CN111848148B - High Bs nickel-zinc ferrite and preparation method thereof - Google Patents
High Bs nickel-zinc ferrite and preparation method thereof Download PDFInfo
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 27
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 27
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 22
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000004615 ingredient Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 10
- 239000011118 polyvinyl acetate Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000001238 wet grinding Methods 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 22
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 11
- 239000011787 zinc oxide Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- 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 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
The invention provides a high Bs nickel-zinc ferrite which comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.5-50.0 mol%, NiO 23.1-26.5 mol%, ZnO 22.8-26.8 mol%, and CuO 0.1-0.2 mol%; the accessory ingredient comprises B2O3、P2O5、Al2O3And SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O3 0.01～0.05wt％，P2O5 0.01～0.05wt％，Al2O3 0.01～0.03wt％，SiO20.01 to 0.02 wt%. The ferrite material adjusts the standing position of an atomic structure by adjusting the content and the proportion of a main component and an auxiliary component, obtains higher atomic magnetic moment and further obtains higher Bs; in addition, the ferrite grains are fused tightly to obtain a compact magnet, so that high sintering density is obtained, and the requirement of power inductance on miniaturization and high current of the ferrite material is met. The invention also provides a preparation method of the nickel-zinc ferrite.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite, in particular to nickel zinc ferrite with high Bs and a preparation method thereof.
Background
Currently, commercial ferrite materials are mainly manganese zinc ferrite and nickel zinc ferrite, wherein the nickel zinc ferrite has the characteristics of high resistivity, high cut-off frequency and the like, and is widely applied to power inductors of DC-DC and AC-DC converters. With the development of miniaturization and high frequency of devices, the requirement for the direct current superposition performance of inductance products is higher and higher. For nickel zinc ferrite materials, Bs requirements of the corresponding materials are also increasing.
Chinese patent application publication No. CN102603279A discloses a high-strength high-Bs nickel suitable for power inductorZinc ferrite and a preparation method thereof. The nickel-zinc ferrite comprises the main components of iron oxide, nickel oxide, zinc oxide and copper oxide, and the contents of the respective standard substances are as follows: fe2O349-52.5 mol% of NiO, 20-29.5 mol% of NiO, 18-28 mol% of ZnO and 2.5-5 mol% of CuO; the accessory components comprise calcium carbonate, cobalt oxide, zirconium oxide, lithium carbonate, vanadium pentoxide and silicon dioxide, and the content of the accessory components relative to the total amount of the main components is as follows by respective standard substances: CaCO3 0.03～0.15wt％，Co2O3 0.01～0.05wt％，ZrO2 0.03～0.13wt％，Li2CO3 0.03～0.10wt％，V2O5 0.03～0.15wt％，SiO20.01 to 0.10 wt%. It is prepared by oxide method, CaCO is added into the auxiliary component3With SiO2The thickness of a crystal boundary is increased in a combined mode, the relative loss factor of a high-frequency band is reduced, sintering is carried out under a certain condition, the size of crystal grains of a sintered product is 3-5 mu m, and the requirements of miniaturization of a power inductor on high strength and high direct current bias of a material are met.
In ferrite materials, the composition and the addition amount of the subcomponents are different, and the subcomponents have influence on the properties of the ferrite such as sintering temperature, crystal structure and the like, so that the components and the mixture ratio of the nickel-zinc ferrite are not studied by persons skilled in the art, and the requirements of miniaturization and large current are met.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a nickel zinc ferrite with high Bs, which is characterized in that the standing position of an atomic structure is adjusted by adjusting the content and the proportion of a main component and an auxiliary component to obtain higher atomic magnetic moment and further obtain higher Bs; in addition, the ferrite grains are fused tightly to obtain a compact magnet, so that high sintering density is obtained, and the requirement of power inductance on miniaturization and high current of the ferrite material is met. The invention also provides a preparation method of the nickel-zinc ferrite.
