CN100466114C - Sintering method of high saturation magnetic flux density MnZn ferrite - Google Patents
Sintering method of high saturation magnetic flux density MnZn ferrite Download PDFInfo
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- CN100466114C CN100466114C CNB2006100519428A CN200610051942A CN100466114C CN 100466114 C CN100466114 C CN 100466114C CN B2006100519428 A CNB2006100519428 A CN B2006100519428A CN 200610051942 A CN200610051942 A CN 200610051942A CN 100466114 C CN100466114 C CN 100466114C
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- 238000005245 sintering Methods 0.000 title claims abstract description 36
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000004907 flux Effects 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 37
- 239000001301 oxygen Substances 0.000 claims abstract description 37
- 229920006395 saturated elastomer Polymers 0.000 claims description 14
- 208000036366 Sensation of pressure Diseases 0.000 claims description 10
- 238000012423 maintenance Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000004576 sand Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000003595 mist Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000005338 frosted glass Substances 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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Abstract
The invention provides a sintering method of high saturation magnetic flux density MnZn ferrite; the method comprises the following steps: a. a first temperature rising stage: b. a second temperature rise stage, a heat preservation stage and a temperature reduction stage; the sintering method can greatly improve the saturation magnetic flux density of the MnZn ferrite by controlling the temperature and the oxygen partial pressure in the whole sintering process of heating, heat preservation and cooling; the high saturation magnetic flux density MnZn ferrite prepared by the sintering method of the invention does not need to add expensive auxiliary components, and the sintering process is simple, thereby greatly reducing the cost of the MnZn ferrite.
Description
Technical field
The present invention relates to the ferritic sintering method of a kind of MnZn, relate in particular to the sintering method of high saturated flux density MnZn ferrite.
Background technology
The MnZn ferrite can be used as soft magnetic material and is widely used in communication apparatus such as power transformer, choke and the household electrical appliance industry.When being used in 100kHz to power transformer magnetic core that hundreds of kHz frequency range is used, compare with metal soft magnetic material with other Ferrite Material, the ferritic power consumption of MnZn is little, and saturation flux density is bigger, so the MnZn ferrite is the important materials as the transformer magnetic core.
But along with the miniaturization of electronic equipment and power supply high-output powerization with in order also normally to use under hot conditions, the saturation flux density of common MnZn Ferrite Material (Bs), particularly high temperature Bs just seem not enough; So increasing people develops and develops the MnZn ferrite of high saturation magnetic flux density (Bs).
Chinese patent application (CN1294099A) discloses a kind of Ferrite Material, it has improved the ferritic Bs of MnZn by add NiO in material, but because the price comparison height of NiO has improved the manufacturing cost of MnZn Ferrite Material greatly, thereby has reduced competition capability.
And for example Chinese patent application (CN1224224A) discloses a kind of Ferrite Material, by Fe
2O
3, MnO, ZnO raw material form and be limited to certain limit, by formed body at the N that controls partial pressure of oxygen
2-O
2Under the atmosphere of mist, sintering was prepared the MnZn ferrite of a kind of high Bs in 5 hours under 1300 ℃ sintering temperature, the occurrence of the partial pressure of oxygen when but this patent application is not announced sintering, but partial pressure of oxygen plays a key effect to the MnZn ferrite of sintering high saturation magnetic flux density, so the content that those of ordinary skill in the art puts down in writing according to this patent application can't obtain high saturated flux density MnZn ferrite.
Summary of the invention
The present invention is directed to prior art in the existing problem of preparation high saturated flux density MnZn ferrite, a kind of sintering method of high saturated flux density MnZn ferrite is provided, through MnZn ferrite behind this method sintering, its saturation flux density Bs obtains raising by a relatively large margin.
The objective of the invention is to be implemented by the following technical programs; A kind of sintering method of high saturated flux density MnZn ferrite, this method is made of following steps:
A, first temperature rise period: this stage is elevated to 600 ℃～800 ℃ with temperature from room temperature in 1 hour to 6 hours time, the temperature rise period carries out in air atmosphere;
B, second temperature rise period, this stage is elevated to 1100～1450 ℃ with temperature from 600 ℃～800 ℃ in 3 hours to 8 hours time, and the partial pressure of oxygen of temperature rise period maintains 0.001～2%;
C, holding stage, this stage, at 1100～1450 ℃, temperature retention time was 30 minutes to 10 hours with temperature maintenance, partial pressure of oxygen maintains 2～10%;
D, temperature-fall period, this stage drops to 100 ℃ with temperature from 1100～1450 ℃ in 6 hours to 20 hours time, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
As preferably, first temperature rise period is elevated to 800 ℃ with temperature from room temperature in 1 hour to 6 hours time in step a.
