CN108640670A - High Bs values, the preparation method of low-power consumption soft magnetic ferrite and magnetic core - Google Patents
High Bs values, the preparation method of low-power consumption soft magnetic ferrite and magnetic core Download PDFInfo
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Abstract
The present invention proposes a kind of high Bs values, the preparation method of low-power consumption soft magnetic ferrite and magnetic core, it is preferred that main formula and effective doping, develop high Bs, low-power consumption soft magnetic ferrite, final products crystallite dimension is 3~4 μm, initial permeability ui reach 2200 or more, 80 DEG C~120 DEG C, under 100kHz, 200mTBs value power attenuation in 380~420kW/m3, 100 DEG C of Bs values are in 450mT or more;Using multisection type balanced atmosphere sintering method, control the density of Ferrite Material, crystallite dimension, the porosity and their distributions between intra-die and crystal grain, the microstructure of soft magnetic ferrite is set more effectively to be controlled, so that it is guaranteed that the key property parameter of material reaches harmonious unification;End product quality is high, and production cost reduces by 20% or more.
Description
Technical field
The present invention relates to soft magnetic ferrite more particularly to a kind of high Bs values, low-power consumption soft magnetic ferrites
And the preparation method of magnetic core.
Background technology
After soft magnetic ferrite is researched and developed successfully from nineteen thirty-five by Dutch Philips laboratory, has more than 80 years go through so far
History, due to ferritic magnetic from ferrimagnetism, saturation magnetization Ms is low compared with metallic magnetic, but than the resistance of metallic magnetic
Rate ρ is again much higher, therefore has good high frequency characteristics.In light current high frequency technique field, soft magnetic ferrite has the advantages that uniqueness.
The magnetic core made of this kind of material is the core of various inductors, electronic transformer, choking-winding, suppressor, filter etc.
Part.Soft magnetic ferrite is put into the announcement of the departments such as National Development and Reform Committee as electronic information technology basic material《It is current excellent
The industrialization of new high-technology major fields guide (2011 year) first developed》And Ministry of Science and Technology's announcement《State key branch
The high-technology field catalogue (2015) held》.It is widely used in computer, household electrical appliance, energy-saving lamp and LED, network communication, vapour
The pillar industries such as vehicle and electric vehicle, high ferro, wind-force and nuclear power generation and new industry.
With the horizontal continuous rapid advances of electronic technology, proposed increasingly to being applied to soft magnetic ferrites therein
High requirement.It is emerging to meet space flight communication, new-energy automobile, clean energy resource, LED green illuminations, portable electronic device etc.
Field minimizes magnetic core and the materials demand of high DC stacked characteristic, magnetic material industry magnetic core manufactory both domestic and external are confused
Confusingly propose the new material research and development plan for both meeting low-loss requirement but also with high saturation magnetic flux density.But it realizes simultaneously
Low-power consumption and the high Bs of high temperature are always the difficult point of soft magnetic ferrite research and development, and this kind of steady operation is badly in need of in electronic market
And it can efficiently provide the material of electronic component conversion power.
The R & D Level of the high Bs materials of domestic manufacturers is compared, otherwise ideal is not achieved in the developmental achievement Bs values of many manufacturers
State or loss are higher or very high for the dependence of sintering process.Domestic Ji Jia manufacturers only few in number at present
The Bs value levels that can accomplish are:Room temperature is 530mT, high temperature 440mT.
Invention content
In view of this, the present invention proposes a kind of preparation of high Bs values, low-power consumption soft magnetic ferrite and magnetic core
Method.
The technical proposal of the invention is realized in this way:
On the one hand, the present invention provides a kind of high Bs values, low-power consumption soft magnetic ferrite, the ferrite powder packets
Include principal component and additive ingredient, wherein
The proportioning of each principal component is respectively:
Fe2O368~72mol%
13~17mol% of MnO
11~15mol% of ZnO
The proportioning of each principal component adds up to 100mol%;
The relatively described principal component total amount, the weight rate of each additive ingredient are respectively:
On the basis of above technical scheme, it is preferred that the Nano-meter SiO_22Particle size range be 50~200nm.
On the other hand, the present invention provides a kind of high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core, packets
Include following steps,
Each principal component and each additive ingredient are mixed, MnZn ferrite material are obtained through ball milling, granulation, pre-burning by S1;
S2 carries out compression molding, sintering to the MnZn ferrite material that step S1 is obtained, obtains final products.