In order to achieve the purpose, the invention provides the following technical scheme:
the high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole:
Fe2O3 49.5～50.0mol％，NiO 23.1～26.5mol％，ZnO 22.8～26.8mol％，CuO 0.1～0.2mol％；
the accessory ingredient comprises B2O3、P2O5、Al2O3And SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows:
B2O3 0.01～0.05wt％，P2O5 0.01～0.05wt％，Al2O3 0.01～0.03wt％，SiO20.01～0.02wt％。
as a further description of the technical solution of the present invention, the contents of the minor components based on the total mass of the major components are: b is2O3 0.03wt％，P2O5 0.03wt％，Al2O3 0.02wt％，SiO20.015wt％。
As a further description of the technical solution of the present invention, the Al2O3Is nano alumina, the SiO2Is nano silicon dioxide.
Nano alumina and nano silica are mainly used for properly inhibiting the excessive growth of crystal grains during sintering, reducing the generation of pores in a magnet, and then rapidly sintering at a high temperature to obtain a high sintering density (Ds).
The invention also provides a preparation method of the nickel-zinc ferrite, which sequentially comprises the following steps:
s1, mixing: preparing the raw materials according to the mol percentage of the main components, and mixing the raw materials by a dry method for 120-180 minutes;
s2, pre-burning: pre-burning the mixed material of S1 in a pushed slab kiln;
s3, crushing: adding the accessory ingredients into the main component pre-fired material obtained in the step S2, and then carrying out wet grinding to obtain slurry;
s4, granulation: adding PVA (polyvinyl acetate) which is 1.4 percent of the weight of the slurry into the slurry of the S3, and performing spray granulation to obtain granules;
s5, pressing: pressing the granules of the S4 by a powder forming machine to obtain a blank;
s6, sintering: and sintering the blank in a resistance furnace, controlling the sintering temperature to be 1200-1250 ℃, preserving the heat for 30-60 minutes, wherein the sintering atmosphere is air, and cooling to room temperature along with the furnace after sintering.
Further, in the step S2, the pre-sintering temperature is controlled to be 800 +/-20 ℃, and the pre-sintering time is 400-600 minutes.
Further, in the step S3, the grinding time is 240 to 360 minutes, and the particle size of the ground slurry is controlled to be 0.6 to 0.8 μm.
Further, in the S5, the pressing density of the blank is controlled to be 3.3 +/-0.15 g/cm3。
The specification parameters of the prepared nickel-zinc ferrite magnetic ring sample are T13 multiplied by 8 multiplied by 3, and the performance indexes are as follows:
(1) initial permeability μi：350(1±10％)
(2) Saturation magnetic induction Bs: 520(1 + -5%) mT, with a test electric field of 8000A/cm.
Based on the technical scheme, the invention has the following technical effects:
(1) the high Bs nickel-zinc ferrite provided by the invention adopts a reasonable formula of main components and auxiliary components, and Fe is adjusted in the main components2O3The contents of NiO and ZnO are used for adjusting the station positions of A position and B position in the atomic structure of the material, thereby obtaining higher atomic magnetic moment and higher Bs; the main component of CuO is mainly to lower the sintering temperature, so that the sintering temperature of the material is lowered to 1300 ℃ or lower.
(2) The nickel-zinc ferrite of the invention is added with nano Al in the accessory components2O3And nano SiO2Mainly for the purpose of properly suppressing the excessive growth of crystal grains during sintering, reducing the generation of pores in the magnet, and then obtaining a high sintering density (Ds) by rapid sintering at a high temperature. The material has the characteristic of high Bs under an electric field of 8000A/m, and meets the requirement of power inductance on miniaturization and high current of a ferrite material.
