CN112430081A - High-saturation-flux-density soft magnetic ferrite material and preparation method thereof - Google Patents
High-saturation-flux-density soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- CN112430081A CN112430081A CN202011338654.7A CN202011338654A CN112430081A CN 112430081 A CN112430081 A CN 112430081A CN 202011338654 A CN202011338654 A CN 202011338654A CN 112430081 A CN112430081 A CN 112430081A
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- 239000000463 material Substances 0.000 title claims abstract description 145
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims description 11
- 230000005291 magnetic effect Effects 0.000 claims abstract description 63
- 230000004907 flux Effects 0.000 claims abstract description 49
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 38
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 38
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 30
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 26
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910002115 bismuth titanate Inorganic materials 0.000 claims abstract description 22
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011787 zinc oxide Substances 0.000 claims abstract description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 18
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 18
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 8
- 239000002075 main ingredient Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 6
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 3
- 229940075630 samarium oxide Drugs 0.000 claims description 3
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 3
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 abstract description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052748 manganese Inorganic materials 0.000 abstract description 4
- 239000011572 manganese Substances 0.000 abstract description 4
- 230000035699 permeability Effects 0.000 description 9
- 239000000696 magnetic material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical group [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 2
- 229940075624 ytterbium oxide Drugs 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005293 ferrimagnetic effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a high saturation magnetic flux density soft magnetic ferrite material, and particularly relates to the technical field of soft magnetic ferrite materials, wherein the high saturation magnetic flux density soft magnetic ferrite material comprises main material components and auxiliary material components, wherein the main material components comprise ferric oxide, manganese oxide and zinc oxide in molar percentage, and the balance is lithium carbonate; the auxiliary material components comprise calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate. According to the invention, the rare earth oxide is added to improve the uniformity of the internal structure of the soft magnetic ferrite material, improve the saturation magnetic flux density of the soft magnetic ferrite material and reduce the coercive force and magnetic loss of the soft magnetic ferrite material, and the bismuth sodium titanate can effectively improve the Curie temperature of the zinc-manganese soft magnetic ferrite material, so that the manganese soft magnetic ferrite material still maintains stable dielectric properties in a high-temperature environment.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite materials, in particular to a high saturation magnetic flux density soft magnetic ferrite material and a preparation method thereof.
Background
When magnetization occurs at Hc of not more than 1000A/m, such a material is called a soft magnetic ferrite. The soft magnetic ferrite is a ferrimagnetic oxide with Fe2O3 as a main component and is produced by a powder metallurgy method. The soft magnetic ferrite refers to a magnetic material which is easy to be magnetized and demagnetized under the action of an external magnetic field, and is often a composite oxide obtained by sintering iron oxide and other metal oxide or metal oxides. The application of soft magnetic materials in industry started from the end of the nineteenth century, appeared with the rise of power electrician and telecommunication technologies, and the application range is extremely wide. The soft magnetic material is not only applied to the fields of household appliances, informationization, automobiles and other matching fields, but also brings continuous requirements for the production of electronic components as a main raw material. The soft magnetic material has a very low coercive force and can be magnetized repeatedly in a magnetic field, and the magnetism obtained after the external electric field is removed can be completely or mostly disappeared.
MnZn ferrite is widely used as a power transformer material in the fields of electronics and communication. The working temperature of the traditional switching power supply transformer is generally 60-100 ℃, and the working frequency is 10-100 kHz. In order to reduce the core loss of ferrite devices in the transformer operating temperature range, various studies such as the addition of additives, element substitution, and optimization of process conditions have been carried out so far to reduce the loss of ferrite cores in the transformer operating temperature range, and as switching power supplies are developed in the direction of miniaturization and energy saving, their operating frequencies are developed in the direction of high frequencies. Due to the heat generated by the transformer itself and the high operating temperature environment, such as electronic components around an automobile engine, the operating temperature of the actual transformer core is often higher, ranging from 80 to 120 ℃. This requires that the ferrite material not only have low core loss but also have a high saturation magnetic flux density in this temperature range.
