CN103664156A - Preparation method of manganese zinc ferrite powder - Google Patents
Preparation method of manganese zinc ferrite powder Download PDFInfo
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- CN103664156A CN103664156A CN201310574134.XA CN201310574134A CN103664156A CN 103664156 A CN103664156 A CN 103664156A CN 201310574134 A CN201310574134 A CN 201310574134A CN 103664156 A CN103664156 A CN 103664156A
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Abstract
The invention discloses a preparation method of manganese zinc ferrite powder. The manganese zinc ferrite powder is prepared by using Fe2O3, Mn3O4 and ZnO as main raw materials and carrying out the following ten procedures: automatic mixing, high-speed dispersion, sanding, filter pressing, double-screw extruding granulation, pre-drying, pre-sintering, coarse grinding, fine grinding and spray granulation. The preparation method has the beneficial effects that the problems of unevenness in pre-sintering in the dry process and relatively high cost in the wet process are solved; meanwhile, acid radical ions such as Cl<1-> in the raw materials can be substantially reduced through filter pressing, thus prolonging the service life cycles of rotary kiln tubes and exhaust ducts, simultaneously solving the problem of waste discharge pollution and improving the properties of the product; the product has relatively high initial permeability and simultaneously has good temperature characteristics and frequency characteristics, low loss, high impedance, good superposition property and the like.
Description
Technical field
The invention belongs to soft magnetic ferrite technical field, be specifically related to a kind of Mn-Zn ferrite material powder, preparation method thereof, is with Fe
2o
3, Mn
3o
4, ZnO is main raw material,, mist projection granulating ten operations broken by automatic blending, high speed dispersion, sand milling, press filtration, twin screw extruder grain, prebake, pre-burning, coarse reduction, fine powder are made MnZn Soft Ferrite Powder.
Background technology
Mn-Zn ferrite claims again magnetic ceramics, it is the soft magnetic ferrite with spinel structure, compare with metallicl magnetic material of the same type, it is high that it has resistivity, the features such as eddy-current loss is little, because of it, there is the physicalies such as high magnetic permeability, low-coercivity and low-power consumption, be widely used in electronic industry, be mainly used to manufacture high-frequency transformer, inductor block, write head and noise filter etc.Along with the develop rapidly of electronic industry, also more and more higher to the requirement of magneticsubstance.The preparation research that is applicable to the high quality magnetic material of different occasions is more and more subject to people's extensive concern.
Summary of the invention
The object of the present invention is to provide a kind of Mn-Zn ferrite material powder, preparation method thereof, improve the performance of material powder integral body by newly-increased sand milling, press filtration, recycling twin screw extruder grain makes the growth of kiln tube lifetime.
Technical scheme of the present invention is:
A Mn-Zn ferrite material powder, preparation method thereof, concrete steps are as follows:
(1) batching: starting material are weighed by following proportioning:
Fe
2O
3 50～80wt%
Mn
3O
4 10～30wt%
ZnO 5～20wt%
Auxiliary material 0～7wt%;
(2) disperse: by the above-mentioned Fe preparing
2o
3, Mn
3o
4even with the wet mixing of ZnO material powder, control solid content at 50～70wt%;
(3) sand milling: gained slip is carried out to sand milling 20～120 minutes with pure water as solvent;
(4) press filtration: by the good slip of sand milling carry out filter-press dehydration to water ratio at 10%～20wt%;
(5) extruder grain: the good filter cake of press filtration is utilized to twin screw extruder granulation after by fragmentation, and granulation diameter is between 1.5-12mm, and length is between 10～50mm;
(6) prebake: the particulate material after extruding is done to preliminary prebake, make the water ratio <3wt% of particulate material;
(7) rotary kiln pre-burning: the particulate material of water ratio <3% is dropped into rotary kiln and carry out pre-burning, calcined temperature is at 800～1000 ℃, the pre-burning time is about 30～60 minutes, and pre-burning flow control is at 2～5Kg/m, and rotary kiln rotating speed is 10～20 turn/m;
(8) coarse reduction: the particle completing through pre-burning is carried out to coarse reduction to particle diameter 1～2 μ m;
(9) fine powder is broken: the material powder through coarse reduction being carried out to fine powder broken, is that solvent drops into material powder and auxiliary material in proportion with pure water, and sand milling 30～120 minutes is to expecting that powder footpath is 0.7～1.5 μ m;
(10) granulation: by through the broken slip mist projection granulating at the temperature of 80～100 ℃ of fine powder, obtain Mn-Zn ferrite spherical particle material powder.
