CN103159469A - Preparation method of Mn-Zn ferrite powder with high permeability - Google Patents
Preparation method of Mn-Zn ferrite powder with high permeability Download PDFInfo
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- CN103159469A CN103159469A CN2011104192100A CN201110419210A CN103159469A CN 103159469 A CN103159469 A CN 103159469A CN 2011104192100 A CN2011104192100 A CN 2011104192100A CN 201110419210 A CN201110419210 A CN 201110419210A CN 103159469 A CN103159469 A CN 103159469A
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Abstract
The invention discloses a preparation method of a Mn-Zn ferrite powder with high permeability. Impurity and particle size control is carried out since raw material mixing, and a main formulation and trace additives of the powder are precisely controlled. The method decreases contents of Cl<-> and trace impurity elements in the powder by different degrees: Cl<-><0.07%, Ca<2+> < 0.01%, K <+> <0.005%, Na<+><0.005% and SO4<2-><0.01%; BET is increased, and mixing uniformity is also improved obviously; and the powder has good moisture content consistency, which is conducive to production of excellent Mn-Zn soft magnetic ferrite material with high permeability.
Description
Technical field
The invention belongs to the powder body material field, be specifically related to a kind of preparation method of high permeability MnZn ferrite material powder.
Background technology
Soft magnetic ferrite is a kind of very important basic function material in national economy, is widely used in each electronic product, and wherein the high-permeability Mn-Zn material is along with the market development variation is the fastest, one of market outlook best material.High Initial Permeability MnZn Ferrite Materials is mainly used in the electronic circuit wide-band transformer, the pulse transformer in the fields such as ISDN (Integrated Services Digital Network) (ISDN), local area network (LAN), wide area network (WAN), background illumination, the fields such as anti-electromagnetic wave wave filter.The magnetic core in these fields is to work under feeble field basically, and at this moment the high magnetic permeability of material will demonstrate unique superiority.At first, when the magnetic permeability of material is higher, the inductance value that less coil turn just can acquiring demand, and then effectively reduce the direct current resistance of coil and by its loss that causes; Secondly, use the high material of magnetic permeability can obviously reduce the volume of transformer, be conducive to miniaturization, the lightweight of device and system.These characteristics have been complied with the development trend of electronic product, and its output has accounted for more than 25% of whole soft magnetic ferrite ultimate productions at present.Along with the high speed development of the electronics and information industries such as communication, computer, network, its market requirement is with average annual speed rapid growth more than 20%.
Batch production high magnetic conductivity ferrite magnetic core has two kinds of different manufacturing process, i.e. coprecipitation technology and oxide process both at home and abroad at present.
The coprecipitation technology route is: with a certain proportion of iron, manganese, zinc and sulfuric acid reaction, generate vitriol, add again ammonium hydrogencarbonate and ammoniacal liquor to carry out chemical reaction under certain condition, generate carbonate sediment, purify through rinsing again, pre-burning is decomposed, and generates oxide compound, as producing the ferritic starting material of high magnetic permeability MnZn.Technical process is: selected raw material → add additional composition → batching dissolving → filtration → carbonate is coprecipitated → and dehydration washing → preparation slip → spraying drying → pre-burning → sand mill fine grinding → preparation slip → mist projection granulating → compression moulding → sintering → mill processing → cleaning → detection.
The key of coprecipitation technology is: (1) dissolving is purified: in enamel reaction still, add a certain amount of sulphuric acid soln, then add successively iron, manganese, zinc, filter purification after having dissolved, obtain the high-purity sulfuric acid salts solution; (2) coprecipitated washing: certain ammonium hydrogencarbonate and ammoniacal liquor Hybrid Heating to certain temperature, are more slowly added sulfate liquor, produce throw out, then through drying washing, generate coprecipitated material; (3) pre-burning powder process: with coprecipitated material oven dry, through the kiln pre-burning, begin to take shape ferrite, then pass through sand milling, slurrying, spray drying granulation, form particulate material.The coprecipitated material Powder Particle Size of Mn-Zn ferrite is thin, impurity is few, the activity is good, is conducive to improve initial permeability.But due to fine size, reached at the nano level that has brings difficulty to moulding; Homogeneity of product also is difficult to control in addition, when building line environmental requirement higher, invest larger.