However, the saturation magnetic flux density and the curie temperature of the common soft magnetic ferrite material at present are not high, and the use requirements of people cannot be met, so that the soft magnetic ferrite material with high saturation magnetic flux density and high curie temperature is urgently needed.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a high saturation magnetic flux density soft magnetic ferrite material and a preparation method thereof, and the problems to be solved by the present invention are: how to improve the high saturation magnetic flux density and the high Curie temperature of the soft magnetic ferrite.
In order to achieve the purpose, the invention provides the following technical scheme: a high saturation magnetic flux density soft magnetic ferrite material comprises main material components and auxiliary material components, wherein the main material components comprise 58.5-62.5 mol% of ferric oxide, 19.7-31.2 mol% of manganese oxide, 9.8-12.7 mol% of zinc oxide and the balance of lithium carbonate according to mol percentage;
the auxiliary material components comprise calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate, and the total weight of the auxiliary material components is 0.13-1.25 wt% of the total weight of the main material components.
In a preferred embodiment, the minor ingredients comprise the following amounts based on the total weight of the major ingredients: 0.01 to 0.05 percent of calcium carbonate, 0.05 to 0.45 percent of molybdenum trioxide, 0.05 to 0.45 percent of bismuth trioxide, 0.01 to 0.2 percent of zirconium dioxide, 0.008 to 0.015 percent of rare earth oxide and 0.05 to 0.1 percent of sodium bismuth titanate.
In a preferred embodiment, the main ingredients comprise 59.5 to 61.5mol percent of ferric oxide, 23.5 to 27.5mol percent of manganese oxide, 10.5 to 11.5mol percent of zinc oxide and the balance of lithium carbonate according to mol percent;
the auxiliary material components comprise 0.02 to 0.04 weight percent of calcium carbonate, 0.15 to 0.35 weight percent of molybdenum trioxide, 0.15 to 0.35 weight percent of bismuth trioxide, 0.08 to 0.12 weight percent of zirconium dioxide, 0.01 to 0.012 weight percent of rare earth oxide and 0.07 to 0.08 weight percent of sodium bismuth titanate.
In a preferred embodiment, the main ingredients comprise, in terms of mole percentage, 60.5 mol% of ferric oxide, 25.5 mol% of manganese oxide, 11.5 mol% of zinc oxide, and the balance of lithium carbonate;
the auxiliary material components comprise 0.03 wt% of calcium carbonate, 0.25 wt% of molybdenum trioxide, 0.25 wt% of bismuth trioxide, 0.1 wt% of zirconium dioxide, 0.012 wt% of rare earth oxide and 0.08 wt% of sodium bismuth titanate.
In a preferred embodiment, the rare earth oxide is one of lanthanum oxide, neodymium oxide, and samarium oxide.
The invention also provides a preparation method of the high saturation magnetic flux density soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing a certain amount of ferric oxide, manganese oxide, zinc oxide, lithium carbonate, calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate according to the content of the main material component and the auxiliary material component;
step two: uniformly mixing ferric oxide, manganese oxide, zinc oxide and lithium carbonate weighed in the step one, putting the mixture into a ball mill, adding deionized water, a dispersing agent and a defoaming agent, mixing and stirring for 20-40min, carrying out ball milling in the ball mill at the rotation speed of 1000r/min at room temperature, screening to obtain nanoscale powder after the ball milling is finished, and carrying out spray granulation by using a PVA (polyvinyl alcohol) granulator for later use;
step three: putting the product obtained in the step two into a rotary kiln for presintering, wherein the presintering temperature is 900-1000 ℃, the presintering time is 2-3h, nitrogen is introduced into the rotary kiln in the presintering process, and the oxygen content in the rotary kiln is controlled to be 6-8%;
step four: uniformly mixing the auxiliary material components weighed in the step one, putting the mixture into a ball mill, performing ball milling for 10-30min under the condition of 1000r/min, adding the screened nanoscale powder into the pre-sintered material in the step three after the ball milling is finished, adding 1-2 times of deionized water, performing ball milling, drying and granulating;
step five: putting the product obtained in the fourth step into a pressing mold, pressing the product into a blank under the pressure of 90-95Mpa, and naturally drying the blank in a dry and ventilated environment after pressing;
step six: putting the blank pressed and molded in the step five into a sintering furnace, heating to 740-760 ℃ at the speed of 210 ℃/h in the nitrogen atmosphere with the volume content of 0.08-0.1 percent of oxygen, and preserving the heat for 1-1.5 hours; in the nitrogen atmosphere with 0.8 to 1 percent of oxygen volume content, when the temperature is raised to 900-temperature and 920-temperature at the speed of 150 ℃/h with 140-temperature and heat preservation for 0.5 to 1 hour; in the nitrogen atmosphere with 3-5% oxygen volume content, the temperature is raised to 1380 and 1430 ℃ at the speed of 90-95 ℃/h, and the sintering heat preservation time is 2.5-3 hours; after sintering, cooling in nitrogen atmosphere with volume content of 0.08-0.1% of ferrite to obtain the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature.
