CN101241793A - Mn-Zn soft magnetic ferrite and production method - Google Patents
Mn-Zn soft magnetic ferrite and production method Download PDFInfo
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- CN101241793A CN101241793A CNA200710019719XA CN200710019719A CN101241793A CN 101241793 A CN101241793 A CN 101241793A CN A200710019719X A CNA200710019719X A CN A200710019719XA CN 200710019719 A CN200710019719 A CN 200710019719A CN 101241793 A CN101241793 A CN 101241793A
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Abstract
The present invention discloses a Mn-Zn series ferrite and the preparing technique thereof. The raw material is prepared with the adjusting of the main formula and the adjusting of the kind and dosage of the adulterant (especially CoO is used). When the raw material is provided higher magnetic conductivity and stable magnetic conductivity change rate in broad temperature range, the raw material is provided with high saturation flux density. The range of the main formula of the material is as follows: Fe2O3 for 53.7-54.4mol, MnO for 36-38mol, and ZnO for 8-10mol The invention is mainly characterized in that the adding amount of CoO is 0.05-0.6wt Therefore the invention has the advantages of small initial permeability variation in broad temperature range and high saturation flux density. The technique of the invention is simple and can be actualized with generalization.
Description
Technical field
The present invention relates to initial permeability (μ i) variation is little in a kind of wide temperature range, saturation flux density is high ferrite sintered product and production method, especially a kind of Mn-Zn series soft magnetic ferrite and production method are applicable to the transformer that uses in the communication equipment and the filter in the digital amplifier.
Background technology
The magnetic core that uses in the transformer of communication usefulness and the filter in the digital amplifier requires the magnetic property of high magnetic permeability, high saturation magnetic flux density, low-loss etc.In recent years, along with the miniaturization of electronic product, highly integrated development, require magnetic core (electric property of magnetic core) will possess certain stability with the variations in temperature that self-heating and variation of ambient temperature cause.Compared with varying with temperature the big high magnetic conductance material that rises and falls, electric property varies with temperature little material and is more being paid attention to now.Particularly the time,, can cause filter frequencies to change and bring bad influence to tonequality if electromagnetic performance varies with temperature greatly as the filter in the digital amplifier.
In addition, owing to magnetic material will use in unsaturated scope, so must calculate, select the physical dimension of product according to saturation flux density.Along with the development of miniaturization, the material with high saturation magnetic flux density is more and more paid close attention to and is expected.
From the above mentioned, the transformer of communication usefulness and the stability of the ferritic electromagnetic performance of the employed Mn-Zn of the filter in the digital amplifier receive much attention, so constantly finding that the temperature characterisitic that adopts cobalt oxide (CoO) can make initial permeability is stable in research and development, the discussion process, but most initial permeability strength can only be in about 1000, and high person only 2000.Simultaneously, because magnetic permeability is low, must reach required sense value by the method that increases number of turns, and being increased in of number of turns increases the loss of the copper cash of coil itself to a certain extent, brought certain problem to power consumption.
Summary of the invention
In order to overcome above-mentioned defective, the invention provides a kind of the initial permeability variation is little in wide temperature range, saturation flux density is high Mn-Zn series soft magnetic ferrite and production method.
The present invention for the technical scheme that solves its technical problem and adopt is: mainly adopt high-purity Fe
2O
3, Mn
3O
4(calculating with MnO), ZnO are main raw material(s), and its proportion is: Fe
2O
3: 53.7～54.4mol%, MnO:36～38mol% and ZnO:8～10mol%.
Also add alloy SiO
2, CaO, Nb
2O
5And V
2O
5, its suitable input amount is: SiO
2: 0.005～0.01wt%, CaO:0.03～0.06wt%, Nb
2O
5: 0.01～0.03wt% and V
2O
5: 0.01～0.06wt%, wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Add alloy CoO in addition, its suitable input amount is: CoO:0.05～0.6wt%, wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Guarantee that the material initial permeability is more than 3000 in the time of 23 ℃, initial permeability is a benchmark during simultaneously with 23 ℃, in-20～150 ℃ scope the rate of change of initial permeability 15% with the ferrite electric property of saturation flux density more than 540mT interior, 23 ℃ the time.