As preferably, second temperature rise period is elevated to 1100～1450 ℃ with temperature from 800 ℃ in 3 hours to 8 hours time in step b, and the partial pressure of oxygen of temperature rise period maintains 0.005～1%.
As preferably, at 1150～1400 ℃, temperature retention time is 2 hours to 8 hours to holding stage with temperature maintenance in step c.
As preferably, temperature-fall period drops to 100 ℃ with temperature from 1150～1400 ℃ in 8 hours to 15 hours time in steps d, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
The MnZn ferrite that can use sintering method of the present invention comprises that those are mainly by Fe
2O
3, the ferrite formed of MnO, ZnO.These ferrites also can contain the other composition, as NiO, Li
2O, MgO and CuO are to improve its characteristic.They can also 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
5And other micro constitutent.
Therefore the present invention compared with prior art has the following advantages:
1, sintering method of the present invention can improve the ferritic saturation flux density of MnZn greatly owing to controlled temperature and partial pressure of oxygen in the whole sintering process that heats up, is incubated and lower the temperature.
2, use sintering method of the present invention and prepare the auxiliary element that high saturated flux density MnZn ferrite need not to add costliness, and sintering process is simple, greatly reduces the ferritic cost of MnZn.
Embodiment
Below be 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
Will be by the Fe of 53mol%
2O
3, the ZnO of 11mol%, the raw material that the MnO of 36mol% forms mixed in sand mill 1 hour, then 800 ℃ of following pre-burnings 2 hours.Add auxiliary element in above-mentioned pre-imitation frosted glass, the auxiliary element of interpolation (wt%) is: the CaCO of 0.1wt%
3, the Nb of 0.03wt%
2O
5, the ZrO of 0.03wt%
2, the SnO of 0.1wt%
2Carried out the secondary sand milling then 2 hours, and carried out mist projection granulating behind the adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In the sintering process, first temperature rise period, this stage is elevated to 600 ℃ from room temperature, and the heating-up time is 4 hours, heats up to carry out in air atmosphere; Second temperature rise period, this stage is elevated to 1300 ℃ from 600 ℃, and the heating-up time is 6 hours, and the partial pressure of oxygen of temperature rise period maintains 0.5%; Be incubated 5 hours down at 1300 ℃, partial pressure of oxygen maintains 6%; Drop to 100 ℃ from 1300 ℃ at last, temperature fall time is 10 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result is 423mT.
Comparative example 1
Identical with embodiment 1, just the partial pressure of oxygen when 600 ℃ are elevated to 1300 ℃ is changed into 3%.With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result has only 412mT.
Embodiment 2
Will be by the Fe of 53.8mol%
2O
3, the ZnO of 7mol%, the raw material that the MnO of 39.2mol% forms mixed in sand mill 1 hour, then 850 ℃ of following pre-burnings 2 hours.Add auxiliary element in above-mentioned pre-imitation frosted glass, the auxiliary element of interpolation (wt%) is: the CaCO of 0.12wt%
3, the Nb of 0.02wt%
2O
5, the ZrO of 0.04wt%
2Carried out the secondary sand milling then 2 hours, and carried out mist projection granulating behind the adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In the sintering process, first temperature rise period, this stage is elevated to 800 ℃ from room temperature, and the heating-up time is 5 hours, heats up to carry out in air atmosphere; Second temperature rise period, this stage is elevated to 1320 ℃ from 800 ℃, and the heating-up time is 5 hours, and the partial pressure of oxygen of temperature rise period maintains 0.1%; Be incubated 3 hours down at 1320 ℃, partial pressure of oxygen maintains 8%; Drop to 100 ℃ from 1320 ℃ at last, temperature fall time is 11 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result is 452mT.
Comparative example 2
Identical with embodiment 2, just the partial pressure of oxygen when 800 ℃ are elevated to 1320 ℃ is changed into 4%.With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result has only 435mT.
