CN108275993A - Temperature resistance rises wide-temperature-ranlow-power low-power soft ferrite material and preparation method thereof - Google Patents
Temperature resistance rises wide-temperature-ranlow-power low-power soft ferrite material and preparation method thereof Download PDFInfo
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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Abstract
The invention discloses a kind of temperature resistances to rise wide-temperature-ranlow-power low-power soft ferrite material and preparation method thereof, including host component and doping component；The doping component accounts for the 3~8% of the host component gross mass；The host component is rich iron formula；The doping component includes CaCO3、CaO、Nb2O5、SiO2、V2O5And Co2O3.The present invention is by preferred main formula and effective doping and uses rational sintering forming process, on the one hand ensure that soft magnetic ferrite has high saturation magnetic flux density, high magnetic permeability；On the other hand it controls the uniformity of crystallite dimension, reduce the porosity and their distributions etc. between intra-die and crystal grain, the microstructure of soft magnetic ferrite is made more effectively to be controlled；Resulting product have excellent high temperature low power capabilities, can effectively avoid transformer generate heat in high frequency burning machine the phenomenon that.
Description
Technical field
The present invention relates to soft magnetic ferrite fields, and wide-temperature-ranlow-power low-power soft ferrite is risen more particularly to a kind of temperature resistance
Material and preparation method thereof.
Background technology
Soft magnetic ferrite is the basic function material of electronics and information industry, has been widely used electronic transformer now
In, such as computer, household electrical appliance, inverter arc welding machine, network communication, automobile field, become leading products, market prospects ten
Divide wide.Currently, with new-energy automobile technology be constantly progressive and national requirements for environmental protection, as charging pile new-energy automobile
The charging infrastructure of " gas station " brings huge space to soft magnetic ferrite market.
Soft magnetic ferrite is in power transformer, main the effects that playing energy storage and resonator, filter.Soft magnetic ferrite magnetic
The utilization of the heart and high-frequency electronic transformer, it will help the promotion and popularization of energy automobile charging pile industry are conducive to energy-saving ring
It protects.But there are the following problems in use for current magnetic ferrite magnetic core material：The inside, particle sizes structure of magnetic core product
Uneven, density is low, it is higher to there is a problem of that apparent temperature rises during high-power transformer use, especially zero load temperature
It increases.
Invention content
The invention mainly solves the technical problem of providing a kind of temperature resistance rise wide-temperature-ranlow-power low-power soft ferrite material and its
Preparation method can solve existing soft magnetic ferrite shortcoming present in high-power power transformer.
In order to solve the above technical problems, one aspect of the present invention is：There is provided a kind of wide temperature of temperature resistance liter low work(
Consume soft magnetic ferrite, including host component and doping component；Wherein, the host component includes following mass percentage
Component：Fe2O371.6~71.8%, ZnO 5.5~5.7%, surplus MnO, total amount 100%；The doping component includes such as
Lower component：CaCO3、CaO、Nb2O5、SiO2、V2O5And Co2O3；The doping component accounts for the 3~8% of the host component gross mass.
In a preferred embodiment of the present invention, the mass ratio of each component is in the doping component：CaCO3：CaO：
Nb2O5：SiO2：V2O5：Co2O3It is 5~8：1~2：3~4：3~5：2~3：1~3.
In a preferred embodiment of the present invention, initial permeability of the soft magnetic ferrite at 25 DEG C be more than etc.
In 3000；Power attenuation at 100KHZ, 200mT, 25~120 DEG C is 350~420KW/m3, and with the raising of temperature, work(
Rate loss is in first to reduce again raised trend；Curie temperature is more than or equal to 230 DEG C；1194A/m, the saturation flux density at 25 DEG C
It is higher than 410mT higher than the saturation flux density at 510mT, 1194A/m, 100 DEG C.
In order to solve the above technical problems, another technical solution used in the present invention is：It is low to provide a kind of wide temperature of temperature resistance liter
The preparation method of power consumption soft magnetic ferrite, includes the following steps：
（1）It weighs：Host component is weighed by formula ratio and doping component is spare；
（2）Host component pre-processes：The host component weighed up is put into strong mixed mill in mixed machine by force and vibrating ball-mill, is then placed in back
Rotary kiln preheating, obtains preburning powder；
（3）Material mixes：By step（2）In obtained preburning powder and step（1）In the mixing of load weighted doping component, then
Grinding is blended by sand mill and obtains the mixed material that grain size is 0.8~1.0 μm, drying is spare；
（4）It is granulated：To step（3）A certain amount of binding sizing agent is added in the middle host component and doping component being blended after grinding,
After mixing, drying is granulated, and pellet is pressed into required base sample with mold；
（5）Sinter molding：By step（4）The base sample of middle gained is put into bell-type furnace, is burnt according to the atmosphere curve of equilibrium oxygen partial pres-sure
Form type, obtains the temperature resistance and rise wide-temperature-ranlow-power low-power soft ferrite material.
