CN106830913B - High-frequency low-loss high-saturation-flux-density soft magnetic ferrite material and preparation method thereof - Google Patents
High-frequency low-loss high-saturation-flux-density soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 41
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 26
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 230000004907 flux Effects 0.000 claims abstract description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 18
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 229910002059 quaternary alloy Inorganic materials 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000011361 granulated particle Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000004576 sand Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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Abstract
The invention discloses a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material and a preparation method thereof2O3:54.5～55.5mol%，ZnO：3.5～6mol%，Co2O3: 0.10-0.25 mol% and the balance MnO; the subcomponent includes Nb2O5、CaCO3、V2O5、ZrO2And Ta2O5One or more of them. The preparation method comprises the steps of material proportioning, sanding, presintering, sanding, heat treatment, granulation, molding and sintering. In the invention, Co is added into the main component2O3And the composition contents of the main component and the accessory component are controlled, and the sintering process is optimized, so that the soft magnetic ferrite material has the performances of high frequency, low loss and high magnetic flux density.
Description
Technical Field
The invention relates to a soft magnetic ferrite material and a preparation method thereof, in particular to a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material and a preparation method thereof.
Background
At present, soft magnetic ferrite is a material with high magnetic conductivity, high resistivity and low loss, so that the soft magnetic ferrite is widely applied to transformers, inductors, switching power supplies, communication equipment and computer electronic rectifying equipment; MnZn ferrite is an important soft magnetic ferrite material, is widely applied to the fields of electronics and communication, and is mainly used for energy storage and conversion. With the development of miniaturization, high efficiency and high energy density of electronic equipment for power conversion, on one hand, the soft magnetic ferrite material for power conversion is required to have higher and higher frequency and low loss under high working frequency, the frequency of the current switching power supply is developed to 1MHZ, and the higher frequency of 5MHz is the development direction of the future market; on the other hand, the soft magnetic ferrite material is required to have high saturation magnetic flux density to improve the direct current superposition resistance of the transformer and improve energy storage.
The MnZn ferrite core loss can be divided into three parts: hysteresis loss (Ph), eddy current loss (Pe), residual loss (Pr), for MnZn ferrite, eddy current loss and residual loss occupy the major part at higher frequencies, reducing the high frequency loss of MnZn ferrite starts mainly from the following aspects: adjusting the formula, adding additives and optimizing the process; the patent publication No. CN1038333344A discloses a high frequency low loss ferrite and its preparation method, by mixing Fe2O3The content of (2) is fixed at 54-57 mol%, the content of ZnO is limited at 0-5 mol%, and high-frequency low loss is realized, but only loss is involved, and the saturation magnetic flux density characteristic is not improved. Therefore, the development of a MnZn ferrite material with high frequency, low loss and high saturation magnetic flux density is a problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material and a preparation method thereof, wherein Co is added into a main component2O3And the composition contents of the main component and the accessory component are controlled, and the sintering process is optimized, so that the soft magnetic ferrite material has the performances of high frequency, low loss and high magnetic flux density.
The technical scheme adopted by the invention for solving the technical problem is as follows: a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O3:54.5～55.5mol%，ZnO ：3.5～6mol%，Co2O30.10 to 0.25mol% and the balance MnO; the subcomponent includes Nb2O5:0.01～0.03wt%、CaCO3:0.04～0.20wt%、V2O5:0.01～0.05wt%、ZrO2:0～0.01wt%、Ta2O50 to 0.05wt% of one or more of them.
The preparation method of the high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material comprises the following steps of:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding;
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 grinding time is 40-90 min, and the particle size is 0.1-1.0 um;
4) and (3) heat treatment: carrying out heat treatment on the ground slurry at 600-900 ℃;
5) and (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank;
7) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.1-0.5% at the temperature rise section of 800-1100 ℃, and the sintering temperature is 1180-1300 ℃.
Preferably, the pre-sintering temperature in the step 2) is 700-1000 ℃, and the heat is preserved for 1-2 hours.
Preferably, the heat treatment temperature in the step 4) is 700-850 ℃, the heat treatment time is 3-5 h, the treated particle size is 0.3-1.1 um, and the particle size distribution is 0.2-2.0 um accounting for more than 90%.
Preferably, the sintering temperature in the step 6) is 1200-1300 ℃, the equilibrium oxygen content is 2.0-4.0%, and the heat preservation time is 3-5 h.