In step (3), accessory package is containing dispersion agent, defoamer and additive, and wherein additive is CaCO
3, Nb
2o
5and SiO
2in one or more mixture.
In step (6), prebake can utilize the tail gas that reclaims mist projection granulating discharge to carry out.
Above-mentioned technique of the present invention is processed by the deep processing to raw material, has solved dry process pre-burning inhomogeneous, and the problem that wet processing cost is higher, meanwhile, can significantly reduce the Cl in starting material by press filtration
-deng acid ion, extended the cycle in work-ing life of rotary kiln boiler tube and exhaust duct, solve the problem of discarded exhaust emission simultaneously, and improved the properties of product; There is higher initial permeability, there is good temperature profile, frequency response characteristic, low loss, high impedance and good stack performance etc. simultaneously.Be in particular in: 1, in whole whipping process, can make Fe in raw material
2o
3, Mn
3o
4, ZnO mix more even, by press filtration, can make SO in raw material
4, Cl
-deng acid ion, there is decline in various degree, extended the cycle in work-ing life of rotary kiln boiler tube and exhaust duct, solved the problem of discarded exhaust emission simultaneously; And the decline of acid ion can improve the properties of product;
2, be difficult for being bonded to boiler tube tube wall during the particle Hou road rotary kiln pre-burning after twin screw extruder grain, make pre-burning more evenly fully, not only promoted the work-ing life of boiler tube, improved the properties of product simultaneously, there is higher initial permeability, there is good temperature profile, frequency response characteristic, low loss, high impedance and good stack performance etc. simultaneously.
Embodiment
Below in conjunction with specific embodiment, further set forth technical characterictic of the present invention and content.
Embodiment 1
(1) by starting material Fe
2o
3, Mn
3o
4, ZnO is by following weight, uses automatic doser to weigh, it is as follows that raw material forms weight proportion:
Fe
2O
3 70wt%
Mn
3O
4 22wt%
ZnO 7wt%
Auxiliary material 1wt%
(2) use high speed dispersor to carry out preliminary wet mixing in the good material powder of counterweight, make Fe
2o
3, Mn
3o
4, ZnO is evenly distributed, and solid content is controlled to 50～60wt%;
(3) slip after high speed dispersion is carried out to sand milling, the defoamer, the dispersion agent that in this process, add 1～7wt% make raw material be more evenly distributed in this process, add micro-CaCO simultaneously
3, Nb
2o
5and SiO
2in one or more mixture, the sand milling time is 20～120 minutes;
(4) the good slip of sand milling is introduced to barrier film pressure filter and carry out filter-press dehydration, the material powder water ratio after requirement dehydration is at 10%～20wt%;
(5) the good filter cake of press filtration, by adopting screw propulsion to enter twin screw Squeezinggranulator after fragmentation, through twin screw Squeezinggranulator, form cylindrical particle, particle diameter is generally between 1.5-12mm, and length is generally between 10～50mm.
