CN102503397A - Manganese oxide doped manganese-zinc ferrite and preparation method thereof - Google Patents
Manganese oxide doped manganese-zinc ferrite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses manganese oxide doped manganese-zinc ferrite, which comprises major materials and additives, wherein the major materials include 50-55mol% of Fe2O3, 35-43mol% of MnO and 2-15mol% of ZnO, and the additives include 0.1-1wt% of Mn3O4 and at least two of 0.02-0.1wt% of CaCO3, 0.02-0.1wt% of V2O5, 0.02-0.40wt% of TiO2, 0.02-0.05wt% of Nb2O5, 0-5wt% of CoO3, 0.02-0.40wt% of ZrO2 and 0.02-0.40wt% of SnO2. The invention further discloses a preparation method of the manganese oxide doped manganese-zinc ferrite. The manganese oxide doped manganese-zinc ferrite has the advantages of quite low power consumption under same conditions.
Description
Technical field
The present invention relates to a kind of magneticsubstance, particularly, relate to Mn-Zn ferrite of a kind of trimanganese tetroxide that mixes and preparation method thereof.
Background technology
Along with developing rapidly of electronics and information industry, the ferritic range of application of MnZn increases day by day.Because the MnZn ferrite has characteristics such as high saturation magnetic flux density, high magnetic permeability, high resistivity, low-loss; Thereby be widely used in the various electronic devices and components, like power transformer, power choke coil, pulse wide-band transformer, magnetic deflection arrangement and transmitter etc.The FERRITE CORE that utilizes characteristics such as MnZn ferrite high saturation magnetic flux density, high resistivity and low-loss to process has become computingmachine, communication, colour TV, video recorder, office automation and the indispensable base components of other electronics.
Introduction report to doped with trace elements in the Mn-Zn ferrite is arranged repeatedly in the prior art, but its power consumption when 80 ℃, 100 ℃ and 120 ℃ all at 300kW/m
3More than, like the MnZn Ferrite Material that one Chinese patent application 03115906.0 is narrated, 100 ℃ power consumption (Pcv) is at 370 kW/m
3About, contribution is little aspect the reduction power consumption.
Summary of the invention
The technical problem that the present invention will solve is to overcome existing defective, and a kind of Mn-Zn ferrite that under 80 ℃, 100 ℃ and 120 ℃ of conditions, has the doping trimanganese tetroxide of lower power consumption is provided, and its preparation method is provided simultaneously.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of Mn-Zn ferrite of the trimanganese tetroxide that mixes, accomplish by following composition preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：50~55mol%；
MnO：?35~43mol%；
ZnO：?2～15?mol%；
Additive is Mn
3O
4With all the other at least 2 kinds of components in weight percentage:
Mn
3O
4：0.1～1?wt％；
CaCO
3：0.02～0.1wt％；
V
2O
5：0.02～0.1?wt％；
TiO
2：0.02～0.40?wt％；
Nb
2O
5：0.02～0.05?wt％；
CoO
3：0～5?wt％；
ZrO
2：0.02～0.40?wt％；
SnO
2：0.02～0.40?wt％。
Preferably, said major ingredient is the component of following molar percentage:
Fe
2O
3：53.28mol%；
MnO：36.96mol%；
ZnO：?9.76mol%。
Preferably, said additive is 6 kinds of components of following weight percent:
Mn
3O
4：0.5wt％；
CaCO
3：0.05wt％；
V
2O
5：0.03?wt％；
TiO
2：0.08wt％；
Nb
2O
5：0.03wt％；
ZrO
2：0.02wt％。
The preparation method of the Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention comprises following technological process:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out first time wet method sand milling more than 30 minutes, the concentration that adds the 10wt% ingredients by weight then is 8 ~ 9% polyvinyl alcohol solution, stirs 2 hours; Spraying drying is processed particle; Carry out pre-burning, calcined temperature is 850 ℃～980 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 0.8～1.0 micron, the concentration that adds the 10wt% ingredients by weight was 8 ~ 9% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40-160 purpose particle powder;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.3-0.5%; Flow angle is less than 30 degree; Form the good finished particle powder of plasticity-, damping is handled the back in 1300 ℃～1400 ℃ sintering 3～5 hours, obtains finished product.
