CN106747394A - A kind of high magnetic permeability lower losses ferrite material and preparation method thereof - Google Patents
A kind of high magnetic permeability lower losses ferrite material and preparation method thereof Download PDFInfo
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- CN106747394A CN106747394A CN201611050197.5A CN201611050197A CN106747394A CN 106747394 A CN106747394 A CN 106747394A CN 201611050197 A CN201611050197 A CN 201611050197A CN 106747394 A CN106747394 A CN 106747394A
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Abstract
The present invention relates to a kind of high magnetic permeability lower losses ferrite material and preparation method thereof, the technique that the present invention is provided includes step：Raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.0 70.5wt%, the ratio of 22 23wt%, 6.5 7.5wt% carries out mixed grinding；Then carry out pre-burning and obtain Preburning material, it is temperature and pre-burning flow to control pre-burning；Pre-burning abrasive lapping is carried out into coarse crushing, particle diameter is controlled；Meal particle, trace mineral supplement, deionized water, dispersant and defoamer are carried out into finely divided and slurrying and obtain prefabricated slurry, be eventually adding polyvinyl alcohol it is uniform after, it is cold to go to room temperature by gained slurry spray granulating and drying, control moisture content.Conventional low-power consumption feed powder magnetic conductivity is set to reach more than 2600 by the above-mentioned technical proposal present invention, so that can be normal to start in cold district not temperature influence using the inductance type magnetic core that the feed powder is produced.It is easy to the production (without refining repeatedly, inductance value being improved by lifting magnetic core surface smoothness) of grinding process simultaneously.
Description
Technical field
The present invention relates to a kind of high magnetic permeability lower losses ferrite material and preparation method thereof.
Background technology
Mn-Zn soft magnetic ferrite has the physicochemical characteristics such as high magnetic permeability, low-coercivity and low-power consumption, quilt
It is widely used in electronics industry, is mainly used to manufacture high frequency transformer, inductor, write head and noise filter etc..With
Electronics industry is developed rapidly, the also more and more higher of the requirement to magnetic material performance, wherein there have a class material requirements to have to be low
With magnetic conductivity higher while power attenuation.So that can be in cold district not using the inductance type magnetic core that the feed powder is produced
Temperature influence is normal to start.
At present the initial permeability of low-power consumption material (non-temperature wide is class) similar both at home and abroad it is general 2000-2600 it
Between, 25 DEG C of power consumptions are in 600-700mw/cm3Between, 100 DEG C of power consumptions are in 300-400mw/cm3Between, saturation induction density Bs：
25 DEG C >=500mT, 100 DEG C >=390mT.Such as PC44 of TDK companies of Japan, the 6H40 of Japanese FDK companies and PHILIPS Co.
3C90.TP4A of DMR44 and Tian Tong companies of domestic Dong Ci companies etc..But the initial permeability of above material is below
2600, saturation induction density is also relatively low.Client portion inductance type magnetic core cannot be met in the normal startup of cold district (by low
Temperature influence).Such as need to meet customer requirement, then will be substantially improved using the material of another series, cost.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation method of high magnetic permeability lower losses ferrite material, using the method one
Aspect can meet demand of the magnetic core client to low-power consumption inductance core high；On the other hand grinding efficiency, resulting low work(are improved
Feed consumption powder magnetic conductivity reaches more than 2600, is easy to grinding to produce.So as to realize the production of high magnetic permeability lower losses ferrite material.
In order to realize above technique effect, the present invention is to be achieved by the steps of：
S1. raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.0-70.5wt%, 22-23wt%,
The ratio of 6.5-7.5wt% carries out mixed grinding, makes feed powder Bulk Specific Gravity in 0.7-1g/cm3, obtain the good material of mixed grinding；Institute
Mixed grinding is stated for mixing and ball milling；The incorporation time 60 minutes, Ball-milling Time 15-25 minutes.
