CN101388269A - Manganese zinc ferrite of high magnetic conductivity high saturation magnetic flux density high Curie temperature - Google Patents
Manganese zinc ferrite of high magnetic conductivity high saturation magnetic flux density high Curie temperature Download PDFInfo
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- CN101388269A CN101388269A CNA2008101232621A CN200810123262A CN101388269A CN 101388269 A CN101388269 A CN 101388269A CN A2008101232621 A CNA2008101232621 A CN A2008101232621A CN 200810123262 A CN200810123262 A CN 200810123262A CN 101388269 A CN101388269 A CN 101388269A
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Abstract
The invention relates to a MnZn ferrite material with high magnetic permeability, high magnetic flux density and high curie temperature, wherein the ferrite material comprises principal component Fe2O3, ZnO, MnO and adding auxiliary components, the main component formulation is that: Fe2O3 is 48-55 mol%, ZnO is 8-16mol%, and MnO is 30-39mol%. The auxiliary components comprise CoO and Bi2O3, and the adding total amount of the auxiliary components is 0.03-0.40 percent of the principal component total amount. CoO:0.005-0.15wt%, Bi2O3:0.008-0.25wt%, one or more of CaO, In2O3, WO3 and MoO3 are added, and CaO:0.008-0.15wt%, In2O3:0.008-0.10wt%, WO3:0.008-0.10wt%, and MoO3:0.005-0.15wt%.
Description
Technical field
The present invention relates to a kind of MnZn ferrite, relate in particular to a kind of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material and preparation method thereof.
Background technology
Along with complete electronic set to digitlization, multifunction and miniaturization development, the networking of electronic system forward, high speed and broadband direction develop, therefore, to magnetic material particularly MnZn Ferrite Material performance more and more higher requirement has been proposed.The coming years,, expanded greatly the high-performance MnZn Ferrite Material magnetic core market demand along with the progressively realization commercialization of the fast development of automotive electronics and Next Generation Internet, next-generation mobile communications, Digital Television.
Automotive electronics is broadly divided into two big classes according to function, i.e. car body electronic control system and vehicle electronics control system (as vehicle-mounted CD/DVD sound system, GPS navigation system etc.).Along with the consumer to the improving constantly of automobile operability, comfortableness and security requirement, automotive electronics develops to directions such as intelligent, integrated, information-based, networkings.According to authoritative institution's prediction, the electronic equipment in the car accounts for 22% of car load value now, will rise to 35% by 2010.On some limousines, electronic product even will account for more than 50% of integral vehicle cost.Therefore automotive electronics is acknowledged as one of electronic industry of development potentiality now most.
On the other hand, along with ISDN(Integrated Service Digital Network) (ISDN), Local Area Network, wide area network network services such as (WAN) and art fast developments such as Aero-Space, satellite communication and satellite navigation, become the huge electronics and information industry of market capacity.
Because above-mentioned field electronic technology is developed by leaps and bounds, traditional MnZn Ferrite Material magnetic core can not adapt to demand for development, must invent out a kind of brand-new high-performance MnZn Ferrite Material, be in particular in that material has: aspects such as high magnetic permeability, high saturation magnetic flux density and high-curie temperature.
Traditional MnZn Ferrite Material, between initial permeability μ i, saturation flux density Bs and Curie temperature Tc, a pair of often contradiction.For example: for the material of μ i=6000, its saturation flux density and Curie temperature be normally: Bs=400mT ± 10%, Tc 〉=140 ℃. this material can not satisfy the requirement of automotive electronics and network service at all, because many Auto Electronic Controlled System are in engine bin, that have even lean on very closely with engine, operational environment is very abominable, highly reliable for guaranteeing, require all components and parts can operate as normal in-40 ℃ to 150 ℃ wide temperature ranges, this just requires material to have high Curie temperature, and from the angle of safety, it is high more good more to wish; On the other hand because the interior installing space of automobile is narrow and small, require the electronic devices and components volume as far as possible little, also must have good electromagnetic performance simultaneously, this just requires material must have higher initial permeability μ i, to reduce coil turn, thereby reach the purpose that reduces volume, in order not influence components and parts service behaviour and efficient, must improve the saturation flux density of material simultaneously.Along with the development of the network communications technology, the ferritic material property of MnZn there is identical requirement.