(6) utilize the tail gas that reclaims mist projection granulating discharge to do preliminary prebake to the particulate material after pushing, make the water ratio <3wt% of particulate material;
(7) particulate material of water ratio <3wt% is dropped into rotary kiln and carry out pre-burning, calcined temperature is at 1000 ℃, the pre-burning time is about 30 minutes, pre-burning flow control is at 2kg/m, rotary kiln rotating speed is 10 turn/m, by pre-burning, allows raw material carry out preliminary solid state reaction, and allows feed particles part Ferrite method, the shrinking percentage of product is burnt till in control, prevents deformation of products;
(8) the black feed particles completing through pre-burning is carried out to coarse reduction to particle diameter 1～2 μ m, employing be vibromill, coarse reduction is regularly about 20 minutes;
(9) the material powder of coarse reduction is carried out to fine powder broken, utilize pure water in sand mill, to drop in proportion material powder, additive, dispersion agent and defoamer as solvent, obtain the black slip of fine powder after broken, whole thin grinding time is about 120 minutes, feed particles relies on steel ball and the collision between it, friction when fine powder is broken, thereby further reduce the median size of material powder, the distribution range of dwindling its particle diameter, extremely thin powder particle diameter is about 0.7 μ m;
(10) by through the broken slip of fine powder at the temperature of 80 ℃, by mist projection granulating tower, make it to become surface drying, centre is slightly moistening, has good fluidity and dispersed spherical particle.
(11) the low-loss manganese zine soft magnetic ferrite particles material property making by above-mentioned technique can be as follows:
Embodiment 2
(1) by starting material Fe
2o
3, Mn
3o
4, ZnO is by following weight, uses automatic doser to weigh, it is as follows that raw material forms weight proportion:
Fe
2O
3 69wt%
Mn
3O
4 14.5wt%
ZnO 15.5wt%
Auxiliary material 1wt%;
(2) use high speed dispersor to carry out preliminary wet mixing in the good material powder of counterweight, make Fe
2o
3, Mn
3o
4, ZnO is evenly distributed, and solid content is controlled to 50～60wt%; ;
(3) use pure water to carry out sand milling as solvent the slip after high speed dispersion, raw material is more evenly distributed in this process, the sand milling time is 20 minutes;
(4) the good slip of sand milling is introduced to barrier film pressure filter and carry out filter-press dehydration, the material powder water ratio after requirement dehydration is at 20wt%;
(5) the good filter cake of press filtration, by adopting screw propulsion to enter twin screw Squeezinggranulator after fragmentation, through twin screw Squeezinggranulator, form cylindrical particle, particle diameter is generally between 1.5-12mm, and length is generally between 10～50mm.
(6) utilize the tail gas that reclaims mist projection granulating discharge to do preliminary prebake to the particulate material after pushing, make the water ratio <3wt% of particulate material;
(7) particulate material of water ratio <3wt% is dropped into rotary kiln and carry out pre-burning, calcined temperature is at 800 ℃, the pre-burning time is about 60 minutes, pre-burning flow control is at 5kg/m, rotary kiln rotating speed is 20 turn/m, by pre-burning, allows raw material carry out preliminary solid state reaction, and allows feed particles part Ferrite method, the shrinking percentage of product is burnt till in control, prevents deformation of products;
(8) the black feed particles completing through pre-burning is carried out to coarse reduction to particle diameter 1～2 μ m, employing be vibromill, coarse reduction is regularly about 60 minutes;
(9) the material powder of coarse reduction is carried out to fine powder broken, utilize pure water in sand mill, to drop in proportion material powder, additive, dispersion agent and defoamer as solvent, obtain the black slip of fine powder after broken, whole thin grinding time is about 30 minutes, feed particles relies on steel ball and the collision between it, friction when fine powder is broken, thereby further reduce the median size of material powder, the distribution range of dwindling its particle diameter, extremely thin powder particle diameter is about 1.5 μ m;
(10) by through the broken slip of fine powder at the temperature of 100 ℃, by mist projection granulating tower, make it to become surface drying, centre is slightly moistening, has good fluidity and dispersed spherical particle.
(11) the high-permeability Mn-Zn soft magnetic ferrite particulate material performance making by above-mentioned technique is as follows:
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So every, do not depart from the equivalence completing under principles of this disclosure or revise, all falling into the scope of protection of the invention.