Drawings
Fig. 1 is a view comparing the microstructure of the nickel zinc ferrite of example 1 of the present invention with that of comparative example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the accompanying drawings and specific examples. The invention provides a preferred embodiment. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
The high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.8 mol%, NiO 25.5 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5Nano Al2O3And nano SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O30.03wt％，P2O50.03 wt% of nano Al2O30.02 wt% of nano SiO20.015wt％。
The nickel-zinc ferrite is prepared by the following preparation method, and sequentially comprises the following steps:
s1, mixing: preparing the raw materials according to the mol percentage of the main components, and mixing the raw materials by a dry method for 150 minutes;
s2, pre-burning: pre-burning the mixed material of S1 in a pushed slab kiln; controlling the presintering temperature to be 800 +/-20 ℃ and the presintering time to be 500 minutes;
s3, crushing: adding the accessory ingredients into the main component pre-fired material obtained in the step S2, and then carrying out wet grinding to obtain slurry; the crushing time is 300 minutes, and the particle size of the ground slurry after crushing is controlled to be 0.6-0.8 mu m;
s4, granulation: adding PVA (polyvinyl acetate) which is 1.4 percent of the weight of the slurry into the slurry of the S3, and performing spray granulation to obtain granules;
s5, pressing: pressing the granules of the S4 by a powder forming machine to obtain a blank; the pressed density of the blank is controlled to be 3.3 +/-0.15 g/cm3；
S6, sintering: and sintering the blank in a resistance furnace, controlling the sintering temperature at 1200 ℃, keeping the temperature for 50 minutes, and cooling the blank to room temperature along with the furnace after sintering is finished.
Example 2
The high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.8 mol%, NiO 25.5 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5Nano Al2O3And nano SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O30.02wt％，P2O50.01 wt% of nano Al2O30.03 wt% of nano SiO20.01wt％。
The nickel-zinc ferrite is prepared by the following preparation method, and sequentially comprises the following steps:
s1, mixing: preparing the materials according to the mol percentage of the main components, and mixing the materials by a dry method for 120 minutes;
s2, pre-burning: pre-burning the mixed material of S1 in a pushed slab kiln; controlling the presintering temperature to be 800 +/-20 ℃ and the presintering time to be 450 minutes;
s3, crushing: adding the accessory ingredients into the main component pre-fired material obtained in the step S2, and then carrying out wet grinding to obtain slurry; the crushing time is 280 minutes, and the particle size of the ground slurry after crushing is controlled to be 0.6-0.8 mu m;
s4, granulation: adding PVA (polyvinyl acetate) which is 1.4 percent of the weight of the slurry into the slurry of the S3, and performing spray granulation to obtain granules;
s5, pressing: pressing the granules of the S4 by a powder forming machine to obtain a blank; the pressed density of the blank is controlled to be 3.3 +/-0.15 g/cm3；
S6, sintering: and sintering the blank in a resistance furnace, controlling the sintering temperature at 1200 ℃, keeping the temperature for 50 minutes, and cooling the blank to room temperature along with the furnace after sintering is finished.
Example 3
The high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.8 mol%, NiO 25.5 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5Nano Al2O3And nano SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O30.04wt％，P2O50.02 wt% of nano Al2O30.01 wt% of nano SiO20.02wt％。
The preparation method of the nickel zinc ferrite is the same as that of the embodiment 2.
Example 4
The high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.8 mol%, NiO 25.5 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5Nano Al2O3And nano SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O30.05wt％，P2O50.05 wt% of nano Al2O30.02 wt% of nano SiO20.01wt％。
The nickel-zinc ferrite is prepared by the following preparation method, and sequentially comprises the following steps:
s1, mixing: preparing the materials according to the mol percentage of the main components, and mixing the materials by a dry method for 180 minutes;
s2, pre-burning: pre-burning the mixed material of S1 in a pushed slab kiln; controlling the presintering temperature to be 800 +/-20 ℃ and the presintering time to be 600 minutes;
s3, crushing: adding the accessory ingredients into the main component pre-fired material obtained in the step S2, and then carrying out wet grinding to obtain slurry; the crushing time is 360 minutes, and the particle size of the ground slurry after crushing is controlled to be 0.6-0.8 mu m;
s4, granulation: adding PVA (polyvinyl acetate) which is 1.4 percent of the weight of the slurry into the slurry of the S3, and performing spray granulation to obtain granules;
s5, pressing: pressing the granules of the S4 by a powder forming machine to obtain a blank; the pressed density of the blank is controlled to be 3.3 +/-0.15 g/cm3；
S6, sintering: and sintering the blank in a resistance furnace, controlling the sintering temperature at 1250 ℃, keeping the temperature for 50 minutes, and cooling the blank to room temperature along with the furnace after sintering, wherein the sintering atmosphere is air.