S2. the good material pre-burning of the mixed grinding of step S1 is obtained into Preburning material (can put into two-tube stove), controls the pre-burning to be
960 DEG C -1300 DEG C of temperature, pre-burning flow 1.8-2.8Kg/ minutes；
S3. the pre-burning abrasive lapping of step S2 is carried out into coarse crushing, control D50 particle diameters are between 2.0-3.5 μm；
S4. fine powder is carried out in meal particle, trace mineral supplement, deionized water, dispersant and defoamer being put into sand mill
Broken and slurrying obtains prefabricated slurry, and it is 1.3-2 μm to be sanded to D50 particle diameters；The meal particle, deionized water, dispersant with disappear
The mass ratio of infusion is 1:0.4-0.7:0.02-0.04:0.002-0.003；The trace mineral supplement is CaCO3,SiO2,V2O5,
Nb2O5And CO3O4；The trace mineral supplement is CaCO with the mass ratio of meal particle3：0.03-0.04wt%, V2O5：
0.025-0.035wt%；Nb2O5：0.02-0.03wt%；CO3O4：0.1-0.2wt%；
S5. it is cold by gained slurry spray granulating and drying after the prefabricated slurry in step S4 adds polyvinyl alcohol uniform
Go to room temperature, control moisture content for 0.15%-0.3%, moisture content fluctuation is ± 0.04%.
Preferably, in step S1, the Bulk Specific Gravity is 0.80-0.9g/cm3, is beneficial to pre-burning operation.
Preferably, in step S2, the furnace tube temperature be 960 DEG C -1000 DEG C, be beneficial to control product contraction distortion and
CL- contents.
Preferably, in step S2, pre-burning flow is 2-2.4Kg/ minutes, is beneficial to control contraction distortion and the CL- of product
Content.
Preferably, in step S3, D50 particle diameters are 2.0-2.8 μm, are beneficial to be sanded and mist projection granulating operation.
Preferably, in step S4, D50 particle diameters are 1.4-1.6 μm, are beneficial to lift product electrical property.
Preferably, in step S4, the mass ratio of the meal particle, deionized water, dispersant and defoamer is 1:0.5:
0.025:0.0025, it is beneficial to the compressing of product and lower road mist projection granulating operation.
Preferably, in step S5, control moisture content for 0.18%-0.25%, be beneficial to compressing.
High magnetic permeability lower losses ferrite material prepared by the preparation method of above-mentioned high magnetic permeability lower losses ferrite material
Fig. 1 is the feed powder technological process of production：The formula weighing one of selected raw material one is dry-mixed-and the sand mill fine grinding one of pre-burning one makes
The slurry packaging and storage of mist projection granulating one.To ensure accurate raw material (di-iron trioxide, mangano-manganic oxide and zinc oxide) formula, it is to avoid
Formula deviation causes penalty or product rejection, and accurate physico-chemical analysis need to be done before in raw material, and strictly by formula
Operation.Three kinds of raw material are well mixed using ball mill.The shrinkage factor of product is controlled by suitable pre-sinter process, is reduced and is produced
Product deform.Coarse crushing is done to Preburning material using ball mill again, is easy to be sanded.Using sand mill, add some trace impurities and enter
Row separating twice, so as to further improve magnetic property.For the ease of being sanded and spraying, also need to add suitable pure aborning
Water, glue, dispersant and defoamer etc., are made slurry.Slurry is made into spherical particles finally by the mode of spray drying to enter
Row packaging.Wherein by according to the requirement of client, the moisture content of particle, Bulk Specific Gravity and distribution of particles are controlled.
The beneficial effects of the invention are as follows：
1) Fe is adjusted by appropriate using in the formula of domestic iron oxide red3+And Zn2+Content, controls valley point and the power consumption of product；
2) a certain proportion of micro- CO is added when being sanded3O4, so as to reach production high magnetic permeability lower losses ferrite material
The purpose of material；
3) 70.0-70.5wt%, 22-23wt%, 6.5- are pressed in di-iron trioxide, mangano-manganic oxide and zinc oxide
In the case of the ratio of 7.5wt%, the mass ratio for being meal particle, deionized water, dispersant and defoamer is 1:0.4-0.7:
0.02-0.04:0.002-0.003；Trace mineral supplement is CaCO with the mass ratio of meal particle3：0.03-0.04wt%,
V2O5：0.025-0.035wt%；Nb2O5：0.02-0.03wt%；CO3O4：During 0.1-0.2wt%, cooperative effect can be produced,
Feed powder magnetic conductivity can be made to reach more than 2600,25 DEG C of power consumptions in 500-550mw/cm3Between, 100 DEG C of power consumptions are in 300-380mw/
cm3Between.