Oxide process that is usually said ceramic process, technical process is: selected raw material → formula weighing → be dry mixed → pelletizing → pre-burning → sand mill fine grinding → slurrying → mist projection granulating → compression moulding → sintering → mill processing → clean → detect.Also there is at present producer to adopt twice mist projection granulating, namely increases an atomizing granulating technology before pre-burning.The characteristics of this technique are that operation is less, are convenient to microcomputer control, can realize that canalization carries out production strictly in line with rules and regulations, and homogeneity of product is more easy to control, but that detrimental impurity is removed is more difficult, and initial permeability is difficult for improving.
Produce high magnetic conductivity soft-magnetic ferrite material, starting material, main formula and trace mineral supplement are internal causes, and what is more important will have advanced manufacturing process and equipment as guarantee.Because this class material is under identical processing condition, material purity is high, impurity is few, fine size and the active high raising that means magnetic permeability.Formula is the key of producing the high-permeability Mn-Zn ferrite material.Usually the ratio that improves Zn in formula can obtain the high product of magnetic permeability.Must strict control composition be offset in actual production, the minor shifts of composition all may produce a very large impact Mn-Zn Ferrite Material performance.Doping is the effective measure of improving the Ferrite Material performance, equally also be applicable to high-permeability material, when pursuing desirable Mn-Zn ferrite grain boundary structure formation condition, significantly control hole and lattice imperfection simultaneously, realize the crystal grain of high density homogeneousization.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of the mixing from starting material just to carry out the control of impurity and particle diameter, can accurately control the Mn-Zn ferrite material powder, preparation method thereof of material powder main formula and trace mineral supplement, to make the High Initial Permeability MnZn Ferrite Materials with various good electric magnetic properties.
The technical solution used in the present invention is as follows:
A kind of preparation method of high permeability MnZn ferrite powder comprises the steps:
1) with raw material and deionized water, dispersion agent according to 1: 0.3～1.2: 0～0.1, preferred 1: 0.4～0.8: 0～0.05 mass ratio mixes, sand milling is to its particle diameter: D50:0.5～1.2 μ m, D90:0.8～3 μ m get slip; Described raw material is Fe
2O
3, Mn
3O
4, ZnO is according to the mixed in molar ratio gained of x: y: z, wherein x is that 0.515～0.525, y is 1-x-z, z is 0.21～0.23;
2) precipitation 20～24h, make the supernatant liquor overflow, and it is 5～15% that the press filtration gained is precipitated to water ratio, preferred 5～10%, with after the fragmentation of gained filter cake at 600 ℃～1100 ℃, carry out pre-burning under preferred 850 ℃～1000 ℃, the pre-burning time, 0.5-1h got Preburning material;
3) the gained Preburning material is carried out coarse reduction, get crushed material, add trace mineral supplement, add deionized water, dispersion agent and defoamer, sand milling is to D50:0.7 μ m～1.5 μ m, D90:1 μ m～3 μ m, preferred D0.8 μ m～1.2 μ m, D90:1.2 μ m～2 μ m; The mass ratio of crushed material and deionized water, dispersion agent, defoamer is 1: 0.1～0.7: 0～0.1: 0～0.05, preferred 1: 0.3～0.4: 0～0.05: 0～0.02;
4) add polyvinyl alcohol, with gained slip mist projection granulating, drying is cooled to room temperature.Control water ratio between 0.1%～1%, preferred 0.15%～0.3%, and control the water ratio fluctuation ± 0.03%.
Step 1) the D50 particle diameter of Raw is respectively: Fe
2O
3: 1.2～1.5 μ m; ZnO:0.8～1.2 μ m; Mn
3O
4: 1.0～1.4 μ m.
Step 3) trace mineral supplement described in is SiO
2, CaCO
3, Mo
2O
3And Bi
2O
3In one or more, the mass ratio of each trace mineral supplement and crushed material is SiO
2: 0-0.00125wt%, CaCO
3: 0-0.0125wt%, Mo
2O
3: 0.045wt%-0.0875wt%, Bi
2O
3: 0.02wt%-0.04wt%.
