CN107555981A - A kind of low-temperature sintering MnZn Ferrite Materials and its prepare sintering method - Google Patents
A kind of low-temperature sintering MnZn Ferrite Materials and its prepare sintering method Download PDFInfo
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Abstract
The present invention provides a kind of low-temperature sintering MnZn Ferrite Materials and its prepares sintering method, and the main component of the Ferrite Material includes Fe2O3, ZnO, MnO and auxiliary additive, content of the principal component in terms of respective reference material are：Fe2O3:49.5mol%~56.5mol%、ZnO:6.5mol%~16mol%、MnO:29.5mol%~41mol%；The auxiliary additive includes：Calcium oxide, sodium peroxide, potassium peroxide, molybdenum sesquioxide, silica and zinc metaborate, it adds 0.1 ~ 0.5wt% that but total amount is principal component total amount.The Ferrite Material obtains Ferrite Material feed powder, after compressing, at a temperature of 1180 DEG C of 30 DEG C of scholars by ball milling, granulation, secondary ball milling, spraying：Sintering obtains sintering magnetic core for 3 ~ 5.5 hours.A kind of low-temperature sintering MnZn Ferrite Materials provided by the invention, sintering temperature decline to a great extent, can be in 1180 DEG C or so sintering, sintered heat insulating duration shortens to 3 ~ 5h, obtains the low-consumption power ferrite of function admirable, and its sintering temperature is low, soaking time is short, and core production energy consumption is low.
Description
Technical field
The present invention relates to electrochemistry and field of metal surface treatment technology, and in particular to a kind of low-temperature sintering MnZn ferrites
Material and its prepare sintering method.
Background technology
With the rapid development of world electronic market, Ferrite Material due to special electromagnetic performance, such as：Electromagnetism
Rate is high, excellent in high-frequency characteristics etc., from various electronic components made of FERRITE CORE, including high frequency magnetic core electronic device, such as：
Deflection coil, kickback transformer, common transformer, rotary transformer, electromagnetism interference transformer, inductor and choke coil
Deng work and control core of these components usually as system or equipment, being widely used in：Computer, mobile phone, communicate, do
Public automation, remote monitoring, audio-visual equipment, household electrical appliance, electromagnetic compatibility, green are according in dawn and electronic information technology (IT).
As modern electronic technology is developed by leaps and bounds, particularly letter is fitted in movement in recent years, first fiber communication, electromagnetic compatibility, electricity are done,
The field such as flat-panel monitor (LCD, PDP), DTV, automotive electronics, novel energy-conserving illuminator, electromagnetism interference application is fast
Speed development, the application to soft magnet oxygen alms bowl open bigger market.Meanwhile higher requirement is it is also proposed to soft magnetic ferrite.
It should be noted that in all these fields dosage it is maximum be MnZn Ferrite Materials and magnetite, account for institute
Have 75% or so of soft magnetic ferrite dosage.In MnZn Ferrite Materials and magnetic core, especially with MnZn power ferrite material and
Based on magnetic core, 85% or so is accounted for.
MnZn power ferrites magnetic core is very wide in state market.According to external expert to global soft magnetic ferrite output
Count nineteen ninety-five whole world illness yield be 210,000 tons, reach 300,000 tons within 2000, to 2005 oneself increase to 450,000 tons, reach within 2010
To 800,000 tons, wherein MnZn power ferrites account for the 60~70% of total amount.Statistics shows, each soft magnetic ferrite application field
Its demand is increased with annual 10~20% amplitude.Also oneself increases the yield of China's soft magnetic ferrite from 30,000 tons of nineteen ninety-five
More than 350,000 tons of 2008 are added to, oneself accounts for more than the 50% of world's total amount.
But because MnZn ferrites need to sinter at high temperature, its usual sintering temperature is at 1330~1400 DEG C, insulation
Time, the sintering process-cycle was up to 26~36 hours, while also to sinter under nitrogen protection, and this just needs great at 4~8 hours
Consume substantial amounts of electric energy and nitrogen.Therefore, MnZn ferrites belong to the industry of high energy consumption.
The content of the invention
For prior art, the invention provides a kind of low-temperature sintering MnZn Ferrite Materials, by Ferrite Material
In appropriate addition zinc metaborate, sodium peroxide, potassium peroxide, molybdenum sesquioxide so that sintering temperature declines to a great extent, Neng Gou
1180 DEG C or so sintering, sintered heat insulating duration shorten to 3~5h, obtain the low-consumption power ferrite of function admirable.
