CN103613370A - Preparation method for high-temperature and high-BS manganese zinc ferrite material with low power consumption - Google Patents
Preparation method for high-temperature and high-BS manganese zinc ferrite material with low power consumption Download PDFInfo
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- CN103613370A CN103613370A CN201310199772.8A CN201310199772A CN103613370A CN 103613370 A CN103613370 A CN 103613370A CN 201310199772 A CN201310199772 A CN 201310199772A CN 103613370 A CN103613370 A CN 103613370A
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Abstract
The invention discloses a preparation method for a high-temperature and high-BS manganese zinc ferrite material with low power consumption. Burdening of 53.5-55 mol% of FeZO3, 39-39.5 mol% of MnO and 6-6.5 mol% of ZnO at mole ratios is carried out. Modification impurities of 480-520 ppm of CaCO3, 380-420 ppm of NiO and 480-520 ppm of V2O5 are added. In the method, the burdening and production technology for optimization of a magnetic core are studied, and the indexes of saturated magnetic flux, power consumption, frequency characteristics, the Curie temperature, saturated magnetic flux density and the like of the obtained magnetic core are improved greatly.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance manganese-zinc MnZn soft magnetic ferrite.
Background technology
High magnetic conductivity ferrite magnetic, magnetic core are to realize in the electronicss such as program control communication, digital technique, network communication colour TV, being used as the products such as inducer, wave filter, pulse transformer and making its miniaturization, the requisite electronic material of lightweight, China has the history of four more than ten years with traditional conventional ceramic technique development high-permeability material, up to the present, and the performance index of material are as all unsatisfactory in saturation flux amount, power loss, frequency response characteristic, Curie temperature etc.
Summary of the invention
In order to alleviate shortcomings and deficiencies of the prior art, the object of the present invention is to provide the preparation method of the high BS low-consumption Mn-Zn ferrite material of high temperature.
The present invention adopts following technical scheme to achieve these goals:
A preparation method for the high BS low-consumption Mn-Zn ferrite material of high temperature, is characterized in that comprising the following steps:
(1) batching: be 53.5-55mol%Fe2O3 in molar ratio, 39-39.5mol%MnO, 6-6.5mol%ZnO prepares burden, and adds modification impurity: 480-520ppmCaCO3; 380-420ppmNiO; 480-520ppmV2O5;
(2) pre-burning: batching pre-burning under the condition of 800 ℃～1000 ℃ obtains Preburning material for 1～3 hour;
(3) ball milling: Preburning material is put into sand mill, add deionized water, the 0.6～1.0wt% polyvinyl alcohol of the 40-60wt% that is equivalent to prepare burden to carry out sand milling simultaneously, sand milling comprises two stages, first stage rotating speed is 50～100 revs/min, ball milling 20～90 minutes, subordinate phase rotating speed is 30～50 revs/min, and ball milling 30～60 minutes, completes ball milling; Sand milling obtains slurry for 0.5～2 hour, and dries;
(4) compression moulding: the powder of oven dry is added to the polyvinyl alcohol of 12-18wt%, the Zinc Stearate of 0.02-0.04wt%, and granulation, packs mould into, is pressed into blank under 75-85Mpa pressure, and during depanning, the density of blank reaches 3g/cm
3be advisable, then, the rear blank of compacting should be placed in environment dry, that ventilate and naturally dry about 48 hours;
(5) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln, sintering in the balanced atmosphere that is 1%～8% in oxygen level, the first temperature rise rate with 250-300 ℃/h of sintering rises to 1200 ℃ by room temperature, with the temperature rise rate of 50-100 ℃/h, by 1200 ℃, rise to 1350～1420 ℃ again, then 1350～1420 ℃ of heat preservation sinterings 2～8 hours; Then cooling, the first rate of temperature fall with 50-100 ℃/h is cooled to 1000 ℃, then is cooled to room temperature with the rate of temperature fall of 200-250 ℃/h.
The preparation method of the high BS low-consumption Mn-Zn ferrite material of described high temperature, it is characterized in that step (1) batching is: be 54.5mol%FeZO3 in molar ratio, 39.25mol%MnO, 6.25mol%ZnO prepares burden, and adds modification impurity: 500ppmCaCO3; 400ppmNiO; 500ppmV2O5.
The preparation method of the high BS low-consumption Mn-Zn ferrite material of described high temperature, is characterized in that sintering in balanced atmosphere that step (6) oxygen level is 4%.
Applicant studies discovery:
Within the scope of 53.5 one 55.Omol%, along with the increase of Fe2O3 ratio, initial permeability first rises and declines afterwards, saturation induction density and Curie temperature monotone increasing; Within the scope of 5.75 one 6.50mol%, along with the increase of ZnO ratio, initial permeability first rises and declines afterwards, and saturation induction density first rises and declines afterwards.