In a preferred embodiment of the present invention, the step（2）In, the process conditions of the preheating are：950~
1050 DEG C, 2~3h.
In a preferred embodiment of the present invention, the step（4）In, the binding sizing agent is that mass concentration is 6~8%
PVA slurries, be added quality account for the 8~10% of the host component and doping component gross mass.
In a preferred embodiment of the present invention, the step（5）In, the process conditions of the sintering are：First in nitrogen
In atmosphere, 800 DEG C are risen to from room temperature with the heating rate of 2~3 DEG C/min, then under conditions of equilibrium oxygen partial pres-sure, first with 1~
The heating rate of 1.5 DEG C/min rises to 1100 DEG C from 800 DEG C, then rises to 1340 from 1100 DEG C with the heating rate of 3~5 DEG C/min
DEG C, keep the temperature 6~8h；Finally under conditions of equilibrium oxygen partial pres-sure, first cooled down from 1340 DEG C with the rate of temperature fall of 1~1.5 DEG C/min
To 1100 DEG C, then in nitrogen atmosphere, room temperature is down to from 1100 DEG C with the rate of temperature fall of 3~5 DEG C/min.
The beneficial effects of the invention are as follows：A kind of temperature resistance of the present invention rises the preparation side of wide-temperature-ranlow-power low-power soft ferrite material
Method by preferred main formula and effective doping and uses rational sintering forming process, on the one hand ensure that soft magnet oxygen
Body material has high saturation magnetic flux density, high magnetic permeability, and power is transmitted to meet its application product in high current, and
It avoids being saturated；On the other hand control the uniformity of crystallite dimension, reduce the porosity and they intra-die and crystal grain it
Between distribution etc., so that the microstructure of soft magnetic ferrite is more effectively controlled, so that it is guaranteed that the key property parameter of material
Reach harmonious unification；Resulting product has excellent high temperature low power capabilities, can effectively avoid transformer and sends out in high frequency
The phenomenon that hot burning machine.
Specific implementation mode
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
The embodiment of the present invention includes：
Embodiment 1
Present invention is disclosed a kind of temperature resistances to rise wide-temperature-ranlow-power low-power soft ferrite material, including host component and doping component；Institute
State doping component accounts for the host component gross mass 3%.
Wherein, the host component is rich iron formula, includes the component of following mass percentage：
Fe2O371.6%, ZnO 5.5%, MnO 22.9%；
The doping component includes following component：CaCO3、CaO、Nb2O5、SiO2、V2O5And Co2O3；And the mass ratio of each component
For：CaCO3：CaO：Nb2O5：SiO2：V2O5：Co2O3It is 5：1：3：3：2：1.
Each ingredient in aforementioned body component and doping component is the raw material of high-purity and high-specific surface area, is contributed to
The density and crystal grain thinning for improving product, ensure high Bs and low-power consumption.
Above-mentioned temperature resistance rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material, includes the following steps：
（1）It weighs：Host component is weighed by formula ratio and doping component is spare；Wherein, host component, including Fe are weighed2O3、
The total 2kg of ZnO and MnO；Weigh the total 0.06kg of each component in doping component；
（2）Host component pre-processes：The host component weighed up is put into strong mixed mill 1h or more in mixed machine by force and vibrating ball-mill, then
It is put into progress preheating 3h in 950 DEG C of pre-burning stove, obtains the preburning powder that average grain diameter is 6~10 μm；
（3）Material mixes：By step（2）In obtained preburning powder and step（1）In the mixing of load weighted doping component, then
Sand mill is blended grinding and obtains the mixed material that grain size is 0.8~1.0 μm, drying, spare；
（4）It is granulated and at base：To step（3）It is added in the middle host component and doping component being blended after grinding and accounts for the main body group
Divide the PVA slurries for being 6% with 8% mass concentration of doping component gross mass as binding sizing agent, is granulated after mixing, uses mould
Tool is pressed into required base sample；
（5）Sinter molding：By step（4）The base sample of middle gained is put into kiln, first in a nitrogen atmosphere, then in equilibrium oxygen partial pres-sure
Under conditions of sinter molding, obtain the temperature resistance and rise wide-temperature-ranlow-power low-power soft ferrite material.The process conditions being specifically sintered are：
First in nitrogen atmosphere, 800 DEG C are risen to from room temperature with the heating rate of 2 DEG C/min, then under conditions of equilibrium oxygen partial pres-sure, first
1100 DEG C are risen to from 800 DEG C with the heating rate of 1 DEG C/min, then rise to 1340 DEG C from 1100 DEG C with the heating rate of 3 DEG C/min,
Keep the temperature 6h；Finally under conditions of equilibrium oxygen partial pres-sure, first 1100 DEG C are cooled to from 1340 DEG C with the rate of temperature fall of 1 DEG C/min, then
In nitrogen atmosphere, room temperature is down to from 1100 DEG C with the rate of temperature fall of 3 DEG C/min.