The invention has the beneficial effects that the power consumption of the prepared high-frequency ferrite core at 100 ℃ under 1MHz 50mT is less than 100kW/m by controlling the composition and the content of the main component and the auxiliary component and optimizing the sintering process3The power consumption of 100 ℃ at 5MHz and 10mT is less than 100kW/m3And the saturation magnetic flux density at 100 ℃ reaches 450mT, so that the soft magnetic ferrite material has the performances of high frequency, low loss and high magnetic flux density.
Detailed Description
Example 1: a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material is composed of main component and auxiliary componentThe main component is a quaternary system, and each is Fe2O3:54.96mol%，ZnO：5.66mol% ，Co2O3: 0.10mol% and the balance MnO; subcomponent Nb2O5:0.02wt%、CaCO3:0.10wt%、V2O5:0.03wt%、ZrO20.01wt%, the above-mentioned auxiliary component is Fe2O3、ZnO、MnO、Co2O3The total weight percent of (c) is calculated.
A preparation method of the high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material of embodiment 1 comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding 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 60min, and the particle size is 0.5 um;
4) and (3) heat treatment: and (3) carrying out heat treatment on the ground slurry at 700 ℃ for 5 hours, wherein the particle size after the heat treatment is 0.7um, and the particle size distribution is 0.2-2.0 um and accounts for more than 90%.
5) And (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank,
7) and (3) sintering: 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 800-1100 ℃, the sintering temperature is 1240 ℃, the balanced oxygen content is 3.5 percent, and the heat preservation time is 4 hours;
example 2: a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O3:55.36mol%，ZnO：4.00mol% ，Co2O3: 0.20mol% and the balance MnO; subcomponent Nb2O5:0.02wt%、CaCO3:0.05wt%、V2O5:0.03wt%、ZrO20.01wt%, the above-mentioned auxiliary component is Fe2O3、ZnO、MnO、Co2O3The total weight percent of (c) is calculated.
A preparation method of the high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material of embodiment 2 includes the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding for 20 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 900 ℃, 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 50min, and the particle size is 0.7 um;
4) and (3) heat treatment: and (3) carrying out heat treatment on the ground slurry at 850 ℃ for 3h, wherein the particle size after the heat treatment is 0.9um, and the particle size distribution is 0.2-2.0 um and accounts for more than 90%.
5) And (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank;
7) and (3) sintering: sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.3 percent at the temperature rise section of 800-1100 ℃, the sintering temperature is 1260 ℃, the balanced oxygen content is 4.0 percent, and the heat preservation time is 5 hours;
example 3: a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O3:55.40mol%，ZnO：3.77mol% ，Co2O3: 0.20mol% and the balance MnO; subcomponent Nb2O5:0.02wt%、CaCO3:0.10wt%、V2O5:0.03wt%、Ta2O50.03wt%, the above-mentioned secondary components being Fe2O3、ZnO、MnO、Co2O3The total weight percent of (c) is calculated.
A preparation method of the high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material of embodiment 3 includes the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding for 15 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 750 ℃, 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 0.2 um;
4) and (3) heat treatment: and (3) carrying out heat treatment on the ground slurry at 700 ℃ for 3 hours, wherein the particle size after the heat treatment is 0.4um, and the particle size distribution is 0.2-2.0 um and accounts for more than 90%.
5) And (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank;
7) and (3) sintering: sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.2 percent at the temperature rise section of 800-1100 ℃, the sintering temperature is 1230 ℃, the balanced oxygen content is 3.2 percent, and the heat preservation time is 4 hours
Example 4: a high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component is a quaternary system and is respectively Fe2O3:55.11mol%，ZnO：3.14mol% ，Co2O3: 0.25mol% and the balance MnO; subcomponent Nb2O5:0.02wt%、CaCO3:0.15wt%、V2O5:0.03wt%、ZrO2:0.005wt%、Ta2O50.02wt%, the above-mentioned secondary components being Fe2O3、ZnO、MnO、Co2O3The total weight percent of (c) is calculated.
A preparation method of the high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material of embodiment 4 comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding for 30 min;
2) pre-burning: pre-burning the mixed powder, wherein the pre-burning temperature is 960 ℃, and keeping the temperature 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 0.3 um;
4) and (3) heat treatment: and (3) carrying out heat treatment on the ground slurry at 800 ℃ for 3 hours, wherein the particle size after the heat treatment is 0.5um, and the particle size distribution is 0.2-2.0 um and accounts for more than 90%.
5) And (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank;
7) 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 rise section of 800-1100 ℃, the sintering temperature is 1200 ℃, the balanced oxygen content is 2.0 percent, and the heat preservation time is 5 hours.
The results of the performance tests on the standard rings prepared in the above four examples are as follows:
the foregoing is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that modifications can be made without departing from the preparation method of the present invention, and these modifications are also considered to be within the protection scope of the present invention.
