CN103011790A - Preparation method of high-permeability manganese zinc ferrite - Google Patents

Preparation method of high-permeability manganese zinc ferrite Download PDF

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Publication number
CN103011790A
CN103011790A CN2012105391248A CN201210539124A CN103011790A CN 103011790 A CN103011790 A CN 103011790A CN 2012105391248 A CN2012105391248 A CN 2012105391248A CN 201210539124 A CN201210539124 A CN 201210539124A CN 103011790 A CN103011790 A CN 103011790A
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preparation
manganese
ferrite
cooling roller
zno
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CN103011790B (en
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李永劬
郭凤鸣
严建强
王士杰
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HAINING LIANFENG MAGNET INDUSTRY Co Ltd
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HAINING LIANFENG MAGNET INDUSTRY Co Ltd
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Abstract

The invention discloses a preparation method of a rapid-quenching amorphous high-permeability manganese zinc ferrite. The method comprises the following steps of: (1) preparing raw materials comprising Fe2O3, ZnO and manganese oxide, wherein the manganese oxide is MnO, Mn3O4 or a mixture of MnO and Mn3O4; (2) smelting after the raw materials are put into a vacuum furnace, subsequently a furnace cover is covered, wherein the temperature for smelting through the vacuum furnace is at 1400-2000 DEG C; (3) rapidly quenching a smelted solution produced after smelting through the vacuum furnace and spraying to form belts to prepare belt materials; and (4) winding the belt materials as a needed manganese zinc ferrite magnetic core and annealing for 1-2h at 500-800 DEG C in a vacuum annealing furnace to obtain the manganese zinc ferrite magnetic core. Due to the adoption of the processes of smelting in vacuum, rapidly quenching and spraying to form belts and finally annealing in vacuum, the additive needed for the traditional manganese zinc ferrite is not included in the high-permeability manganese zinc ferrite, the raw material cost is saved, the preparation process is simple, the production process is shortened and the production efficiency is enhanced.