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention has following beneficial effect:
1, the Mn-Zn ferrite of doping trimanganese tetroxide power consumption≤300 kW/m under 80 ℃ and 120 ℃ of (100KHz, 200mT) conditions
3, power consumption≤260kW/m when 100 ℃ (100KHz, 200mT)
3, (power consumption is 300 kW/m under the same terms with common Mn-Zn ferrite
3More than) compare, its power consumption is quite low, has adapted to the demand of multiple special industry;
2, in the prescription of the Mn-Zn ferrite of the doping trimanganese tetroxide of the present invention's proposition, added an amount of Mn
3O
4, on the basis of saving production cost and reduction processing requirement, improved the resistivity of Mn-Zn ferrite, reduced its power loss; CaCO
3Have crystal grain thinning, it is excessive to suppress grain growth, improves resistivity, reduces the effect of high-frequency loss; TiO
2Then have very strong adhesive capacity, make ferrite have stronger hardness; Nb
2O
5Can improve ferritic resistivity, reduce its sintering temperature, make it be beneficial to environmental protection more;
3, common soft magnetic ferrite is in when batching, prepares burden in ratio accurately, when the secondary sand milling, adds needed additive, and such production technique can obtain when 100 ℃ (100KHz, 200mT) power consumption near 300kW/m
3Material; But the product power consumption of this material when 80 ℃ and 120 ℃ can be very high, and the MnO that reserves about the 0.5wt% of major ingredient gross weight adds when follow-up secondary wet process sand milling, so not only on the material at high temperature curve, can play good effect; And because the MnO of process pre-burning does not add; Make the particle powder have certain plasticity-, so both can reduce the pressure of material when moulding, prevent that again material from producing the rimose phenomenon when sintering;
4, can find out that from the Mn-Zn ferrite of doping trimanganese tetroxide and the power consumption comparison diagram under each temperature of common ferrite under 20 ℃-120 ℃, product proposed by the invention all has lower power consumption, is applicable to the demand of different industries.
Description of drawings
Accompanying drawing is used to provide further understanding of the present invention, and constitutes the part of specification sheets, is used to explain the present invention with embodiments of the invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is Mn-Zn ferrite and common Mn-Zn ferrite power consumption comparison diagram under 100KHz, 200mT working conditions of doping trimanganese tetroxide among the embodiment 1.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for explanation and explains the present invention, and be not used in qualification the present invention.
Embodiment 1
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：50mol%；
MnO：?43mol%；
ZnO：?7?mol%；
Additive is Mn
3O
4With all the other 2 kinds of components in weight percentage:
Mn
3O
4：0.1wt％；
CaCO
3：0.02wt％；
V
2O
5：0.03?wt％；
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish through following prepared:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out the wet method sand milling 30 minutes first time, the concentration that adds the 10wt% ingredients by weight then is 9% polyvinyl alcohol solution, stirs 2 hours, and spraying drying is processed particle, carries out pre-burning, and calcined temperature is 850 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 1 micron, the concentration that adds the 10wt% ingredients by weight was 9% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40 orders ~ 160 purpose particle powders;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.5%, and flow angle is 30 degree, forms the good finished particle powder of plasticity-, and damping is handled the back in 1300 ℃ of sintering 5 hours, obtains finished product.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, initial permeability is μ i=2320, the high temperature saturation magnetic flux density is Bs=430mT;
As shown in Figure 1; Fig. 1 is through the Mn-Zn ferrite of the doping trimanganese tetroxide of process method preparation proposed by the invention and the contrast of common Mn-Zn ferrite power consumption under each temperature condition; Can find out that on scheming from 20 ℃-120 ℃, the power consumption of two kinds of Mn-Zn ferrites is along with the rising of temperature; The trend that all is first decline, rises again during to 100 ℃, 100 ℃ is the power consumption valley point.The power consumption of the Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention all is starkly lower than common Mn-Zn ferrite from 20 ℃-120 ℃; When working conditions was 100KHz, 200mT, both power consumptions contrasted as follows:
80 ℃ and 120 ℃: power consumption of the present invention is 300 kW/m
3Common Mn-Zn ferrite power consumption is 320 kW/m
3
100 ℃: power consumption of the present invention is 260 kW/m
3Common Mn-Zn ferrite power consumption is 290 kW/m
3
Embodiment 2
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：53.28mol%；
MnO：36.96mol%；
ZnO：?9.76mol%；
Additive is 6 kinds of components of following weight percent:
Mn
3O
4：0.5wt％；
CaCO
3：0.05wt％；
V
2O
5：0.03?wt％；
TiO
2：0.08wt％；
Nb
2O
5：0.03wt％；
ZrO
2：0.02wt％；