In a preferred embodiment, the ball mill used in the second step and the fourth step adopts a variable frequency planetary ball mill, and when the materials are ground, the ball-to-material ratio is 3: 1.
In a preferred embodiment, the rotating speed of the rotary kiln in the pre-burning process in the step three is 3-6r/min, and the discharge amount is 350-650 kg/h.
In a preferred embodiment, the density of the blank pressed and formed in the step five is 2.85-3.06g/cm3。
In a preferred embodiment, the magnetic permeability of the soft magnetic ferrite material with high saturation magnetic flux density and high curie temperature obtained in the sixth step is 1300-2000 at room temperature, the saturation magnetic flux density is greater than or equal to 630mT, and the curie temperature is greater than or equal to 330 ℃.
The invention has the technical effects and advantages that:
1. according to the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature, which is prepared by adopting the raw material formula, lithium carbonate is added into the main material component of the traditional zinc-manganese soft magnetic ferrite material, and rare earth oxide and sodium bismuth titanate are added into the auxiliary material component, compared with the traditional zinc-manganese soft magnetic ferrite material, a small amount of lithium carbonate is added into the auxiliary material component, more lithium carbonate is added into the main material component and is mixed with the auxiliary material component after ball milling and presintering, the microstructure of the soft magnetic ferrite material can be changed, the grain size is reduced, the initial permeability of the soft magnetic ferrite material can be improved, the loss of the soft magnetic ferrite material is reduced, the rare earth oxide and sodium bismuth titanate are added into the auxiliary material component, the rare earth oxide can improve the uniformity of the internal structure of the soft magnetic ferrite material, and the saturation magnetic flux density of the soft magnetic ferrite material can be improved, the coercive force and the magnetic loss of the soft magnetic ferrite material are reduced, and the Curie temperature of the zinc-manganese soft magnetic ferrite material can be effectively improved by the bismuth sodium titanate, so that the manganese soft magnetic ferrite material still keeps stable dielectric property in a high-temperature environment;
2. according to the invention, the main material components and the auxiliary material components are ground into nanoscale powder through the variable frequency planetary ball mill, and then pre-sintering, mixing, press forming and sintering are carried out, so that the particle sizes of the main material components and the auxiliary material components can be effectively reduced, when the grain size is smaller than 100nm, the diffraction line can be widened due to grain refinement, a better nanocrystalline structure can be formed, the saturation magnetic flux density of the manganese soft magnetic ferrite material can be effectively improved, the coercive force is lower, and the magnetic loss is less.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a high saturation magnetic flux density soft magnetic ferrite material, which comprises main material components and auxiliary material components, wherein the main material components comprise 58.5 mol% of ferric oxide, 19.7 mol% of manganese oxide, 9.8 mol% of zinc oxide and the balance of lithium carbonate according to mol percentage;
the auxiliary material components comprise calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate, and the total weight of the auxiliary material components is 0.13 wt% of the total weight of the main material components.
In a preferred embodiment, the minor ingredients comprise the following amounts based on the total weight of the major ingredients: 0.01 wt% of calcium carbonate, 0.05 wt% of molybdenum trioxide, 0.05 wt% of bismuth trioxide, 0.01 wt% of zirconium dioxide, 0.008 wt% of rare earth oxide and 0.05 wt% of sodium bismuth titanate.
In a preferred embodiment, the rare earth oxide is lanthanum oxide.