Description

A kind of preparation method of high permeability MnZn ferrite
Technical field
The present invention relates to a kind of preparation method of Mn-Zn ferrite.
Background technology
Electronic industry constantly develops, so that the volume of magnetic elements more and more is tending towards microminiaturized, thereby the research of high permeability MnZn ferrite day by day becomes an important directions of soft magnetic ferrite research.Because when initial permeability is higher, just can reach the inductance value that needs with less coil turn, thereby can effectively reduce the direct current resistance of coil and the loss of introducing thereof, and can also reduce significantly device volume simultaneously, be conducive to miniaturization and the lightweight of device.
The described Mn-Zn ferrite soft magnetism of China Patent Publication No. 1619719A and manufacture method, preparation flow is the links such as pre-burning, pulverizing, mist projection granulating, compression moulding, sintering.Production Flow Chart is complicated, and efficient is low, and 1100～1250 ℃ of sintering temperatures, soaking time 3～5 hours, and energy consumption is larger.Though described its sintering temperature of Mn-Zn ferrite sintering method of another China Patent Publication No. CN1623953A is lower than above-mentioned patent, but still need 1000～1200 ℃, soaking time still is 3～5 hours, and energy consumption is also larger.
The described manganese of China publication CN1447356A-zinc power soft ferrite powder and preparation method thereof has added the organism such as di(2-ethylhexyl)phosphate octanol, polyvinyl alcohol and defoamer, very easily decomposes contaminate environment when high temperature sintering; And when crushing material, mist projection granulating, the workshop dust pollution is very serious, work under bad environment.
Above-mentioned each patent is all used powder pressing forming, and then high temperature sintering is prepared from, and energy consumption is high like this, preparation flow is complicated, and cost is high; Contain additive, at high temperature easily decompose contaminate environment.Therefore, how to shorten the preparation flow of soft magnetic manganese-zinc ferrite, reduce production energy consumption and become problem demanding prompt solution.
Summary of the invention
Technical problem to be solved by this invention just provides a kind of preparation method of fast quenching amorphous high permeability MnZn ferrite, simplifies preparation flow, reduces the low and environmental pollution of production energy consumption.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of preparation method of fast quenching amorphous high permeability MnZn ferrite is characterized in that comprising the steps:
1) batching: raw material is Fe 2O 3, ZnO and manganese oxide compound, the oxide compound of described manganese is MnO or Mn 3O 4Perhaps MnO and Mn 3O 4Mixture;
2) smelt: raw material is put into vacuum oven, then cover bell and vacuumize and smelt, the temperature that vacuum oven is smelted is 1400～2000 ℃;
3) vacuum oven is smelted after the smelting liquation of output carry out fast quenching spray band and make band;
4) the required manganese-zinc ferrite core of above-mentioned strip coil coiled, 500～800 ℃ of annealing 1～2h can obtain the manganese-zinc ferrite core finished product in vacuum annealing furnace.
As preferably, the molar percentage of each component is the Fe of 51～53mol% in the described raw material 2O 3, the oxide compound of the manganese of 25～27mol%, all the other are ZnO.
As preferably, the molar percentage of each component is the Fe of 52mol% in the described raw material 2O 3, the oxide compound of the manganese of 26mol%, the ZnO of 22mol%.
As preferably, described ZnO is nano particle.
As preferably, described Fe 2O 3, ZnO, manganese oxide compound put into vacuum oven by order from the bottom up.
As preferably, the temperature that described vacuum oven is smelted is 1600～1800 ℃.
As preferably, the strip width that described fast quenching spray band is made is 15～40mm, and thickness is 20～40 μ m.
As preferably, the concrete technology of fast quenching spray band is in the described step 3): the smelting liquation of output was poured the Sheng ladle into after vacuum oven was smelted, the nozzle ejection of wrapping by bleed-out again, traction throws away and can make required Mn-Zn ferrite band through cooling roller, through the follow-up magnetic core that is wound into different size.
As preferably, described bleed-out bag is provided with the liquid level that liquid-level measuring-controlling apparatus is adjusted the bleed-out bag, is provided with roller mouth spacing measuring and control device between described bleed-out bag nozzle and cooling roller and adjusts the spacing of bleed-out bag nozzle and cooling roller and make nozzle spray molten steel constant voltage, constant current.
As preferably, described cooling roller outer circumferential sides is provided with the turning cutter, and the complete band of every spray uses turning cutter car cooling roller outer circumference surface one circle, with sand paper the cooling roller outer circumference surface is polished smooth, described cooling roller outer circumferential sides also is provided with online coping device cooling roller is carried out online reconditioning again.
The present invention changes traditional powder pressing forming, and then the preparation technology of high temperature sintering, vacuum is smelted, the fast quenching spray is with, the technique of last vacuum annealing and adopt, and the high permeability MnZn ferrite test performance that the present invention prepares is: μ i 〉=10000, Bs 〉=300mT.Wherein, calculate initial permeability after the inductance value with HP4284A type LCR Meter specimen, test condition is 1kHz, 0.1V, 20Ts; Adopt the saturation magnetic flux density Bs of SY8258BH/ μ analytical system specimen, test condition is 50Hz, H=1200A/m, 25 ℃.Thereby the present invention has the following advantages:
