CN108059451A - A kind of high frequency power soft magnetic ferrite and preparation method thereof - Google Patents
A kind of high frequency power soft magnetic ferrite and preparation method thereof Download PDFInfo
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- CN108059451A CN108059451A CN201711285910.9A CN201711285910A CN108059451A CN 108059451 A CN108059451 A CN 108059451A CN 201711285910 A CN201711285910 A CN 201711285910A CN 108059451 A CN108059451 A CN 108059451A
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- magnetic ferrite
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 9
- 238000005245 sintering Methods 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 13
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 12
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- 239000004615 ingredient Substances 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000003595 mist Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 230000002411 adverse Effects 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000008188 pellet Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009472 formulation Methods 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 2
- 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 2
- 238000004891 communication Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- TWFZGCMQGLPBSX-UHFFFAOYSA-N carbendazim Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
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- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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Abstract
A kind of high frequency power soft magnetic ferrite, including following component:Major ingredient:Fe2O3:52~56mol%、MnO:34~38 mol%、ZnO:10~15 mol%;Auxiliary material:Bi2O3:100~400ppm、TiO2:50~150ppm、Co2O3:150~200ppm、SiO2:10~50ppm、CaO:10~50ppm、SnO2:10~30ppm、Cr2O3:10~30ppm.Inventive formulation is reasonable, can effectively improve the power of soft magnetic ferrite, reduces power attenuation and magnetic hystersis loss;The present invention adds in butyl stearate in grinding as lubricant, advantageously reduces grinding time, improves production efficiency.1h is kept the temperature during sintering at 1100 DEG C, is conducive to the growth of crystal.
Description
Technical field
The invention belongs to soft magnetic ferrite fields, and in particular to a kind of high frequency power soft magnetic ferrite and its system
Preparation Method.
Background technology
With the development of electronics science and information technology, Mn-Zn soft magnetic ferrite increasingly becomes a kind of extremely important electricity
Sub- component magnetic material, since it is with high initial permeability, high saturation magnetic flux density, low-coercivity, low-power consumption etc.
Excellent characteristic, Mn-Zn soft magnetic ferrite are widely used in the electronic devices such as the communication technology, power-supply device, computer product.
In recent years, since electronic component constantly develops to high density, miniaturization, chip type, integrated direction, MnZn is correspondingly required
The various characteristics of soft magnetic ferrite will also improve.
Powerful Mn-Zn soft magnetic ferrite is mainly used for magnetic core of transformer, works in high-power state, therefore
The power for improving Mn-Zn soft magnetic ferrite is of great significance to the development in the even entire electronic component field of transformer.
The content of the invention
In order to solve the problems, such as that prior art exists, the power of manganese-zinc ferrite is improved, improves manganese-zinc ferrite material
The stability of material, adapts to performance requirement of the communications industry to soft magnetic ferrite, and the present invention proposes a kind of high frequency power soft magnet oxygen
Body material, mainly including following component:
Major ingredient
Fe2O3:52~56mol%、MnO:34~38 mol%、ZnO:10~15 mol%.
Auxiliary material
Bi2O3:100~400ppm、TiO2:50~150ppm、Co2O3:150~200ppm、SiO2:10~50ppm、CaO:10~
50ppm、SnO2:10~30ppm、Cr2O3:10~30ppm.
The present invention also provides a kind of above-mentioned preparation methods of high frequency power soft magnetic ferrite, include the following steps:
(1)Dispensing, by each component according to said ratio dispensing;
(2)The raw material prepared is put into adverse current batch mixer and mixes by batch mixing and slurrying, 1 ~ 2h of mixing time;
(3)Pre-burning carries out pre-burning, 700 ~ 1000 DEG C of calcined temperature, burn-in time in rotary kiln:3~5h;
(4)Mixture after pre-burning is put into 20 ~ 40min of ball mill coarse powder essence by coarse crushing;
(5)Mist projection granulating, using spray drying granulation, the temperature for being passed through hot-air is 260 ~ 280 DEG C;
(6)It is finely divided, it is sanded using circulation type sand mill, 3 ~ 6h of time is sanded, while adds in above-mentioned raw materials gross mass
0.2 ~ 0.5% butyl stearate is as lubricant;
(7)Secondary mist projection granulating:Using spray drying granulation, the temperature for being passed through hot-air is 300 ~ 350 DEG C;
(8)Shaping, by step(7)The pellet compression moulding of acquisition;
(9)Sintering carries out atmosphere sintering using nitrogen list push plate sintering furnace, and sintering temperature is 1300 ~ 1500 DEG C.
Further, the step(9)In keep the temperature 1h at 1100 DEG C.