On the basis of above technical scheme, it is preferred that in the step S1, in ball milling process be added pure water, dispersant,
Adhesive and antifoaming agent, Control granularity are distributed 100~300 μm, and aqueous weight percent is 0.15~0.25%.
On the basis of above technical scheme, it is preferred that in the step S1, addition 7wt%~10wt% when granulation
PVA solution, and using spray drying.
On the basis of above technical scheme, it is preferred that in the step S1, calcined temperature is 950~1050 DEG C, pre-burning
Time is 30~90min.
On the basis of above technical scheme, it is preferred that in the step S2, sintering process includes,
S2-1 rises to 900 DEG C with the heating rate of 0.5~2.0 DEG C/min in air atmosphere from room temperature;
S2-2, adjustment partial pressure of oxygen is 0.4~0.5%, and 1200 are risen to from 900 DEG C with the heating rate of 1.0~3.0 DEG C/min
℃;
S2-3, adjustment partial pressure of oxygen is 5~7%, and 1350~1370 are risen to from 1200 DEG C with the heating rate of 3~10 DEG C/min
DEG C, keep the temperature 4.2~7h;
S2-4 cools down under the conditions of equilibrium oxygen partial pres-sure, and it is 4.75~5kg/m to obtain sintered density3Magnetic core.
On the basis of above technical scheme, it is preferred that in step S2-4, first drop to 900 DEG C from maximum sintering temperature, drop
Warm rate is 2.5~5 DEG C/min, and partial pressure of oxygen is controlled 0.02%~0.5%;Then again from 900 DEG C to room temperature, rate of temperature fall is
1.5~4 DEG C/min, partial pressure of oxygen is controlled 0~0.005%.
On the basis of above technical scheme, it is preferred that final products crystallite dimension is 3~4 μm, and initial permeability ui reaches
Power attenuation is in 380~420kW/m under to 2200 or more, 80 DEG C~120 DEG C, 100kHz, 200mT Bs values3, 100 DEG C of Bs values exist
450mT or more.
The high Bs values of the present invention, the preparation method of low-power consumption soft magnetic ferrite and magnetic core are compared with the existing technology
It has the advantages that:
(1) preferably main formula and effective doping, develop high Bs, low-power consumption soft magnetic ferrite, final products are brilliant
Particle size is 3~4 μm, and initial permeability ui reaches 2200 or more, 80 DEG C~120 DEG C, 100kHz, power damages under 200mT Bs values
Consumption is in 320~420kW/m3, 100 DEG C of Bs values are in 450mT or more;
(2) use multisection type balanced atmosphere sintering method, control the density, crystallite dimension, the porosity of Ferrite Material with
And their distributions between intra-die and crystal grain, so that the microstructure of soft magnetic ferrite is more effectively controlled, to
Ensure that the key property parameter of material reaches harmonious unification;
(3) end product quality is high, and production cost reduces by 20% or more.
Specific implementation mode
Below in conjunction with embodiment of the present invention, the technical solution in embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only some embodiments of the invention, rather than whole embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all
Other embodiment shall fall within the protection scope of the present invention.
Embodiment 1
The soft magnetic ferrite of the present embodiment, including principal component and additive ingredient, wherein
The proportioning of each principal component is respectively:
Fe2O3 68mol
MnO 17mol
ZnO 15mol
The relatively described principal component total amount, the weight rate of each additive ingredient are respectively:
Particle size range is the Nano-meter SiO_2 of 50~100nm2 50PPM。
High Bs values, the preparation process of low-power consumption magnetic ferrite magnetic core are as follows:
First, each principal component and each additive ingredient are weighed, is uniformly mixed.
Secondly, pure water, dispersant, adhesive and antifoaming agent will be added in mixed material, carries out ball milling, Control granularity distribution
100~300 μm, aqueous weight percent is 0.15%.
Then, the PVA solution of 7wt% is added to the powder that ball milling obtains, and uses spray drying granulation.
Then, in air atmosphere, in 950 DEG C of pre-burnings, burn-in time 30min obtains MnZn ferrite material.
