CN103382104B - Rare-earth-doped soft-magnetic ferrite and preparation method thereof - Google Patents
Rare-earth-doped soft-magnetic ferrite and preparation method thereof Download PDFInfo
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- CN103382104B CN103382104B CN201310259016.XA CN201310259016A CN103382104B CN 103382104 B CN103382104 B CN 103382104B CN 201310259016 A CN201310259016 A CN 201310259016A CN 103382104 B CN103382104 B CN 103382104B
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Abstract
The invention provides a rare-earth-doped soft-magnetic ferrite and a preparation method thereof. The invention is characterized in that main components of the rare-earth-doped soft-magnetic ferrite comprise, by mol, 1.2 to 1.3 mol of ZrO2, 54 to 54.5 mol of Fe3O4, 3.5 to 5.5 mol of ZnO, 2 to 2.5 mol of NiO, 0.2 to 0.3 mol of tantalum carbide and 0.4 to 0.5 mol of Na2O, and modification impurities added in the main components comprise, in terms of the weight of the rare-earth-doped soft-magnetic ferrite, 450 to 480 ppm of Bi, 310 to 330 ppm of La2O3, 630 to 680 ppm of CaCO3, 330 to 360 ppm of As, 410 to 480 ppm of Cr, 220 to 250 ppm of Te, 340 to 360 ppm of TeO2, 350 to 380 ppm of iron powder and 450 to 480 ppm of Nb2O5. The rare-earth-doped soft-magnetic ferrite provided by the invention has Curie temperature of more than 250 DEG C, and magnetic permeability of the rare-earth-doped soft-magnetic ferrite is increased by more than 40% compared with magnetic permeability of common ferrite magnetic cores of a same specification.
Description
Technical field
The present invention relates to technical field of magnetic materials, particularly, the present invention relates to a kind of rear-earth-doped soft magnetic ferrite and preparation method thereof.
Background technology
The high ferromagnetic oxide powder of magnetic flux density, magnetic core are to realize in the electronic equipments such as program control communication, digital technology, network communication colour TV, being used as the products such as inductor, filter, pulse transformer and making its miniaturization, the requisite electronic material of lightweight, improve constantly the magnetic flux density in magnetic material, it is the pursuit of being engaged in these professional engineers and technicians and production firm always, and the performance index of material are as all unsatisfactory in loss, frequency characteristic, Curie temperature etc.
Summary of the invention
The object of this invention is to provide a kind of rear-earth-doped soft magnetic ferrite and preparation method thereof.
The technical solution adopted in the present invention is:
A kind of rear-earth-doped soft magnetic ferrite, is characterized in that, principal component counts by molar and comprises: 1.2-1.3mol ZrO
2, 54-54.5mol Fe
2o
3, 5-5.5molZnO, 2-2.5molNiO, 0.2-0.3mol ramet, 0.4-0.5molNa
2o, the modification impurity adding in principal component comprises according to the weighing scale that accounts for described rear-earth-doped soft magnetic ferrite: 450-480ppm Bi, 310-330ppm La
2o
3, 630-680ppm CaCO
3, 330-360ppm As, 410-480ppm Cr, 220-250ppm Te, 340-360ppm TeO
2, 350-380ppm iron powder, 450-480ppm Nb
2o
5;
The preparation method of described rear-earth-doped soft magnetic ferrite, is characterized in that comprising the following steps:
(1) batching: principal component is prepared burden, and add modification impurity;
(2) once sintered: batching is mixed, under nitrogen atmosphere protection, pre-burning 1-2 hour under the condition of 560 DEG C-590 DEG C, then be warming up to pre-burning 2-3 hour under the condition of 930 DEG C-970 DEG C, obtain Preburning material;
(3) ball milling, pressed compact: Preburning material is put into sand mill, add the 0.6-1.0wt% polyvinyl alcohol that is equivalent to prepare burden, 1.0-1.2wt% disperse materials, appropriate amount of deionized water to carry out sand milling 90-120 minute simultaneously, obtain slurry, and dry; The powder of oven dry is added to the polyvinyl alcohol of 1.2-1.8wt%, the stearic acid of 0. 2-0. 4wt%, and granulation, packs mould into, under 75-85Mpa pressure, is pressed into blank, naturally dries;
