CN112573912A - Preparation method of medium-wide-band wide-temperature low-loss MnZn ferrite material - Google Patents
Preparation method of medium-wide-band wide-temperature low-loss MnZn ferrite material Download PDFInfo
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- CN112573912A CN112573912A CN202011357656.0A CN202011357656A CN112573912A CN 112573912 A CN112573912 A CN 112573912A CN 202011357656 A CN202011357656 A CN 202011357656A CN 112573912 A CN112573912 A CN 112573912A
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 30
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 30
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 16
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 16
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 15
- 235000010216 calcium carbonate Nutrition 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 9
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- 239000007788 liquid Substances 0.000 claims abstract description 7
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 40
- 239000001301 oxygen Substances 0.000 claims description 40
- 229910052760 oxygen Inorganic materials 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 30
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- 239000002002 slurry Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
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- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
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- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000011858 nanopowder Substances 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- -1 CO2O3 Chemical compound 0.000 claims description 3
- 230000035699 permeability Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims 2
- 239000011029 spinel Substances 0.000 claims 2
- 238000000265 homogenisation Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000000696 magnetic material Substances 0.000 abstract description 3
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- 229910002601 GaN Inorganic materials 0.000 description 2
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 2
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 241000656145 Thyrsites atun Species 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
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Abstract
The invention relates to a medium-broadband MnZn ferrite material with wide-temperature range and low-loss characteristics and a preparation method thereof. The additive is composed of Fe2O3, MnO and ZnO as main components and additive auxiliary components, wherein the mole percentage of the main components is as follows: 52.5-53.5 mol% of Fe2O3, 8.8-9.8 mol% of ZnO and the balance of MnO; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: 0.04-0.06% of CaCO3, 0.02-0.03% of Nb2O5, 0.35-0.45% of Co2O3, 0.01-0.03% of ZrO2 and 30-120 ppm of SiO2, wherein the Si element is added in a nano-scale gas atomization SiO2 mode. And performing secondary ball milling on the pre-sintered material, settling and sorting the pre-sintered material with a liquid medium, and performing granulation, pressure forming, sintering under an atmosphere/temperature control condition and the like to prepare the medium-broadband MnZn ferrite material with the characteristics of wide temperature range and low loss. The microstructure is compact and uniform in crystal grain, the power loss is low in the wide temperature range of 0-140 ℃ and the working frequency of 100-500 KHz, and the magnetic material has high saturation magnetic flux density and high magnetic conductivity.
Description
Technical Field
The invention belongs to the field of advanced preparation and application of high-performance power ferrite soft magnetic materials, relates to a preparation method of a wide-temperature (0-140 ℃) low-loss MnZn power ferrite material applied under the condition of medium and wide frequency (100-500 KHz), and relates to a material crushing process and a sintering process. The medium-frequency wide-temperature low-loss MnZn ferrite material is particularly suitable for the related application of a third-generation semiconductor device GaN high-power density converter.
Background
MnZn ferrite is a soft magnetic material widely applied to the fields of modern communication, computers, automobile electronics, national defense science and technology and the like. In recent years, with the development of third-generation semiconductor technology and microelectronic technology, there has been a demand for higher frequency and smaller size of magnetic functional devices, and in the fields of new energy vehicles, 5G communication, cloud computing servers, high-end consumer electronics, and the like, magnetic components such as transformers, inductors, and choke coils are generally operated at medium-high frequency and in a wide range of environmental temperature. The power consumption of conventional soft magnetic power ferrite materials varies greatly with temperature. In pursuit of high efficiency, low temperature rise, high power density, and high reliability, it is desirable to use magnetic components that can maintain low power consumption over a wide range of operating frequencies and operating temperatures. In recent decades, a series of wide-temperature low-power-consumption ferrite materials at home and abroad are widely applied, such as PC95 series of TDK and 3C97 series of femtomagnetic, and the working frequency is about 100KHz generally. The working frequency of the third-generation semiconductor gallium nitride device is 100-500 KHz, and in order to meet the market demand, a wide-temperature low-power-consumption MnZn ferrite material with more excellent power consumption characteristics under the frequency condition of 100-500 KHz needs to be developed.