Preferably, the Fe2O3For 53.1 mol%.
Preferably, the MnO is 36.2 mol%.
Preferably, the ZnO is 11 mol%.
The present invention cardinal principle be:CaO and SiO is added in major ingredient2, the two reaction generation CaSiO3The shape in crystal boundary
Into resistive formation, the loss factor of soft magnetic ferrite can be reduced.However excessively high CaO can increase soft magnetic ferrite
Disaccommodation, excessively high SiO2It is easy to cause that crystal grain is discontinuous to grow up in the sintering of soft magnetic ferrite, it is magnetic to reduce its.
TiO2Can and SiO2, Mn generate another phase in crystal boundary, form grain boundary layer, advantageously reduce soft magnetic ferrite
Power attenuation.In addition Ti ionic portions substitution Fe ions, can be by body sintering temperature, without promoting grain growth, convenient for obtaining
Smaller even grained and low-porosity are obtained, so as to reduce magnetic hystersis loss.
Add Co2O3The temperature characterisitic of material can be controlled, reduces magnetic hystersis loss.
Butyl stearate is added in when finely divided can play the role of lubrication, reduce grinding time, improve production efficiency.
The beneficial effects of the invention are as follows:
1st, inventive formulation is reasonable, can effectively improve the power of soft magnetic ferrite, reduces power attenuation and magnetic hystersis loss;
2nd, the present invention adds in butyl stearate in grinding as lubricant, advantageously reduces grinding time, improves production efficiency.
1h is kept the temperature when the 3rd, being sintered at 1100 DEG C, is conducive to the growth of crystal.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, it elaborates with reference to specific embodiment to the present invention.
Embodiment 1
A kind of high frequency power soft magnetic ferrite, mainly including following component:
Major ingredient
Fe2O3:56mol%、MnO:38 mol%、ZnO:10 mol%.
Auxiliary material
Bi2O3:100ppm、TiO2:130ppm、Co2O3:150ppm、SiO2:30ppm、CaO:30ppm、SnO2:20ppm、
Cr2O3:20ppm.
A kind of preparation method of high frequency power soft magnetic ferrite, includes the following steps:
(1)Dispensing, by each component according to said ratio dispensing;
(2)The raw material prepared is put into adverse current batch mixer and mixes by batch mixing and slurrying, mixing time 1.5h;
(3)Pre-burning carries out pre-burning, 700 DEG C of calcined temperature, burn-in time in rotary kiln:4h;
(4)Mixture after pre-burning is put into ball mill coarse powder essence 30min by coarse crushing;
(5)Mist projection granulating, using spray drying granulation, the temperature for being passed through hot-air is 250 DEG C;
(6)It is finely divided, it is sanded using circulation type sand mill, time 5h is sanded, while add in 0.3% butyl stearate work
For lubricant;
(7)Secondary mist projection granulating:Using spray drying granulation, the temperature for being passed through hot-air is 320 DEG C;
(8)Shaping, by step(7)The pellet compression moulding of acquisition;
(9)Sintering carries out atmosphere sintering using nitrogen list push plate sintering furnace, and sintering temperature is 1400 DEG C, and is protected at 1100 DEG C
Warm 1h.
Embodiment 2
A kind of high frequency power soft magnetic ferrite, mainly including following component:
Major ingredient
Fe2O3:52mol%、MnO:35 mol%、ZnO:15 mol%.
Auxiliary material
Bi2O3:400ppm、TiO2:50ppm、Co2O3:150ppm、SiO2:50ppm、CaO:50ppm、SnO2:10ppm、Cr2O3:
30ppm。
A kind of preparation method of high frequency power soft magnetic ferrite, includes the following steps:
(1)Dispensing, by each component according to said ratio dispensing;
(2)The raw material prepared is put into adverse current batch mixer and mixes by batch mixing and slurrying, mixing time 1h;
(3)Pre-burning carries out pre-burning, 1000 DEG C of calcined temperature, burn-in time in rotary kiln:3h;
(4)Mixture after pre-burning is put into ball mill coarse powder essence 20min by coarse crushing;
(5)Mist projection granulating, using spray drying granulation, the temperature for being passed through hot-air is 260 DEG C;
(6)It is finely divided, it is sanded using circulation type sand mill, time 4h is sanded, while adds in above-mentioned raw materials gross mass
0.3% butyl stearate is as lubricant;
(7)Secondary mist projection granulating:Using spray drying granulation, the temperature for being passed through hot-air is 300 DEG C;
(8)Shaping, by step(7)The pellet compression moulding of acquisition;
(9)Sintering carries out atmosphere sintering using nitrogen list push plate sintering furnace, and sintering temperature is 1300 DEG C, and is protected at 1100 DEG C
Warm 1h.