The invention also provides a preparation method of the high saturation magnetic flux density soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing a certain amount of ferric oxide, manganese oxide, zinc oxide, lithium carbonate, calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate according to the content of the main material component and the auxiliary material component;
step two: uniformly mixing ferric oxide, manganese oxide, zinc oxide and lithium carbonate weighed in the step one, putting the mixture into a ball mill, adding deionized water, a dispersing agent and a defoaming agent, mixing and stirring for 30min, carrying out ball milling in the ball mill at the rotating speed of 1000r/min at room temperature, screening to obtain nanoscale powder after the ball milling is finished, and carrying out spray granulation by using a PVA (polyvinyl alcohol) granulator for later use;
step three: putting the product obtained in the step two into a rotary kiln for presintering, wherein the presintering temperature is 950 ℃, the presintering time is 2.5 hours, nitrogen is introduced into the rotary kiln in the presintering process, and the oxygen content in the rotary kiln is controlled to be 7%;
step four: uniformly mixing the auxiliary material components weighed in the step one, putting the mixture into a ball mill, carrying out ball milling for 20min under the condition of 1000r/min, adding the screened nanoscale powder into the pre-sintered material in the step three after the ball milling is finished, adding 1.5 times of deionized water, carrying out ball milling, drying and granulating;
step five: putting the product obtained in the fourth step into a pressing mold, pressing the product into a blank under the pressure of 93Mpa, and naturally drying the blank in a dry and ventilated environment after pressing;
step six: putting the blank pressed and molded in the step five into a sintering furnace, heating to 750 ℃ at the speed of 200 ℃/h in a nitrogen atmosphere with the volume content of 0.09% of oxygen, and preserving heat for 1.5 hours; heating to 910 ℃ at the speed of 145 ℃/h in a nitrogen atmosphere with the volume content of 0.9 percent of oxygen, and preserving heat for 1 hour; in a nitrogen atmosphere with 4 percent of oxygen volume content, heating to 1400 ℃ at the speed of 93 ℃/h, and sintering and preserving heat for 3 hours; and cooling in a nitrogen atmosphere with the volume content of 0.09 percent of ferrite after sintering to obtain the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature.
In a preferred embodiment, the ball mill used in the second step and the fourth step adopts a variable frequency planetary ball mill, and when the materials are ground, the ball-to-material ratio is 3: 1.
In a preferred embodiment, the rotating speed of the rotary kiln in the pre-burning process in the step three is 5r/min, and the discharge amount is 500 kg/h.
In a preferred embodiment, the density of the blank pressed and formed in the step five is 2.95g/cm3。
In a preferred embodiment, the high saturation magnetic flux density and high curie temperature soft magnetic ferrite material obtained in the sixth step has a magnetic permeability of 1500 at room temperature, a saturation magnetic flux density of 635mT, and a curie temperature of 330 ℃.
Example 2:
different from the embodiment 1, the main ingredients comprise 60.5mol percent of ferric oxide, 25.5mol percent of manganese oxide, 11.5mol percent of zinc oxide and the balance of lithium carbonate according to the mol percent;
based on the total weight of the main material components, the auxiliary material components comprise 0.03 wt% of calcium carbonate, 0.25 wt% of molybdenum trioxide, 0.25 wt% of bismuth trioxide, 0.1 wt% of zirconium dioxide, 0.012 wt% of rare earth oxide and 0.08 wt% of sodium bismuth titanate.
In a preferred embodiment, the obtained high saturation magnetic flux density and high curie temperature soft magnetic ferrite material has a magnetic permeability of 1920 at room temperature, 645mT saturation magnetic flux density and 345 ℃.
Example 3:
different from the examples 1-2, the main ingredients comprise 60.5mol percent of ferric oxide, 26.5mol percent of manganese oxide, 11.5mol percent of zinc oxide and the balance of lithium carbonate according to mol percent;
based on the total weight of the main material components, the auxiliary material components have the following percentage contents: 0.05 wt% of calcium carbonate, 0.45 wt% of molybdenum trioxide, 0.45 wt% of bismuth trioxide, 0.2 wt% of zirconium dioxide, 0.015 wt% of rare earth oxide and 0.1 wt% of sodium bismuth titanate.
