CN112723873B - Broadband high-impedance high-permeability MnZn soft magnetic ferrite and preparation method thereof - Google Patents
Broadband high-impedance high-permeability MnZn soft magnetic ferrite and preparation method thereof Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 43
- 238000000227 grinding Methods 0.000 claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 23
- 239000001301 oxygen Substances 0.000 claims abstract description 23
- 239000011324 bead Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004321 preservation Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 12
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 230000005484 gravity Effects 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000696 magnetic material Substances 0.000 abstract description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 2
- 235000010216 calcium carbonate Nutrition 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract description 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 229910052682 stishovite Inorganic materials 0.000 abstract description 2
- 229910052905 tridymite Inorganic materials 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract 1
- 230000035699 permeability Effects 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 239000011572 manganese Substances 0.000 description 6
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 3
- 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 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002075 main ingredient Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical class [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of magnetic materials, and discloses a broadband high-impedance high-permeability MnZn soft magnetic ferrite material and a preparation method thereof. The broadband high-impedance high-permeability MnZn soft magnetic ferrite material comprises a main component and an auxiliary component, wherein the main component comprises Fe2O3:52.5mol percent to 53.9mol percent, znO:21.3 to 23.3mol percent, the balance of Mn3O4, and the auxiliary components comprise, based on the total weight of the main components: nano CaCO3:400ppm to 1000ppm, nano Bi2O3:100ppm to 600ppm, nano Nb2O5:100ppm to 350ppm, nano SiO2:20ppm to 150ppm, nanometer MoO3:100ppm to 500ppm. The MnZn ferrite material adopts the processes of grinding by a bead mill and oxygen-enriched sintering through proper main components and nanometer doping. The Mn-Zn ferrite material has the characteristics of wide frequency band, high magnetic conductivity, high impedance and the like, so that the Mn-Zn ferrite material has better comprehensive magnetic performance and is better used for an EMI resistant assembly.
Description
Technical Field
The invention relates to a broadband high-impedance high-permeability MnZn soft magnetic ferrite and a preparation method thereof, belonging to the technical field of magnetic materials.
Background
Manganese zinc ferrite is a typical soft magnetic material and is widely applied to the fields of various recording magnetic heads for multiplex communication, switch power supplies, transformer cores, filters, audio and video recording, information storage systems, medical diagnosis, military industry and civil electromagnetic interference resistant materials. With the increasing frequency and digital of electronic equipment, the energy density of interference signals is increased, so that the electromagnetic environment in a limited space is deteriorated, and the personal safety and military safety are greatly compromised. The high-performance MnZn ferrite core is used as a magnetic medium type wave absorbing material, has unique advantages in the aspect of EMI resistance, has the function of low-pass filtering, can better solve the problem of high-frequency interference suppression of a power line, a signal line and a connector, and has good market prospect.
Researches show that the material sintering temperature can be reduced, the material frequency characteristic can be improved and the method has important guiding significance for preparing the MnZn soft magnetic ferrite with wide frequency, high impedance and high magnetic conductivity through reasonable doping, sanding and oxygen-enriched sintering processes.
The patent with publication No. CN101859621B discloses a MnZn ferrite material with high magnetic conductivity and a preparation method thereof, compared with the patent, the invention introduces Nb 2 O 5 The preparation method has the advantages that the preparation method has the effects of refining grains and improving low-frequency impedance, but can reduce the magnetic conductivity of the material, so that the growth of the grains can be promoted, the uniformity of the grains can be improved, the purpose of broadband high-impedance high-magnetic conductivity can be achieved, and the formula and the process complement each other. The patent with publication number CN101475366B discloses a broadband manganese-zinc ferrite material with high magnetic permeability, high saturation induction and high Curie temperature and a preparation method thereof, and the patent does not mention an oxygen-enriched sintering process and a high impedance direction. The patent with publication number CN101857426B discloses a preparation technology of a broadband high-impedance MnZn ferrite material, which is greatly different from the preparation technology in component technology and high-impedance application frequency band. Patent publication No. CN111056830A discloses a wide-temperature high-frequency high-impedance high-permeability Mn-Zn ferrite material and a preparation method thereof, and TiO is used in the formula 2 And NiO, which is greatly different from the formula in the technical scheme of the invention, and the process in the aspect of oxygen-enriched sintering is not mentioned. The patent with publication number CN101419858B discloses a broadband high-permeability low-loss Mn-Zn soft magnetic ferrite material and a preparation method thereof, compared with the invention, different auxiliary component systems are adopted, and the initial permeability in the patent is 9000-12000 (10 kHz), so that the ferrite material has high cutoff frequency. The initial permeability in the invention is above 15000 (10 kHz), and the high impedance characteristic, impedance coefficient ZN, is emphasized max And is more than or equal to 42.0 omega/mm. The patent publication No. CN1677579B discloses a broadband manganese-zinc series high-permeability soft magnetic ferrite material, compared with the invention, the initial permeability of the material disclosed by the patent is 10000 (10 kHz), the cutoff frequency fr is more than or equal to 400kHz, the impedance characteristic is not shown, the invention adopts an oxygen-enriched sintering process, the initial permeability of the prepared material is more than 15000 (10 kHz), and the cutoff frequency fr is lower, emphasizing the impedance characteristics: impedance coefficient ZN max And is more than or equal to 42.0 omega/mm. The above comparison document has larger difference with the invention in the aspects of formulation and process, and the MnZn soft magnetic ferrite prepared by the preparation method of the invention has better effects of wide frequency, high impedance and high magnetic permeability, which is the result obtained by the great creative labor of technicians.