Obtain higher initial permeability μ i, then saturation flux density Bs and Curie temperature Tc are often lower, this is because from material prescription, high initial magnetoconductivity μ i material and high saturation magnetic flux density Bs and high-curie temperature Tc material belong to two big MnZn Ferrite Material systems, and it is filled a prescription, and often difference is bigger.The present invention starts with from the following aspects, ferrite material material formula boundary at first breaks traditions, by a large amount of experiments, work out a new prescription, can take into account two kinds of MnZn Ferrite Material performance characteristics such as high initial magnetoconductivity μ i material and high saturation magnetic flux density Bs and high-curie temperature Tc material simultaneously.Secondly, by adding trace element, particularly some nano materials are optimized and modification the Ferrite Material performance.And, the kind and the addition of trace element are groped by a large amount of experiments.Thereby obtain high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material.
Summary of the invention
The present invention seeks to: propose a kind of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material and preparation method.The index of material is reached: saturation induction density Bs 〉=510mT, initial permeability μ under Curie temperature Tc 〉=220 ℃, the normal temperature
i〉=5500.
Technical scheme of the present invention is: a kind of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material, this Ferrite Material comprises principal component Fe
2O
3, ZnO, MnO and add auxiliary element, the principal component prescription is: Fe
2O
3: 48～55mol%, ZnO:8～16mol%, MnO:30～39mol%; Described auxiliary element comprises CoO, Bi
2O
3, also add CaO, In in addition
2O
3, WO
3, and MoO
3In one or more, it is 0.03～0.40wt% of principal component total amount that auxiliary element adds total amount.
The preparation method of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material of the present invention may further comprise the steps: 1) with principal component Fe in proportion
2O
3: 48～55mol%, ZnO:8～16mol%, MnO:30～39mol%; Mixing, grinding, dry, pre-burning obtain the principal component through pre-burning; 2) mix the grinding of holding concurrently through the principal component of pre-burning together with the auxiliary element that adds and make the composite material that average grain diameter is 0.9～1.3 μ m, carry out drying subsequently; C) dried particles is pressed down at press to make density be 3.0 ± 0.2g/cm
3Blank, blank is put into the bell jar stove, in partial pressure of oxygen is 1～8% balanced atmosphere,, promptly obtain the ferrite finished product 1320～1420 ℃ of sintering temperatures 3～7 hours.
Prescription of the present invention especially cooperates corresponding preparation method to make the ferrite finished product obtain following index: Curie temperature Tc 〉=220 ℃, and under the normal temperature, described ferritic initial permeability μ
i〉=5500, saturation induction density Bs 〉=510mT.
The concrete steps of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn ferrite material preparation method for material: 1) with principal component Fe
2O
3, Mn
3O
4, ZnO adds and to carry out sand milling in the sand mill be added with deionized water in advance and then through spray drying granulation, 800～1000 ℃ of pre-burnings in rotary kiln or box type furnace, to obtain ferrite prefiring material; 2) ferrite prefiring material is added with auxiliary element carry out sand milling in the sand mill that is added with deionized water in advance, obtain the ferrite slurry that average grain diameter is 1.0 ± 0.3 μ m, add 10% PVA solution (concentration is 10%) subsequently and carry out spray drying granulation, obtain ferrite powder; 3) ferrite powder being obtained density through the press compacting is 3.0 ± 0.2g/cm
3The ferrite blank, with blank in vacuum sintering furnace or bell jar stove or atmosphere protection pushed bat kiln, in partial pressure of oxygen is 1～8% balanced atmosphere, 1320～1420 ℃ of sintering temperatures 3～7 hours.
As the stronger a kind of specific embodiment of practicality, described relatively principal component total amount in the product, the content of reference material is as follows separately in it for described auxiliary adding ingredient, CaO:0.008～0.15wt%, In
2O
3: 0.008～0.10wt%, WO
3: 0.008～0.10wt%, CoO:0.005～0.15wt%, Bi
2O
3: 0.008～0.25wt%, MoO
3: 0.005～0.15wt%.
Result of study shows that CaO content can not be too high in the ferrite, and excessive CaO can cause the discontinuous growth of ferrite crystal grains, thereby influences material initial permeability μ
iRaising.The CaO of Jia Ruing is 0～0.15wt% in the present invention.Especially be 0.01-0.08wt%.The present invention studies an example and shows: do not adding under any auxiliary element situation, raw-material CaO (impurity content) still reaches 0.018wt%, and above-mentioned CaO content is the total content of CaO in the raw material.
Adopt In
2O
3, Bi
2O
3, CoO, WO
3And MoO
3Enter Deng adding as basic auxiliary element, these additives since characteristics separately the electromagnetic performance of MnZn Ferrite Material is played an important role.