Sintering method is prepared present invention also offers a kind of low-temperature sintering MnZn Ferrite Materials, what it was prepared
MnZn Ferrite Materials can reach following index：Initial permeability μ ≈ 1800 under normal temperature, the strong Bs >=380mT of saturation induction,
100KHz, 200mT, power consumption≤290mW/cm under the conditions of 100 DEG C3Function admirable low-power dissipation soft magnetic ferrite material.
A kind of low-temperature sintering MnZn Ferrite Materials disclosed by the invention, main component include Fe2O3, ZnO, MnO and auxiliary
Additive is helped, content of the principal component in terms of respective reference material is：Fe2O3:49.5mol%~56.5mol%, ZnO:
6.5mol%~16mol%, MnO:29.5mol%~41mol%；The auxiliary additive includes：Calcium oxide, sodium peroxide,
Potassium peroxide, molybdenum sesquioxide, silica and zinc metaborate, it adds 0.1~0.5wt% that but total amount is principal component total amount.
The addition of the auxiliary additive is：Calcium oxide：0.01~0.15wt%, sodium peroxide：0.05~
0.1wt%, 0.05~0.1wt% of potassium peroxide, 0.01~0.05wt% of molybdenum sesquioxide, 0.01~0.05wt% of nickel oxide,
Silica：0.005~0.02wt%, zinc metaborate：0.005~0.045wt%.
The auxiliary additive also includes rare earth addition, reduce loss of the Ferrite Material in the range of frequency applications because
Son, make its application wider.The rare earth addition includes lanthana, cerium oxide, thorium oxide.
The addition of the rare earth addition is：0.002~0.005wt% of lanthana, cerium oxide 0.002~
0.005wt%, 0.002~0.005wt% of thorium oxide.
The content of principal component is in the Ferrite Material：
Fe2O354mol%
ZnO 10.8mol%
MnO 35.2mol%；
The addition of each component is in auxiliary additive in the Ferrite Material：
A kind of low-temperature sintering MnZn Ferrite Materials disclosed by the invention, it prepares sintering method and is：
By following component：Fe2O3:54mol%, ZnO:10.8mol%, MnO:35.2mol% weighs raw material；Input is pre-
First steel ball grinding in ball mill added with deionized water, controls 0.5 ± 0.1 μm of average grain diameter, after a mist projection granulating, 850
Electricity consumption heating revolving kiln carries out pre-burning at a temperature of ± 20 DEG C, 0.9~1.2mm of particle diameter pre-burning particle is obtained, then by pre-burning
Grain addition ball mill secondary ball milling, mentioned component content, addition auxiliary additive calcium oxide press in mechanical milling process：0.05~
0.10wt%, sodium peroxide：0.02~0.03wt%, potassium peroxide：0.08~0.10wt%, molybdenum sesquioxide：0.02~
0.045wt%, silica：0.01~0.015wt%, zinc metaborate：0.025~0.035wt%, lanthana：0.003~
0.005wt%, cerium oxide：0.003~0.005wt%, thorium oxide：0.003~0.005wt%；And pure water is added, control in ball
The average grain diameter of mill is 1.0 ± 0.2 μm, finally carries out secondary spraying and obtains MnZn ferrite particle feed powders, takes the particle feed powder
According to shape of product it is compressing after, be put into vacuum drying oven, clock hood type furnace or N2In gas shielded pushed bat kiln, in partial pressure of oxygen less than 3%
In balanced atmosphere, at a temperature of 30 DEG C of 1180 scholar：Sintering 3~5.5 hours.
Beneficial effect：
(1) a kind of low-temperature sintering MnZn Ferrite Materials provided by the invention, are added in right amount using in Ferrite Material
Zinc metaborate, sodium peroxide, potassium peroxide, molybdenum sesquioxide, so that sintering temperature declines to a great extent, can be at 1180 DEG C or so
Sintering, sintered heat insulating duration shorten to 3~5h, obtain the low-consumption power ferrite of function admirable.
(2) a kind of low-temperature sintering MnZn Ferrite Materials provided by the invention, rare earth addition is also added, reduces iron oxygen
Fissipation factor of the body material in the range of frequency applications, make its application wider.
(2) low-temperature sintering MnZn Ferrite Materials provided by the invention prepare sintering method, and sintering temperature is low, during insulation
Between short, obtained magnetic core product function admirable, reduce MnZn Ferrite Materials prepare needed for energy consumption.
Embodiment
Technical scheme is further described below by embodiment.
