CN111689770A - High-temperature high-BsLow-loss soft magnetic ferrite material and preparation method thereof - Google Patents
High-temperature high-BsLow-loss soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 29
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 14
- 229910002059 quaternary alloy Inorganic materials 0.000 claims description 14
- 230000004907 flux Effects 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000011361 granulated particle Substances 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 238000000280 densification Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 230000005415 magnetization Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention provides a high-temperature high-BsA low-loss soft magnetic ferrite material and a preparation method thereof, wherein the ferrite material consists of a main component and a secondary component, and the main component is Fe respectively calculated by respective oxides2O3: 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO3、Nb2O5、Li2CO3And one or more of MgO. The preparation method comprises the steps of proportioning, mixing, presintering, sanding, granulating, molding and sintering. The invention mainly selects a high-iron formula, NiO is added into the main component, the composition contents of the main component and the auxiliary component are controlled, and particularly Li with higher specific magnetization intensity is added2CO3MgO additive and low-temperature densification sintering process are adopted to enable the soft magnetic ferrite material to have high temperature and high BsLow loss performance.
Description
Technical Field
The invention belongs to the technical field of soft magnetic ferrite materials, and particularly relates to a high-temperature high-B ferrite materialsA low-loss soft magnetic ferrite material and a preparation method thereof.
Background
With the rapid development of personal computers, information appliances, automotive electronics, and the like, demands for miniaturization and flattening of electronic devices have been made. Increase the high-temperature saturation magnetic flux density B of the magnetic coresThe converter is beneficial to reducing the volume of the converter and ensuring the normal operation of electronic devices under complex conditions such as high temperature and the like. Meanwhile, the high-temperature power consumption of the material is not too high, the power consumption is required to be a negative temperature coefficient in order to avoid the rapid increase of the temperature rise caused by the power consumption, and the temperature at the lowest point of the power consumption is higher than the working temperature, so that the electronic device is in a low-loss state when working at the working temperature, and the vicious circle between the power consumption and the temperature rise caused by the power consumption is prevented.
In recent years, high temperature high BsLow-loss soft magnetic ferrite materials have become a focus of attention in the magnetic industry.
In a Chinese published patent CN101090017A, a high saturation magnetic flux density low loss MnZn power ferrite and a preparation method thereof are disclosed, the invention relates to a high saturation magnetic flux density low loss MnZn power ferrite and a preparation method thereof; the invention develops the power consumption valley point of less than or equal to 260mW/cm under the conditions of 90 ℃, 100kHz and 200mT by accurately controlling the components and the preparation method of the material3A MnZn power ferrite having a saturation magnetic flux density of 530mT or more at 25 ℃ under 1000A/m and 50Hz and a saturation magnetic flux density of 420mT or more at 100 ℃ under 1000A/m and 50 Hz.
In chinese published patent CN102054552A, a NiMnZn ferrite material is disclosed, which is composed of a main component and an accessory component, and is characterized in that: the main component raw materials are as follows: fe2O353.2-55.7 mol%, ZnO 2-11 mol%, NiO 0-2.5 mol% but not 0, and the balance MnO; what is needed isThe accessory ingredient raw materials comprise the following components in percentage by weight of the total weight of the main ingredient raw materials: SiO 2250～200ppm，CaCO3200～1500ppm，ZrO250～500ppm，Nb2O550 to 500ppm and Na2O50 to 300 ppm. The invention also provides a preparation method of the NiMnZn ferrite material, wherein in the sintering procedure, the heating rate is 4-7 ℃/min in the temperature rise stage of 1000-1300 ℃, and the oxygen partial pressure concentration is below 0.2%; the temperature is 1300-1350 ℃, and the sintering time is 2-8 hours. The ferrite core provided by the invention has a saturation magnetic flux density of more than 450mT at 100 ℃ and a loss of 320KW/m at 100 DEG C3The following.
