferrite has a wide market application prospect. The invention adopts a completely different technical scheme from the wide-temperature low-loss and high-frequency low-loss of the publication No. CN101964233A, and realizes the low-loss characteristic of the material in the wide-temperature, medium-high frequency range.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite material firstly, and aims to provide a preparation method of the material secondly.
In order to achieve the purpose of the invention, the inventor provides the following technical scheme.
The invention is realized in such a way that the MnZn power ferrite with variable frequency, wide temperature, low loss and high magnetic flux density consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O 3: 52.00-54.00 mol%, ZnO: 9.00-12.0 mol%, MnO: 35.5-38.5 mol% and 0.3-0.6 wt% of Co2O 3;
the auxiliary components based on the total weight of the main components are as follows: CaCO 3: 0.05 to 0.10 wt%, SiO 2: 0.008 to 0.03 wt%, Sb2O 3: 0.03 to 0.10 wt%, Ta2O 5: 0.01 to 0.08 wt%, V2O 5: 0.005 to 0.02 wt%, In2O 3: 0.01 to 0.08 wt%, Nb2O 5: more than four of 0.01 to 0.06 wt%.
Preferably, the main components and the contents thereof are calculated by oxides as follows: fe2O 3: 52.50-53.50 mol%, ZnO: 9.00-11.50 mol%, MnO: 36.00-37.50 mol% and 0.35-0.50 wt% of Co2O 3.
Preferably, the auxiliary components based on the total weight of the main components are as follows: CaCO 3: 0.08 wt%, SiO 2: 0.01 wt%, Sb2O 3: 0.06 wt%, Ta2O 5: 0.03 wt%, In2O 3: 0.04 wt%, Nb2O 5: 0.02 wt%.
The invention also provides a preparation method of the variable-frequency wide-temperature low-loss high-magnetic-flux-density MnZn power ferrite, which comprises the following steps of:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, the steel balls and water according to a certain proportion, and sanding for 60-240 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln, wherein the presintering temperature is 850-980 ℃, and the presintering time is 90-240 minutes;
s5, secondary sanding: mixing the presintering, the steel ball and water according to a certain proportion, adding auxiliary components, sanding for 240-420 minutes, and then passing through a magnetic mill with the frequency of 80-300 Hz;
s6, spray granulation: adding PVA (polyvinyl alcohol) with the weight of 8-10% of the secondary sand abrasive and the concentration of 5-10 wt% into the slurry in the sanding process for spray granulation, wherein the inlet temperature is 280-400 ℃, the outlet temperature is 80-150 ℃, and the process particle size is 40-200 meshes;
s7, molding: adding zinc stearate accounting for 0.08-0.10% of the weight of the granular material into the granular material, uniformly stirring, and pressing into a blank;
s8, sintering: comprises the following steps:
s81, heating the room temperature to 350-450 ℃, wherein the heating time is 8-12 hours;
s82, continuously heating to 930-1150 ℃, and reducing the oxygen content to 0-2%;
s83, continuously heating to 1280-1360 ℃, and preserving heat for 4-8 hours until the oxygen content is reduced to 1-8%;
s84, reducing the sintering temperature to 900-1050 ℃;
s85, continuously reducing the temperature to 100-200 ℃;
and S86, continuously cooling to room temperature.
Preferably, in the one-time sanding in S2, the raw materials: steel ball: the water weight ratio is 1: (4-6): (0.7-1.2).
Preferably, when sanding again in S5, the raw materials: steel ball: the water weight ratio is 1: (4-7): (0.8 to 1.2).
Preferably, the pressure at the time of molding in S7 is 3 to 10 MPa.
Preferably, the sintering in S8 comprises the steps of:
s81, heating the room temperature to 350 ℃ for 9-11 hours;
s82, continuously heating to 930 ℃, reducing the oxygen content to 0-2%, and keeping the temperature to 1100 ℃ along with the heating;
s83, heating from 1100 ℃ to 1280-1360 ℃, and preserving heat for 4-8 hours until the oxygen content is reduced to 1-8%;
s84, reducing the sintering temperature to 1050 ℃;
s85, continuously reducing the temperature to 150 ℃;
and S86, continuously cooling to room temperature.