Disclosure of Invention
The invention aims to provide a MnZn soft magnetic ferrite with broadband high impedance and high magnetic conductivity and a preparation method thereof. The specific technical scheme of the invention is as follows: a manganese zinc ferrite material with wide frequency band, high impedance and high magnetic conductivity is prepared from main components and auxiliary components, wherein the main components are as follows: fe (Fe) 2 O 3 :52.5mol% -53.9 mol%, znO:21.3mol percent to 23.3mol percent, the balance being Mn 3 O 4 The method comprises the steps of carrying out a first treatment on the surface of the The auxiliary components comprise, by weight based on the total mass of the main components: nano CaCO 3 :400 ppm-1000 ppm, nano Bi 2 O 3 :100 ppm-600 ppm, nano Nb 2 O 5 :100 ppm-350 ppm, nano SiO 2 :20 ppm-150 ppm, nanometer MoO 3 :100ppm to 500ppm. After the formula (particularly the formula of auxiliary components) and the preparation process (particularly the sintering process) of the magnetic material are deeply researched, the preparation method of the MnZn soft magnetic ferrite with wide frequency band and high impedance and high magnetic conductivity is developed under the condition that the adjustment of the formula content and the process parameters do not have obvious regularity.
The specific performance of the method is improved as follows: at 8mV,10kHz, magnetic permeability μ i Not less than 15000; at 200kHz, permeability μ i More than or equal to 10000; mu at 500kHz i And more than or equal to 5000. Under the test condition of 8mV, when the frequency is 100kHz, the impedance coefficient ZN is more than or equal to 8.0 omega/mm; at 500kHz, the impedance coefficient ZN is more than or equal to 34.0 omega/mm; impedance coefficient ZN in the range of 0.5MHz to 1MHz max Not less than 42.0 omega/mm; the Curie temperature Tc is more than or equal to 130 ℃. By doping nano Bi 2 O 3 Nano SiO 2 And adopting an oxygen-enriched sintering mode, reducing the sintering temperature to 1300-1400 ℃, and simultaneously having smaller grains of 15-20 mu m.
The preparation method of the MnZn soft magnetic ferrite with broadband high impedance and high magnetic conductivity comprises the following steps:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.5mol% -53.9 mol%, znO:21.3mol percent to 23.3mol percent, the balance being Mn 3 O 4 Then carrying out wet ball milling mixing for 10-40 min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering at 700-1000 ℃ at a heating rate of 1-5 ℃/min;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :400 ppm-1000 ppm, nano Bi 2 O 3 :100 ppm-600 ppm, nano Nb 2 O 5 :100 ppm-350 ppm, nano SiO 2 :20 ppm-150 ppm, nanometer MoO 3 :100 Grinding the mixture for 30 to 120 minutes by a bead mill according to the ppm to 500 ppm;
step 4: granulating: adding 3-20wt% of polyvinyl alcohol according to the total weight of the powder obtained after grinding, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm, and the density of 3.15g/cm 3 ～3.35g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300-1400 ℃, the heat preservation time is 4-8 hours, the equilibrium oxygen content is divided into two sections, and the two sections are respectively: 10.0% -20.0%, 3.0% -8.0%.
