CN103524124A - Sintering method of high-magnetic-permeability MnZn ferrite material - Google Patents
Sintering method of high-magnetic-permeability MnZn ferrite material Download PDFInfo
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- CN103524124A CN103524124A CN201310419245.3A CN201310419245A CN103524124A CN 103524124 A CN103524124 A CN 103524124A CN 201310419245 A CN201310419245 A CN 201310419245A CN 103524124 A CN103524124 A CN 103524124A
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Abstract
The invention discloses a sintering method of a high-magnetic-permeability MnZn ferrite material, which comprises the following four stages: a. first temperature rise stage; b. second temperature rise stage; c. holding stage; and d. cooling stage. Since the temperature and partial oxygen pressure are controlled in the whole sintering process of temperature rise, holding and cooling, the high-magnetic-permeability MnZn ferrite can be obtained at lower sintering temperature. The sintering method of the high-magnetic-permeability MnZn ferrite has the advantages of low sintering temperature and short sintering period, and greatly lowers the sintering cost of the MnZn ferrite.
Description
Technical field
The present invention relates to a kind of sintering method of MnZn Ferrite Material, relate in particular to a kind of sintering method of MnZn ferrite material with high magnetic conductivity.
Background technology
Be accompanied by the universal of Portable mobile electronic device, the high speed development of multimedia communication, digital network, and the demand in the field such as electromagnetic compatibility and anti-electromagnetic interference, proposed the more requirement of Gao Gengxin to MnZn ferrite material with high magnetic conductivity at present.Along with the miniaturization of electronic devices and components, wish that the ferritic magnetic permeability of high magnetic permeability MnZn is more high better.The ferritic preparation of high magnetic permeability MnZn, except selecting suitable main formula design and suitable indium addition beyond the region of objective existence, the control of sintering process is also very important.
Mainly by selecting, main formula forms, additive designs and combination improves the ferritic magnetic permeability of MnZn for Chinese patent application CN200710071536.2, CN200810037005.6, CN200810123262.1, CN200910133726.1, CN200910194706.5, CN201010150330.0 etc., but sintering process is not studied in great detail, and the inventor finds, the control of sintering process is extremely important to improving magnetic permeability.
Summary of the invention
The present invention is directed to prior art and preparing the existing problem of MnZn ferrite material with high magnetic conductivity, a kind of sintering method of MnZn ferrite material with high magnetic conductivity is provided, the MnZn ferrite obtaining after the method sintering, its magnetic permeability obtains raising by a relatively large margin.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:
The sintering method that a kind of MnZn ferrite material with high magnetic conductivity is provided, consists of following steps:
A, first temperature rise period: from room temperature, rise to 500 ℃ ~ 700 ℃, temperature rise rate is 0.5 ~ 1.0 ℃/min, in air atmosphere, carries out;
B, second temperature rise period: be warmed up to 1300 ~ 1450 ℃ from 500 ℃ ~ 700 ℃, temperature rise rate is 3.0 ~ 10.0 ℃/min, and oxygen partial pressure maintains below 2%;
C, holding stage: temperature is maintained to 1300 ~ 1450 ℃, and soaking time is 1 ~ 12 hour, and oxygen partial pressure maintains 5 ~ 100%;
D, temperature-fall period: temperature is dropped to room temperature from 1300 ~ 1450 ℃, and rate of temperature fall is 0.5 ~ 4.0 ℃/min, maintains equilibrium oxygen partial pres-sure.
In a preferred embodiment of the present invention, in step a, described first temperature rise period is elevated to 700 ℃ by temperature from room temperature under the temperature rise rate of 0.5 ~ 0.8 ℃/min.
In a preferred embodiment of the present invention, in step b, described second temperature rise period is elevated to 1300 ~ 1450 ℃ by temperature from 700 ℃ under the temperature rise rate of 3.0 ~ 10.0 ℃/min,, oxygen partial pressure maintains below 1%.
In a preferred embodiment of the present invention, in step c, described holding stage maintains 1350 ~ 1400 ℃ by temperature, and soaking time is 7 ~ 12 hours, and oxygen partial pressure maintains 21 ~ 100%.