In basic auxiliary element, primary study Bi
2O
3Composite mixed (the Bi in composite mixed of-CoO
2O
3With the ratio of CoO be 1～2: 1) to material initial permeability μ
iInfluence with saturation induction density Bs experimental results show that: suitable Bi
2O
3(0.01～0.13wt%) can improve the initial permeability μ of material to the composite mixed amount of-CoO
i, also can improve saturation induction density Bs simultaneously, initial permeability μ is considered in overall balance
iWith saturation induction density Bs, we select Bi
2O
3The composite mixed amount of-CoO is 0.015～0.25wt%.And Bi
2O
3Have fluxing action, in ferritic sintering process, micro-Bi
2O
3The affiliation that adds facilitate liquid-phase sintering.Liquid-phase sintering helps improving reaction rate, promotes the carrying out of solid phase reaction, improves the sintered density of material, reduces the crystal boundary and the intragranular porosity, finally makes the initial permeability μ of material
iImprove.The CoO that adds trace in experiment impels to generate CoFe
2O
4Ferrite, CoFe
2O
4K
1, K
2Just be, in the MnZn ferrite, can play the compensating action of positive and negative K value, make its K
1Just becoming by negative zero passage with composition (or temperature); Simultaneously, CoFe
2O
4λ
1110, can reduce material magnetostriction coefficient λ so in the MnZn ferrite, add CoO
s, make μ
iIncrease.
The invention has the beneficial effects as follows: obtained the high high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material of a kind of performance index by the present invention.Its characteristic is: saturation induction density Bs 〉=510mT, initial permeability μ under Curie temperature Tc 〉=220 ℃, the normal temperature
i〉=5500.
Embodiment
Ferrite preparation method's of the present invention typical embodiment, with following step:
1) raw material mix: press with following composition of raw materials: Fe
2O
3: 54.1mol%, ZnO:13mol%, MnO:32.9mol% takes by weighing raw material;
2) sand milling:
Load weighted raw material are put into sand mill, and at the deionized water of weight such as adding in advance, sand milling 0.5 hour;
3) spray drying granulation:
In the raw material slip, add about 10%PVA solution (concentration is 10%), carry out spray drying granulation one time;
4) pre-burning: a spray drying granulation powder is carried out pre-burning by rotary kiln, and burning temperature is 900 ℃;
5) impurity (composition) adds: add following auxiliary element: CoO:0.08wt%, Bi
2O
3: 0.03wt%; And MoO
3: 0.02wt%, CaO:0.045wt%, In
2O
3: 0.035wt% and WO
3: four kinds of adding ingredients of 0.02wt% can appoint select one, two, three or whole four kinds of compositions add.
6) secondary sand milling: ferrite prefiring material and above-mentioned auxiliary element are put into sand mill, and at the deionized water of weight such as adding in advance, sand milling 1.5 hours, the particle mean size that makes pre-imitation frosted glass is less than 1.3 μ m;
7) secondary spray drying granulation:
In ferrite slurry, add about 10%PVA solution (concentration is 10%), carry out the secondary spray drying granulation;
8) moulding: secondary spray drying granulation ferrite powder is pressed into the ferrite blank;
9) sintering: the ferrite blank is put into the bell jar stove, in partial pressure of oxygen is 4.5% balanced atmosphere, 1395 ℃ of sintering temperatures 5 hours.Above-mentioned prescription and preparation method make finished material reach described index.
Embodiment 1: take by weighing 54.1mol%Fe
2O
3, 32.9mol%MnO (the raw material form is Mn3O4), 13mol%ZnO.Drop in the sand mill that is added with deionized water in advance and grind, control average grain diameter 0.8 ± 0.2 μ m, once spraying back electricity consumption heating revolving kiln under 900 ± 20 ℃ of temperature carries out pre-burning.Pre-subsequently imitation frosted glass drops into sand mill and carries out the secondary sand milling, and described relatively principal component content in the sand grinding process adds pure water 35%, dispersant 0.008% and defoamer 0.005%, and adds addition of C aO:0.045wt%, WO
3: 0.02wt%, CoO:0.08wt%, Bi
2O
3: the average grain diameter of 0.03wt% control sand milling is 1.0 ± 0.2 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm
3Annulus, the ferrite blank is put into the bell jar stove, in partial pressure of oxygen is 4.5% balanced atmosphere, 1395 ℃ of sintering temperatures 5 hours.The product correlated performance is listed in the table one.The present invention can select to add MoO in addition
3: 0.02wt% or In
2O
3: 0.035wt%, or the two all is added on and does not all have significantly difference on the performance.