By adopting technique scheme, the present invention makes Cl in powder
-The decline of content and the large degree of micro impurity element: Cl
-＜0.07%, Ca
2+＜0.01%, K
+＜0.005%, Na
+＜0.005%, SO
4 2-＜0.01%; BET is improved, and mixes consistence and also be significantly improved, and material powder water ratio high conformity is conducive to produce the Mn-Zn soft magnetic ferrite of good high magnetic permeability.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1:
Press Fe
2O
3: ZnO: Mn
3O
4Be the molar ratio ingredient of 52.1: 21.8: 26.1, the initial D50 particle diameter of raw material is: Fe
2O
3: 1.4 μ m; ZnO:1.0 μ m; Mn
3O
4: 1.2 μ m;
With above-mentioned three kinds of starting material altogether 1000kg join high speed dispersor and mix tentatively with 400kg deionized water, 10kg dispersion agent triammonium citrate and disperse, raw material after dispersion enters into the horizontal sand mill sand milling to be mixed, particle diameter after sand milling is D50:0.8 μ m, D90:1.3 μ m;
Slip is precipitated 1 day, make the supernatant liquor overflow, mud after precipitation carries out filter-press dehydration with diaphragm filter press, controlling feed pressure during charging is 0.1Mpa, and progressively improve feed pressure to 0.8Mpa, advanced to be filled with barrier film with high pressure water after material and again to dewater, eardrum pressure is 1.5Mpa, the filter cake moisture content 12% after dehydration; The micronutrient levels that records in filter cake is: Cl
-0.06%, Ca
2+0.005%, K
+0.003%, Na
+0.002%, SO
4 2-0.005%;
To adopt rotary kiln to carry out pre-burning after the fragmentation of gained filter cake under 850 ℃, the pre-burning time, 0.5h got Preburning material, when chlorion during higher than 200ppm, after being shaped, the finished product material powder can cause product seriously to be bonded together in sintering process, deformation of products is scrapped, and the chloride ion content that the present embodiment records Preburning material is 60ppm; Preburning material is carried out coarse reduction get the meal particle, get 400Kg meal particle, add CaCO
3: 20g, Mo
2O
3: 280g, Bi
2O
3: 80g, SiO
2: 5g, add deionized water 200kg, dispersion agent 2kg, defoamer 100g, then be broken to D50:1.0 μ m, D90:1.5 μ m through the horizontal sand mill fine powder;
Add the PVA of the model 1799 of 45kg Kingsoft petrochemical iy produced, carry out mist projection granulating, drying and cooling, gained material powder water ratio is 0.02%～0.025%.
The above-mentioned material powder that makes is pressed into external diameter 30*1.18, internal diameter 19*1.18, the annular sample of height 8*1.18, sintering under 1390 ℃ of standard equilibrium oxygen partial pres-sures, the sinter that obtains is tested its power loss and saturation magnetic flux density with SY8258, HP8242 tests its initial permeability, and test result is as shown in table 1:
Table 1
Embodiment 2:
Press Fe
2O
3: ZnO: Mn
3O
4Be the molar ratio ingredient of 52.1: 21.8: 26.1, the initial D50 particle diameter of raw material is: Fe
2O
3: 1.4 μ m; ZnO:1.0 μ m; Mn
3O
4: 1.2 μ m;
With above-mentioned three kinds of starting material altogether 1000kg join high speed dispersor and mix tentatively with 400kg deionized water, 10kg dispersion agent triammonium citrate and disperse, raw material after dispersion enters into the horizontal sand mill sand milling to be mixed, particle diameter after sand milling is: D50:0.7 μ m, D90:1.2 μ m;
Slip is precipitated 1 day, make the supernatant liquor overflow, mud after precipitation carries out filter-press dehydration with diaphragm filter press, controlling feed pressure during charging is 0.1Mpa, and progressively improve feed pressure to 0.8Mpa, advanced to be filled with barrier film with high pressure water after material and again to dewater, eardrum pressure is 1.5Mpa, the filter cake moisture content 10% after dehydration; Micronutrient levels in filter cake is: Cl
-0.05%, Ca
2+0.003%, K
+0.004%, Na
+0.003%, SO
4 2-0.004%;
To adopt rotary kiln to carry out pre-burning after the fragmentation of gained filter cake under 1000 ℃, pre-burning time 1h gets Preburning material, and the chloride ion content that records Preburning material is 55ppm; Preburning material is carried out coarse reduction get the meal particle, get 400Kg meal particle, add CaCO
3: 30g, Mo
2O
3: 300g, Bi
2O
3: 100g, add deionized water 220kg, dispersion agent 2.5kg, defoamer 100g, then be broken to D50:1.0 μ m, D90:1.5 μ m through the horizontal sand mill fine powder;
Add the PVA of the model 1799 of 45kg Kingsoft petrochemical iy produced, carry out mist projection granulating, drying and cooling, gained material powder water ratio is 0.02%～0.025%.