In a preferred embodiment of the present invention, in steps d, described temperature-fall period drops to room temperature by temperature from 1350 ~ 1400 ℃ in the rate of temperature fall of 1.0 ~ 3.0 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
Can be applicable to MnZn ferrite material with high magnetic conductivity of the present invention comprises mainly by Fe
2o
3, the high magnetic conductivity ferrite that forms of MnO, ZnO.These ferrites also can contain SiO
2, CaO, V
2o
5, Bi
2o
3, MoO
3, TiO
2, SnO
2, Co
2o
3, Nb
2o
5, ZrO
2, Ta
2o
5deng other trace mineral supplement composition, to improve its characteristic.
The invention has the beneficial effects as follows:
1, the sintering method of a kind of MnZn ferrite material with high magnetic conductivity of the present invention, owing to having controlled temperature and oxygen partial pressure in the whole sintering process heating up, be incubated and lowering the temperature, can improve the ferritic magnetic permeability of MnZn greatly.
2, application the present invention prepares high magnetic permeability MnZn ferrite, and sintering temperature can reduce by 20 ~ 50 ℃, greatly reduces sintering cost, extends kiln work-ing life.
Embodiment
Be below the specific embodiment of the present invention, technical characterictic of the present invention is described further, but the present invention is not limited to these embodiment.
Embodiment 1
By the Fe by 52mol%
2o
3, the ZnO of 23mol%, the starting material that the MnO of 25mol% forms mix 1 hour in sand mill, then pre-burning 2 hours at 850 ℃.In the powder of take after pre-burning, quality is benchmark, in above-mentioned Preburning material, adds ancillary component, and the ancillary component of interpolation (wt%) is: the CaCO of 0.01wt%
3, the Bi of 0.04wt%
2o
3, the MoO of 0.04wt%
3.Then carry out secondary sand milling 2 hours, carry out mist projection granulating after adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In sintering process, first temperature rise period, this stage is elevated to 700 ℃ from room temperature, and temperature rise rate is 0.8 ℃/min, heats up and carries out in air atmosphere; Second temperature rise period, this stage is elevated to 1370 ℃ from 700 ℃, and temperature rise rate is 5 ℃/min, and the oxygen partial pressure of temperature rise period maintains 0.7%; At 1370 ℃, be incubated 8 hours, oxygen partial pressure maintains 100%; Finally drop to room temperature from 1370 ℃, rate of temperature fall is 2 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result is 16418.
Comparative example 1
Identical with embodiment 1, oxygen partial pressure when just handle is elevated to 1370 ℃ from 700 ℃ changes 21% into.With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result only has 11539.
Embodiment 2
By the Fe by 52.5mol%
2o
3, the ZnO of 23.5mol%, the starting material that the MnO of 24mol% forms mix 1 hour in sand mill, then pre-burning 2 hours at 750 ℃.In the powder of take after pre-burning, quality is benchmark, in above-mentioned Preburning material, adds ancillary component, and the ancillary component of interpolation (wt%) is: the CaCO of 0.02wt%
3, the Bi of 0.03wt%
2o
3, the MoO of 0.03wt%
3.Then carry out secondary sand milling 2 hours, carry out mist projection granulating after adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In sintering process, first temperature rise period, this stage is elevated to 700 ℃ from room temperature, and temperature rise rate is 0.8 ℃/min, heats up and carries out in air atmosphere; Second temperature rise period, this stage is elevated to 1360 ℃ from 700 ℃, and temperature rise rate is 6 ℃/min, and the oxygen partial pressure of temperature rise period maintains 0.5%; At 1360 ℃, be incubated 10 hours, oxygen partial pressure maintains 21%; Finally drop to room temperature from 1360 ℃, rate of temperature fall is 3 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result is 15369.
Comparative example 2
Identical with embodiment 2, temperature rise rate when just handle is elevated to 1360 ℃ from 700 ℃ changes 1 ℃/min into.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result only has 10287.
Embodiment 3
By the Fe by 52.2mol%
2o
3, the ZnO of 23.8mol%, the starting material that the MnO of 24mol% forms mix 1 hour in sand mill, then pre-burning 2 hours at 800 ℃.In the powder of take after pre-burning, quality is benchmark, in above-mentioned Preburning material, adds ancillary component, and the ancillary component of interpolation (wt%) is: the CaCO of 0.01wt%
3, the Bi of 0.05wt%
2o
3, the MoO of 0.05wt%
3.。Then carry out secondary sand milling 2 hours, carry out mist projection granulating after adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In sintering process, first temperature rise period, this stage is elevated to 700 ℃ from room temperature, and temperature rise rate is 0.8 ℃/min, heats up and carries out in air atmosphere; Second temperature rise period, this stage is elevated to 1360 ℃ from 700 ℃, and temperature rise rate is 6 ℃/min, and the oxygen partial pressure of temperature rise period maintains 0.5%; At 1360 ℃, be incubated 10 hours, oxygen partial pressure maintains 21%; Finally drop to room temperature from 1360 ℃, rate of temperature fall is 3 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result is 15908.