(4) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln sintering, first rise to 530-570 DEG C with the heating rate of 90-110 DEG C/h, then with the heating rate with 120-130 DEG C/h, rise to 730-770 DEG C, sintering 2-3 hour; Adjusting oxygen content in blanket of nitrogen is 0.4%-0.6%, then rises to 920-950 DEG C with the heating rate of 150-170 DEG C/h, sintering 2-3 hour; Rise to 1350-1430 DEG C with the heating rate of 120-130 DEG C/h again, heat preservation sintering 3-4 hour; Then cooling, adjusting oxygen content in blanket of nitrogen is 0.3%-0.4%, is cooled to 720-740 DEG C with the rate of temperature fall of 150-180 DEG C/h, insulation 2-3 hour, then be cooled to room temperature with the rate of temperature fall of 200-210 DEG C/h;
Disperse materials described in step (3) is made by the raw material of following weight portion: microcrystalline wax 3-4, zinc stearate 2-3, aminopropyl triethoxysilane 0.5-0.8, SnO
20.3-0.5, Nano titanium dioxide 0.3-0.5, iron powder 1.2-1.5, glycerol glycerinate 2.3-2.5;
Preparation method is: by each mixing of materials, grinding distribution evenly.
The Curie temperature of magnetic core of the present invention reaches more than 250, and magnetic permeability reaches more general same specification FERRITE CORE and improves more than 40%.
embodiment
A kind of rear-earth-doped soft magnetic ferrite, is characterized in that, principal component counts by molar and comprises: 1.3mol ZrO
2, 54.5mol Fe
2o
3, 5.5molZnO, 2molNiO, 0.3mol ramet, 0.4-0.5molNa
2o, the modification impurity adding in principal component comprises according to the weighing scale that accounts for described rear-earth-doped soft magnetic ferrite: 480ppm Bi, 330ppm La
2o
3, 680ppm CaCO
3, 360ppm As, 480ppm Cr, 250ppm Te, 360ppm TeO
2, 350ppm iron powder, 480ppm Nb
2o
5;
The preparation method of rear-earth-doped soft magnetic ferrite, comprises the following steps:
(1) batching: principal component is prepared burden, and add modification impurity;
(2) once sintered: batching is mixed, under nitrogen atmosphere protection, pre-burning 1-2 hour under the condition of 560 DEG C-590 DEG C, then be warming up to pre-burning 2-3 hour under the condition of 930 DEG C-970 DEG C, obtain Preburning material;
(3) ball milling, pressed compact: Preburning material is put into sand mill, add the 0.6-1.0wt% polyvinyl alcohol that is equivalent to prepare burden, 1.0-1.2wt% disperse materials, appropriate amount of deionized water to carry out sand milling 90-120 minute simultaneously, obtain slurry, and dry; The powder of oven dry is added to the polyvinyl alcohol of 1.2-1.8wt%, the stearic acid of 0. 2-0. 4wt%, and granulation, packs mould into, under 75-85Mpa pressure, is pressed into blank, naturally dries;
(4) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln sintering, first rise to 530-570 DEG C with the heating rate of 90-110 DEG C/h, then with the heating rate with 120-130 DEG C/h, rise to 730-770 DEG C, sintering 2-3 hour; Adjusting oxygen content in blanket of nitrogen is 0.4%-0.6%, then rises to 920-950 DEG C with the heating rate of 150-170 DEG C/h, sintering 2-3 hour; Rise to 1350-1430 DEG C with the heating rate of 120-130 DEG C/h again, heat preservation sintering 3-4 hour; Then cooling, adjusting oxygen content in blanket of nitrogen is 0.3%-0.4%, is cooled to 720-740 DEG C with the rate of temperature fall of 150-180 DEG C/h, insulation 2-3 hour, then be cooled to room temperature with the rate of temperature fall of 200-210 DEG C/h;
Disperse materials described in step (3) by following weight portion (kilogram) raw material make: microcrystalline wax 4, zinc stearate 3, aminopropyl triethoxysilane 0.8, SnO
20.5, Nano titanium dioxide 0.5, iron powder 1.2-1.5, glycerol glycerinate 2.5;
Preparation method is: by each mixing of materials, grinding distribution evenly.