The present invention provides a kind of low-temperature sintering MnZn Ferrite Materials：Main component includes Fe2O3, ZnO, MnO and auxiliary
Additive, content of the principal component in terms of respective reference material are：Fe2O3:49.5mol%~56.5mol%, ZnO:
6.5mol%~16mol%, MnO:29.5mol%~41mol%；The auxiliary additive includes：Calcium oxide, sodium peroxide,
Potassium peroxide, molybdenum sesquioxide, silica and zinc metaborate, it adds 0.1~0.5wt% that but total amount is principal component total amount.
The addition of the auxiliary additive is：Calcium oxide：0.01~0.15wt%, sodium peroxide：0.05~
0.1wt%, 0.05~0.1wt% of potassium peroxide, 0.01~0.05wt% of molybdenum sesquioxide, 0.01~0.05wt% of nickel oxide,
Silica：0.005~0.02wt%, zinc metaborate：0.005~0.045wt%.
The auxiliary additive also includes rare earth addition, reduce loss of the Ferrite Material in the range of frequency applications because
Son, make its application wider.The rare earth addition includes lanthana, cerium oxide, thorium oxide.
The addition of the rare earth addition is：0.002~0.005wt% of lanthana, cerium oxide 0.002~
0.005wt%, 0.002~0.005wt% of thorium oxide.
Its specific embodiment is：
Embodiment 1
Each component in Ferrite Material is carried out by formula as below to weigh.
Fe2O354mol%
ZnO 10.8mol%
MnO 35.2mol%；
The addition of each component is in auxiliary additive in the Ferrite Material：
The Fe that will have been weighed2O3, steel ball grinding in the ball mill added with deionized water, control are average in advance for ZnO, MnO input
0.5 ± 0.1 μm of particle diameter, after a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning at a temperature of 850 ± 20 DEG C, obtains grain
0.9~1.2mm of footpath pre-burning particle, pre-burning particle is then added into ball mill secondary ball milling, mentioned component is pressed in mechanical milling process
Content, add auxiliary additive calcium oxide, sodium peroxide, potassium peroxide, molybdenum sesquioxide, silica, zinc metaborate；And add
Enter pure water, control ball milling average grain diameter be 1.0 ± 0.2 μm, finally carry out it is secondary spraying obtain MnZn ferrite particle materials
Powder, take the particle feed powder according to shape of product it is compressing after, be put into vacuum drying oven, clock hood type furnace or N2In gas shielded pushed bat kiln,
In balanced atmosphere of the partial pressure of oxygen less than 3%, at a temperature of 1150 DEG C：Sintering 3.5 hours.
Embodiment 2
Each component in Ferrite Material is carried out by formula as below to weigh.
Fe2O354mol%
ZnO 10.8mol%
MnO 35.2mol%；
The addition of each component is in auxiliary additive in the Ferrite Material：
The Fe that will have been weighed2O3, steel ball grinding in the ball mill added with deionized water, control are average in advance for ZnO, MnO input
0.5 ± 0.1 μm of particle diameter, after a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning at a temperature of 850 ± 20 DEG C, obtains grain
0.9~1.2mm of footpath pre-burning particle, pre-burning particle is then added into ball mill secondary ball milling, mentioned component is pressed in mechanical milling process
Content, add auxiliary additive calcium oxide, sodium peroxide, potassium peroxide, molybdenum sesquioxide, silica, zinc metaborate, oxidation
Lanthanum, cerium oxide, thorium oxide；And add pure water, control ball milling average grain diameter be 1.0 ± 0.2 μm, finally carry out secondary spraying
Obtain MnZn ferrite particle feed powders, take the particle feed powder according to shape of product it is compressing after, be put into vacuum drying oven, clock hood type furnace or
N2In gas shielded pushed bat kiln, in balanced atmosphere of the partial pressure of oxygen less than 3%, at a temperature of 1180 DEG C：Sintering 4.5 hours.
The electromagnetic performance of obtained product：Initial permeability μ under normal temperature:1750~1826, the strong Bs of saturation induction:382
~401mT, the power consumption under the conditions of 100KHz, 200mT, 100 DEG C:260~281mW/cm3。
Embodiment 3
Each component in Ferrite Material is carried out by formula as below to weigh.