Suitable main formula is: Fe2O3:MnO:ZnO=54.5mol%:39.25mol%:6.25mol%.In 800 1 920 ℃ of temperature ranges, along with the rising of calcined temperature, powder active reduces gradually, and saturation induction density and sintered density first rise and decline afterwards.Suitable calcined temperature is 890 ℃.
A small amount of CaC03 that adds, contributes to the reduction of ferrite power consumption, and sintered density first rises and reduces afterwards, and saturation induction density first rises and reduces afterwards.Suitable addition is 500ppm, NiO add can acceleration of sintering density raising, ferritic saturation induction density first rises and declines afterwards, the △ B at 100 ℃ of high temperature first rises and declines afterwards.Suitable addition is 400ppm.When adding V2O5, the sintered density of material and saturation induction density are all the rear downward trend that first rises, the loss of material first declines and rises afterwards, when ferritic DC superposition characteristic is 5OOppm with the consistent V2O5 additive of variation of Δ B, and the initial permeability of material.High temperature Bs has maximum value, is respectively 2035,446mT.High temperature power consumption has minimum value, is 385mw/cm3.
Along with the raising of forming pressure, green density improves constantly, but sintered density can't continue raising, the variation tendency that having first raises reduces afterwards.When forming pressure is 80MPa, ferritic saturation induction density obtains maximum value.
Beneficial effect of the present invention:
The present invention optimizes batching and the production technique of magnetic core by research, the indexs such as the saturation flux amount of the magnetic core obtaining, power loss, frequency response characteristic, Curie temperature, saturation magnetic flux density all have greatly improved.
Embodiment
Embodiment 1:
The preparation method of the high BS low-consumption Mn-Zn ferrite material of high temperature, is characterized in that comprising the following steps:
(1) batching: be 54.5mol%FeZO3 in molar ratio, 39.25mol%MnO, 6.25mol%ZnO prepares burden, and adds modification impurity: 500ppmCaCO3; 400ppmNiO; 500ppmV2O5.
(2) pre-burning: batching pre-burning under the condition of 890 ℃ obtains Preburning material for 2 hours;
(3) ball milling: Preburning material is put into sand mill, add deionized water, the 0.6～1.0wt% polyvinyl alcohol of the 50wt% that is equivalent in right amount to prepare burden to carry out sand milling simultaneously, sand milling comprises two stages, first stage rotating speed is 50～100 revs/min, ball milling 20～90 minutes, subordinate phase rotating speed is 30～50 revs/min, and ball milling 30～60 minutes, completes ball milling; Sand milling obtains slurry for 0.5～2 hour, and dries;
(4) compression moulding: the powder of oven dry is added to the polyvinyl alcohol of 16wt%, the Zinc Stearate of 0.03-0.04wt%, and granulation, packs mould into, is pressed into blank under 80Mpa pressure, and during depanning, the density of blank reaches 3g/cm
3be advisable, then, the rear blank of compacting should be placed in environment dry, that ventilate and naturally dry about 48 hours;
(5) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln, sintering in the balanced atmosphere that is 4% in oxygen level, the first temperature rise rate with 250-300 ℃/h of sintering rises to 1200 ℃ by room temperature, with the temperature rise rate of 50-100 ℃/h, by 1200 ℃, rise to 1350～1420 ℃ again, then 1350～1420 ℃ of heat preservation sinterings 2～8 hours; Then cooling, the first rate of temperature fall with 50-100 ℃/h is cooled to 1000 ℃, then is cooled to room temperature with the rate of temperature fall of 200-250 ℃/h.