Preferably, in S8:
the temperature rise rate of the S81 sintering procedure is 2.0 ℃/min;
the temperature rise rate of the S82 sintering procedure is 1.5 ℃/min;
the temperature rise rate of the S83 sintering procedure is 2.0 ℃/min;
the cooling rate of the S84 sintering procedure is 1.5 ℃/min;
the cooling rate of the S85 sintering procedure is 2.0 ℃/min;
s86 naturally cooling to the temperature.
Preferably, in S8, S84 and S85 are performed in an environment with an oxygen content of less than 0.01% when the temperature is decreased.
Compared with the prior art, the invention has the beneficial effects that:
1. the MnZn ferrite material prepared by the power of the invention has the characteristics of high frequency band, wide temperature range and low loss. By simultaneous addition of an auxiliary component Ta2O5、V2O5、Sb2O3、CaCO3、SiO2、In2O3、Nb2O5The ferrite can obtain lower material loss within a wider temperature range of 25-120 ℃ and a frequency range of 150-300 KHZ, and the performance of the ferrite is further optimized, so that the ferrite has better comprehensive performance.
Losses of MnZn power ferrite are composed of hysteresis losses, eddy current losses and residual losses. In order to obtain low loss in a wide temperature range of 25 ℃ to 120 ℃, CoFe with a large K1 positive value can be produced by adding Co2O3 to the main component2O4The compensation effect of Fe and Co on K1 is comprehensively utilized, the proper proportion of Fe and Co is adjusted, the corresponding mu i-T curve is relatively flat in a relatively wide temperature range, and therefore a wide-temperature low-temperature coefficient material can be obtained, in addition, a certain corresponding relation exists between the hysteresis coefficient and the magnetic permeability, the hysteresis coefficient of the material with high magnetic permeability is also small, the hysteresis coefficient of the material with low opposite magnetic permeability is large, the hysteresis coefficient has an internal relation with K1, the content of Fe and Co is adjusted, the value of K1 is close to zero, the hysteresis coefficient is reduced, and the magnetic permeability is improved, so that relatively small hysteresis loss can be obtained. In addition, Sb, Zr, Nb, Ca, In, Si and the like are addedThe element optimizes the crystal boundary, refines the grain growth and improves the loss coefficient of the material.
3. Under different frequencies, the dependence of the loss and the temperature is caused by the fact that the power loss is related to the frequency, as is known, under the low-frequency condition, the residual loss is caused by the magnetic after effect, and in order to improve the lower loss in the frequency range of 150-300 KHz, on one hand, the sintering atmosphere is controlled to ensure that the oxygen partial pressure meets the minimum value of cation keeping vacancy, and Fe must be controlled2+In an amount to destroy and provide Fe2+Conditional vacancy participation in diffusion, controlling the number of vacancies, and then adding Nb2O5、Sb2O3、Ta2O5、In2O3、V2O5And the micro oxides have the crystal structures with uniform crystal grains, few pores, high density and small internal stress, reduce the loss peak value, adjust the temperature and frequency range of the peak value application, avoid the loss peak value falling in the application temperature and frequency range, and obtain the ferrite material with small magnetic after-effect loss.
4. According to the preparation method of the ferrite material, a great deal of research is carried out on the sintering process, the sintering temperature, the heat preservation time, the sintering oxygen content and the temperature rise and drop curve are improved, the process production has the characteristics of low cost and stable process, and the MnZn power ferrite with medium-high frequency conversion, wide temperature and low loss can be prepared.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of the variable frequency wide temperature low loss high magnetic flux density MnZn power ferrite of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the invention, if not specifically, all main components are molar percentage units, all auxiliary components are weight percentage units, and all equipment, raw materials and the like can be directly purchased from the market or materials commonly used in the industry.