The broadband high-impedance high-permeability MnZn soft magnetic ferrite disclosed by the invention has the following technical performances, indexes and parameters:
(1) Initial permeability mu i ≥15000(T＝25℃，B<0.25mT，10kHz)；μ i ≥10000(T＝25℃，B<0.25mT，200kHz)；μ i ≥5000(T＝25℃，B<0.25mT，500kHz)；
(2) Quality factor Q <0.7 (500 khz,10ts, t25 x 15 x 7.5);
(3) At 100kHz, the impedance coefficient ZN is more than or equal to 8.0 omega/mm; at 500kHz, the impedance coefficient ZN is more than or equal to 34.0 omega/mm; resistance in the range of 0.5 to 1MHzCoefficient of resistance ZN max ≥42.0Ω/mm；
(4) Saturation induction intensity B S ≥420mT(25℃，H＝1194A/m)；
(5) Curie temperature T C ≥130℃。
Detailed Description
The broadband high-impedance high-permeability MnZn soft magnetic ferrite prepared by the invention and the preparation process are further described below through specific implementation cases. Three MnZn ferrite materials of example 1, example 2 and example 3 and four MnZn ferrite materials of comparative example 1, comparative example 2, comparative example 3 and comparative example 4 were prepared according to the following preparation methods.
Example 1: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.6mol%, znO:22.3mol% and the remainder of Mn 3 O 4 Proportioning, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: the mixture obtained in the step 1 is baked and presintered, the presintering temperature is 900 ℃, the heating rate is 5 ℃/min, and the heat preservation is carried out for 2 hours;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :700ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :150ppm, nano SiO 2 :60ppm, nanometer MoO 3 :100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300 ℃, the balance oxygen content is 15%, the temperature is kept for 1h, the oxygen content is 4%, and the temperature is kept for 5h.
Example 2: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: adopting the same main ingredient formula as in example 1, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering at 950 ℃ at a heating rate of 5 ℃/min;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :900ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :100ppm, nano SiO 2 :80ppm, nanometer MoO 3 :100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300 ℃, the heat preservation time is 6 hours, the balanced oxygen content is 10%, the heat preservation is 1 hour, the oxygen content is 4%, and the heat preservation is 5 hours.
Example 3: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.5mol%, znO:22.1mol% and the remainder of Mn 3 O 4 Proportioning, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering at 900 ℃ at a heating rate of 5 ℃/min;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: caCO (CaCO) 3 :900ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :100ppm, nano SiO 2 :80ppm, nanometer MoO 3 :100ppm, which was ground with a bead mill to 80min；
Step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: step 6: sintering: the sintering temperature is 1300 ℃, the heat preservation time is 6 hours, the balanced oxygen content is 10%, the heat preservation is 1 hour, the oxygen content is 4%, and the heat preservation is 5 hours.
Comparative example 1: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.6mol%, znO:22.3mol% and the remainder of Mn 3 O 4 Proportioning, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: the mixture obtained in the step 1 is baked and presintered, the presintering temperature is 900 ℃, the heating rate is 5 ℃/min, and the heat preservation is carried out for 2 hours;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :700ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :150ppm, nano SiO 2 :60ppm, nanometer MoO 3 :100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300 ℃, the balance oxygen content is 15%, the temperature is kept for 1h, the oxygen content is 4%, and the temperature is kept for 5h.
Comparative example 2: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.9mol%, znO:21.4mol% and the remainder of Mn 3 O 4 Proportioning, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: the mixture obtained in the step 1 is baked and presintered, the presintering temperature is 900 ℃, the heating rate is 5 ℃/min, and the heat preservation is carried out for 2 hours;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :700ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :150ppm, nano SiO 2 :60ppm, nanometer MoO 3 :100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300 ℃, the balance oxygen content is 15%, the temperature is kept for 1h, the oxygen content is 4%, and the temperature is kept for 5h.
Comparative example 3: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: adopting the same main ingredient formula as in comparative example 1, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering at 950 ℃ at a heating rate of 5 ℃/min;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO 3 :900ppm, nano Bi 2 O 3 :200ppm, nano Nb 2 O 5 :100ppm, nano SiO 2 :120ppm, nanometer MoO 3 :100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green body with the size phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300 ℃, the heat preservation time is 6 hours, the balanced oxygen content is 10%, the heat preservation is 1 hour, the oxygen content is 4%, and the heat preservation is 5 hours.