Disclosure of Invention
The invention establishes the relationship of ferrite component composition, structural characteristics and magnetic property based on the loss mechanism of MnZn ferrite and the Snoek limit relationship of magnetic permeability and resonant frequency, and regulates and controls the magnetocrystalline anisotropy coefficient K of material grains by main component adjustment, composite doping of oxide particles and optimization of technological process1The ferrite has uniform grain refinement, magnetic domain state, grain boundary structure and components, and the like, and the purposes of wide frequency, wide temperature and low loss are achieved. Particularly, through the particle sorting in the technical process and the matching of a proper sintering system, the loss caused by the dispersion of the ferrite grain size is effectively reduced, and particularly the eddy current loss of the ferrite is reduced while the grain size of the sintered ferrite is regulated and controlled and the grain refinement is realized. The method has important guiding significance for improving and enhancing the performance of other ferrite materials.
The invention has the technical scheme that the medium-broadband wide-temperature low-loss MnZn ferrite material comprises the following main components in mole percentage: 52.5-53.5 mol% of Fe2O3, 8.8-9.8 mol% of ZnO and the balance of MnO; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: 0.04-0.06% of CaCO3, 0.02-0.03% of Nb2O5, 0.35-0.45% of Co2O3, 0.01-0.03% of ZrO2 and 30-120 ppm of SiO2, wherein the Si element is added in a nano-scale gas atomization SiO2 mode.
The invention also provides a preparation method of the medium-broadband wide-temperature low-loss MnZn ferrite material, which comprises the following specific steps:
(1) taking Fe2O3, MnO and ZnO as raw materials, carrying out metering burdening on the raw materials according to the proportion, and respectively grinding and mixing to obtain mixed powder with proper and uniform granularity; further, drying and briquetting the mixed powder, and presintering in air to synthesize partially spinel-petrochemical MnZn ferrite presintering powder;
(2) crushing the pre-sintered and synthesized materials, performing secondary ball milling in an ethanol medium, and performing sedimentation and separation on secondary ball-milled particles through a proper liquid medium (deionized water and absolute ethanol) to obtain ferrite slurry with uniform particle size; further, nano-scale additives of CaCO3, Nb2O5, CO2O3, ZrO2 and SiO2 are introduced into the ferrite slurry, and are mixed and homogenized to obtain uniformly doped ferrite powder through a spray drying process;
(3) loading the doped ferrite powder into a 25 x 15 x 8 annular die, and pressing under uniaxial pressure to prepare a ferrite annular blank, wherein the molding pressure is 300-350 Mpa, and the pressure maintaining time is 1-2 minutes;
(4) and sintering the ferrite ring biscuit subjected to compression molding in an experimental bell jar furnace to obtain the medium-broadband wide-temperature low-loss MnZn ferrite material.
In the preferable step (1), the respective grinding and mixing processes comprise independently grinding raw materials such as Fe2O3, MnO, ZnO and the like until the average particle size reaches 0.8-1.2 μm, and then mixing and grinding for 0.5-1.0 hour; preferably, the mixed powder is pressed into a material block under the pressing pressure of 50-100 MPa, and is presintered in air at the presintering temperature of 780-880 ℃ for 1-3 hours.