Example 1
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 52.60 mol%, ZnO: 10.20 mol%, MnO: 37.20 mol% and 0.3 wt% Co by weight2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.08wt％、SiO2：0.01wt％、Sb2O3：0.06wt％、Ta2O5：0.03wt％、In2O3：0.04wt％、Nb2O5：0.02wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln at the presintering temperature of 930 ℃ for 120 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 4.5: 1, adding auxiliary components, sanding for 180 minutes, and then passing through a magnetic mill with the frequency of 250 Hz;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank at the room temperature to 450 ℃ at the heating rate of 0.6 ℃/min for 11 hours;
s82, continuously heating the blank to 960 ℃ at the heating rate of 2.0 ℃/min, reducing the oxygen content to 0.5 percent, and keeping the temperature to 1100 ℃;
s83, continuously heating the blank to 1300 ℃ at the heating rate of 2.5 ℃/min, and preserving the heat for 5 hours until the oxygen content is reduced to 2.85%;
s84, reducing the sintering temperature of the blank to 1050 ℃ at the cooling rate of 2.5 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 3.3 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Example 2
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 53.00 mol%, ZnO: 9.50 mol%, MnO: 37.50 mol% and 0.3 wt% Co by weight2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.08wt％、SiO2：0.01wt％、Sb2O3：0.08wt％、Ta2O5：0.03wt％、In2O3：0.05wt％、Nb2O5：0.03wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln, wherein the presintering temperature is 950 ℃, and the presintering time is 120 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 5: 1, adding auxiliary components, sanding for 180 minutes, and then passing through a magnetic mill with the frequency of 250 Hz;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank at the room temperature to 450 ℃ at the heating rate of 0.6 ℃/min for 11 hours;
s82, continuously heating the blank to 980 ℃ at the heating rate of 2.0 ℃/min, reducing the oxygen content to 0.3%, and keeping the temperature to 1100 ℃;
s83, continuously heating the blank to 1320 ℃ at the heating rate of 2.5 ℃/min, and preserving the heat for 5 hours until the oxygen content is reduced to 3.0%;
s84, reducing the sintering temperature of the blank to 1050 ℃ at the cooling rate of 2.5 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 3.3 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Example 3
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 53.50 mol%, ZnO: 9.50 mol%, MnO: 37.00 mol% and 0.35 wt% Co by weight2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.06wt％、SiO2：0.02wt％、Sb2O3：0.06wt％、Ta2O5：0.03wt％、In2O3：0.05wt％、Nb2O5：0.05wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln, wherein the presintering temperature is 980 ℃, and the presintering time is 120 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 5: 1, adding auxiliary components, sanding for 180 minutes, and then passing through a magnetic mill with the frequency of 250 Hz;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank at the room temperature to 450 ℃ at the heating rate of 0.6 ℃/min for 11 hours;
s82, continuously heating the blank to 1000 ℃ at the heating rate of 2.0 ℃/min, reducing the oxygen content to 0.2%, and keeping the temperature to 1100 ℃;
s83, continuously heating the blank to 1330 ℃ at the heating rate of 2.5 ℃/min, and preserving the heat for 5 hours until the oxygen content is reduced to 3.2%;
s84, reducing the sintering temperature of the blank to 1050 ℃ at the cooling rate of 2.5 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 3.3 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Example 4
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 54.00 mol%, ZnO: 10.0 mol%, MnO: 36.00 mol% and 0.4 wt% Co by weight2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.08wt％、SiO2：0.01wt％、Sb2O3：0.08wt％、Ta2O5：0.05wt％、In2O3：0.05wt％、Nb2O5：0.05wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5.5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln, wherein the presintering temperature is 980 ℃, and the presintering time is 150 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 5: mixing according to the proportion of 0.8, adding auxiliary components, sanding for 210 minutes, and then passing through a magnetic mill with the frequency of 250 Hz;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank at the room temperature to 450 ℃ at the heating rate of 0.6 ℃/min for 11 hours;
s82, continuously heating the blank to 930 ℃ at the heating rate of 2.0 ℃/min, reducing the oxygen content to 0.3%, and keeping the temperature to 1100 ℃;
s83, continuously heating the blank to 1320 ℃ at the heating rate of 2.5 ℃/min, and preserving the heat for 5 hours until the oxygen content is reduced to 3.0%;
s84, reducing the sintering temperature of the blank to 1050 ℃ at the cooling rate of 2.5 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 3.3 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Comparative example 1