1, the present invention does not contain the required additive of traditional Mn-Zn ferrite, saves material cost;
2, preparation technology is simple, shortens Production Flow Chart, has improved production efficiency;
3 compare with traditional preparation method, without pre-burning, sintering process, have reduced production energy consumption in the preparation process.
4, environmental protection does not have the additives decompose contaminate environment; The workshop no dust pollution.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments:
Fig. 1 is the fast quenching spray carrying equipment structural representation of high permeability MnZn ferrite.
Embodiment
The preparation method of Mn-Zn ferrite of the present invention comprises the steps:
1) batching: raw material is Fe 2O 3, ZnO and manganese oxide compound, the oxide compound of described manganese is MnO or Mn 3O 4Perhaps MnO and Mn 3O 4Mixture; The molar percentage of each component is the Fe of 51～53mol% in the described raw material 2O 3, the oxide compound of the manganese of 25～27mol%, all the other are ZnO, described ZnO is nano particle.
2) smelt: raw material is put into vacuum oven, then cover bell and vacuumize and smelt, the temperature that vacuum oven is smelted is 1400～2000 ℃; Wherein, described Fe 2O 3, ZnO, manganese oxide compound put into vacuum oven by order from the bottom up.
3) vacuum oven is smelted after the smelting liquation of output carry out fast quenching spray band and make band; The strip width that described fast quenching spray band is made is 15～40mm, and thickness is 20～40 μ m.
4) the required manganese-zinc ferrite core of above-mentioned strip coil coiled, 500～800 ℃ of annealing 1～2h can obtain the manganese-zinc ferrite core finished product in vacuum annealing furnace.
Below in conjunction with specific embodiment the present invention is made and to specify:
Embodiment one:
Adopt Fe 2O 351mol%, ZnO22mol%, MnO27mol% are Fe 2O 3, ZnO, MnO put into vacuum oven by order from the bottom up, then cover bell and vacuumize and smelt 1700 ℃ of smelting temperatures; Above-mentioned smelting liquation fast quenching spray 15mm wide strip, thickness of strip 20 μ m.The required fast quenching amorphous manganese-zinc ferrite core of above-mentioned strip coil coiled, in vacuum annealing furnace 800 ℃, the 1h anneal gets final product to get the manganese-zinc ferrite core of characteristic conforms product requirement.
Embodiment two:
Adopt Fe 2O 353mol%, ZnO22mol%, Mn 3O 425mol% is Fe 2O 3, ZnO, Mn 3O 4Put into vacuum oven by order from the bottom up, then cover bell and vacuumize and smelt 1600 ℃ of smelting temperatures; Above-mentioned smelting liquation fast quenching spray 40mm wide strip, thickness of strip 40 μ m.The required fast quenching amorphous manganese-zinc ferrite core of above-mentioned strip coil coiled, in vacuum annealing furnace 500 ℃, the 3h anneal gets final product to get the manganese-zinc ferrite core of characteristic conforms product requirement.
Embodiment three:
Adopt Fe 2O 351mol%, ZnO24mol%, MnO25mol% are Fe 2O 3, ZnO, MnO and Mn 3O 4Mixture is put into vacuum oven by order from the bottom up, then covers bell and vacuumizes and smelt 1800 ℃ of smelting temperatures; Above-mentioned smelting liquation fast quenching spray 25mm wide strip, thickness of strip 30 μ m.The required fast quenching amorphous manganese-zinc ferrite core of above-mentioned strip coil coiled, in vacuum annealing furnace 650 ℃, the 1.5h anneal gets final product to get the manganese-zinc ferrite core of characteristic conforms product requirement.
Below in conjunction with Fig. 1 the fast quenching spray carrying equipment of high permeability MnZn ferrite is explained:
This fast quenching spray carrying equipment is comprised of intermediate frequency furnace 1, Sheng ladle 2, liquid-level measuring-controlling apparatus 3, bleed-out bag 4, roller mouth spacing measuring and control device 5, turning cutter 6, online coping device 7, cooling roller 8, reeling machine 9.Bleed-out bag 4 is located at and is contained ladle 2 belows, and cooling roller 8 is located at bleed-out bag 4 belows, and turning cutter 6, online coping device 7 are located at cooling roller 8 outer circumferential sides, the amorphous Mn-Zn ferrite strip coil that reeling machine 9 throws away cooling roller 8 tractions.
At first, Fe 2O 3, ZnO, MnO(or Mn 3O 4) put into vacuum oven by order from the bottom up, then cover bell and vacuumize and smelt 1600～1800 ℃ of smelting temperatures.
The mother alloy of above-mentioned vacuum metling is put into intermediate frequency furnace 1 fusing fully, pour into and contain ladle 2, by the ejection of the nozzle on the bleed-out bag 4,8 tractions throw away and can make required amorphous fast quenching Mn-Zn ferrite band through cooling roller, through the follow-up magnetic core that is wound into different size again.
Wherein, liquid-level measuring-controlling apparatus 3 is liquid levels of adjusting bleed-out bag 4, and roller mouth spacing measuring and control device 5 practical situation according to bleed-out bag 4 are constantly adjusted roller mouth spacing, makes nozzle ejection molten steel constant voltage, constant current, thereby makes even thickness on strip width, the length direction.The complete band of every spray, cooling roller 8 all can be caused roll surface rough by molten steel, uses turning cutter 6 cars once, uses sand papering smooth again; When the spray band, cooling roller can will can improve surface quality of strips with online coping device 7 online reconditionings constantly by molten steel, increases magnetic core lamination coefficient, thereby improves the comprehensive magnetic energy of magnetic core.
Above-mentioned three examples test initial permeability μ i, saturation magnetic flux density Bs contrast is as shown in the table:
? μ i Bs（mT）
Embodiment one 12000 310
Embodiment two 11800 335
Embodiment three 10000 350
As can be seen from the above table, the μ of the embodiment of the invention i〉=10000, prepared FERRITE CORE is the high permeability MnZn ferrite magnetic core.