4) knowable to the ferritic three-phase constituent phasors of MnZn, Fe is worked as2O3When content is more than 5O%, its λsBe on the occasion of
With the λ of ferrite other partssNegative value plays local negative function, makes ferritic λsWith relatively low value.ZnO content increase can
To lower K1Value, but corresponding Fe2O3Content is accomplished by slightly subtracting, and could so maintain K1=0 and λs=0 occurs simultaneously, so as to carry
The ferritic initial permeabilities of MnZn high, reduction power consumption.Therefore the present invention have selected suitable main formula, make product it is existing compared with
Initial permeability high, there is relatively low power consumption again.
5) doping is the effective measures for improving Ferrite Material performance, has important to improving ferritic performance
Meaning.Experiment shows, is keeping adding appropriate V in MnZn ferrites in the case that premise is constant2O5Crystal grain refinement can be made, dropped
Low Br, so as to reduce magnetic hystersis loss.The addition of Ca and Si can equally improve resistivity, reduce eddy-current loss.It is of the invention mainly to exist
Appropriate Co is mixed with after selection basic recipe2O3, comprehensively utilize Fe2+And Co2+To the compensating action of K1, and reasonable adjusting
Fe2+With Co2+Content K1 values is leveled off to zero, reduce Steinmetz's constant, improve magnetic conductivity, obtain less magnetic hystersis loss.
6) conventional low-power consumption feed powder magnetic conductivity is made to reach more than 2600 by the above-mentioned technical proposal present invention, so that adopting
The magnetic core produced with the feed powder can be in cold district not temperature influence.It is easy to the production of grinding process simultaneously (without essence repeatedly
Mill, inductance value is improved by lifting magnetic core surface smoothness).Domestic and international low-power consumption conventional products, because initial permeability is equal
Less than 2600, saturation induction density is also relatively low.Normal startup of the client portion inductance type magnetic core in cold district cannot be met
(receiving low temperature effect).Such as need to meet customer requirement, then will be substantially improved using the material of another temperature series wide, cost.
7) it is applied on magnetic core using the feed powder 2K8D of present invention production, fully meets the requirement of particular customer, and produce
Considerable economic benefit.
Brief description of the drawings
Fig. 1 is the feed powder technological process of production；1 is the inspection of raw and process materials and to receive, and 2 is sub-material and dispensing, and 3 ball milling mixings are (red
Shake), 4 two-tube kiln pre-burnings, 5 ball milling meal are pure, and 6 are sanded (finely divided), 7 mist projection granulatings, 8 bags of packaging packaging and storages.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
1. raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.12wt%：22.8wt%：7.08wt%
Ratio enter conical mixer and carry out mixing 60 minutes, then using ball milling 25 minutes, control feed powder Bulk Specific Gravity is in 0.80-
0.9g/cm3Between.
2. the good material of mixing and ball milling is put into two-tube stove carries out pre-burning, controls 980 DEG C of furnace tube temperature, pre-burning flow 2-
2.4Kg/ minutes.
3. Preburning material input straight-line ball mill is carried out into coarse crushing, control D50 particle diameters are at 2.0-2.8 μm.
4. finely divided and slurrying is carried out in meal particle being put into sand mill.Wherein need add trace mineral supplement, plus go from
Sub- water, bonus point powder and plus defoamer.It is sanded to D50 particle diameters：1.4-1.6μm.Meal particle and deionized water, dispersant and disappear
The mass ratio of infusion is 1:0.5:0.025:0.0025.Wherein additive is CaCO3,SiO2,V2O5,Nb2O5With micro- A,
All kinds of trace mineral supplements are CaCO with the mass ratio of crushed material3：0.0325wt%, V2O5：0.025wt%, Nb2O5：
0.025wt%, CO3O4：0.15wt%.
5. polyvinyl alcohol is added, it is cold to go to room temperature by gained slurry spray granulating and drying.Control moisture content is in 0.2%-
0.25%.And control moisture content to fluctuate ± 0.04%.The pressure rings of Φ 30.