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish through following prepared:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out the wet method sand milling 35 minutes first time, the concentration that adds the 10wt% ingredients by weight then is 8% polyvinyl alcohol solution, stirs 2 hours, and spraying drying is processed particle, carries out pre-burning, and calcined temperature is 950 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 0.9 micron, the concentration that adds the 10wt% ingredients by weight was 9% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40 orders ~ 160 purpose particle powders;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.3%, and flow angle 29 degree form the good finished particle powder of plasticity-, and damping is handled the back in 1365 ℃ of sintering 4 hours, obtains finished product.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Initial permeability: μ i=2380
Saturation magnetic flux density: Bs=436mT
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 285kW/m
3
100 ℃, power consumption: 255kW/m
3
Embodiment 3
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：?55mol%；
MnO：?35mol%；
ZnO：?10?mol%；
Additive is Mn
3O
4Component with all the other 3 kinds of weight fractions:
Mn
3O
4：1wt％；
CaCO
3：0.1wt％；
V
2O
5：?0.02?wt％；
Nb
2O
5：0.02?wt％；
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish through following prepared:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out the wet method sand milling 40 minutes first time, the concentration that adds the 10wt% ingredients by weight then is 9% polyvinyl alcohol solution, stirs 2 hours, and spraying drying is processed particle, carries out pre-burning, and calcined temperature is 980 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 1 micron, the concentration that adds the 10wt% ingredients by weight was 9% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40 orders ~ 160 purpose particle powders;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.4%, and flow angle forms the good finished particle powder of plasticity-less than 26 degree, and damping is handled the back in 1350 ℃ of sintering 4 hours, obtains finished product.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Initial permeability: μ i=2310
Saturation magnetic flux density: Bs=432mT
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 295kW/m
3
100 ℃, power consumption: 260kW/m
3
Embodiment 4
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：55mol%；
MnO：?43mol%；
ZnO： 2mol%；
Additive is Mn
3O
4Component with all the other 4 kinds of weight fractions:
Mn
3O
4：0.8?wt％；
V
2O
5：?0.1?wt％；
TiO
2：?0.40?wt％；
CoO
3：1?wt％；
ZrO
2：0.03?wt％；
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish through following prepared:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out the wet method sand milling 50 minutes first time, the concentration that adds the 10wt% ingredients by weight then is 9% polyvinyl alcohol solution, stirs 2 hours, and spraying drying is processed particle, carries out pre-burning, and calcined temperature is 920 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 0.9 micron, the concentration that adds the 10wt% ingredients by weight was 8% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40 orders ~ 160 purpose particle powders;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.3%, and flow angle 28 degree form the good finished particle powder of plasticity-, and damping is handled the back in 1400 ℃ of sintering 3 hours, obtains finished product.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Initial permeability: μ i=2360
Saturation magnetic flux density: Bs=435mT
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 292kW/m
3
100 ℃, power consumption: 258kW/m
3
Embodiment 5
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：50mol%；
MnO：?35mol%；
ZnO：?15?mol%；
Additive is Mn
3O
4Component with all the other 5 kinds of weight fractions:
Mn
3O
4：0.2?wt％；
V
2O
5：?0.1?wt％；
TiO
2：?0.1?wt％；
Nb
2O
5：0.04?wt％；
CoO
3：?5?wt％；
SnO
2：?0.?2wt％；
The preparation method is with embodiment 1 said technological process.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Initial permeability: μ i=2330
Saturation magnetic flux density: Bs=434mT
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 290kW/m
3
100 ℃, power consumption: 260kW/m
3
Embodiment 6
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：52mol%；
MnO：?42mol%；
ZnO：?6?mol%；
Additive is Mn
3O
4Component with all the other 6 kinds of weight fractions:
Mn
3O
4：0.6wt％
CaCO
3：0.06wt％；
V
2O
5：0.06?wt％；
TiO
2：0.22wt％；
CoO
3：2wt％；
ZrO
2：0.1?wt％；
SnO
2：0.1?wt％；
The preparation method is with technological process described in the embodiment 2.。
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Initial permeability: μ i=2320
Saturation magnetic flux density: Bs=435mT
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 290kW/m
3
100 ℃, power consumption: 260kW/m
3
Embodiment 7
The Mn-Zn ferrite of doping trimanganese tetroxide proposed by the invention, accomplish by following component preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：52mol%；
MnO：?40mol%；
ZnO：?8?mol%；
Additive is Mn
3O
4Component with all the other 4 kinds of weight fractions:
Mn
3O
4：0.6wt％
TiO
2：0.02wt％；
Nb
2O
5：0.05?wt％；
ZrO
2：0.4?wt％；
SnO
2：0.02?wt％；
The preparation method is with technological process described in the embodiment 3.