Claims (10)

1. the preparation method of a high permeability MnZn ferrite is characterized in that comprising the steps:
1) batching: raw material is Fe 2O 3, ZnO and manganese oxide compound, the oxide compound of described manganese is MnO or Mn 3O 4Perhaps MnO and Mn 3O 4Mixture;
2) smelt: raw material is put into vacuum oven, then cover bell and vacuumize and smelt, the temperature that vacuum oven is smelted is 1400～2000 ℃;
3) vacuum oven is smelted after the smelting liquation of output carry out fast quenching spray band and make band;
4) the required manganese-zinc ferrite core of above-mentioned strip coil coiled, 500～800 ℃ of annealing 1～2h can obtain the manganese-zinc ferrite core finished product in vacuum annealing furnace.
2. the preparation method of Mn-Zn ferrite according to claim 1, it is characterized in that: the molar percentage of each component is the Fe of 51～53mol% in the described raw material 2O 3, the oxide compound of the manganese of 25～27mol%, all the other are ZnO.
3. the preparation method of Mn-Zn ferrite according to claim 2, it is characterized in that: the molar percentage of each component is the Fe of 52mol% in the described raw material 2O 3, the oxide compound of the manganese of 26mol%, the ZnO of 22mol%.
4. the preparation method of Mn-Zn ferrite according to claim 3, it is characterized in that: described ZnO is nano particle.
5. the preparation method of Mn-Zn ferrite according to claim 1 is characterized in that: described Fe 2O 3, ZnO, manganese oxide compound put into vacuum oven by order from the bottom up.
6. the preparation method of Mn-Zn ferrite according to claim 5 is characterized in that: the temperature that described vacuum oven is smelted is 1600～1800 ℃.
7. the preparation method of Mn-Zn ferrite according to claim 1 is characterized in that: the strip width that described fast quenching spray band is made is 15～40mm, and thickness is 20～40 μ m.
8. the preparation method of Mn-Zn ferrite according to claim 1, it is characterized in that: the concrete technology of fast quenching spray band is in the described step 3): the smelting liquation of output was poured into and is contained ladle (2) after vacuum oven was smelted, spray by the nozzle on the bleed-out bag (4) again, traction throws away and can make required Mn-Zn ferrite band through cooling roller (8), through the follow-up magnetic core that is wound into different size.
9. the preparation method of Mn-Zn ferrite according to claim 8, it is characterized in that: described bleed-out bag (4) is provided with the liquid level that liquid-level measuring-controlling apparatus (3) is adjusted bleed-out bag (4), and the spacing that is provided with roller mouth spacing measuring and control device (5) adjustment bleed-out bag (4) nozzle and cooling roller (8) between described bleed-out bag (4) nozzle and cooling roller (8) makes nozzle ejection molten steel constant voltage, constant current.
10. the preparation method of Mn-Zn ferrite according to claim 9, it is characterized in that: described cooling roller (8) outer circumferential sides is provided with turning cutter (6), the complete band of every spray, use turning cutter car cooling roller outer circumference surface one circle, with sand paper the cooling roller outer circumference surface is polished smooth, described cooling roller (8) outer circumferential sides also is provided with online coping device (7) cooling roller is carried out online reconditioning again.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503397A (en) * 2011-11-29 2012-06-20 无锡斯贝尔磁性材料有限公司 Manganese oxide doped manganese-zinc ferrite and preparation method thereof
CN108655352A (en) * 2017-03-29 2018-10-16 鞍钢股份有限公司 Preparation method of iron foil
CN113563062A (en) * 2021-09-24 2021-10-29 天通控股股份有限公司 Ultrahigh-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method thereof
CN114315336A (en) * 2021-12-28 2022-04-12 南通华兴磁性材料有限公司 Preparation method of high-magnetic-property manganese-zinc ferrite