In the optimization step (2), sedimentation and separation of particles are carried out on the ferrite slurry subjected to secondary ball milling by using a proper liquid medium (deionized water and absolute ethyl alcohol) to obtain the ferrite slurry with the average particle size of 0.7-1.2 mu m and the deviation of 16-20%; preparing measured nano-scale powder of CaCO3, Nb2O5, CO2O3, ZrO2 and SiO2 into ethanol-based suspension by stirring and ultrasonic dispersion, wherein the average size distribution of oxide nano-crystalline grains of each component is within the range of 30-60 nm, and the addition amount of the nano-crystalline grains is based on the solid content and mass of the secondary ball-milled material obtained after sedimentation, and the mass ratio of the nano-crystalline grains is respectively as follows: 0.04-0.06% of CaCO3, 0.02-0.03% of Nb2O5, 0.35-0.45% of Co2O3, 0.01-0.03% of ZrO2 and 30-120 ppm of SiO 2; the ethanol dosage in the process is enough to meet the rheological property requirement of the slurry; further, the spherical granular powder with the average grain diameter of 0.9-1.3 mm is obtained by spray drying.
In the optimization step (3), the ferrite biscuit molding pressure is 300-350 Mpa, and the pressure maintaining time is 1-2 minutes.
In the above preferred step (4), the control of the atmosphere and temperature in the ferrite sintering process is composed of three main stages:
1) a temperature rising stage: room temperature is 5-25 ℃ to 300-400 ℃, heating rate is 1.5-2.5 ℃/min, oxygen content: 21.0 vol%; 300-400-800-900 ℃, the heating rate is 2.5-4.5 ℃/min, and the oxygen content is as follows: 21.0 vol%; 800-900 to 1250-1320 ℃, oxygen content: 0.2-0.05 vol%;
2) and (3) a heat preservation stage: keeping the temperature of 1250-1320 ℃ for 1-2 h, then quickly cooling to 1230-1280 ℃ after 0.5-1.0 h, keeping the temperature for 6-8 h, and obtaining the oxygen content: 3.0-5.0 vol%;
3) and (3) cooling: 1250-1300 ℃ to 1100-1200 ℃, cooling rate of 1.5-5.0 ℃/min, oxygen partial pressure: 2.0-1.0 vol%; keeping the temperature of 1100-1200 ℃ for 1-2 hours, and keeping the oxygen content: 2.0-1.0 vol%; 1100-1200 ℃ to 900-1000 ℃, and the oxygen content below 950 ℃ is controlled below 50ppm by adopting the equilibrium oxygen partial pressure.
Has the advantages that:
the invention provides a medium-broadband wide-temperature low-loss MnZn ferrite material and a preparation method thereof. The MnZn ferrite material has lower power loss in the use frequency of 100-500 KHz and the temperature range of 0-140 ℃. Compared with most of the existing manganese zinc ferrite materials with wide temperature range and low power consumption, the manganese zinc ferrite material can adapt to wider use frequency and temperature and has lower power loss. The power consumption Pcv of the material under different conditions is as follows:
the saturation magnetic flux density Bs under the conditions of 1194A/m and 1KHz is as follows:
25℃Bs≥540mT
100℃Bs≥420 mT
140℃Bs≥360mT
the initial permeability μ i at 25 ℃ was 3300. + -. 25%.
Drawings
FIG. 1 is a graph illustrating a sintering process of example 1;
FIG. 2 is a graph illustrating a sintering process of example 3.