In a preferred embodiment, the obtained high saturation magnetic flux density and high Curie temperature soft magnetic ferrite material has the magnetic permeability of 1560 at room temperature, the saturation magnetic flux density of 642mT and the Curie temperature of 338 ℃.
Example 4
In the preferred technical scheme, the invention provides a high saturation magnetic flux density soft magnetic ferrite material, which comprises a main material component and an auxiliary material component, wherein the main material component comprises 60.5 mol% of ferric oxide, 25.5 mol% of manganese oxide, 11.5 mol% of zinc oxide and the balance of lithium carbonate according to mol percentage;
based on the total weight of the main ingredients, the auxiliary ingredients comprise the following contents: 0.03 weight percent of calcium carbonate, 0.25 weight percent of molybdenum trioxide, 0.25 weight percent of bismuth trioxide, 0.1 weight percent of zirconium dioxide, 0.012 weight percent of rare earth oxide and 0.08 weight percent of sodium bismuth titanate.
In a preferred embodiment, the rare earth oxide is ytterbium oxide.
The invention also provides a preparation method of the high saturation magnetic flux density soft magnetic ferrite material, which comprises the following specific preparation steps:
the method comprises the following steps: weighing a certain amount of ferric oxide, manganese oxide, zinc oxide, lithium carbonate, calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate according to the content of the main material component and the auxiliary material component;
step two: uniformly mixing ferric oxide, manganese oxide, zinc oxide and lithium carbonate weighed in the step one, putting the mixture into a ball mill, adding deionized water, a dispersing agent and a defoaming agent, mixing and stirring for 30min, carrying out ball milling in the ball mill at the rotating speed of 1000r/min at room temperature, screening to obtain nanoscale powder after the ball milling is finished, and carrying out spray granulation by using a PVA (polyvinyl alcohol) granulator for later use;
step three: putting the product obtained in the step two into a rotary kiln for presintering, wherein the presintering temperature is 950 ℃, the presintering time is 2.5 hours, nitrogen is introduced into the rotary kiln in the presintering process, and the oxygen content in the rotary kiln is controlled to be 7%;
step four: uniformly mixing the auxiliary material components weighed in the step one, putting the mixture into a ball mill, carrying out ball milling for 20min under the condition of 1000r/min, adding the screened nanoscale powder into the pre-sintered material in the step three after the ball milling is finished, adding 1.5 times of deionized water, carrying out ball milling, drying and granulating;
step five: putting the product obtained in the fourth step into a pressing mold, pressing the product into a blank under the pressure of 93Mpa, and naturally drying the blank in a dry and ventilated environment after pressing;
step six: putting the blank pressed and molded in the step five into a sintering furnace, heating to 750 ℃ at the speed of 200 ℃/h in a nitrogen atmosphere with the volume content of 0.09% of oxygen, and preserving heat for 1.5 hours; heating to 910 ℃ at the speed of 145 ℃/h in a nitrogen atmosphere with the volume content of 0.9 percent of oxygen, and preserving heat for 1 hour; in a nitrogen atmosphere with 4 percent of oxygen volume content, heating to 1400 ℃ at the speed of 93 ℃/h, and sintering and preserving heat for 3 hours; and cooling in a nitrogen atmosphere with the volume content of 0.09 percent of ferrite after sintering to obtain the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature.
In a preferred embodiment, the ball mill used in the second step and the fourth step adopts a variable frequency planetary ball mill, and when the materials are ground, the ball-to-material ratio is 3: 1.
In a preferred embodiment, the rotating speed of the rotary kiln in the pre-burning process in the step three is 5r/min, and the discharge amount is 500 kg/h.
In a preferred embodiment, the density of the blank pressed and formed in the step five is 2.95g/cm3。
In a preferred embodiment, the high saturation magnetic flux density and high curie temperature soft magnetic ferrite material obtained in the sixth step has a magnetic permeability of 1500 at room temperature, a saturation magnetic flux density of 635mT, and a curie temperature of 330 ℃.
Example 5
Unlike example 4, the rare earth oxide is samarium oxide.