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US6200493B1 (en) * 1998-05-20 2001-03-13 Tdk Corporation MnMgCuZn ferrite material
CN1402266A (en) * 2002-09-13 2003-03-12 无锡晶石磁性电子器件有限公司 Magnanese-zinc ferrite magnetic core
CN1793019A (en) * 2005-11-01 2006-06-28 淄博宇星电子材料有限公司 Process for mfg, 18k manganese zine iron oxygen body magnetic powder magnetic core
JP2010173888A (en) * 2009-01-29 2010-08-12 Tdk Corp METHOD FOR PRODUCING MnZn FERRITE
CN102060518A (en) * 2010-11-29 2011-05-18 苏州天铭磁业有限公司 High-resistivity low-loss nanocrystal manganese-zinc (MnZn) ferrite material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6200493B1 (en) * 1998-05-20 2001-03-13 Tdk Corporation MnMgCuZn ferrite material
CN1402266A (en) * 2002-09-13 2003-03-12 无锡晶石磁性电子器件有限公司 Magnanese-zinc ferrite magnetic core
CN1793019A (en) * 2005-11-01 2006-06-28 淄博宇星电子材料有限公司 Process for mfg, 18k manganese zine iron oxygen body magnetic powder magnetic core
JP2010173888A (en) * 2009-01-29 2010-08-12 Tdk Corp METHOD FOR PRODUCING MnZn FERRITE
CN102060518A (en) * 2010-11-29 2011-05-18 苏州天铭磁业有限公司 High-resistivity low-loss nanocrystal manganese-zinc (MnZn) ferrite material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503397A (en) * 2011-11-29 2012-06-20 无锡斯贝尔磁性材料有限公司 Manganese oxide doped manganese-zinc ferrite and preparation method thereof
CN108655352A (en) * 2017-03-29 2018-10-16 鞍钢股份有限公司 Preparation method of iron foil
CN113563062A (en) * 2021-09-24 2021-10-29 天通控股股份有限公司 Ultrahigh-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method thereof
CN113563062B (en) * 2021-09-24 2021-11-30 天通控股股份有限公司 Ultrahigh-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method thereof
CN114315336A (en) * 2021-12-28 2022-04-12 南通华兴磁性材料有限公司 Preparation method of high-magnetic-property manganese-zinc ferrite

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