The Mn-Zn ferrite of the doping trimanganese tetroxide through above prepared, concrete parameter is following:
Power consumption under 100KHz, 200mT working conditions:
80 ℃ and 120 ℃, power consumption (Pcv): 300kW/m
3
100 ℃, power consumption: 260kW/m
3
What should explain at last is: the above is merely the preferred embodiments of the present invention; Be not limited to the present invention; Although the present invention has been carried out detailed explanation with reference to previous embodiment; For a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the Mn-Zn ferrite of the trimanganese tetroxide that mixes, accomplish by following composition preparation:
Major ingredient is the component of following molar percentage:
Fe
2O
3：50~55mol%；
MnO：?35~43mol%；
ZnO：?2～15?mol%；
Additive is Mn
3O
4With all the other at least 2 kinds of components in weight percentage:
Mn
3O
4：0.1～1?wt％；
CaCO
3：0.02～0.1wt％；
V
2O
5：0.02～0.1?wt％；
TiO
2：0.02～0.40?wt％；
Nb
2O
5：0.02～0.05?wt％；
CoO
3：0～5?wt％；
ZrO
2：0.02～0.40?wt％；
SnO
2：0.02～0.40?wt％。
2. the Mn-Zn ferrite of doping trimanganese tetroxide according to claim 1, said major ingredient are the component of following molar percentage:
Fe
2O
3：53.28mol%；
MnO：36.96mol%；
ZnO：?9.76mol%。
3. the Mn-Zn ferrite of doping trimanganese tetroxide according to claim 1 and 2, said additive are 6 kinds of components of following weight percent:
Mn
3O
4：0.5wt％；
CaCO
3：0.05wt％；
V
2O
5：0.03?wt％；
TiO
2：0.08wt％；
Nb
2O
5：0.03wt％；
ZrO
2：0.02wt％。
4. the preparation method of the Mn-Zn ferrite of each described doping trimanganese tetroxide of claim 1-3 comprises following technological process:
(1) preparation of pre-burning material:, take by weighing Fe respectively according to formula rate of the present invention
2O
3, MnO, ZnO, wherein, before first time wet method sand milling, the MnO of 0.5wt% that reserves the major ingredient gross weight adds during in order to follow-up secondary wet process sand milling;
To reserve the remaining major ingredient in back and carry out first time wet method sand milling more than 30 minutes, the concentration that adds the 10wt% ingredients by weight then is 8 ~ 9% polyvinyl alcohol solution, stirs 2 hours; Spraying drying is processed particle; Carry out pre-burning, calcined temperature is 850 ℃～980 ℃, obtains the pre-burning material;
(2) preparation of particulate material: the pre-burning material is carried out the wet method sand milling second time, proportionally add the MnO that reserves in additive and the step (1) this moment; When wet method sand milling to particulate median size was 0.8～1.0 micron, the concentration that adds the 10wt% ingredients by weight was 8 ~ 9% polyvinyl alcohol solution, adopted atomizing granulating technology to process 40-160 purpose particle powder;
(3) material sintering: before the moulding, earlier particulate material is carried out damping and handle, making its water cut is 0.3-0.5%; Flow angle is less than 30 degree; Form the good finished particle powder of plasticity-, damping is handled the back in 1300 ℃～1400 ℃ sintering 3～5 hours, obtains finished product.
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| WO2015000098A1 (en) * | 2013-07-05 | 2015-01-08 | 无锡斯贝尔磁性材料有限公司 | Broad-band low-loss magnesium-zinc ferrite magnetic material and manufacturing method thereof |
| CN109437877A (en) * | 2018-10-23 | 2019-03-08 | 无锡斯贝尔磁性材料有限公司 | A kind of production technology of high solids content manganese-zinc ferrite slurry |
| CN111138182A (en) * | 2019-12-31 | 2020-05-12 | 天长市中德电子有限公司 | Method for preparing manganese-zinc ferrite with high magnetic conductivity |
| CN111302780A (en) * | 2018-12-12 | 2020-06-19 | 泰州茂翔电子器材有限公司 | Soft magnetic material with high Q, wide temperature and low loss and production method thereof |
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