6. ring is sintered in bell-jar atmosphere sintering furnace, and sintering temperature is incubated 4h, partial pressure of oxygen 3.0%, using flat at 1360 DEG C
Weighing apparatus oxygen platen press cooling down.
7. 8258 type power consumption instrument are respectively adopted and 4284 type inductance instrument survey electrical property.
8. experimental result and analysis
The initial permeability of this programme product is 2280,25 DEG C of power consumption 665mw/cm3, 100 DEG C of power consumption 382mw/cm3, saturation
Magnetic induction density B s：25℃：502mT, 100 DEG C：396mT.
Embodiment 2
1. raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.2wt%：22.8wt%：The ratio of 7wt%
Example enters conical mixer carries out mixing 60 minutes, and then using ball milling 25 minutes, control feed powder Bulk Specific Gravity is in 0.80-0.9g/cm3
Between.
2. the good material of mixing and ball milling is put into two-tube stove carries out pre-burning, controls 980 DEG C of furnace tube temperature, pre-burning flow 2-
2.4Kg/ minutes.
3. Preburning material input straight-line ball mill is carried out into coarse crushing, control D50 particle diameters are at 2.0-2.8 μm.
4. finely divided and slurrying is carried out in meal particle being put into sand mill.Wherein need add trace mineral supplement, plus go from
Sub- water, bonus point powder and plus defoamer.It is sanded to D50 particle diameters：1.4-1.6μm.Meal particle and deionized water, dispersant and disappear
The mass ratio of infusion is 1:0.5:0.025:0.0025.Wherein additive is CaCO3,SiO2,V2O5,Nb2O5With micro- A,
All kinds of trace mineral supplements are CaCO with the mass ratio of crushed material3：0.0325wt%, V2O5：0.025wt%, Nb2O5：
0.025wt%, CO3O4：0.15wt%.
5. polyvinyl alcohol is added, it is cold to go to room temperature by gained slurry spray granulating and drying.Control moisture content is in 0.2%-
0.25%.And control moisture content to fluctuate ± 0.04%.The pressure rings of Φ 30.
6. ring is sintered in bell-jar atmosphere sintering furnace, and sintering temperature is incubated 4h, partial pressure of oxygen 3.0%, using flat at 1360 DEG C
Weighing apparatus oxygen platen press cooling down.
7. 8258 type power consumption instrument are respectively adopted and 4284 type inductance instrument survey electrical property.
The initial permeability of this programme product is 2820,25 DEG C of power consumption 520mw/cm3, 100 DEG C of power consumption 337mw/cm3, saturation
Magnetic induction density B s：25℃：524mT, 100 DEG C：422mT.
Embodiment 3
1. raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.2wt%：22.8wt%：The ratio of 7wt%
Example enters conical mixer carries out mixing 60 minutes, and then using ball milling 25 minutes, control feed powder Bulk Specific Gravity is in 0.80-0.9g/cm3
Between.
2. the good material of mixing and ball milling is put into two-tube stove carries out pre-burning, controls 980 DEG C of furnace tube temperature, pre-burning flow 2-
2.4Kg/ minutes.
3. Preburning material input straight-line ball mill is carried out into coarse crushing, control D50 particle diameters are at 2.0-2.8 μm.
4. finely divided and slurrying is carried out in meal particle being put into sand mill.Wherein need add trace mineral supplement, plus go from
Sub- water, bonus point powder and plus defoamer.It is sanded to D50 particle diameters：1.4-1.6μm.Meal particle and deionized water, dispersant and disappear
The mass ratio of infusion is 1:0.5:0.025:0.0025.Wherein additive is CaCO3,SiO2,V2O5,Nb2O5With micro- A,
All kinds of trace mineral supplements are CaCO with the mass ratio of crushed material3：0.0125wt%, V2O5：0.015wt%, Nb2O5：
0.015wt%, CO3O4：0.05wt%.
5. polyvinyl alcohol is added, it is cold to go to room temperature by gained slurry spray granulating and drying.Control moisture content is in 0.2%-
0.25%.And control moisture content to fluctuate ± 0.04%.The pressure rings of Φ 30.