Finally, compression molding is carried out to the MnZn ferrite material that pre-burning obtains, is then sintered under the following conditions,
Obtain final products:
S2-1 rises to 900 DEG C with the heating rate of 0.5 DEG C/min in air atmosphere from room temperature;
S2-2, adjustment partial pressure of oxygen is 0.4%, and 1200 DEG C are risen to from 900 DEG C with the heating rate of 1.0 DEG C/min;
S2-3, adjustment partial pressure of oxygen are 5%, rise to 1350 DEG C from 1200 DEG C with the heating rate of 3 DEG C/min, keep the temperature 4.2h;
S2-4 first drops to 900 DEG C from maximum sintering temperature, and rate of temperature fall is 2.5 DEG C/min, and partial pressure of oxygen is controlled 0.02%
~0.5%;Then again from 900 DEG C to room temperature, rate of temperature fall is 1.5 DEG C/min, and partial pressure of oxygen is controlled 0~0.005%, burnt
Knot density is 4.75kg/m3Magnetic core.
Embodiment 2
The soft magnetic ferrite of the present embodiment, including principal component and additive ingredient, wherein
The proportioning of each principal component is respectively:
Fe2O3 70mol
MnO 15mol
ZnO 15mol
The relatively described principal component total amount, the weight rate of each additive ingredient are respectively:
Particle size range is the Nano-meter SiO_2 of 100~200nm2 70PPM。
High Bs values, the preparation process of low-power consumption magnetic ferrite magnetic core are as follows:
First, each principal component and each additive ingredient are weighed, is uniformly mixed.
Secondly, pure water, dispersant, adhesive and antifoaming agent will be added in mixed material, carries out ball milling, Control granularity distribution
100~300 μm, aqueous weight percent is 0.2%.
Then, the PVA solution of 8wt% is added to the powder that ball milling obtains, and uses spray drying granulation.
Then, in air atmosphere, in 1000 DEG C of pre-burnings, burn-in time 60min obtains MnZn ferrite material.
Finally, compression molding is carried out to the MnZn ferrite material that pre-burning obtains, is then sintered under the following conditions,
Obtain final products:
S2-1 rises to 900 DEG C with the heating rate of 1.5 DEG C/min in air atmosphere from room temperature;
S2-2, adjustment partial pressure of oxygen is 0.4~0.5%, and 1200 DEG C are risen to from 900 DEG C with the heating rate of 2 DEG C/min;
S2-3, adjustment partial pressure of oxygen are 5~7%, 1360 DEG C are risen to from 1200 DEG C with the heating rate of 6 DEG C/min, heat preservation
5.5h;
S2-4 first drops to 900 DEG C from maximum sintering temperature, and rate of temperature fall is 3.5 DEG C/min, and partial pressure of oxygen is controlled 0.02%
~0.5%;Then again from 900 DEG C to room temperature, rate of temperature fall is 3 DEG C/min, and partial pressure of oxygen is controlled 0~0.005%, is sintered
Density is 4.85kg/m3Magnetic core.
Embodiment 3
The soft magnetic ferrite of the present embodiment, including principal component and additive ingredient, wherein
The proportioning of each principal component is respectively:
Fe2O3 72mol
MnO 17mol
ZnO 11mol
The relatively described principal component total amount, the weight rate of each additive ingredient are respectively:
Particle size range is the Nano-meter SiO_2 of 50~200nm2 100PPM。
High Bs values, the preparation process of low-power consumption magnetic ferrite magnetic core are as follows:
First, each principal component and each additive ingredient are weighed, is uniformly mixed.
Secondly, pure water, dispersant, adhesive and antifoaming agent will be added in mixed material, carries out ball milling, Control granularity distribution
100~300 μm, aqueous weight percent is 0.25%.
Then, the PVA solution of 10wt% is added to the powder that ball milling obtains, and uses spray drying granulation.
Then, in air atmosphere, in 1050 DEG C of pre-burnings, burn-in time 90min obtains MnZn ferrite material.
Finally, compression molding is carried out to the MnZn ferrite material that pre-burning obtains, is then sintered under the following conditions,
Obtain final products:
S2-1 rises to 900 DEG C with the heating rate of 2.0 DEG C/min in air atmosphere from room temperature;
S2-2, adjustment partial pressure of oxygen is 0.4~0.5%, and 1200 DEG C are risen to from 900 DEG C with the heating rate of 3.0 DEG C/min;
S2-3, adjustment partial pressure of oxygen are 7%, rise to 1370 DEG C from 1200 DEG C with the heating rate of 10 DEG C/min, keep the temperature 7h;
S2-4 first drops to 900 DEG C from maximum sintering temperature, and rate of temperature fall is 5 DEG C/min, partial pressure of oxygen control 0.02%~
0.5%;Then again from 900 DEG C to room temperature, rate of temperature fall is 4 DEG C/min, and partial pressure of oxygen controls 0~0.005%, obtains being sintered close
Degree is 4.90kg/m3Magnetic core.