Comparative example 3
Identical with embodiment 1, just the oxygen partial pressure of 1360 ℃ of holding-zones is changed into 5%.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result only has 10891.
Embodiment 4
By the Fe by 51.5mol%
2o
3, the ZnO of 23mol%, the starting material that the MnO of 25.5mol% forms mix 1 hour in sand mill, then pre-burning 2 hours at 800 ℃.In the powder of take after pre-burning, quality is benchmark, in above-mentioned Preburning material, adds ancillary component, and the ancillary component of interpolation (wt%) is: the CaCO3 of 0.01wt%, the Bi of 0.05wt%
2o
3, the MoO of 0.05wt%
3.。Then carry out secondary sand milling 2 hours, carry out mist projection granulating after adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In sintering process, first temperature rise period, this stage is elevated to 700 ℃ from room temperature, and temperature rise rate is 0.8 ℃/min, heats up and carries out in air atmosphere; Second temperature rise period, this stage is elevated to 1380 ℃ from 700 ℃, and temperature rise rate is 5 ℃/min, and the oxygen partial pressure of temperature rise period maintains 0.6%; At 1380 ℃, be incubated 8 hours, oxygen partial pressure maintains 100%; Finally drop to room temperature from 1380 ℃, rate of temperature fall is 2 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result is 16533.
Comparative example 4
Identical with embodiment 4, just changing 5 ℃/min into from 1380 ℃ of rate of temperature fall to temperature descending section.
With the initial permeability of TH2816A type LCR test set specimen at 10kHz/0.25V, 25 ℃, result only has 9874.
Specific embodiment described in the present invention is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various modifications or supplement or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made a detailed description and has quoted as proof some specific exampless, to those skilled in the art, only otherwise it is obvious leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (7)
1. a sintering method for MnZn ferrite material with high magnetic conductivity, is characterized in that, comprises the following steps:
A, first temperature rise period: from room temperature, rise to 500 ℃ ~ 700 ℃, temperature rise rate is 0.5 ~ 1.0 ℃/min, in air atmosphere, carries out;
B, second temperature rise period: be warmed up to 1300 ~ 1450 ℃ from 500 ℃ ~ 700 ℃, temperature rise rate is 3.0 ~ 10.0 ℃/min, and oxygen partial pressure maintains below 2%;
C, holding stage: temperature is maintained to 1300 ~ 1450 ℃, and soaking time is 1 ~ 12 hour, and oxygen partial pressure maintains 5 ~ 100%;
D, temperature-fall period: temperature is dropped to room temperature from 1300 ~ 1450 ℃, and rate of temperature fall is 0.5 ~ 4.0 ℃/min, maintains equilibrium oxygen partial pres-sure.
2. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 1, is characterized in that, in step a, described first temperature rise period is elevated to 700 ℃ by temperature from room temperature under the temperature rise rate of 0.5 ~ 0.8 ℃/min.
3. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 1, it is characterized in that, in step b, described second temperature rise period is elevated to 1300 ~ 1450 ℃ by temperature from 700 ℃ under the temperature rise rate of 3.0 ~ 10.0 ℃/min, and oxygen partial pressure maintains below 1%.
4. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 1, is characterized in that, in step c, described holding stage maintains 1350 ~ 1400 ℃ by temperature, and soaking time is 7 ~ 12 hours, and oxygen partial pressure maintains 21 ~ 100%.
5. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 1, it is characterized in that, in steps d, described temperature-fall period drops to room temperature by temperature from 1350 ~ 1400 ℃ in the rate of temperature fall of 1.0 ~ 3.0 ℃/min, and temperature-fall period maintains equilibrium oxygen partial pres-sure.
6. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 1, is characterized in that, the main raw of described MnZn ferrite material with high magnetic conductivity comprises Fe
2o
3, MnO and ZnO.