The performance data of the soft magnetic ferrite making by above-described embodiment:
| Sequence number | Technical indicator title | Technical indicator | Remarks |
| 1 | Initial permeability (25 ± 3 ℃) | 2400±25% | ? |
| 2 | Power loss (100Kc, 200mT) unit: KW/m 3 | 683(25±2℃), 305(100±2℃) | ? |
| 3 | Saturation magnetic flux density mT(100 ℃) | 453 | ? |
| 4 | Curie temperature ℃ | >260 | ? |
| 5 | Apparent density Kg/m3 | 4.95 | ? |
Claims (3)
1. a preparation method for the high BS low-consumption Mn-Zn ferrite material of high temperature, is characterized in that comprising the following steps:
(1) batching: be 53.5-55mol%Fe2O3 in molar ratio, 39-39.5mol%MnO, 6-6.5mol%ZnO prepares burden, and adds modification impurity: 480-520ppmCaCO3; 380-420ppmNiO; 480-520ppmV2O5;
(2) pre-burning: batching pre-burning under the condition of 800 ℃～1000 ℃ obtains Preburning material for 1～3 hour;
(3) ball milling: Preburning material is put into sand mill, add deionized water, the 0.6～1.0wt% polyvinyl alcohol of the 40-60wt% that is equivalent to prepare burden to carry out sand milling simultaneously, sand milling comprises two stages, first stage rotating speed is 50～100 revs/min, ball milling 20～90 minutes, subordinate phase rotating speed is 30～50 revs/min, and ball milling 30～60 minutes, completes ball milling; Sand milling obtains slurry for 0.5～2 hour, and dries;
(4) compression moulding: the powder of oven dry is added to the polyvinyl alcohol of 12-18wt%, the Zinc Stearate of 0.02-0.04wt%, and granulation, packs mould into, is pressed into blank under 75-85Mpa pressure, and during depanning, the density of blank reaches 3g/cm
3be advisable, then, the rear blank of compacting should be placed in environment dry, that ventilate and naturally dry about 48 hours;
(5) double sintering: magnetic core blank is put into nitrogen atmosphere protection pushed bat kiln, sintering in the balanced atmosphere that is 1%～8% in oxygen level, the first temperature rise rate with 250-300 ℃/h of sintering rises to 1200 ℃ by room temperature, with the temperature rise rate of 50-100 ℃/h, by 1200 ℃, rise to 1350～1420 ℃ again, then 1350～1420 ℃ of heat preservation sinterings 2～8 hours; Then cooling, the first rate of temperature fall with 50-100 ℃/h is cooled to 1000 ℃, then is cooled to room temperature with the rate of temperature fall of 200-250 ℃/h.
2. the preparation method of the high BS low-consumption Mn-Zn ferrite material of high temperature according to claim 1, it is characterized in that step (1) batching is: be 54.5mol%FeZO3 in molar ratio, 39.25mol%MnO, 6.25mol%ZnO prepares burden, and adds modification impurity: 500ppmCaCO3; 400ppmNiO; 500ppmV2O5.
3. the preparation method of the high BS low-consumption Mn-Zn ferrite material of high temperature according to claim 1, is characterized in that sintering in balanced atmosphere that step (6) oxygen level is 4%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249908A (en) * | 2018-01-18 | 2018-07-06 | 常熟市三佳磁业有限公司 | Low-power consumption high magnetic permeability and magnetic hysteresis are stretched manganese-zinc ferrite and preparation method thereof |
| CN108911733A (en) * | 2018-07-10 | 2018-11-30 | 横店集团东磁股份有限公司 | A kind of high Bs high frequency MnZn Ferrite Material of low-power consumption and preparation method thereof |
| CN109437877A (en) * | 2018-10-23 | 2019-03-08 | 无锡斯贝尔磁性材料有限公司 | A kind of production technology of high solids content manganese-zinc ferrite slurry |
| CN109704744A (en) * | 2019-01-23 | 2019-05-03 | 深圳顺络电子股份有限公司 | A kind of wireless charging RX end iron ferrite and magnetic sheet and its manufacturing method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102219488A (en) * | 2011-04-16 | 2011-10-19 | 江门安磁电子有限公司 | High-temperature high-Bs low-loss MnZn ferrite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219488A (en) * | 2011-04-16 | 2011-10-19 | 江门安磁电子有限公司 | High-temperature high-Bs low-loss MnZn ferrite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 丁川等: "Mn-Zn铁氧体掺杂与结构-性能的研究进展", 《电子元件与材料》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249908A (en) * | 2018-01-18 | 2018-07-06 | 常熟市三佳磁业有限公司 | Low-power consumption high magnetic permeability and magnetic hysteresis are stretched manganese-zinc ferrite and preparation method thereof |
| CN108911733A (en) * | 2018-07-10 | 2018-11-30 | 横店集团东磁股份有限公司 | A kind of high Bs high frequency MnZn Ferrite Material of low-power consumption and preparation method thereof |
| CN109437877A (en) * | 2018-10-23 | 2019-03-08 | 无锡斯贝尔磁性材料有限公司 | A kind of production technology of high solids content manganese-zinc ferrite slurry |
| CN109704744A (en) * | 2019-01-23 | 2019-05-03 | 深圳顺络电子股份有限公司 | A kind of wireless charging RX end iron ferrite and magnetic sheet and its manufacturing method |
| CN109704744B (en) * | 2019-01-23 | 2021-08-10 | 东莞顺络电子有限公司 | RX end ferrite material and magnetic sheet for wireless charging and manufacturing method thereof |
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Application publication date: 20140305 |