The specific implementation mode is as follows:
example 1
The method for preparing the medium-wide-band wide-temperature low-loss MnZn ferrite annular magnetic core provided by the invention comprises the following preparation steps:
(1) taking high-purity Fe2O3, MnO and ZnO as raw materials, and taking 53.20 mol% of Fe2O3, 9.00 mol% of ZnO and the balance of MnO as the raw materials; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: the raw materials of 0.06 percent of CaCO3, 0.03 percent of Nb2O5, 0.45 percent of Co2O3, 0.15 percent of ZrO2 and 80ppm of SiO2 are metered and proportioned. Firstly, separately grinding raw materials such as Fe2O3, MnO, ZnO and the like until the average particle size of the raw materials reaches 0.8-1.2 mu m, and then carrying out a ball milling process for 0.5 hour to obtain uniformly mixed powder. Further, the mixed powder is pressed into blocks under 50MPa, and presintering is carried out in the air, the presintering temperature is 880 ℃, and the synthesis time is 2.5 hours;
(2) grinding and performing secondary wet ball milling on the presintered and synthesized material in an ethanol medium for 1.5 hours, settling and sorting secondary ball milling slurry particles through a liquid medium (deionized water and absolute ethanol) to obtain slurry with the average particle size of 0.7-1.2 mu m, preparing ethanol-based suspension from CaCO3, SiO2, Nb2O5, ZrO2 and Co2O3 oxide nano powder through stirring and ultrasonic dispersion, adding glue, performing ball milling and mixing for 0.5 hour, and then performing spray drying to obtain spherical particle powder with the average particle size of 1.2 mm;
(3) loading the granulated ferrite powder into an annular die, and pressing under uniaxial pressure to obtain an annular ferrite biscuit with the outer diameter of 25mm, the inner diameter of 15mm and the height of 8mm, wherein the molding pressure is 300MPa, and the pressure maintaining time is 1.5 minutes;
(4) and sintering the ferrite ring biscuit in a test bell jar furnace. The atmosphere and temperature regulation and control in the sintering process are set according to the following three main stages:
1) a temperature rising stage: room temperature 25 ℃ to 400 ℃, heating rate 1.5 ℃/min, oxygen content: 21.0 vol%; 400-900 ℃, heating rate of 2.5 ℃/min, oxygen content: 21.0 vol%; 900 to 1320 ℃, oxygen content: 0.1 vol%;
2) and (3) a heat preservation stage: keeping the temperature at 1320 ℃ for 1.5h, quickly cooling to 1250 ℃ after 50min, keeping the temperature for 8 h, wherein the oxygen content: 3.5 vol%;
3) and (3) cooling: 1250 ℃ to 1100 ℃, cooling rate 1.5 ℃/min, oxygen partial pressure: 1.5 vol%; heat preservation at 1100 ℃ for 1.0h, oxygen partial pressure: 1.5 vol%; 1100-900 deg.C, cooling rate of 1.0 deg.C/min, and oxygen content below 950 deg.C controlled to below 50ppm by adopting balanced oxygen partial pressure.
The annular magnetic core sample prepared by the steps is subjected to electromagnetic performance test, the performance parameters are shown in table 1, and the schematic diagram of the sintering process curve of the embodiment 1 is shown in fig. 1.
Table 1 example 1 magnetic ring sample performance parameters
Example 2
The method for preparing the medium-wide-band wide-temperature low-loss MnZn ferrite annular magnetic core provided by the invention comprises the following preparation steps:
(1) taking high-purity Fe2O3, MnO and ZnO as raw materials, and taking 53.20 mol% of Fe2O3, 9.00 mol% of ZnO and the balance of MnO as the raw materials; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: the raw materials of 0.06 percent of CaCO3, 0.03 percent of Nb2O5, 0.45 percent of Co2O3, 0.15 percent of ZrO2 and 80ppm of SiO2 are metered and proportioned. Firstly, separately grinding raw materials such as Fe2O3, MnO, ZnO and the like until the average particle size of the raw materials reaches 0.8-1.2 mu m, and then carrying out a ball milling process for 0.5 hour to obtain uniformly mixed powder. Further, the mixed powder is pressed into blocks under 50MPa, and presintering is carried out in the air, the presintering temperature is 880 ℃, and the synthesis time is 2.5 hours;
(2) grinding and performing secondary wet ball milling on the presintered and synthesized materials in a deionized water medium for 1.5 hours, preparing ethanol-based suspension from CaCO3, SiO2, Nb2O5, ZrO2 and Co2O3 oxide nano powder through stirring and ultrasonic dispersion, adding glue, performing ball milling and mixing for 0.5 hour, and then performing spray drying to obtain spherical particle powder with the average particle size of 1.2 mm;