Example 5
The high Bs nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.8 mol%, NiO 25.5 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5Nano Al2O3And nano SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O30.01wt％，P2O50.02 wt% of nano Al2O30.05 wt% of nano SiO20.05wt％。
The preparation method of the nickel zinc ferrite is the same as that of the embodiment 4.
The composition ratio data of the nickel zinc ferrite of examples 1 to 5 are summarized in Table 1.
TABLE 1 compositional proportions of the nickel zinc ferrites of examples 1 to 5
| Unit of | mol％ | mol％ | mol％ | mol％ | wt％ | wt％ | wt％ | wt％ |
| Composition (I) | Fe2O3 | NiO | ZnO | CuO | B2O3 | P2O5 | Al2O3 | SiO2 |
| Example 1 | 49.8 | 25.5 | 24.55 | 0.15 | 0.03 | 0.03 | 0.02 | 0.015 |
| Example 2 | 49.8 | 25.5 | 24.55 | 0.15 | 0.02 | 0.01 | 0.03 | 0.01 |
| Example 3 | 49.8 | 25.5 | 24.55 | 0.15 | 0.04 | 0.02 | 0.01 | 0.02 |
| Example 4 | 49.8 | 25.5 | 24.55 | 0.15 | 0.05 | 0.05 | 0.02 | 0.01 |
| Example 5 | 49.8 | 25.5 | 24.55 | 0.15 | 0.01 | 0.04 | 0.02 | 0.02 |
Comparative example 1
The nickel-zinc ferrite comprises a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole: fe2O349.4 mol%, NiO 25.9 mol%, ZnO 24.55 mol%, CuO 0.15 mol%; the accessory ingredient comprises B2O3、P2O5、Al2O3And SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows: b is2O3 0.03wt％，P2O5 0.02wt％，Al2O3 0.05wt％，SiO20.05wt％。
The preparation method of the nickel zinc ferrite is the same as that of the embodiment 1.
The nickel zinc ferrites of examples 1 to 5 and the nickel zinc ferrite of comparative example 1 were sintered to form a magnetic ring, and the test and evaluation were performed, respectively. Under the condition that the turn number N is 20Ts, an HP-4284A type LCR tester is used for testing the initial permeability mu of the magnetic ring samplei(ii) a The samples were tested for saturation magnetic induction Bs at an electric field of 8000A/m with a model SY-8258B-H analyzer. The results of the tests and evaluations are shown in table 2.
TABLE 2 tables for testing and evaluating the properties of nickel zinc ferrites of examples 1 to 5, and comparative example 1
| Item | Initial permeability μ i | Bs(100℃) | Evaluation of |
| Unit of | ％ | mT | - |
| Index (I) | 350(1±10％) | 520(1±5％) | - |
| Example 1 | 355 | 521 | OK |
| Example 2 | 345 | 510 | OK |
| Example 3 | 343 | 505 | OK |
| Example 4 | 325 | 511 | OK |
| Example 5 | 335 | 508 | OK |
| Comparative example 1 | *200 | *480 | NG |
Exceeding lower limit of specification
As can be seen from Table 2, the nickel-zinc ferrites of examples 1-5 added nano Al in the subcomponent2O3And nano SiO2It is possible to suitably suppress the excessive growth of crystal grains, reduce the generation of pores in the magnet, and obtain a high sintered density (Ds). The nickel-zinc ferrite of the embodiments 1 to 5 has the characteristic of high Bs under an electric field of 8000A/m, and meets the requirement of power inductance on miniaturization and large current of ferrite materials.