Claims (3)
1. a Mn-Zn ferrite material powder, preparation method thereof, is characterized in that, concrete steps are as follows:
(1) batching: starting material are weighed by following proportioning:
Fe
2O
3 50～80wt%
Mn
3O
4 10～30wt%
ZnO 5～20wt%
Auxiliary material 0～7wt%;
(2) disperse: by the above-mentioned Fe preparing
2o
3, Mn
3o
4even with the wet mixing of ZnO material powder, control solid content at 50～70wt%;
(3) sand milling: gained slip is carried out to sand milling 20～120 minutes with pure water as solvent;
(4) press filtration: by the good slip of sand milling carry out filter-press dehydration to water ratio at 10%～20wt%;
(5) extruder grain: the good powder of press filtration is utilized to twin screw extruder granulation, and granulation diameter is between 1.5-12mm, and length is between 10～50mm;
(6) prebake: the particulate material after extruding is done to preliminary prebake, make the water ratio <3wt% of particulate material;
(7) rotary kiln pre-burning: the particulate material of water ratio <3% is dropped into rotary kiln and carry out pre-burning, calcined temperature is at 800～1000 ℃, and the pre-burning time is about 30～60 minutes, and pre-burning flow control is at 2～5Kg/m, and rotary kiln rotating speed is 5～20 turn/m;
(8) coarse reduction: the particle completing through pre-burning is carried out to coarse reduction to particle diameter 1～2 μ m;
(9) fine powder is broken: the material powder through coarse reduction being carried out to fine powder broken, is that solvent drops into material powder and auxiliary material in proportion with pure water, and sand milling 30～120 minutes is to expecting that powder footpath is 0.7～1.5;
(10) granulation: by through the broken slip mist projection granulating at the temperature of 80～100 ℃ of fine powder, obtain Mn-Zn ferrite spherical particle material powder.
2. Mn-Zn ferrite material powder, preparation method thereof according to claim 1, is characterized in that, the tail gas that in step (6), prebake utilization recovery mist projection granulating is discharged carries out.
3. Mn-Zn ferrite material powder, preparation method thereof according to claim 1, is characterized in that, in step (9), accessory package is containing dispersion agent, defoamer and additive, and wherein additive is CaCO
3, Nb
2o
5and SiO
2in one or more mixture.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104084586A (en) * | 2014-06-05 | 2014-10-08 | 浙江大学 | Filter-pressing preparation method for soft-magnetic composite material |
| CN105060875A (en) * | 2015-08-19 | 2015-11-18 | 无锡斯贝尔磁性材料有限公司 | Thin film type MnZn ferrite magnetic material special powder |
| CN107573025A (en) * | 2017-09-12 | 2018-01-12 | 成都新柯力化工科技有限公司 | A kind of architectural pottery dry method flouring technology of green energy conservation |
| CN114133234A (en) * | 2021-12-07 | 2022-03-04 | 鞍山安特磁材有限公司 | Novel process for producing pressure-resistant ferrite powder |
| CN117438206A (en) * | 2023-11-15 | 2024-01-23 | 南通悦立磁业有限公司 | Preparation device and process of wide-temperature low-power-consumption manganese zinc ferrite powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531559A (en) * | 2010-12-22 | 2012-07-04 | 上海宝钢磁业有限公司 | Preparation method for high-performance manganese zinc ferrite powder |
-
2013
- 2013-11-15 CN CN201310574134.XA patent/CN103664156A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531559A (en) * | 2010-12-22 | 2012-07-04 | 上海宝钢磁业有限公司 | Preparation method for high-performance manganese zinc ferrite powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104084586A (en) * | 2014-06-05 | 2014-10-08 | 浙江大学 | Filter-pressing preparation method for soft-magnetic composite material |
| CN105060875A (en) * | 2015-08-19 | 2015-11-18 | 无锡斯贝尔磁性材料有限公司 | Thin film type MnZn ferrite magnetic material special powder |
| CN107573025A (en) * | 2017-09-12 | 2018-01-12 | 成都新柯力化工科技有限公司 | A kind of architectural pottery dry method flouring technology of green energy conservation |
| CN114133234A (en) * | 2021-12-07 | 2022-03-04 | 鞍山安特磁材有限公司 | Novel process for producing pressure-resistant ferrite powder |
| CN117438206A (en) * | 2023-11-15 | 2024-01-23 | 南通悦立磁业有限公司 | Preparation device and process of wide-temperature low-power-consumption manganese zinc ferrite powder |
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Application publication date: 20140326 |
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