Embodiment 2: take by weighing 53.5mol%Fe
2O
3, (the raw material form is Mn to 34.5mol%MnO
3O
4), 12mol%ZnO.Drop in the sand mill that is added with deionized water in advance and grind, control average grain diameter 0.8 ± 0.2 μ m, once spraying back electricity consumption heating revolving kiln under 900 ± 20 ℃ of temperature carries out pre-burning.Pre-subsequently imitation frosted glass drops into sand mill and carries out the secondary sand milling, and described relatively principal component content in the sand grinding process adds pure water 35%, dispersant 0.008% and defoamer 0.005%, and adds addition of C aO:0.045wt%, In
2O
3: 0.035wt%, WO
3: 0.02wt%, CoO:0.08wt%, Bi
2O
3: 0.03wt%, MoO
3: 0.02wt%, the average grain diameter of control sand milling is 1.0 ± 0.2 μ m.Carry out the secondary spraying at last and obtain Mn-Zn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm
3Annulus, the ferrite blank is put into the bell jar stove, in partial pressure of oxygen is 4.5% balanced atmosphere, 1395 ℃ of sintering temperatures 5 hours.The product correlated performance is listed in the table 1.Table 1
By table 1 as seen, ferrite product of the present invention has three high characteristics such as high magnetic conductivity high saturation magnetic flux density high-curie temperature
Claims (6)
1, a kind of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material is characterized in that Ferrite Material comprises principal component Fe
2O
3, ZnO, MnO and add auxiliary element, the principal component prescription is: Fe
2O
3: 48～55mol%, ZnO:8～16mol%, MnO:30～39mol%; Described auxiliary element comprises CoO, Bi
2O
3, it is 0.03～0.40wt% of principal component total amount that auxiliary element adds total amount.
2, high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material according to claim 1 is characterized in that auxiliary element CoO addition 0.005～0.15wt%, Bi
2O
3Addition is 0.008～0.25wt%.
3, high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material according to claim 1 is characterized in that auxiliary element adds CaO, In again
2O
3, WO
3, and MoO
3In one or more, CaO:0.008～0.15wt%, In
2O
3: 0.008～0.10wt%, WO
3: 0.008～0.10wt%,, MoO
3: 0.005～0.15wt%.
4, high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material according to claim 1 is characterized in that CaO content is 0.01-0.08wt%.
5, the preparation method of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material is characterized in that may further comprise the steps: 1) with principal component Fe in proportion
2O
3: 48～55mol%, ZnO:8～16mol%, MnO:30～39mol%; Mixing, grinding, dry, pre-burning obtain the principal component through pre-burning; 2) carry out mixing for the second time double the grinding through the principal component of pre-burning together with the auxiliary element that adds and make the composite material that average grain diameter is 0.9～1.3 μ m, carry out drying subsequently; C) dried particles is pressed down at press to make density be 3.0 ± 0.2g/cm
3Blank, blank is put into the bell jar stove, in partial pressure of oxygen is 1～8% balanced atmosphere,, promptly obtain the ferrite finished product 1320～1420 ℃ of sintering temperatures 3～7 hours.
6, the preparation method of high magnetic conductivity high saturation magnetic flux density high-curie temperature MnZn Ferrite Material according to claim 5 is characterized in that concrete steps are that mixing, grinding technics are with principal component Fe
2O
3, Mn
3O
4, ZnO adds and to carry out sand milling in the sand mill add deionized water in advance and then through spray drying granulation, 800～1000 ℃ of pre-burnings in rotary kiln or box type furnace, to obtain ferrite prefiring material; Mixing for the second time holds concurrently grinds is ferrite prefiring material to be added with auxiliary element carry out sand milling in the sand mill that is added with deionized water in advance, obtain the ferrite slurry that average grain diameter is 1.0 ± 0.3 μ m, the PVA solution that adds 10wt% subsequently carries out spray drying granulation, obtains ferrite powder.