Embodiment 3
Will be by the Fe of 53.2mol%
2O
3, the ZnO of 9mol%, the raw material that the MnO of 37.8mol% forms mixed in sand mill 1 hour, then 900 ℃ of following pre-burnings 2 hours.Add auxiliary element in above-mentioned pre-imitation frosted glass, the auxiliary element of interpolation (wt%) is: the CaCO of 0.13wt%
3, the Nb of 0.015wt%
2O
5, the ZrO of 0.05wt%
2Carried out the secondary sand milling then 2 hours, and carried out mist projection granulating behind the adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In the sintering process, first temperature rise period, this stage is elevated to 600 ℃ from room temperature, and the heating-up time is 1 hour, heats up to carry out in air atmosphere; Second temperature rise period, this stage is elevated to 1150 ℃ from 600 ℃, and the heating-up time is 3 hours, and the partial pressure of oxygen of temperature rise period maintains 2%; Be incubated 8 hours down at 1150 ℃, partial pressure of oxygen maintains 10%; Drop to 100 ℃ from 1150 ℃ at last, temperature fall time is 6 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result is 428mT.
Comparative example 3
Identical with embodiment 1, just the partial pressure of oxygen when 600 ℃ are elevated to 1150 ℃ is changed into 4%.With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result has only 407mT.
Embodiment 4
Will be by the Fe of 52.7mol%
2O
3, the ZnO of 13.2mol%, the raw material that the MnO of 34.1mol% forms mixed in sand mill 1 hour, then 850 ℃ of following pre-burnings 2 hours.Add auxiliary element in above-mentioned pre-imitation frosted glass, the auxiliary element of interpolation (wt%) is: the CaCO of 0.08wt%
3, the Nb of 0.018wt%
2O
5, the ZrO of 0.03wt%
2, the SnO of 0.012wt%
2Carried out the secondary sand milling then 2 hours, and carried out mist projection granulating behind the adding PVA, the standard toroidal core that is shaped to Φ 25 is carried out sintering.In the sintering process, first temperature rise period, this stage is elevated to 800 ℃ from room temperature, and the heating-up time is 6 hours, heats up to carry out in air atmosphere; Second temperature rise period, this stage is elevated to 1450 ℃ from 800 ℃, and the heating-up time is 8 hours, and the partial pressure of oxygen of temperature rise period maintains 0.001%; Be incubated 30 minutes down at 1450 ℃, partial pressure of oxygen maintains 2%; Drop to 100 ℃ from 1450 ℃ at last, temperature fall time is 20 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result is 438mT.
Comparative example 4
Identical with embodiment 2, just the partial pressure of oxygen when 800 ℃ are elevated to 1450 ℃ is changed into 3%.With the Bs of SY-8258 type B-H tester in 50Hz, 1194/m, 100 ℃ of following specimen, the result has only 418mT.
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.The technical staff of the technical field of the invention can make various modifications or replenishes 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 detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (7)
1, a kind of sintering method of high saturated flux density MnZn ferrite, this method is made of following steps:
A, first temperature rise period: this stage is elevated to 600 ℃～800 ℃ with temperature from room temperature in 1 hour to 6 hours time, the temperature rise period carries out in air atmosphere;
B, second temperature rise period, this stage is elevated to 1100～1450 ℃ with temperature from 600 ℃～800 ℃ in 3 hours to 8 hours time, and the partial pressure of oxygen of temperature rise period maintains 0.001～2%;
C, holding stage, this stage, at 1100～1450 ℃, temperature retention time was 30 minutes to 10 hours with temperature maintenance, partial pressure of oxygen maintains 2～10%;
D, temperature-fall period, this stage drops to 100 ℃ with temperature from 1100～1450 ℃ in 6 hours to 20 hours time, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
2, the sintering method of high saturated flux density MnZn ferrite according to claim 1 is characterized in that first temperature rise period is elevated to 800 ℃ with temperature from room temperature among the step a in 1 hour to 6 hours time.
3, the sintering method of high saturated flux density MnZn ferrite according to claim 2, it is characterized in that among the step b that second temperature rise period be elevated to 1100～1450 ℃ with temperature from 800 ℃ in 3 hours to 8 hours time, the partial pressure of oxygen of temperature rise period maintains 0.005～1%.
4, according to the sintering method of claim 1 or 2 or 3 described high saturated flux density MnZn ferrites, it is characterized in that among the step c holding stage with temperature maintenance at 1150～1400 ℃, temperature retention time is 2 hours to 8 hours.