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 53.80 mol%, ZnO: 8.00 mol%, MnO: 36.70 mol% and 0.4 wt% Co by weight2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.10wt％、SiO2：0.01wt％、Sb2O3：0.03wt％、Ta2O5：0.03wt％、In2O3：0.03wt％、Nb2O5：0.05wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln at the presintering temperature of 850 ℃ for 90 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 5: 1, mixing in proportion, adding auxiliary components, and sanding for 180 minutes;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank to 650 ℃ at the heating rate of 2.0 ℃/min, and heating for 11 hours;
s82, continuously heating the blank to 1000 ℃ at the heating rate of 2.5 ℃/min, reducing the oxygen content to 0.5 percent, and keeping the temperature to 1100 ℃;
s83, continuously heating the blank to 1310 ℃ at a heating rate of 3.0 ℃/min, and preserving heat for 5 hours until the oxygen content is reduced to 5.0%;
s84, reducing the sintering temperature of the blank to 1000 ℃ at a cooling rate of 3.0 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 4.0 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Comparative example 2
A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite consists of a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 53.50 mol%, ZnO: 10.05 mol%, MnO: 36.00 mol% and 0.3 wt% Co by weight2O3；
Auxiliary ingredients based on the total weight of the main ingredientThe auxiliary components are as follows: CaCO3：0.06wt％、SiO2：0.005wt％、TiO2：0.10wt％、In2O3：0.02wt％、Nb2O5：0.02wt％。
A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite comprises the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, steel balls and water according to the proportion of 1: 5.5: after mixing according to the proportion of 0.8, sanding for 180 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln at the presintering temperature of 900 ℃ for 90 minutes;
s5, secondary sanding: pre-burning, steel balls and water are mixed according to the proportion of 1: 5: mixing at a ratio of 0.8, adding auxiliary components, and sanding for 180 minutes;
s6, spray granulation: adding PVA with the weight of 8% of the secondary sand grinding material and the concentration of 10 wt% into the slurry in the sand grinding for spray granulation to obtain granulation powder;
s7, molding: adding zinc stearate with the weight of 0.08 percent of the weight of the granular material into the granular material, uniformly stirring, and pressing into a green body under the pressure of 5 Mpa;
s8, sintering: comprises the following steps:
s81, heating the blank to 650 ℃ at the heating rate of 2.5 ℃/min, and the heating time is 9 hours;
s82, continuously heating the blank to 1000 ℃ at the heating rate of 3.0 ℃/min, reducing the oxygen content to 0.3%, and keeping the temperature to 1150 ℃;
s83, continuously heating the blank to 1320 ℃ at the heating rate of 3.3 ℃/min, and preserving the heat for 5 hours until the oxygen content is reduced to 3.50%;
s84, reducing the sintering temperature of the blank to 1000 ℃ at a cooling rate of 3.0 ℃/min;
s85, continuously reducing the temperature of the blank to 150 ℃ at a temperature reduction rate of 4.0 ℃/min;
and S86, continuing naturally cooling the blank to room temperature.
Performance testing
The loss values (temperature of 25-120 ℃ and frequency of 100-300 KHz) of the MnZn ferrite material samples prepared in the above examples 1-4 and comparative examples 1-2 are passed through an X fluorescence analyzer, and the final composition of the detected ferrite is consistent with the designed composition. Testing the power consumption of the ferrite by an IWATSU-8232 alternating current B-H analyzer under the conditions of 100 kHz-300 KHz and 25-120 ℃; the saturation magnetic flux density of the ferrite is tested by an IWATSU-8232 flow B-H analyzer under the conditions of 50Hz and 1194A/m.
The results of the performance tests are given in the following table:
example 1
Figure BDA0002929567130000131
Example 2
Figure BDA0002929567130000141
Example 3
Figure BDA0002929567130000142
Example 4
Figure BDA0002929567130000151
Comparative example 1
Figure BDA0002929567130000152
Comparative example 2
Figure BDA0002929567130000153
The performance test results show that compared with the comparative example, the MnZn ferrite prepared by the formula and the process has higher wide-temperature (25-120 ℃) loss characteristic and (100-300 KHz) frequency characteristic.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite is characterized by comprising a main component and an auxiliary component;
the main components and the contents thereof are calculated by oxides as follows: fe2O3: 52.00-54.00 mol%, ZnO: 9.00-12.0 mol%, MnO: 35.5 to 38.5 mol% and 0.3 to 0.6 wt% of Co2O3；
The auxiliary components based on the total weight of the main components are as follows: CaCO3：0.05～0.10wt％、SiO2：0.008～0.03wt％、Sb2O3：0.03～0.10wt％、Ta2O5：0.01～0.08wt％、V2O5：0.005～0.02wt％、In2O3：0.01～0.08wt％、Nb2O5: more than four of 0.01 to 0.06 wt%.