Embodiment 2
Present invention is disclosed a kind of temperature resistances to rise wide-temperature-ranlow-power low-power soft ferrite material, including host component and doping component；Institute
State doping component accounts for the host component gross mass 8%.
Wherein, the host component is rich iron formula, includes the component of following mass percentage：
Fe2O371.8%, ZnO 5.7%, MnO 22.5%；
The doping component includes following component：CaCO3、CaO、Nb2O5、SiO2、V2O5And Co2O3；And the mass ratio of each component
For：CaCO3：CaO：Nb2O5：SiO2：V2O5：Co2O3It is 8：2：4：5：3：3.
Each ingredient in aforementioned body component and doping component is the raw material of high-purity and high-specific surface area, is contributed to
The density and crystal grain thinning for improving product, ensure high Bs and low-power consumption.
Above-mentioned temperature resistance rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material, includes the following steps：
（1）It weighs：Host component is weighed by formula ratio and doping component is spare；Wherein, host component, including Fe are weighed2O3、
The total 2kg of ZnO and MnO；Weigh the total 0.16kg of each component in doping component；
（2）Host component pre-processes：Host component pre-processes：The host component weighed up is mixed by force to strong mixed mill in machine and vibrating ball-mill
1h or more is then placed in progress preheating 23h in 1050 DEG C of pre-burning stove, obtains the pre-burning powder that average grain diameter is 6~10 μm
End；
（3）Material mixes：By step（2）In obtained preburning powder and step（1）In the mixing of load weighted doping component, then
Sand mill is blended grinding and obtains the mixed material that grain size is 0.8~1.0 μm, drying, spare；
（4）It is granulated and at base：To step（3）It is added in the middle host component and doping component being blended after grinding and accounts for the main body group
Divide the PVA slurries for being 8% with 10% mass concentration of doping component gross mass as binding sizing agent, is granulated after mixing, grain
Material is pressed into required base sample with mold；
（5）Sinter molding：By step（4）The base sample of middle gained is put into kiln, first in a nitrogen atmosphere, then in equilibrium oxygen partial pres-sure
Under conditions of sinter molding, obtain the temperature resistance and rise wide-temperature-ranlow-power low-power soft ferrite material.The process conditions being specifically sintered are：
First in nitrogen atmosphere, 800 DEG C are risen to from room temperature with the heating rate of 3 DEG C/min, then under conditions of equilibrium oxygen partial pres-sure, first
1100 DEG C are risen to from 800 DEG C with the heating rate of 1.5 DEG C/min, then rise to 1340 from 1100 DEG C with the heating rate of 5 DEG C/min
DEG C, keep the temperature 8h；Finally under conditions of equilibrium oxygen partial pres-sure, first 1100 are cooled to from 1340 DEG C with the rate of temperature fall of 1.5 DEG C/min
DEG C, then in nitrogen atmosphere, room temperature is down to from 1100 DEG C with the rate of temperature fall of 5 DEG C/min.
The soft magnetic ferrite obtained by the above method, after tested, density 4.98g/cm3, Curie temperature is big
In equal to 230 DEG C；
With higher initial permeability, the initial permeability at 25 DEG C is more than or equal to 3000；
Low, 100KHZ, 200mT is lost with lower power attenuation, especially high temperature power, the power damage at 25~120 DEG C
Consumption is 350~420KW/m3, and with the raising of temperature, power attenuation is in first to reduce again raised trend；Specifically,
Under 100KHZ, 200mT, 25 DEG C of test conditions, the KW/m of P≤4203;
Under 100KHZ, 200mT, 80 DEG C of test conditions, the KW/m of P≤3803;
Under 100KHZ, 200mT, 100 DEG C of test conditions, the KW/m of P≤3503;
Under 100KHZ, 200mT, 120 DEG C of test conditions, the KW/m of P≤3803;
With higher saturation flux density and magnetic conductivity, the saturation flux density at 1194A/m, 25 DEG C is higher than 510mT,
Saturation flux density at 1194A/m, 100 DEG C is higher than 410mT.