The above-mentioned material powder that makes is pressed into external diameter 30*1.18, internal diameter 19*1.18, the annular sample of height 8*1.18, sintering under 1375 ℃ of standard equilibrium oxygen partial pres-sures, the sinter that obtains is tested its power loss and saturation magnetic flux density with SY8258, HP8242 tests its initial permeability, and test result is as shown in table 2:
Table 2
Embodiment 3:
Press Fe
2O
3: ZnO: Mn
3O
4Be the molar ratio ingredient of 51.7: 23: 25.3, the initial D50 particle diameter of raw material is: Fe
2O
3: 1.4 μ m; ZnO:1.0 μ m; Mn
3O
4: 1.2 μ m;
With above-mentioned three kinds of starting material altogether 1000kg join high speed dispersor and mix tentatively with 400kg deionized water, 10kg dispersion agent triammonium citrate and disperse, raw material after dispersion enters into the horizontal sand mill sand milling to be mixed, particle diameter D50:0.6 μ m after sand milling, D90:1.2 μ m;
Slip is precipitated 1 day, make the supernatant liquor overflow, mud after precipitation carries out filter-press dehydration with diaphragm filter press, controlling feed pressure during charging is 0.1Mpa, and progressively improve feed pressure to 0.8Mpa, and having advanced to be filled with barrier film with high pressure water after material and again to dewater, eardrum pressure is 1.5Mpa, micronutrient levels in filter cake moisture content 5% after dehydration, filter cake is: Cl
-0.04%, Ca
2+0.003%, K
+0.003%, Na
+0.004%, SO
4 2-0.005%;
To adopt rotary kiln to carry out pre-burning after the fragmentation of gained filter cake under 1100 ℃, pre-burning time 0.5h gets Preburning material, and the chloride ion content that records Preburning material is 50ppm; Preburning material gets the meal particle through coarse reduction, gets 400Kg meal particle, adds CaCO
3: 40g, Mo
2O
3: 320g, Bi
2O
3: 120g, add deionized water 250kg, dispersion agent 2.5kg, defoamer 100g, then be broken to D50:1.0 μ m, D90:1.5 μ m through the horizontal sand mill fine powder;
Add the PVA of the model 1799 of 45kg Kingsoft petrochemical iy produced, carry out mist projection granulating, drying and cooling, get water ratio and be 0.02%～0.025% material powder.
Above-mentioned material powder is pressed into external diameter 30*1.18, internal diameter 19*1.18, the annular sample of height 8*1.18, sintering under 1365 ℃ of standard equilibrium oxygen partial pres-sures, the sinter that obtains is tested its power loss and saturation magnetic flux density with SY8258, HP8242 tests its initial permeability, and test result is as shown in table 3:
Table 3
Above-described embodiment is interpreted as only being used for explanation the present invention and is not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modification falls into claim limited range of the present invention equally.
Claims (11)
1. the preparation method of a high permeability MnZn ferrite powder, comprise the steps:
1) raw material and deionized water, dispersion agent are mixed according to 1: 0.3～1.2: 0～0.1 mass ratio, sand milling is to its particle diameter: D50:0.5～1.2 μ m, and D90:0.8～3 μ m get slip; Described raw material is Fe
2O
3, Mn
3O
4, ZnO is according to the mixed in molar ratio gained of x: y: z, wherein x is that 0.515～0.525, y is 1-x-z, z is 0.21～0.23;
2) precipitation 20～24h, make the supernatant liquor overflow, and it is 5～15% that the press filtration gained is precipitated to water ratio, will carry out pre-burning after the fragmentation of gained filter cake under 600 ℃～1100 ℃, and pre-burning time 0.5～1h gets Preburning material;
3) the gained Preburning material is carried out coarse reduction, get crushed material, add trace mineral supplement, add deionized water, dispersion agent and defoamer, sand milling is to D50:0.7 μ m～1.5 μ m, D90:1 μ m～3 μ m; The mass ratio of crushed material and deionized water, dispersion agent, defoamer is 1: 0.1～0.7: 0～0.1: 0～0.05;
4) add polyvinyl alcohol, with gained slip mist projection granulating, drying is cooled to room temperature, controls water ratio between 0.1%～1%, and controls the water ratio fluctuation ± 0.03%.
2. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 1) the D50 particle diameter of Raw is respectively: Fe
2O
3: 1.2～1.5 μ m; ZnO:0.8～1.2 μ m; Mn
3O
4: 1.0～1.4 μ m.
3. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 1) mass ratio of Raw and deionized water, dispersion agent is 1: 0.4～0.8: 0～0.05.
4. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 2) in will precipitate water ratio and be adjusted to 5～10%.
5. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 2) in calcined temperature be 850 ℃～1000 ℃.
6. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 3) medium sand is milled to D0.8 μ m～1.2 μ m, D90:1.2 μ m～2 μ m.
7. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 3) in the mass ratio of crushed material and deionized water, dispersion agent, defoamer be 1: 0.3～0.4: 0～0.05: 0～0.02.
8. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that step 3) described in trace mineral supplement be SiO
2, CaCO
3, Mo
2O
3And Bi
2O
3In one or more, the mass ratio of each trace mineral supplement and crushed material is SiO
2: 0-0.00125wt%, CaCO
3: 0-0.0125wt%, Mo
2O
3: 0.045wt%-0.0875wt%, Bi
2O
3: 0.02wt%-0.04wt%.
9. the preparation method of high permeability MnZn ferrite powder according to claim 8, is characterized in that, the mass ratio of each trace mineral supplement and crushed material is SiO
2: 0-0.00125wt%, CaCO
3: 0.005-0.0125wt%, Mo
2O
3: 0.045wt%-0.0875wt%, Bi
2O
3: 0.02wt%-0.04wt%.
10. the preparation method of high permeability MnZn ferrite powder according to claim 1, is characterized in that, controls water ratio between 0.1%～1%, and control the water ratio fluctuation ± 0.03%.
11. the preparation method of high permeability MnZn ferrite powder according to claim 10 is characterized in that, controls water ratio between 0.15%～0.3%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601504A (en) * | 2013-11-14 | 2014-02-26 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Powder for preventing manganese-zinc ferrite from adhesion and deformation in sintering process |
| CN104402423A (en) * | 2014-10-23 | 2015-03-11 | 苏州市宝玛数控设备有限公司 | Preparation method of high stability high frequency wide temperature magnetic core material used for numerical control magnetic core pendulum feeder |
| CN105367048A (en) * | 2015-11-12 | 2016-03-02 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material and preparation technology thereof |
| CN108249907A (en) * | 2018-01-25 | 2018-07-06 | 浙江朗基新材料科技有限公司 | A kind of ferrite material preparation method for material |
| CN110957124A (en) * | 2019-12-18 | 2020-04-03 | 横店集团东磁股份有限公司 | Preparation method of casting slurry and casting slurry prepared by same |
| CN112390636A (en) * | 2020-11-16 | 2021-02-23 | 南通三优佳磁业有限公司 | Method for manufacturing manganese-zinc ferrite small magnetic core |
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| CN101962209A (en) * | 2009-07-24 | 2011-02-02 | 上海宝钢磁业有限公司 | Post treatment technique of iron oxide red for high-performance Mn-Zn soft magnetic ferrite |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601504A (en) * | 2013-11-14 | 2014-02-26 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Powder for preventing manganese-zinc ferrite from adhesion and deformation in sintering process |
| CN103601504B (en) * | 2013-11-14 | 2015-03-18 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Powder for preventing manganese-zinc ferrite from adhesion and deformation in sintering process |
| CN104402423A (en) * | 2014-10-23 | 2015-03-11 | 苏州市宝玛数控设备有限公司 | Preparation method of high stability high frequency wide temperature magnetic core material used for numerical control magnetic core pendulum feeder |
| CN105367048A (en) * | 2015-11-12 | 2016-03-02 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material and preparation technology thereof |
| CN105367048B (en) * | 2015-11-12 | 2018-03-20 | 横店集团东磁股份有限公司 | A kind of MnZn ferrite material and its preparation technology |
| CN108249907A (en) * | 2018-01-25 | 2018-07-06 | 浙江朗基新材料科技有限公司 | A kind of ferrite material preparation method for material |
| CN110957124A (en) * | 2019-12-18 | 2020-04-03 | 横店集团东磁股份有限公司 | Preparation method of casting slurry and casting slurry prepared by same |
| CN110957124B (en) * | 2019-12-18 | 2021-05-14 | 横店集团东磁股份有限公司 | Preparation method of casting slurry and casting slurry prepared by same |
| CN112390636A (en) * | 2020-11-16 | 2021-02-23 | 南通三优佳磁业有限公司 | Method for manufacturing manganese-zinc ferrite small magnetic core |
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Application publication date: 20130619 |