Taking the soft magnetic ferrite materials with high saturation magnetic flux density and high Curie temperature produced in the above examples 1, 2, 3, 4 and 5 respectively, measuring the magnetic permeability and Curie temperature of the soft magnetic ferrite material by an Agilent-4284A precision LCR instrument, and testing the saturation magnetic flux density Bs of the sample at different temperatures by a SY8218.BH analyzer, wherein the measurement results are shown in the table I:
watch 1
As can be seen from the above table, the soft magnetic ferrite material produced by the method of the present invention can be obtained by the embodiments 1, 2 and 3, and under the same processing conditions, the product obtained by using the material ratio of the embodiment 2 has the advantages of good magnetic permeability, high saturation magnetic flux density and curie temperature, and can meet the use requirements of people; through the embodiment 2, the embodiment 4 and the embodiment 5, under the condition of the same material proportion, the same amount of lanthanum oxide, ytterbium oxide and alumina is added, the action effect of the alumina on the soft magnetic ferrite material is better, and the promotion effect on the saturation magnetic flux density and Curie temperature of the soft magnetic ferrite material is better, lithium carbonate is added into the main material component of the traditional zinc-manganese soft magnetic ferrite material, rare earth oxide and bismuth sodium titanate are added into the auxiliary material component, compared with the traditional zinc-manganese soft magnetic ferrite material, a small amount of lithium carbonate is added into the auxiliary material component, the invention adds more lithium carbonate into the main material component, and the lithium carbonate is mixed with the auxiliary material component after ball milling and presintering, thereby changing the microstructure of the soft magnetic ferrite material, reducing the grain size, improving the initial permeability of the soft magnetic ferrite material and reducing the loss of the soft magnetic ferrite material, the rare earth oxide and the sodium bismuth titanate are added into the auxiliary material components, the rare earth oxide can improve the uniformity of the internal structure of the soft magnetic ferrite material, the saturation magnetic flux density of the soft magnetic ferrite material can be improved, the coercive force and the magnetic loss of the soft magnetic ferrite material are reduced, and the sodium bismuth titanate can effectively improve the Curie temperature of the zinc-manganese soft magnetic ferrite material, so that the manganese soft magnetic ferrite material still keeps stable dielectric properties in a high-temperature environment.
And finally: 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, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (10)
1. A high saturation magnetic flux density soft magnetic ferrite material comprises main material components and auxiliary material components, and is characterized in that: the main components comprise 58.5 to 62.5mol percent of ferric oxide, 19.7 to 31.2mol percent of manganese oxide, 9.8 to 12.7mol percent of zinc oxide and the balance of lithium carbonate according to mol percent;
the auxiliary material components comprise calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate, and the total weight of the auxiliary material components is 0.13-1.25 wt% of the total weight of the main material components.
2. The high saturation magnetic flux density soft magnetic ferrite material according to claim 1, wherein: based on the total weight of the main ingredients, the auxiliary ingredients comprise the following contents: 0.01 to 0.05 percent of calcium carbonate, 0.05 to 0.45 percent of molybdenum trioxide, 0.05 to 0.45 percent of bismuth trioxide, 0.01 to 0.2 percent of zirconium dioxide, 0.008 to 0.015 percent of rare earth oxide and 0.05 to 0.1 percent of sodium bismuth titanate.
3. The high saturation magnetic flux density soft magnetic ferrite material according to claim 2, wherein: the main ingredients comprise 59.5 to 61.5mol percent of ferric oxide, 23.5 to 27.5mol percent of manganese oxide, 10.5 to 11.5mol percent of zinc oxide and the balance of lithium carbonate according to the mol percent;
the auxiliary material components comprise 0.02 to 0.04 weight percent of calcium carbonate, 0.15 to 0.35 weight percent of molybdenum trioxide, 0.15 to 0.35 weight percent of bismuth trioxide, 0.08 to 0.12 weight percent of zirconium dioxide, 0.01 to 0.012 weight percent of rare earth oxide and 0.07 to 0.08 weight percent of sodium bismuth titanate.