Claims (4)
1. A high-frequency low-loss high-saturation magnetic flux density soft magnetic ferrite material is composed of a main component and auxiliary components, and is characterized in that the main component is a quaternary system and is respectively Fe2O3:54.5～55.5mol%，ZnO ：3.5～6mol%，Co2O30.10 to 0.25mol% and the balance MnO; the subcomponent includes Nb2O5:0.01～0.03wt%、CaCO3:0.04～0.20wt%、V2O5:0.01～0.05wt%、ZrO2:0～0.01wt%、Ta2O50 to 0.05wt% of one or more of; the preparation method comprises the following steps:
1) preparing materials: adopting quaternary system formula according to main formula Fe2O3、ZnO、Co2O3Weighing the mixture according to the proportion of MnO, mixing and sanding;
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 grinding time is 40-90 min, and the particle size is 0.1-1.0 um;
4) and (3) heat treatment: carrying out heat treatment on the ground slurry at 600-900 ℃;
5) and (3) granulation: drying the ground slurry and then granulating;
6) molding: pressing the granulated particles to obtain a required blank;
7) and (3) sintering: and sintering the blank in a kiln by adopting balanced oxygen partial pressure, wherein the oxygen content is 0.1-0.5% at the temperature rise section of 800-1100 ℃, and the sintering temperature is 1180-1300 ℃.
2. The high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material as claimed in claim 1, wherein: the pre-sintering temperature in the step 2) is 700-1000 ℃, and the heat is preserved for 1-2 hours.
3. The high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material as claimed in claim 1, wherein: the heat treatment temperature in the step 4) is 700-850 ℃, the heat treatment time is 3-5 h, the treated particle size is 0.3-1.1 um, and the particle size distribution is 0.2-2.0 um, which accounts for more than 90%.
4. The high-frequency low-loss high-saturation-flux-density soft magnetic ferrite material as claimed in claim 1, wherein: the sintering temperature in the step 6) is 1200-1260 ℃, the equilibrium oxygen content is 2.0-4.0%, and the heat preservation time is 3-5 h.
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| CN109273231B (en) * | 2018-08-28 | 2021-02-12 | 江西尚朋电子科技有限公司 | Preparation method of soft magnetic electronic material |
| CN111233451A (en) * | 2018-11-28 | 2020-06-05 | 泰州茂翔电子器材有限公司 | High Bs, high frequency and low loss magnetic material |
| CN110444361B (en) * | 2019-09-09 | 2020-09-22 | 天通瑞宏科技有限公司 | Preparation method of high-frequency high-saturation magnetic flux density ferrite, inductor and transformer |
| CN111233452B (en) * | 2019-10-18 | 2021-09-17 | 横店集团东磁股份有限公司 | High-frequency high-impedance lean iron manganese zinc ferrite and preparation method thereof |
| CN111039666A (en) * | 2019-12-26 | 2020-04-21 | 天通控股股份有限公司 | Manganese zinc ferrite material with ultrahigh saturation magnetic flux density and preparation method thereof |
| CN111892395B (en) * | 2020-07-29 | 2021-09-14 | 天通控股股份有限公司 | High-frequency high-impedance manganese-zinc ferrite material and preparation method thereof |
| JP2022067365A (en) * | 2020-10-20 | 2022-05-06 | 株式会社トーキン | MnZn-based ferrite |
| CN112552037B (en) * | 2020-12-11 | 2024-05-24 | 江门安磁电子有限公司 | Low-loss ferrite material and preparation method thereof |
| CN112723873B (en) * | 2021-02-05 | 2023-06-02 | 天通控股股份有限公司 | Broadband high-impedance high-permeability MnZn soft magnetic ferrite and preparation method thereof |
| CN113121218A (en) * | 2021-04-06 | 2021-07-16 | 南通冠优达磁业股份有限公司 | Wide-temperature high-frequency low-loss soft magnetic ferrite material and preparation method thereof |
| CN113277840B (en) * | 2021-05-10 | 2023-05-12 | 天通控股股份有限公司 | High-frequency high-working-density low-loss manganese zinc ferrite and preparation method thereof |
| CN113480302B (en) * | 2021-09-03 | 2021-11-09 | 天通控股股份有限公司 | Wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and preparation method thereof |
| CN113563062B (en) | 2021-09-24 | 2021-11-30 | 天通控股股份有限公司 | Ultrahigh-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method thereof |
| CN115536379B (en) * | 2022-10-24 | 2023-09-05 | 苏州天源磁业股份有限公司 | High-frequency low-loss soft magnetic ferrite material and preparation method and application thereof |
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