7. the sintering method of MnZn ferrite material with high magnetic conductivity according to claim 6, is characterized in that, described MnZn ferrite material with high magnetic conductivity also comprises SiO
2, CaO, V
2o
5, Bi
2o
3, MoO
3, TiO
2, SnO
2, Co
2o
3, Nb
2o
5, ZrO
2, Ta
2o
5in one or more trace mineral supplement compositions.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104051111A (en) * | 2014-06-24 | 2014-09-17 | 铜陵三佳变压器有限责任公司 | Zirconium-based ferrite core material used for transformer |
| CN104064310A (en) * | 2014-06-24 | 2014-09-24 | 安徽皖宏电气设备有限公司 | Copper-based ferrite magnetic core material for transformer |
| CN104072120A (en) * | 2014-06-12 | 2014-10-01 | 天长市中德电子有限公司 | High-magnetic-strength manganese zinc ferrite material |
| CN104124030A (en) * | 2014-06-25 | 2014-10-29 | 蚌埠市英路光电有限公司 | Cobalt-based rare earth ferromagnetic core material |
| CN107176830A (en) * | 2017-04-01 | 2017-09-19 | 浙江工业大学 | A kind of preparation method of high permeability MnZn ferrite |
| CN107200572A (en) * | 2017-05-08 | 2017-09-26 | 中国计量大学 | A kind of ferrite sintered methods of low magnetic permeability temperature coefficient MnZn |
| CN107316728A (en) * | 2017-05-08 | 2017-11-03 | 泰州茂翔电子器材有限公司 | A kind of MH10kW magnetic materials with good low temperature characteristic |
| CN110183221A (en) * | 2019-05-05 | 2019-08-30 | 南京中电熊猫磁电科技有限公司 | The preparation method of the Mn-Zn soft magnetic ferrite of ultra low temperature magnetic conductivity stability |
| CN110386813A (en) * | 2019-07-21 | 2019-10-29 | 昆山凌泽电子有限公司 | A kind of manganese-zinc ferrite magnetic sheet and preparation method thereof |
| CN112094115A (en) * | 2020-09-21 | 2020-12-18 | 临沂春光磁业有限公司 | Manganese-zinc ferrite material with ultrahigh magnetic conductivity and preparation method thereof |
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| CN101259999B (en) * | 2008-03-31 | 2011-05-04 | 横店集团东磁股份有限公司 | High magnetic conductivity soft-magnetic ferrite material and manufacturing method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072120A (en) * | 2014-06-12 | 2014-10-01 | 天长市中德电子有限公司 | High-magnetic-strength manganese zinc ferrite material |
| CN104051111A (en) * | 2014-06-24 | 2014-09-17 | 铜陵三佳变压器有限责任公司 | Zirconium-based ferrite core material used for transformer |
| CN104064310A (en) * | 2014-06-24 | 2014-09-24 | 安徽皖宏电气设备有限公司 | Copper-based ferrite magnetic core material for transformer |
| CN104124030A (en) * | 2014-06-25 | 2014-10-29 | 蚌埠市英路光电有限公司 | Cobalt-based rare earth ferromagnetic core material |
| CN107176830A (en) * | 2017-04-01 | 2017-09-19 | 浙江工业大学 | A kind of preparation method of high permeability MnZn ferrite |
| CN107200572A (en) * | 2017-05-08 | 2017-09-26 | 中国计量大学 | A kind of ferrite sintered methods of low magnetic permeability temperature coefficient MnZn |
| CN107316728A (en) * | 2017-05-08 | 2017-11-03 | 泰州茂翔电子器材有限公司 | A kind of MH10kW magnetic materials with good low temperature characteristic |
| CN110183221A (en) * | 2019-05-05 | 2019-08-30 | 南京中电熊猫磁电科技有限公司 | The preparation method of the Mn-Zn soft magnetic ferrite of ultra low temperature magnetic conductivity stability |
| CN110183221B (en) * | 2019-05-05 | 2021-11-30 | 南京中电熊猫磁电科技有限公司 | Preparation method of manganese-zinc soft magnetic ferrite material with ultralow temperature magnetic conductivity stability |
| CN110386813A (en) * | 2019-07-21 | 2019-10-29 | 昆山凌泽电子有限公司 | A kind of manganese-zinc ferrite magnetic sheet and preparation method thereof |
| CN112094115A (en) * | 2020-09-21 | 2020-12-18 | 临沂春光磁业有限公司 | Manganese-zinc ferrite material with ultrahigh magnetic conductivity and preparation method thereof |
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Application publication date: 20140122 |