Comparative example 4: a kind of wide band high impedance high permeability MnZn soft magnetic ferrite material, is made up of main component and auxiliary component, the preparation method is as follows:
step 1: and (3) batching: adopting the same main ingredient formula as in comparative example 1, and then carrying out wet ball milling and mixing for 20min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering at 950 ℃ at a heating rate of 5 ℃/min;
step 3: and (5) sanding: vibration grinding is carried out on the obtained presintered material, and then auxiliary components are added: nano CaCO3:900ppm, nano Bi2O3:300ppm, nano Nb2O5:100ppm, nano SiO2:80ppm, nano MoO3:100ppm, grinding it for 80min with a bead mill;
step 4: granulating: according to the total weight of the powder obtained after grinding, adding 15wt% of polyvinyl alcohol, grinding and sieving to obtain particles with a certain size;
step 5: and (5) press forming: pressing into annular green bodies with the dimensions phi 25mm phi 15mm phi 7.5mm and the density of 3.2g/cm3;
step 6: sintering: the sintering temperature is 1300 ℃, the heat preservation time is 6 hours, and the oxygen content is 4 percent.
The test results of the magnetic permeability at different frequencies of the examples and the comparative examples are shown in the following table:
the results of the frequency impedance coefficient tests for the examples and comparative examples are shown in the following table:
the comparison examples and comparative examples show that: by adopting proper composition of main components and auxiliary components and optimizing the sintering process of the material (oxygen-enriched sintering), the impedance and the magnetic permeability of the material are greatly improved. The initial magnetic permeability of the comparative examples is about 11000, the initial magnetic permeability of the examples can reach more than 15000, the impedance coefficient of the examples at 500 kHz-800 kHz has great advantages, and the impedance of the 500kHz is improved by more than 25% compared with that of the comparative examples.
The foregoing is merely some embodiments of the present invention, and the scope of the present invention is not limited thereto.
Claims (3)
1. A broadband high-impedance high-permeability MnZn ferrite material is characterized by comprising a main component and an auxiliary component, wherein the main component comprises Fe 2 O 3 :52.5mol percent to 53.9mol percent, znO:21.3mol% to 23.3mol% and the balance Mn 3 O 4 The auxiliary components comprise, by total weight of the main components: nano CaCO 3 :400ppm to 1000ppm, nano Bi 2 O 3 :100ppm to 600ppm, nano Nb 2 O 5 :100ppm to 350ppm, nano SiO 2 :20 ppm-150 ppm, nanometer MoO 3 :100ppm to 500ppm, the grain size is smaller than 20 mu m,
the preparation method of the MnZn ferrite material with broadband high impedance and high magnetic conductivity comprises the following steps:
step 1: and (3) batching: fe (Fe) 2 O 3 :52.5mol percent to 53.9mol percent, znO:21.3mol% to 23.3mol% and the balance of Mn 3 O 4 Proportioning, and then carrying out wet ball milling and mixing for 10-40 min;
step 2: presintering: drying the mixture obtained in the step 1, and presintering for 1-3 hours at 700-1000 ℃;
step 3: and (5) sanding: vibration grinding is carried out on the presintering material obtained in the step 2, and then auxiliary components are added: nano CaCO 3 :400ppm to 1000ppm, nano Bi 2 O 3 :100ppm to 600ppm, nano Nb 2 O 5 :100ppm to 350ppm, nano SiO 2 :20 ppm-150 ppm, nanometer MoO 3 : grinding for 30-120 min by a bead mill with the concentration of 100-500 ppm;
step 4: granulating: drying and granulating the ground slurry;
step 5: and (5) press forming: pressing into annular green body with the dimensions of phi 25mm multiplied by phi 15mm multiplied by 7.5mm, and the density of 3.15g/cm 3 ～3.35g/cm 3 ；
Step 6: sintering: the sintering temperature is 1300-1400 ℃, the heat preservation time is 4-8 hours, and the balanced oxygen content is divided into two sections, which are respectively: 10.0 to 20.0 percent and 3.0 to 8.0 percent, and the reaction can be fully carried out by an oxygen-enriched sintering mode to ensure that Fe 3+ Increase, inhibit zinc volatilization at the same time, promote grain growth, improve grain uniformity, and reduce sintering temperature.
2. The broadband high-impedance high-permeability MnZn ferrite material according to claim 1, wherein the presintering is carried out in air in the step 2, the presintering temperature is 700-1000 ℃, and the heating rate is 1-5 ℃/min.
3. The broadband high-impedance high-permeability MnZn ferrite material according to claim 1, wherein the grinding time of the bead mill in the step 3 is 30-120 min, and the grinding beads have a heavier specific gravity and fall down in the grinding process by using the bead mill, so that the raw material generates up-and-down convection in a grinding cylinder with pressure, the raw material is pressurized in a gap between the grinding beads and rotated at a high speed to form a more uniform particle size distribution in the cross-over impact, and the particle size of the raw material is reduced.
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