In chinese published patent CN102690106A, a high saturation magnetic flux density MnZn ferrite material is disclosed, which is composed of a main component and a subcomponent, wherein the main component and the content are calculated as oxides: fe2O360-68 mol%, 10-20 mol% of ZnO and the balance of MnO; the auxiliary components based on the total weight of the main components are as follows: SiO 2250～200ppm、CaCO3200～1500ppm、ZrO250～500ppm、Nb2O550 to 500ppm and V2O550 to 500 ppm. The invention also provides a preparation method of the ferrite material. The ferrite core provided by the invention has a saturation magnetic flux density of above 560mT at 25 ℃ and above 460mT at 100 ℃; volume loss at 25 ℃ is 1800kW/m3The volume loss at 100 ℃ is below 1600kW/m3The following.
High temperature saturation magnetic flux density B of the prior artsAlthough the improvement is provided, the high-temperature power consumption is still large, and the requirements of miniaturization of electronic devices and development of high output power of power supplies cannot be well met. Therefore, a high temperature high B was developedsA low loss soft magnetic ferrite material is very necessary.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-temperature high-BsA low-loss soft magnetic ferrite material and its preparing process, wherein the high-iron formula is mainly selected, NiO is added to main component, and the contents of main and auxiliary components are controlledIn particular, addition of Li having a higher specific magnetization2CO3MgO additive and low-temperature densification sintering process are adopted to enable the soft magnetic ferrite material to have high temperature and high BsLow loss performance.
The technical scheme adopted by the invention for solving the technical problem is as follows: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of main component and subsidiary component, the main component is quaternary system, and each main material includes Fe2O3: 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO3：0.04 wt%～0.12wt%、 Nb2O5：0.01wt%～0.03wt%、Li2CO3:0.01wt% -0.14 wt%, MgO: 0.005wt% -0.03 wt% of one or more of the components.
A high temperature high BsThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing;
2) pre-burning: pre-burning the mixed powder;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding and then performing secondary mixing treatment, wherein the sand grinding time is 60-100 min, and the particle size is 0.4-1.5 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank;
6) and (3) sintering: the blank is sintered in a kiln by adopting balanced oxygen partial pressure, the oxygen content is 0.1-0.5 percent at the temperature rising section of 800-1200 ℃, and the sintering temperature is 1340-1390 ℃.
Preferably, the pre-sintering temperature in the step 2) is 850-1000 ℃, and the temperature is kept for 1-2 h.
Preferably, the sintering temperature in the step 5) is 1350-1390 ℃, the equilibrium oxygen content is 1.0-4.0%, and the heat preservation time is 4-6 h.
The invention has the beneficial effects that: by controlling the composition and content of the main component and the subcomponent, Li having a high specific magnetization is added2CO3MgO additive and high-temperature high-B prepared by adopting low-temperature densification sintering processsThe power consumption of the low-loss soft magnetic ferrite core is less than 550kW/m at 100kHz and 200mT at 100 DEG C3B at 100 ℃ at 1kHz,1194A/msReaching 480mT, and the soft magnetic ferrite material has high temperature and high BsLow loss performance.
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited to these examples.
Example 1: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O356.6mol%, ZnO: 8.92mol%, NiO: 3.5mol% and the balance MnO; accessory ingredient CaCO3:0.08wt%、Li2CO30.01wt%, the above-mentioned auxiliary component is Fe2O3And calculating the total weight percentage of ZnO, MnO and NiO.
Preparation of high temperature high B described in example 1sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing for 15 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 950 ℃, and keeping the temperature for 2 hours;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 70min, and the particle size is 1.0 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank,
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.1 percent at the temperature rise section of 800-1200 ℃, the sintering temperature is 1370 ℃, the balanced oxygen content is 3.5 percent, and the heat preservation time is 5 hours.
Example 2: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O356.85mol%, ZnO: 8.6mol%, NiO: 4.0mol% and the balance MnO; accessory ingredient CaCO3:0 .05wt%、Nb2O50.02 wt%, MgO 0.03wt%, and the above-mentioned auxiliary components are Fe2O3And calculating the total weight percentage of ZnO, MnO and NiO.
Preparation of high temperature high B described in example 2sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing for 25 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 980 ℃, and keeping the temperature for 2 h;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 60min, and the particle size is 1.2 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank,
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.4 percent at the temperature rising section of 800-1200 ℃, the sintering temperature is 1390 ℃, the balanced oxygen content is 4.0 percent, and the heat preservation time is 6 hours.