(3) loading the granulated ferrite powder into an annular die, and pressing under uniaxial pressure to obtain an annular ferrite biscuit with the outer diameter of 25mm, the inner diameter of 15mm and the height of 8mm, wherein the molding pressure is 300MPa, and the pressure maintaining time is 1.5 minutes;
(4) and sintering the ferrite ring biscuit in a test bell jar furnace. The atmosphere and temperature regulation and control in the sintering process are set according to the following three main stages:
1) a temperature rising stage: room temperature 25 ℃ to 400 ℃, heating rate 1.5 ℃/min, oxygen content: 21.0 vol%; 400-900 ℃, heating rate of 2.5 ℃/min, oxygen content: 21.0 vol%; 900 to 1320 ℃, oxygen content: 0.1 vol%;
2) and (3) a heat preservation stage: keeping the temperature at 1320 ℃ for 1.5h, quickly cooling to 1250 ℃ after 50min, keeping the temperature for 8 h, wherein the oxygen content: 3.5 vol%;
3) and (3) cooling: 1250 ℃ to 1100 ℃, cooling rate 1.5 ℃/min, oxygen partial pressure: 1.5 vol%; heat preservation at 1100 ℃ for 1.0h, oxygen partial pressure: 1.5 vol%; 1100-900 deg.C, cooling rate of 1.0 deg.C/min, and oxygen content below 950 deg.C controlled to below 50ppm by adopting balanced oxygen partial pressure.
And (3) carrying out electromagnetic performance test on the annular magnetic core sample prepared by the steps, wherein the performance parameters are shown in table 2.
Table 2 example 2 magnetic ring sample performance parameters
Example 3
The method for preparing the medium-wide-band wide-temperature low-loss MnZn ferrite annular magnetic core provided by the invention comprises the following preparation steps:
1) taking high-purity Fe2O3, MnO and ZnO as raw materials, and taking 53.20 mol% of Fe2O3, 9.00 mol% of ZnO and the balance of MnO as the raw materials; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: the raw materials of 0.06 percent of CaCO3, 0.03 percent of Nb2O5, 0.45 percent of Co2O3, 0.15 percent of ZrO2 and 80ppm of SiO2 are metered and proportioned. Firstly, separately grinding raw materials such as Fe2O3, MnO, ZnO and the like until the average particle size of the raw materials reaches 0.8-1.2 mu m, and then carrying out a ball milling process for 0.5 hour to obtain uniformly mixed powder. Further, the mixed powder is pressed into blocks under 50MPa, and presintering is carried out in the air, the presintering temperature is 880 ℃, and the synthesis time is 2.5 hours;
2) grinding and performing secondary wet ball milling on the presintered and synthesized material in an ethanol medium for 1.5 hours, settling and sorting secondary ball milling slurry particles through a liquid medium (deionized water and absolute ethanol) to obtain slurry with the average particle size of 0.7-1.2 mu m, preparing ethanol-based suspension from CaCO3, SiO2, Nb2O5, ZrO2 and Co2O3 oxide nano powder through stirring and ultrasonic dispersion, adding glue, performing ball milling and mixing for 0.5 hour, and then performing spray drying to obtain spherical particle powder with the average particle size of 1.2 mm;
3) loading the granulated ferrite powder into an annular die, and pressing under uniaxial pressure to obtain an annular ferrite biscuit with the outer diameter of 25mm, the inner diameter of 15mm and the height of 8mm, wherein the molding pressure is 300MPa, and the pressure maintaining time is 1.5 minutes;
4) and sintering the ferrite ring biscuit in a test bell jar furnace. The atmosphere and temperature regulation and control in the sintering process are set according to the following three main stages:
1) a temperature rising stage: room temperature 25 ℃ to 400 ℃, heating rate 1.5 ℃/min, oxygen content: 21.0 vol%; 400-900 ℃, heating rate of 2.5 ℃/min, oxygen content: 21.0 vol%; 900 to 1320 ℃, oxygen content: 0.1 vol%;
2) and (3) a heat preservation stage: keeping the temperature at 1250 ℃ for 10 hours, wherein the oxygen content is as follows: 3.5 vol%;
3) and (3) cooling: 1250 ℃ to 1100 ℃, cooling rate 1.5 ℃/min, oxygen partial pressure: 1.5 vol%; heat preservation at 1100 ℃ for 1.0h, oxygen partial pressure: 1.5 vol%; 1100-900 deg.C, cooling rate of 1.0 deg.C/min, and oxygen content below 950 deg.C controlled to below 50ppm by adopting balanced oxygen partial pressure.