Fe2O354mol%
ZnO 10.8mol%
MnO 35.2mol%；
The addition of each component is in auxiliary additive in the Ferrite Material：
The Fe that will have been weighed2O3, steel ball grinding in the ball mill added with deionized water, control are average in advance for ZnO, MnO input
0.5 ± 0.1 μm of particle diameter, after a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning at a temperature of 850 ± 20 DEG C, obtains grain
0.9~1.2mm of footpath pre-burning particle, pre-burning particle is then added into ball mill secondary ball milling, mentioned component is pressed in mechanical milling process
Content, add auxiliary additive calcium oxide, sodium peroxide, potassium peroxide, molybdenum sesquioxide, silica, zinc metaborate, oxidation
Lanthanum, cerium oxide, thorium oxide；And add pure water, control ball milling average grain diameter be 1.0 ± 0.2 μm, finally carry out secondary spraying
Obtain MnZn ferrite particle feed powders, take the particle feed powder according to shape of product it is compressing after, be put into vacuum drying oven, clock hood type furnace or
N2In gas shielded pushed bat kiln, in balanced atmosphere of the partial pressure of oxygen less than 3%, at a temperature of 1210 DEG C：Sintering 5.5 hours.
The electromagnetic performance of obtained product：Initial permeability μ under normal temperature:1821~1895, the strong Bs of saturation induction:389
~411mT, the power consumption under the conditions of 100KHz, 200mT, 100 DEG C:255~270mW/cm3。
The present invention is not limited to above-mentioned preferred forms, and anyone can show that other are various under the enlightenment of the present invention
The product of form, however, make any change in its shape or structure, it is every that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (6)
1. a kind of low-temperature sintering MnZn Ferrite Materials, its main component includes Fe2O3, ZnO, MnO and auxiliary additive, its
It is characterised by：Content of the principal component in terms of respective reference material be：Fe2O3:49.5mol%~56.5mol%, ZnO:
6.5mol%~16mol%, MnO:29.5mol%~41mol%；The auxiliary additive includes：Calcium oxide, sodium peroxide,
Potassium peroxide, molybdenum sesquioxide, silica and zinc metaborate, it adds 0.1~0.5wt% that but total amount is principal component total amount.
A kind of 2. low-temperature sintering MnZn Ferrite Materials according to claim 1, it is characterised in that：The auxiliary additive
Addition be：Calcium oxide：0.01~0.15wt%, sodium peroxide：0.05~0.1wt%, potassium peroxide 0.05~
0.1wt%, 0.01~0.05wt% of molybdenum sesquioxide, 0.01~0.05wt% of nickel oxide, silica：0.005~
0.02wt%, zinc metaborate：0.005~0.045wt%.
A kind of 3. low-temperature sintering MnZn Ferrite Materials according to claim 1, it is characterised in that：The auxiliary additive
Also include rare earth addition, the rare earth addition includes lanthana, cerium oxide, thorium oxide.
A kind of 4. low-temperature sintering MnZn Ferrite Materials according to claim 3, it is characterised in that：The rare earth addition
Addition be：0.002~0.005wt% of lanthana, 0.002~0.005wt% of cerium oxide, thorium oxide 0.002~
0.005wt%.
A kind of 5. low-temperature sintering MnZn Ferrite Materials according to claim 4, it is characterised in that：The Ferrite Material
The content of middle principal component is：
Fe2O354mol%
ZnO 10.8mol%
MnO 35.2mol%；
The addition of each component is in auxiliary additive in the Ferrite Material：
6. a kind of low-temperature sintering MnZn Ferrite Materials according to claim 5 prepare sintering method, it is characterised in that：
By following component：Fe2O3:54mol%, ZnO:10.8mol%, MnO:35.2mol% weighs raw material；Input is in advance added with going
Steel ball grinding in the ball mill of ionized water, 0.5 ± 0.1 μm of average grain diameter is controlled, after a mist projection granulating, in 850 ± 20 DEG C of temperature
The lower electricity consumption heating revolving kiln of degree carries out pre-burning, obtains 0.9~1.2mm of particle diameter pre-burning particle, pre-burning particle then is added into ball
Grinding machine secondary ball milling, mentioned component content is pressed in mechanical milling process, add auxiliary additive calcium oxide：0.05~0.10wt%, mistake
Sodium oxide molybdena：0.02~0.03wt%, potassium peroxide：0.08~0.10wt%, molybdenum sesquioxide：0.02~0.045wt%, dioxy
SiClx：0.01~0.015wt%, zinc metaborate：0.025~0.035wt%, lanthana：0.003~0.005wt%, oxidation
Cerium：0.003~0.005wt%, thorium oxide：0.003~0.005wt%；And pure water is added, control the average grain diameter in ball milling to be
1.0 ± 0.2 μm, finally carry out secondary spraying and obtain MnZn ferrite particle feed powders, take the particle feed powder according to shape of product pressure
After type is made, vacuum drying oven, clock hood type furnace or N are put into2In gas shielded pushed bat kiln, in balanced atmosphere of the partial pressure of oxygen less than 3%,
At a temperature of 1180 30 DEG C of scholars：Sintering 3~5.5 hours.
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Application publication date: 20180109 |