Embodiment 3
A kind of high frequency power soft magnetic ferrite, mainly including following component:
Major ingredient
Fe2O3:53.1mol%、MnO:36.2mol%、ZnO:11 mol%.
Auxiliary material
Bi2O3:200ppm、TiO2:120ppm、Co2O3:200ppm、SiO2:15ppm、CaO:15ppm、SnO2:20ppm、
Cr2O3:10ppm.
A kind of preparation method of high frequency power soft magnetic ferrite, includes the following steps:
(1)Dispensing, by each component according to said ratio dispensing;
(2)The raw material prepared is put into adverse current batch mixer and mixes by batch mixing and slurrying, mixing time 1h;
(3)Pre-burning carries out pre-burning, 750 DEG C of calcined temperature, burn-in time in rotary kiln:5h;
(4)Mixture after pre-burning is put into ball mill coarse powder essence 40min by coarse crushing;
(5)Mist projection granulating, using spray drying granulation, the temperature for being passed through hot-air is 280 DEG C;
(6)It is finely divided, it is sanded using circulation type sand mill, time 2h is sanded, while adds in above-mentioned raw materials gross mass
0.5% butyl stearate is as lubricant;
(7)Secondary mist projection granulating:Using spray drying granulation, the temperature for being passed through hot-air is 350 DEG C;
(8)Shaping, by step(7)The pellet compression moulding of acquisition;
(9)Sintering carries out atmosphere sintering using nitrogen list push plate sintering furnace, and sintering temperature is 1500 DEG C, and is protected at 1100 DEG C
Warm 1h.
The performance of soft magnetic ferrite obtained in above-described embodiment is tested, using SY8232-BH
Analyzer testers measure saturation flux density(Bs):Initial permeability is tested with HP42484A LCR tables(μi), use
Protek digital Multimeter testers measured power is lost(Pc).Test result is as shown in the table:
As can be seen from the above table according to soft magnetic ferrite made from formula of the present invention and method, from initial magnetic conductance
Rate, power attenuation, the core capabilities index of three soft magnetic materials of saturation flux density are good to weigh performance, wherein embodiment
3 property indices are optimal.
Claims (6)
1. a kind of high frequency power soft magnetic ferrite, which is characterized in that including following component:
Major ingredient:Fe2O3:52~56mol%、MnO:34~38 mol%、ZnO:10~15 mol%;Auxiliary material:Bi2O3:100~400ppm、
TiO2:50~150ppm、Co2O3:150~200ppm、SiO2:10~50ppm、CaO:10~50ppm、SnO2:10~30ppm、Cr2O3:
10~30ppm。
2. a kind of preparation method of high frequency power soft magnetic ferrite as described in claim 1, which is characterized in that including
Following steps:
(1)Dispensing, by each component according to said ratio dispensing;
(2)The raw material prepared is put into adverse current batch mixer and mixes by batch mixing and slurrying, 1 ~ 2h of mixing time;
(3)Pre-burning carries out pre-burning, 700 ~ 1000 DEG C of calcined temperature, burn-in time in rotary kiln:3~5h;
(4)Mixture after pre-burning is put into 20 ~ 40min of ball mill coarse powder essence by coarse crushing;
(5)Mist projection granulating, using spray drying granulation, the temperature for being passed through hot-air is 260 ~ 280 DEG C;
(6)It is finely divided, it is sanded using circulation type sand mill, 3 ~ 6h of time is sanded, while adds in above-mentioned raw materials gross mass
0.2 ~ 0.5% butyl stearate is as lubricant;
(7)Secondary mist projection granulating:Using spray drying granulation, the temperature for being passed through hot-air is 300 ~ 350 DEG C;
(8)Shaping, by step(7)The pellet compression moulding of acquisition;
(9)Sintering carries out atmosphere sintering using nitrogen list push plate sintering furnace, and sintering temperature is 1300 ~ 1500 DEG C.
3. a kind of preparation method of high frequency power soft magnetic ferrite as described in claim 2, which is characterized in that described
Step(9)In keep the temperature 1h at 1100 DEG C.
A kind of 4. high frequency power soft magnetic ferrite as described in claim 1, which is characterized in that the Fe2O3For 53.1
mol%。
5. a kind of high frequency power soft magnetic ferrite as described in claim 1, which is characterized in that the MnO is 36.2
mol%。
6. a kind of high frequency power soft magnetic ferrite as described in claim 1, which is characterized in that the ZnO is 11
mol%。
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