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|---|---|---|---|
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|---|---|---|---|
| CN2008101232621A CN101388269B (en) | 2008-07-11 | 2008-07-11 | Manganese zinc ferrite of high magnetic conductivity high saturation magnetic flux density high Curie temperature |
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| CN101388269B CN101388269B (en) | 2011-09-28 |
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ID=40477615
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|---|---|---|---|---|
| CN101870578A (en) * | 2010-04-14 | 2010-10-27 | 湖北凯立德新材料有限公司 | Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof |
| CN101921103A (en) * | 2010-08-19 | 2010-12-22 | 上海电力学院 | Manganese zinc ferrite with high magnetic conductivity and preparation method thereof |
| CN102173767A (en) * | 2011-01-17 | 2011-09-07 | 临沂中瑞电子有限公司 | Magnetic material for photovoltaic inverter |
| CN102390986A (en) * | 2011-08-09 | 2012-03-28 | 临沂中瑞电子有限公司 | Low-power-consumption MnZn ferrite material |
| WO2012097481A1 (en) * | 2011-01-17 | 2012-07-26 | 临沂中瑞电子有限公司 | MnZn FERRITE MATERIAL |
| WO2013174100A1 (en) * | 2012-05-25 | 2013-11-28 | 南通华兴磁性材料有限公司 | Mnzn ferrite material for broadband anti-electromagnetic interference and manufacturing method thereof |
| CN104051106A (en) * | 2014-06-24 | 2014-09-17 | 铜陵三佳变压器有限责任公司 | Boron-oxide-based ferrite core material used for transformer |
| CN105461296A (en) * | 2015-11-20 | 2016-04-06 | 无锡斯贝尔磁性材料有限公司 | A high-BS low-loss manganese zinc ferrite magnetic material and a preparing method thereof |
| CN108892501A (en) * | 2018-08-02 | 2018-11-27 | 西华大学 | Ferrite material and preparation method thereof |
| CN108950345A (en) * | 2018-08-16 | 2018-12-07 | 安徽信息工程学院 | inorganic functional composite material |
| CN111138179A (en) * | 2019-12-25 | 2020-05-12 | 江门安磁电子有限公司 | Broadband high-impedance manganese-zinc ferrite material and preparation method thereof |
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| CN100340524C (en) * | 2005-03-21 | 2007-10-03 | 乳源东阳光磁性材料有限公司 | Ferrite in manganese zinc series in both five thousands of high curie temperature and lowloss and preparing process thereof |
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| CN101870578A (en) * | 2010-04-14 | 2010-10-27 | 湖北凯立德新材料有限公司 | Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof |
| CN101870578B (en) * | 2010-04-14 | 2013-06-05 | 湖北凯立德新材料有限公司 | Wide-temperature manganese zinc ferrite material with high-magnetic conductivity of 12,000 mu i and preparation method thereof |
| CN101921103A (en) * | 2010-08-19 | 2010-12-22 | 上海电力学院 | Manganese zinc ferrite with high magnetic conductivity and preparation method thereof |
| CN102173767A (en) * | 2011-01-17 | 2011-09-07 | 临沂中瑞电子有限公司 | Magnetic material for photovoltaic inverter |
| WO2012097481A1 (en) * | 2011-01-17 | 2012-07-26 | 临沂中瑞电子有限公司 | MnZn FERRITE MATERIAL |
| CN102173767B (en) * | 2011-01-17 | 2013-05-15 | 临沂中瑞电子有限公司 | Magnetic material for photovoltaic inverter |
| CN102390986A (en) * | 2011-08-09 | 2012-03-28 | 临沂中瑞电子有限公司 | Low-power-consumption MnZn ferrite material |
| CN102390986B (en) * | 2011-08-09 | 2013-05-15 | 临沂中瑞电子有限公司 | Low-power-consumption MnZn ferrite material |
| WO2013174100A1 (en) * | 2012-05-25 | 2013-11-28 | 南通华兴磁性材料有限公司 | Mnzn ferrite material for broadband anti-electromagnetic interference and manufacturing method thereof |
| CN104051106A (en) * | 2014-06-24 | 2014-09-17 | 铜陵三佳变压器有限责任公司 | Boron-oxide-based ferrite core material used for transformer |
| CN104051106B (en) * | 2014-06-24 | 2016-08-24 | 铜陵三佳变压器有限责任公司 | A kind of boron oxide based ferrite core material for transformer |
| CN105461296A (en) * | 2015-11-20 | 2016-04-06 | 无锡斯贝尔磁性材料有限公司 | A high-BS low-loss manganese zinc ferrite magnetic material and a preparing method thereof |
| CN105461296B (en) * | 2015-11-20 | 2018-12-14 | 无锡斯贝尔磁性材料有限公司 | A kind of high BS low-loss manganese zine ferrite magnetic material and preparation method thereof |
| CN108892501A (en) * | 2018-08-02 | 2018-11-27 | 西华大学 | Ferrite material and preparation method thereof |
| CN108950345A (en) * | 2018-08-16 | 2018-12-07 | 安徽信息工程学院 | inorganic functional composite material |
| CN111138179A (en) * | 2019-12-25 | 2020-05-12 | 江门安磁电子有限公司 | Broadband high-impedance manganese-zinc ferrite material and preparation method thereof |
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