After tested, obtained magnetic core of the present invention can effectively inhibit high-power transformer temperature to rise higher problem, especially suitable
The requirement for closing the low-power consumption under the conditions of wide temperature, is suitble at 25 DEG C -- within the scope of 120 DEG C.
The present invention ensures that soft magnetic ferrite has high saturation magnetic flux close by preferred main formula and effective doping
Degree, high magnetic permeability, transmit power, and avoid being saturated to meet its application product in high current；And its power attenuation
Especially high temperature power loss it is relatively low, avoid transformer generate heat in high frequency burning machine the phenomenon that.
The sintering process that the present invention uses, can control its crystallite dimension uniformity, reduce the porosity and they
Distribution etc. between intra-die and crystal grain, makes the microstructure of soft magnetic ferrite more effectively be controlled, so that it is guaranteed that material
The key property parameter of material reaches harmonious unification.
The soft magnetic ferrite of gained of the invention can be applicable to the necks such as inverter arc welding machine, DC/DC converters, charger
Domain, it is over-the-counter in addition to meeting high-power power transformer city, mini power power transformer can be more competent at, application field is wide.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of temperature resistance rises wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that including host component and doping component；Its
In, the host component includes the component of following mass percentage：Fe2O371.6~71.8%, ZnO 5.5~5.7%, surplus
For MnO, total amount 100%；The doping component includes following component：CaCO3、CaO、Nb2O5、SiO2、V2O5And Co2O3；It is described
Doping component accounts for the 3~8% of the host component gross mass.
2. temperature resistance according to claim 1 rises wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that the doping group
The mass ratio of each component is in point：CaCO3：CaO：Nb2O5：SiO2：V2O5：Co2O3It is 5~8：1~2：3~4：3~5：2~3：1
~3.
3. temperature resistance according to claim 1 rises wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that the soft magnet
Initial permeability of the ferrite at 25 DEG C is more than or equal to 3000；Power attenuation at 100KHZ, 200mT, 25~120 DEG C
For 350~420KW/m3, and with the raising of temperature, power attenuation is in first to reduce again raised trend；Curie temperature is more than or equal to
230℃；1194A/m, saturation flux density at 25 DEG C higher than 510mT, 1194A/m, 100 DEG C at saturation flux density be higher than
410mT。
4. a kind of temperature resistance as described in any one of claims 1-3 rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material,
It is characterised in that it includes following steps：
（1）It weighs：Host component is weighed by formula ratio and doping component is spare；
（2）Host component pre-processes：The host component weighed up is put into strong mixed mill in mixed machine by force and vibrating ball-mill, is then placed in back
Rotary kiln preheating, obtains preburning powder；
（3）Material mixes：By step（2）In obtained preburning powder and step（1）In the mixing of load weighted doping component, then
Grinding is blended by sand mill and obtains the mixed material that grain size is 0.8~1.0 μm, drying is spare；
（4）It is granulated：To step（3）A certain amount of binding sizing agent is added in the middle host component and doping component being blended after grinding,
After mixing, drying is granulated, and pellet is pressed into required base sample with mold；
（5）Sinter molding：By step（4）The base sample of middle gained is put into bell-type furnace, is burnt according to the atmosphere curve of equilibrium oxygen partial pres-sure
Form type, obtains the temperature resistance and rise wide-temperature-ranlow-power low-power soft ferrite material.
5. temperature resistance according to claim 4 rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that
The step（2）In, the process conditions of the preheating are：950~1050 DEG C, 2~3h.
6. temperature resistance according to claim 4 rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that
The step（4）In, the binding sizing agent is the PVA slurries that mass concentration is 6~8%, and quality is added and accounts for the host component
With the 8~10% of doping component gross mass.
7. temperature resistance according to claim 4 rises the preparation method of wide-temperature-ranlow-power low-power soft ferrite material, which is characterized in that
The step（5）In, the process conditions of the sintering are：First in nitrogen atmosphere, with the heating rate of 2~3 DEG C/min from room
Temperature rises to 800 DEG C, then under conditions of equilibrium oxygen partial pres-sure, is first risen to from 800 DEG C with the heating rate of 1~1.5 DEG C/min
1100 DEG C, then 1340 DEG C are risen to from 1100 DEG C with the heating rate of 3~5 DEG C/min, keep the temperature 6~8h；Finally in equilibrium oxygen partial pres-sure
Under conditions of, 1100 DEG C first are cooled to from 1340 DEG C with the rate of temperature fall of 1~1.5 DEG C/min, then in nitrogen atmosphere, with 3~5
DEG C/rate of temperature fall of min is down to room temperature from 1100 DEG C.
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