The performance data of the magnetic ferrite magnetic core making by above-described embodiment:
| Sequence number | Technical indicator title | Technical indicator | Remarks |
| 1 | Initial permeability (25 ± 3 DEG C) | 7800±25% | ? |
| 2 | Power loss (100Kc, 200mT) unit: KW/m 3 | 563(25±2℃), 265(100±2℃) | ? |
| 3 | Saturation flux density mT(100 DEG C) | 460 | ? |
| 4 | Curie temperature DEG C | >250 | ? |
Claims (1)
1. a rear-earth-doped soft magnetic ferrite, is characterized in that, principal component counts by molar and comprises: 1.2-1.3mol ZrO
2, 54-54.5mol Fe
2o
3, 5-5.5molZnO, 2-2.5molNiO, 0.2-0.3mol ramet, 0.4-0.5molNa
2o, the modification impurity adding in principal component comprises according to the weighing scale that accounts for described rear-earth-doped soft magnetic ferrite: 450-480ppm Bi, 310-330ppm La
2o
3, 630-680ppm CaCO
3, 330-360ppm As, 410-480ppm Cr, 220-250ppm Te, 340-360ppm TeO
2, 350-380ppm iron powder, 450-480ppm Nb
2o
5;
Its preparation method comprises the following steps:
(1) batching: principal component is prepared burden, and add modification impurity;
(2) once sintered: batching is mixed, under nitrogen atmosphere protection, pre-burning 1-2 hour under the condition of 560 DEG C-590 DEG C, then be warming up to pre-burning 2-3 hour under the condition of 930 DEG C-970 DEG C, obtain Preburning material;
(3) sand milling, pressed compact: Preburning material is put into sand mill, add the 0.6-1.0wt% polyvinyl alcohol that is equivalent to prepare burden, 1.0-1.2wt% disperse materials, appropriate amount of deionized water to carry out sand milling 90-120 minute simultaneously, obtain slurry, and dry; The powder of oven dry is added to the polyvinyl alcohol of 1.2-1.8wt%, the stearic acid of 0. 2-0. 4wt%, and granulation, packs mould into, under 75-85MPa pressure, is pressed into blank, naturally dries;
(4) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln sintering, first rise to 530-570 DEG C with the heating rate of 90-110 DEG C/h, then with the heating rate of 120-130 DEG C/h, rise to 730-770 DEG C, sintering 2-3 hour; Adjusting oxygen content in blanket of nitrogen is 0.4%-0.6%, then rises to 920-950 DEG C with the heating rate of 150-170 DEG C/h, sintering 2-3 hour; Rise to 1350-1430 DEG C with the heating rate of 120-130 DEG C/h again, heat preservation sintering 3-4 hour; Then cooling, adjusting oxygen content in blanket of nitrogen is 0.3%-0.4%, is cooled to 720-740 DEG C with the rate of temperature fall of 150-180 DEG C/h, insulation 2-3 hour, then be cooled to room temperature with the rate of temperature fall of 200-210 DEG C/h;
Disperse materials described in step (3) is made by the raw material of following weight portion: microcrystalline wax 3-4, zinc stearate 2-3, aminopropyl triethoxysilane 0.5-0.8, SnO
20.3-0.5, Nano titanium dioxide 0.3-0.5, iron powder 1.2-1.5, glycerol glycerinate 2.3-2.5;
Preparation method is: by each mixing of materials, grinding distribution evenly.
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| CN104058735B (en) * | 2014-06-09 | 2015-06-24 | 青岛东方循环能源有限公司 | Iron-zirconium-tungsten complex ferrite and preparation method thereof |
| CN104058737B (en) * | 2014-06-10 | 2015-06-24 | 青岛东方循环能源有限公司 | Preparation method of nickel and tungsten ferrite |
| CN104058739B (en) * | 2014-06-24 | 2015-06-24 | 安徽皖宏电气设备有限公司 | Tantalum-based ferrite magnetic core material used for transformer |
| CN104891976A (en) * | 2015-04-24 | 2015-09-09 | 马鞍山科信咨询有限公司 | Low-loss nickel-zinc ferrite material and preparation method |
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