4. The high saturation magnetic flux density soft magnetic ferrite material according to claim 2, wherein: the main ingredients comprise, by mole percentage, 60.5 mol% of ferric oxide, 25.5 mol% of manganese oxide, 11.5 mol% of zinc oxide, and the balance of lithium carbonate;
the auxiliary material components comprise 0.03 wt% of calcium carbonate, 0.25 wt% of molybdenum trioxide, 0.25 wt% of bismuth trioxide, 0.1 wt% of zirconium dioxide, 0.012 wt% of rare earth oxide and 0.08 wt% of sodium bismuth titanate.
5. The high saturation magnetic flux density soft magnetic ferrite material according to claim 1, wherein: the rare earth oxide is one of lanthanum oxide, neodymium oxide and samarium oxide.
6. The method for preparing a high saturation magnetic flux density soft magnetic ferrite material according to any one of claims 1 to 5, wherein: the preparation method comprises the following specific steps:
the method comprises the following steps: weighing a certain amount of ferric oxide, manganese oxide, zinc oxide, lithium carbonate, calcium carbonate, molybdenum trioxide, bismuth trioxide, titanium dioxide, zirconium dioxide, rare earth oxide and sodium bismuth titanate according to the content of the main material component and the auxiliary material component;
step two: uniformly mixing ferric oxide, manganese oxide, zinc oxide and lithium carbonate weighed in the step one, putting the mixture into a ball mill, adding deionized water, a dispersing agent and a defoaming agent, mixing and stirring for 20-40min, carrying out ball milling in the ball mill at the rotation speed of 1000r/min at room temperature, screening to obtain nanoscale powder after the ball milling is finished, and carrying out spray granulation by using a PVA (polyvinyl alcohol) granulator for later use;
step three: putting the product obtained in the step two into a rotary kiln for presintering, wherein the presintering temperature is 900-1000 ℃, the presintering time is 2-3h, nitrogen is introduced into the rotary kiln in the presintering process, and the oxygen content in the rotary kiln is controlled to be 6-8%;
step four: uniformly mixing the auxiliary material components weighed in the step one, putting the mixture into a ball mill, performing ball milling for 10-30min under the condition of 1000r/min, adding the screened nanoscale powder into the pre-sintered material in the step three after the ball milling is finished, adding 1-2 times of deionized water, performing ball milling, drying and granulating;
step five: putting the product obtained in the fourth step into a pressing mold, pressing the product into a blank under the pressure of 90-95Mpa, and naturally drying the blank in a dry and ventilated environment after pressing;
step six: putting the blank pressed and molded in the step five into a sintering furnace, heating to 740-760 ℃ at the speed of 210 ℃/h in the nitrogen atmosphere with the volume content of 0.08-0.1 percent of oxygen, and preserving the heat for 1-1.5 hours; in the nitrogen atmosphere with 0.8 to 1 percent of oxygen volume content, when the temperature is raised to 900-temperature and 920-temperature at the speed of 150 ℃/h with 140-temperature and heat preservation for 0.5 to 1 hour; in the nitrogen atmosphere with 3-5% oxygen volume content, the temperature is raised to 1380 and 1430 ℃ at the speed of 90-95 ℃/h, and the sintering heat preservation time is 2.5-3 hours; after sintering, cooling in nitrogen atmosphere with volume content of 0.08-0.1% of ferrite to obtain the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature.
7. The method for preparing a high saturation magnetic flux density soft magnetic ferrite material according to claim 6, wherein: and the ball mills used in the second step and the fourth step are variable frequency planetary ball mills, and the ball-material ratio is 3:1 when the materials are ground.
8. The method for preparing a high saturation magnetic flux density soft magnetic ferrite material according to claim 6, wherein: in the third step, the rotating speed of the rotary kiln in the presintering process is 3-6r/min, and the discharge amount is 350-650 kg/h.
9. The method for preparing a high saturation magnetic flux density soft magnetic ferrite material according to claim 6, wherein: the density of the blank pressed and formed in the step five is 2.85-3.06g/cm3。
10. The method for preparing a high saturation magnetic flux density soft magnetic ferrite material according to claim 6, wherein: the magnetic conductivity of the soft magnetic ferrite material with high saturation magnetic flux density and high Curie temperature obtained in the sixth step is 1300-2000 at room temperature, the saturation magnetic flux density is more than or equal to 630mT, and the Curie temperature is more than or equal to 330 ℃.
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