The annular magnetic core sample prepared by the steps is subjected to electromagnetic performance test, the performance parameters are shown in figure 2 in table 3, and the sintering process curve schematic diagram in example 3 is shown in figure 2.
Table 3 example 3 magnetic ring sample performance parameters
Claims (6)
1. A medium-broadband wide-temperature low-loss MnZn ferrite material is characterized by comprising the following components: the material consists of a spinel structure main crystal phase, a crystal boundary and a doping component in the crystal, wherein the spinel structure main crystal phase comprises the following chemical components: 52.5-53.5 mol% of Fe2O3, 8.8-9.8 mol% of ZnO and the balance of MnO; the additive comprises the following auxiliary components in percentage by weight of the total weight of the main components: 0.04-0.06% of CaCO3, 0.02-0.03% of Nb2O5, 0.35-0.45% of Co2O3, 0.01-0.03% of ZrO2 and 30-120 ppm of SiO2, wherein Si is added in a nano-scale gas atomization SiO2 mode, and the density of a sintered body is as follows: 4.92 +/-0.03 g/cm3The main properties are as follows:
the saturation magnetic flux density Bs under the conditions of 1194A/m and 1KHz is as follows:
25℃Bs≥540mT
100℃Bs≥420 mT
140℃Bs≥360mT
the initial permeability μ i at 25 ℃ was 3300. + -. 25%.
2. The method for preparing the MnZn ferrite material with medium broadband, wide temperature and low loss according to claim 1 comprises the following specific steps:
1) fe2O3, MnO and ZnO are used as raw materials, and the raw materials are proportioned according to the measurement of each component, and are respectively ground and mixed to obtain mixed powder with proper and uniform granularity; further pressing the mixed powder into a material block, and presintering in air to synthesize the spinel-structured MnZn ferrite powder;
2) grinding and secondarily ball-milling the pre-sintered and synthesized material in an ethanol medium, and settling and sorting secondary ball-milled slurry particles through a liquid medium (deionized water and absolute ethanol) to obtain ferrite slurry with uniform particle size; then, introducing the oxide nano powder of CaCO3, SiO2, Nb2O5, ZrO2 and Co2O3 into the ferrite slurry, mixing, performing ball milling homogenization, and performing spray drying to obtain uniformly doped ferrite powder;
3) loading the doped ferrite powder into a mold, and pressing under uniaxial pressure to form a circular ferrite biscuit with the outer diameter of 25mm, the inner diameter of 15mm and the height of 8mm, wherein the molding pressure is 300-350 MPa, and the pressure maintaining time is 1-2 minutes;
and (3) sintering the ferrite ring biscuit subjected to compression molding in an experimental bell jar furnace to obtain the medium-broadband wide-temperature low-loss MnZn ferrite material.
3. The method according to claim 2, wherein the respective grinding and mixing processes in the step (1) are that the raw materials of Fe2O3, MnO and ZnO are separately ground until the average particle size reaches 0.8-1.2 μm, and then mixed and ground for 0.5-1.0 hour; pressing the mixed powder into a material block under the pressing pressure of 50-100 MPa; the pre-sintering temperature in the air is 780-880 ℃, and the pre-sintering synthesis time is 1-3 hours.