In comparison with the nickel-zinc ferrite of comparative example 1, the nickel-zinc ferrite of example 1 has a significantly better magnet compactness than that of comparative example 1, mainly because the magnet of example 1 has uniform grain growth and fewer pores, so that Bs value is greatly increased compared to that of comparative example 1, in comparison with the microstructure comparison diagram of fig. 1.
The foregoing is illustrative and explanatory only, and is described in greater detail and detail, but is not to be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications are possible without departing from the inventive concept, and such obvious alternatives fall within the scope of the invention.
Claims (3)
1. The high Bs nickel-zinc ferrite is characterized by comprising a main component and an auxiliary component, wherein the main component comprises the following raw materials in percentage by mole:
Fe2O349.5-50.0 mol%, NiO 23.1-26.5 mol%, ZnO 22.8-26.8 mol%, and CuO 0.1-0.2 mol%; the sum of the mole percentages of the main components is 100 percent;
the accessory ingredient comprises B2O3、P2O5、Al2O3And SiO2(ii) a Based on the total mass of the main component, the contents of the auxiliary components are as follows:
B2O3 0.01～0.05wt％，P2O5 0.01～0.05wt％，Al2O3 0.01～0.03wt％，SiO2 0.01～0.02wt％；
the Al is2O3Is nano alumina, the SiO2Is nano silicon dioxide.
2. The nickel zinc ferrite according to claim 1, wherein the contents of the subcomponents are, based on the total mass of the main component: b is2O3 0.03wt％，P2O5 0.03wt％，Al2O3 0.02wt％，SiO2 0.015wt％。
3. A method for preparing a nickel zinc ferrite as claimed in any one of claims 1 to 2, comprising the following steps in sequence:
s1, mixing: preparing the raw materials according to the mol percentage of the main components, and mixing the raw materials by a dry method for 120-180 minutes;
s2, pre-burning: pre-burning the mixed material of S1 in a pushed slab kiln;
s3, crushing: adding the accessory ingredients into the main component pre-fired material obtained in the step S2, and then carrying out wet grinding to obtain slurry;
s4, granulation: adding PVA (polyvinyl acetate) which is 1.4 percent of the weight of the slurry into the slurry of the S3, and performing spray granulation to obtain granules;
s5, pressing: pressing the granules of the S4 by a powder forming machine to obtain a blank;
s6, sintering: sintering the blank in a resistance furnace, controlling the sintering temperature at 1200-1250 ℃, preserving the heat for 30-60 minutes, wherein the sintering atmosphere is air, and cooling the blank to room temperature along with the furnace after sintering;
in the step S2, the pre-sintering temperature is controlled to be 800 +/-20 ℃, and the pre-sintering time is 400-600 minutes;
in the step S3, the crushing time is 240-360 minutes, and the particle size of the ground slurry is controlled to be 0.6-0.8 mu m;
in the S5, the pressing density of the blank is controlled to be 3.3 +/-0.15 g/cm3。
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| CN102682946A (en) * | 2012-05-30 | 2012-09-19 | 江门安磁电子有限公司 | MnZn ferrite magnetic core with double characteristics and manufacture method |
| CN110357610A (en) * | 2019-07-26 | 2019-10-22 | 横店集团东磁股份有限公司 | A kind of nickel-zinc-ferrite material, and its preparation method and application |
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| CN102603279A (en) * | 2012-03-07 | 2012-07-25 | 天通控股股份有限公司 | High-strength high-Bs (saturation magnetic induction intensity) nickel-zinc ferrite and preparation method thereof |
| CN102682946A (en) * | 2012-05-30 | 2012-09-19 | 江门安磁电子有限公司 | MnZn ferrite magnetic core with double characteristics and manufacture method |
| CN110357610A (en) * | 2019-07-26 | 2019-10-22 | 横店集团东磁股份有限公司 | A kind of nickel-zinc-ferrite material, and its preparation method and application |
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