6. ring is sintered in bell-jar atmosphere sintering furnace, and sintering temperature is incubated 4h, partial pressure of oxygen 3.0%, using flat at 1360 DEG C
Weighing apparatus oxygen platen press cooling down.
7. 8258 type power consumption instrument are respectively adopted and 4284 type inductance instrument survey electrical property.
The initial permeability of this programme product is 2166,25 DEG C of power consumption 733mw/cm3, 100 DEG C of power consumption 425mw/cm3, saturation
Magnetic induction density B s：25℃：504mT, 100 DEG C：401mT.
Find that the conventional low-power consumption feed powder magnetic conductivity that example 2 is produced reaches more than 2600,25 DEG C by the embodiment above
Power consumption is in 500-550mw/cm3Between, 100 DEG C of power consumptions are in 300-380mw/cm3Between, saturation induction density Bs：25℃≥
520mT, 100 DEG C >=420mT.So that can be in cold district not temperature influence using the magnetic core that the feed powder is produced.Just simultaneously
In the production (without refining repeatedly, inductance value being improved by lifting magnetic core surface smoothness) of grinding process.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment
Content.So every do not depart from the lower equivalent or modification for completing of spirit disclosed in this invention, the model of present invention protection is both fallen within
Enclose.
Claims (10)
1. a kind of preparation method of high magnetic permeability lower losses ferrite material, it is characterised in that：
S1. raw material di-iron trioxide, mangano-manganic oxide and zinc oxide are pressed into 70.0-70.5wt%, 22-23wt%, 6.5-
The ratio of 7.5wt% carries out mixed grinding, makes feed powder Bulk Specific Gravity in 0.7-1g/cm3, obtain the good material of mixed grinding；
S2. the good material of the mixed grinding of step S1 is carried out into pre-burning and obtains Preburning material, control pre-burning for 960 DEG C -1300 DEG C of temperature,
Pre-burning flow 1.8-2.8Kg/ minutes；
S3. the pre-burning abrasive lapping of step S2 is carried out into coarse crushing, control D50 particle diameters are between 2.0-3.5 μm；
S4. meal particle, trace mineral supplement, deionized water, dispersant and defoamer are carried out into finely divided and slurrying and obtains prefabricated
Slurry, it is 1.3-2 μm to be sanded to D50 particle diameters；The mass ratio of the meal particle, deionized water, dispersant and defoamer is 1:
0.4-0.7:0.02-0.04:0.002-0.003；The trace mineral supplement is CaCO3,V2O5,Nb2O5And CO3O4；It is described micro
Additive is CaCO with the mass ratio of meal particle3：0.03-0.04wt%, V2O5：0.025-0.035wt%；Nb2O5：
0.02-0.03wt%；CO3O4：0.1-0.2wt%；
S5. after the prefabricated slurry in step S4 adds polyvinyl alcohol uniform, gained slurry spray granulating and drying is cooled to
Room temperature, it is 0.15%-0.3% to control moisture content.
2. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S1
In, the mixed grinding is mixing and ball milling；The incorporation time 60 minutes, Ball-milling Time 15-25 minutes.
3. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S1
In, the Bulk Specific Gravity is 0.80-0.9g/cm3。
4. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S2
In, the furnace tube temperature is 960 DEG C -1000 DEG C, and pre-burning flow is 2-2.4Kg/ minutes.
5. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S3
In, D50 particle diameters are 2.0-2.8 μm.
6. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S4
In, D50 particle diameters are 1.4-1.6 μm.
7. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S4
In, the mass ratio of the meal particle, deionized water, dispersant and defoamer is 1:0.5:0.025:0.0025.
8. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S4
In, preferably 0.2%-0.25%.
9. the preparation method of high magnetic permeability lower losses ferrite material according to claim 1, it is characterised in that：Step S5
In, moisture content is controlled for 0.2%-0.25%, moisture content stability bandwidth is ± 0.04%.
10. the height that prepared by the preparation method of any one high magnetic permeability lower losses ferrite material according to claim 1-9
Magnetic conductivity lower losses ferrite material.
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| CN117438205A (en) * | 2023-11-13 | 2024-01-23 | 南通三优佳磁业有限公司 | Preparation process and application of rare earth doped manganese zinc ferrite magnetic material |
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