5, the sintering method of high saturated flux density MnZn ferrite according to claim 4 is characterized in that in the steps d that temperature-fall period drops to 100 ℃ with temperature from 1150～1400 ℃ in 8 hours to 15 hours time, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
6, the sintering method of high saturated flux density MnZn ferrite according to claim 1 is characterized in that:
A, first temperature rise period: this stage is elevated to 800 ℃ with temperature from room temperature, and the heating-up time is 5 hours, heats up to carry out in air atmosphere;
B, second temperature rise period: this stage is elevated to 1320 ℃ from 800 ℃, and the heating-up time is 5 hours, and the temperature rise period partial pressure of oxygen maintains 0.1%;
C, holding stage: this stage, at 1320 ℃, temperature retention time was 3 hours with temperature maintenance, and partial pressure of oxygen maintains 8%;
D, temperature-fall period: this stage drops to 100 ℃ from 1320 ℃, and temperature fall time is 11 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
7, the sintering method of high saturated flux density MnZn ferrite according to claim 1 is characterized in that:
A, first temperature rise period: this stage is elevated to 800 ℃ with temperature from room temperature, and the heating-up time is 6 hours, heats up to carry out in air atmosphere;
B, second temperature rise period: this stage is elevated to 1450 ℃ from 800 ℃, and the heating-up time is 8 hours, and the temperature rise period partial pressure of oxygen maintains 0.001%;
C, holding stage: this stage, at 1450 ℃, temperature retention time was 30 minutes with temperature maintenance, and partial pressure of oxygen maintains 2%;
D, temperature-fall period: this stage drops to 100 ℃ with temperature from 1450 ℃, and temperature fall time is 20 hours, and temperature-fall period is kept equilibrium oxygen partial pres-sure.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101483092B (en) * | 2008-01-16 | 2011-08-24 | 横店集团东磁股份有限公司 | Producing method of high saturation magnetic flux density low loss soft magnetic ferrite material |
| CN101429017B (en) * | 2008-12-06 | 2011-12-28 | 广东风华高新科技股份有限公司 | Ferrite magnetic core for network communication and method for producing the same |
| CN102010192B (en) * | 2010-10-29 | 2013-01-23 | 宜宾金川电子有限责任公司 | Mangan zinc ferrite resintering process |
| CN102531560A (en) * | 2011-12-30 | 2012-07-04 | 南通鼎源电子磁材有限公司 | Magnetism, copper and zinc-iron soft magnetic ferrite material and preparation method thereof |
| CN103172358B (en) * | 2013-03-21 | 2014-10-15 | 电子科技大学 | High BsHigh TcMnZn ferrite material and preparation method thereof |
| 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 |
| CN109896848A (en) * | 2019-04-22 | 2019-06-18 | 南通冠优达磁业有限公司 | A kind of preparation method of low-consumption Mn-Zn ferrite |
| CN113470963B (en) * | 2021-08-16 | 2022-04-29 | 四川大学 | Method for preparing MnZn ferrite U-shaped magnetic core |
| CN114085086A (en) * | 2021-11-02 | 2022-02-25 | 宝钢磁业（江苏）有限公司 | Sintering process of iron-rich ultrahigh Bs material |
| CN116283262B (en) * | 2023-01-28 | 2024-09-13 | 山东春光磁电科技有限公司 | High-temperature-resistant high-permeability high-impedance MnZn ferrite material and preparation method and application thereof |
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| CN1061395A (en) * | 1990-11-15 | 1992-05-27 | 川崎制铁株式会社 | Produce the method for Mn-Zn ferrite |
| CN1623953A (en) * | 2003-12-01 | 2005-06-08 | 浙江天通电子股份有限公司 | Manganese zinc ferrite soft magnetic sinitering method |
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2006
- 2006-06-14 CN CNB2006100519428A patent/CN100466114C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061395A (en) * | 1990-11-15 | 1992-05-27 | 川崎制铁株式会社 | Produce the method for Mn-Zn ferrite |
| CN1623953A (en) * | 2003-12-01 | 2005-06-08 | 浙江天通电子股份有限公司 | Manganese zinc ferrite soft magnetic sinitering method |
Non-Patent Citations (1)
| Title |
|---|
| 工艺因素及添加剂对锰锌铁氧体磁性能的影响. 谭维.硕士学位论文. 2002 * |
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