2. The frequency-conversion wide-temperature low-loss high-flux-density MnZn power ferrite as claimed in claim 1, wherein the main components and the contents thereof calculated as oxides are: fe2O3: 52.50-53.50 mol%, ZnO: 9.00-11.50 mol%, MnO: 36.00 to 37.50 mol% and 0.35 to 0.50 wt% of Co2O3。
3. The frequency conversion wide-temperature low-loss high-magnetic flux density MnZn as claimed in claim 1The power ferrite is characterized in that the power ferrite comprises the following auxiliary components in percentage by weight of the total weight of the main components: CaCO3：0.08wt％、SiO2：0.01wt％、Sb2O3：0.06wt％、Ta2O5：0.03wt％、In2O3：0.04wt％、Nb2O5：0.02wt％。
4. A preparation method of a frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite is characterized by comprising the following steps:
s1, batching and mixing: weighing the main components according to the proportion, mixing and uniformly mixing;
s2, primary sanding: mixing the raw materials, the steel balls and water according to a certain proportion, and sanding for 60-240 minutes;
s3, primary spray granulation: spraying and granulating the slurry which is ground and uniformly mixed for the first time, and removing water in the slurry to prepare a granular material;
s4, pre-burning: presintering the granular materials in a rotary kiln, wherein the presintering temperature is 850-980 ℃, and the presintering time is 90-240 minutes;
s5, secondary sanding: mixing the presintering, the steel ball and water according to a certain proportion, adding auxiliary components, sanding for 240-420 minutes, and then passing through a magnetic mill with the frequency of 80-300 Hz;
s6, spray granulation: adding PVA (polyvinyl alcohol) with the weight of 8-10% of the secondary sand abrasive and the concentration of 5-10 wt% into the slurry in the sanding process for spray granulation, wherein the inlet temperature is 280-400 ℃, the outlet temperature is 80-150 ℃, and the process particle size is 40-200 meshes;
s7, molding: adding zinc stearate accounting for 0.08-0.10% of the weight of the granular material into the granular material, uniformly stirring, and pressing into a blank;
s8, sintering: comprises the following steps:
s81, heating the room temperature to 350-450 ℃, wherein the heating time is 8-12 hours;
s82, continuously heating to 930-1150 ℃, and reducing the oxygen content to 0-2%;
s83, continuously heating to 1280-1360 ℃, and preserving heat for 4-8 hours until the oxygen content is reduced to 1-8%;
s84, reducing the sintering temperature to 900-1050 ℃;
s85, continuously reducing the temperature to 100-200 ℃;
and S86, continuously cooling to room temperature.
5. The preparation method of the frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite as claimed in claim 4, wherein when in S2 primary sanding, raw materials: steel ball: the water weight ratio is 1: (4-6): (0.7-1.2).
6. The preparation method of the frequency conversion wide-temperature low-loss high-magnetic flux density MnZn power ferrite as claimed in claim 4, wherein during secondary sanding in S5, raw materials: steel ball: the water weight ratio is 1: (4-7): (0.8 to 1.2).
7. The preparation method of the variable-frequency wide-temperature low-loss high-flux-density MnZn power ferrite as claimed in claim 4, wherein the pressure during molding in S7 is 3-10 MPa.
8. The method for preparing a variable frequency wide temperature low loss high flux density MnZn power ferrite as claimed in claim 4, wherein the sintering in S8 comprises the steps of:
s81, heating the room temperature to 350 ℃ for 9-11 hours;
s82, continuously heating to 930 ℃, reducing the oxygen content to 0-2%, and keeping the temperature to 1100 ℃ along with the heating;
s83, heating from 1100 ℃ to 1280-1360 ℃, and preserving heat for 4-8 hours until the oxygen content is reduced to 1-8%;
s84, reducing the sintering temperature to 1050 ℃;
s85, continuously reducing the temperature to 150 ℃;
and S86, continuously cooling to room temperature.
9. The method for preparing a variable frequency wide temperature low loss high flux density MnZn power ferrite as claimed in claim 4, wherein in S8:
the temperature rise rate of the S81 sintering procedure is 2.0 ℃/min;
the temperature rise rate of the S82 sintering procedure is 1.5 ℃/min;
the temperature rise rate of the S83 sintering procedure is 2.0 ℃/min;
the cooling rate of the S84 sintering procedure is 1.5 ℃/min;
the cooling rate of the S85 sintering procedure is 2.0 ℃/min;
s86 naturally cooling to the temperature.
10. The method for preparing a variable frequency wide temperature range low loss high flux density MnZn power ferrite as claimed in claim 4, wherein in S8, the temperature of S84 and S85 is decreased in an environment with an oxygen content of less than 0.01%.
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CN116813320A (en) * 2023-06-08 2023-09-29 浙江工业大学 MnZn ferrite for MHz frequency
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