Example 3: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O357mol%, ZnO: 8.0mol%, NiO: 4.2mol% and the balance MnO; accessory ingredient CaCO3:0 .08wt%、Nb2O5:0 .02wt%、Li2CO30.09 wt%, the aboveComponent (b) is Fe2O3And calculating the total weight percentage of ZnO, MnO and NiO.
Preparation of high temperature high B described in example 3sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing for 15 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 850 ℃, and keeping the temperature for 2 h;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 80min, and the particle size is 0.5 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank,
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.3 percent at the temperature rising section of 800-1200 ℃, the sintering temperature is 1360 ℃, the balanced oxygen content is 2.0 percent, and the heat preservation time is 5 hours.
Example 4: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O357.2mol%, ZnO: 7.5mol%, NiO: 4.8mol% and the balance MnO; accessory ingredient CaCO3:0 .1wt%、Nb2O50.02 wt% and MgO 0.01wt%, the above-mentioned auxiliary components being Fe2O3And calculating the total weight percentage of ZnO, MnO and NiO.
Preparation of high temperature high B described in example 4sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing for 35 min;
2) pre-burning: pre-burning the mixed powder at 990 ℃ for 1 h;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 90min, and the particle size is 1.4 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank,
6) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.5 percent at the temperature rise section of 800-1200 ℃, the sintering temperature is 1350 ℃, the balanced oxygen content is 1.5 percent, and the heat preservation time is 6 hours.
Example 5: high-temperature high-BsThe low-loss soft magnetic ferrite material consists of a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O357.4mol%, ZnO: 7.1mol%, NiO: 5.0mol% and the balance MnO; accessory ingredient CaCO3:0 .12wt%、Li2CO30.14wt%, the above-mentioned secondary components being Fe2O3And calculating the total weight percentage of ZnO, MnO and NiO.
Preparation of high temperature high B described in example 5sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing for 35 min;
2) pre-burning: pre-burning the mixed powder at 1000 deg.c for 1 hr;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding, and then performing secondary mixing treatment, wherein the sand grinding time is 100min, and the particle size is 1.3 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank,
6) and (3) sintering: sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.5 percent at the temperature rising section of 800-1200 ℃, the sintering temperature is 1340 ℃, the balanced oxygen content is 1.0 percent, and the heat preservation time is 6 hours.
The results of the performance tests on the standard rings prepared in the above five examples are as follows:
the described embodiments of the present invention are intended to be illustrative only, and various modifications, additions and substitutions may be made by those skilled in the art without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (3)
1. High-temperature high-BsThe low-loss soft magnetic ferrite material consists of main component and subsidiary component, and features that the main component is quaternary system and the main material includes Fe2O3: 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO3：0.04 wt%～0.12wt%、Nb2O5：0.01 wt%～0.03wt%、Li2CO3:0.01wt% -0.14 wt%, MgO: 0.005wt% -0.03 wt% of one or more of the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3Weighing ZnO, NiO and MnO in proportion, mixing and crushing;
2) pre-burning: pre-burning the mixed powder;
3) sanding: adding the additive into the pre-sintered material, performing vibration grinding and then performing secondary mixing treatment, wherein the sand grinding time is 60-100 min, and the particle size is 0.4-1.5 um;
4) and (3) granulation: drying the ground slurry and then granulating;
5) molding: pressing the granulated particles to obtain a required blank;
6) and (3) sintering: the blank is sintered in a kiln by adopting balanced oxygen partial pressure, the oxygen content is 0.1-0.5 percent at the temperature rising section of 800-1200 ℃, and the sintering temperature is 1340-1390 ℃.
2. High temperature high saturation magnetic flux density B according to claim 1sThe low-loss soft magnetic ferrite material is characterized in that: the pre-sintering temperature in the step 2) is 850-1000 ℃, and the heat preservation is carried out for 1-2 h.
3. High temperature high saturation magnetic flux density B according to claim 1sThe low-loss soft magnetic ferrite material is characterized in that: the sintering temperature in the step 5) is 1350-1390 ℃, the equilibrium oxygen content is 1.0-4.0 percent, and the heat preservation time is 4-6 hours.
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| CN114284023A (en) * | 2021-12-21 | 2022-04-05 | 江苏佰迪凯磁性材料有限公司 | BP52 soft magnetic material with high frequency, low loss and high Bs and preparation method thereof |
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