The magnetic core obtained to embodiment 2 is tested, and following result is obtained:
As can be seen that final products crystallite dimension is 3~4 μm, initial permeability ui reaches 2200 or more, 80 DEG C~120
DEG C, under 100kHz, 200mT Bs values power attenuation in 320~420kW/m3, 100 DEG C of Bs values are in 450mT or more.
The foregoing is merely the better embodiments of the present invention, are not intended to limit the invention, all the present invention's
Within spirit and principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of high Bs values, low-power consumption soft magnetic ferrite, it is characterised in that:The ferrite powder include principal component and
Additive ingredient, wherein
The proportioning of each principal component is respectively:
Fe2O368~72mol%
13~17mol% of MnO
11~15mol% of ZnO
The proportioning of each principal component adds up to 100mol%;
The relatively described principal component total amount, the weight rate of each additive ingredient are respectively:
CaCO3100~1000PPM
SnO2100~500PPM
MoO350~100PPM
ZrO2100~500PPM
Bi2O350~100PPM
Nano-meter SiO_2250~100PPM.
2. high Bs values described in claim 1, low-power consumption soft magnetic ferrite, it is characterised in that:The Nano-meter SiO_22's
Particle size range is 50~200nm.
3. high Bs values described in claim 1, the preparation method of low-power consumption magnetic ferrite magnetic core, it is characterised in that:Packet
Include following steps,
Each principal component and each additive ingredient are mixed, MnZn ferrite material are obtained through ball milling, granulation, pre-burning by S1;
S2 carries out compression molding, sintering to the MnZn ferrite material that step S1 is obtained, obtains final products.
4. high Bs values, the preparation method of low-power consumption soft magnetic ferrite as claimed in claim 3, it is characterised in that:
In the step S1, pure water, dispersant, adhesive and antifoaming agent are added in ball milling process, Control granularity is distributed 100~300 μm,
Aqueous weight percent is 0.15~0.25%.
5. high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core as claimed in claim 3, it is characterised in that:
In the step S1, the PVA solution of 7wt%~10wt% is added when granulation, and using spray drying.
6. high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core as claimed in claim 3, it is characterised in that:
In the step S1, calcined temperature is 950~1050 DEG C, and burn-in time is 30~90min.
7. high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core as claimed in claim 3, it is characterised in that:
In the step S2, sintering process includes,
S2-1 rises to 900 DEG C with the heating rate of 0.5~2.0 DEG C/min in air atmosphere from room temperature;
S2-2, adjustment partial pressure of oxygen is 0.4~0.5%, and 1200 DEG C are risen to from 900 DEG C with the heating rate of 1.0~3.0 DEG C/min;
S2-3, adjustment partial pressure of oxygen is 5~7%, and 1350~1370 DEG C are risen to from 1200 DEG C with the heating rate of 3~10 DEG C/min,
Keep the temperature 4.2~7h;
S2-4 cools down under the conditions of equilibrium oxygen partial pres-sure, and it is 4.75~5kg/m to obtain sintered density3Magnetic core.
8. high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core as claimed in claim 7, it is characterised in that:
In step S2-4,900 DEG C first are dropped to from maximum sintering temperature, rate of temperature fall is 2.5~5 DEG C/min, and partial pressure of oxygen control exists
0.02%~0.5%;Then again from 900 DEG C to room temperature, rate of temperature fall is 1.5~4 DEG C/min, partial pressure of oxygen control 0~
0.005%.
9. high Bs values, the preparation method of low-power consumption magnetic ferrite magnetic core as claimed in claim 3, it is characterised in that:
Final products crystallite dimension be 3~4 μm, initial permeability ui reach 2200 or more, 80 DEG C~120 DEG C, 100kHz, 200mT Bs
The lower power attenuation of value is in 320~420kW/m3, 100 DEG C of Bs values are in 450mT or more.
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