4. The method according to claim 2, wherein in the step (2), the ferrite slurry after the secondary ball milling is subjected to sedimentation separation of particles by using a suitable liquid medium (deionized water and absolute ethyl alcohol) to obtain the ferrite slurry with the average particle size of 0.7-1.2 μm and the deviation of 16% -20%; preparing measured nano-scale powder of CaCO3, Nb2O5, CO2O3, ZrO2 and SiO2 into ethanol-based suspension by stirring and ultrasonic dispersion, wherein the average size distribution of oxide nano-crystalline grains of each component is within the range of 30-60 nm, and the addition amount of the nano-crystalline grains is based on the solid content and mass of the secondary ball-milled material obtained after sedimentation, and the mass ratio of the nano-crystalline grains is respectively as follows: 0.04-0.06% of CaCO3, 0.02-0.03% of Nb2O5, 0.35-0.45% of Co2O3, 0.01-0.03% of ZrO2 and 30-120 ppm of SiO 2; the ethanol dosage in the process is enough to meet the rheological property requirement of the slurry; further, the spherical granular powder with the average grain diameter of 0.9-1.3 mm is obtained by spray drying.
5. The method according to claim 2, wherein in the step (3), the ferrite biscuit molding pressure is 300 to 350MPa, and the dwell time is 1 to 2 minutes.
6. The method according to claim 2, wherein in step (4), the ferrite sintering process atmosphere and temperature regulation consists of three main stages:
1) a temperature rising stage: room temperature is 5-25 ℃ to 300-400 ℃, heating rate is 1.5-2.5 ℃/min, oxygen content: 21.0 vol%; 300-400-800-900 ℃, the heating rate is 2.5-4.5 ℃/min, and the oxygen content is as follows: 21.0 vol%; 800-900 to 1250-1320 ℃, oxygen content: 0.2-0.05 vol%;
2) and (3) a heat preservation stage: keeping the temperature of 1250-1320 ℃ for 1-2 h, then quickly cooling to 1230-1280 ℃ after 0.5-1.0 h, keeping the temperature for 6-8 h, and obtaining the oxygen content: 3.0-5.0 vol%;
3) and (3) cooling: 1250-1300 ℃ to 1100-1200 ℃, cooling rate of 1.5-5.0 ℃/min, oxygen partial pressure: 2.0-1.0 vol%; keeping the temperature of 1100-1200 ℃ for 1-2 hours, and keeping the oxygen content: 2.0-1.0 vol%; 1100-1200 ℃ to 900-1000 ℃, and the oxygen content below 950 ℃ is controlled below 50ppm by adopting the equilibrium oxygen partial pressure.
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| CN113956031A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | Low-loss MnZn power ferrite and preparation method thereof |
| CN113956028A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | High-temperature low-loss MnZn power ferrite and preparation method thereof |
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| CN113716950A (en) * | 2021-11-01 | 2021-11-30 | 天通控股股份有限公司 | Low-temperature sintered flexible magnetic sheet and preparation method thereof |
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| CN113956031A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | Low-loss MnZn power ferrite and preparation method thereof |
| CN113956028A (en) * | 2021-11-25 | 2022-01-21 | 横店集团东磁股份有限公司 | High-temperature low-loss MnZn power ferrite and preparation method thereof |
| CN113956031B (en) * | 2021-11-25 | 2023-02-21 | 横店集团东磁股份有限公司 | Low-loss MnZn power ferrite and preparation method thereof |
| CN114477988A (en) * | 2022-03-28 | 2022-05-13 | 天通控股股份有限公司 | Easily-formed and high-strength ferrite material and preparation method thereof |
| WO2024109951A1 (en) * | 2022-11-25 | 2024-05-30 | 横店集团东磁股份有限公司 | Wide-temperature-range material for use in low-frequency band and preparation method therefor |
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