Process conditions involved in the present invention:
1), weighing: there emerged a raw-material weight by the correct weighing of aforementioned proportion;
2), mix: the raw material after the weighing is put into the dry type vibratory ball mill successively, carry out mixing in 20～30 minutes, require to mix, do not have tangible aberration;
3), give burning: the raw material input push type that mixes is given firing, give the burning temperature and be set at 850～1100 ℃, it is 2～5 hours that high temperature gives the burning time;
4), pulverize: adopt vibrator to carry out 10～40 minutes pulverizing, make it comment equal particle directly to reach below the 2.5 μ m giving the powder that burns down;
5), sand milling: in sand mill, drop into an amount of powder, drop into the impurity that measures in advance, and drop into following additives and carry out sand milling (meticulous pulverizing), averaged particles is directly reached below the 2.2 μ m by 40～80 minutes grindings;
The deionization pure water of additive use amount: 40～50wt%;
0.5 the binding agent of～1.5wt%;
0.1 the dispersant of～0.5wt%;
0.1wt% with interior defoamer and value greater than zero;
Wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
6), granulation: adopt the spray granulating and drying tower to make the particulate material that out of roundness is good, mobile performance is good, the loose specific weight of raw material is at 1.20～1.40g/cm3 usually, and angle of repose (flow angle) is smaller or equal to 30 degree, and pellet moisture content is in 0.5wt%;
Mn-Zn ferrite with this method production, initial permeability was more than 3000 when magnetic core possessed 23 ℃, initial permeability is a benchmark during simultaneously with 23 ℃, in-20～150 ℃ scope the rate of change of initial permeability 15% with interior, saturation flux density 23 ℃ the time more than 540mT.
The invention has the beneficial effects as follows: the initial permeability variation is little in wide temperature range, saturation flux density is high for this example, can bring stability to the digital amplifier that uses under the big condition of variations in temperature and the work loop of communication equipment.
Description of drawings
The temperature variant curve chart of initial permeability that Fig. 1 forms for the CoO content;
The temperature variant curve chart of initial permeability when Fig. 2 changes for main formula
Embodiment
Embodiment 1: a kind of Mn-Zn series soft magnetic ferrite, and mainly by Fe
2O
3, Mn
3O
4Form with ZnO, wherein Mn
3O
4Calculate with MnO, press Fe
2O
3: 54.1mol%, MnO:37.1mol% and ZnO:8.8mol% measure, mix, and give the burning stove with push type and give burning (950 ℃ * 2 hours), through 20 minutes pulverizing, add alloy: SiO again
2: 0.005wt%, CaO:0.04wt%, Nb
2O
5: 0.02wt%, V
2O
5: 0.05wt%, alloy wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
The CoO that adds simultaneously alloy such as following table 1 again drops into sand mill, and (CoOwt% is meant with respect to Fe in the table 1
2O
3, Mn
3O
4Total weight ratio with ZnO.)
Add additive according to following ratio: deionization pure water: 40～50wt%, binding agent: 0.5～1.5wt%, dispersant: 0.1～0.5wt% and defoamer: 0.1wt% greater than zero, carries out sand milling with interior and value, and additive wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Carry out drying-granulating about 100 ℃ with the mist projection granulating tower.Form, in the control partial pressure of oxygen, carry out sintering with prepared raw material, obtain external diameter and be 22mm, internal diameter and be 14mm, highly be the annular sample of 8mm with 1300 ℃ * 5 hours heat-retaining condition.With LCR and B-H analyzer the initial permeability of sample ring is measured (magnetic field intensity during mensuration is 800A/m) with variation of temperature rate and saturation flux density, measurement result is charged to table 1 respectively, is made the characteristic curve of Fig. 1.
Table 1:
The explanation of embodiment 1:, form suitable example 1,2,3 and comparative example 1,2 in the table 1 respectively according to the difference of CoO content; Wherein be suitable for example 1,2,3 and be CoO content within the scope of the present invention, comparative example 1,2 be CoO content not within the scope of the present invention.
Initial permeability was more than 3000 when these three suitable addition all can satisfy 23 ℃ as can be seen from The above results, initial permeability is a benchmark during simultaneously with 23 ℃, in-20～150 ℃ scope the rate of change of initial permeability 15% with the performance requirement of saturation flux density more than 540mT interior, 23 ℃ the time.But the tracing pattern that wherein is suitable for example 2 is the most desirable, thinks that this addition is an optimum addition.When the addition of CoO is less than the scope of application, its effect can be not too obvious, initial permeability when causing 23 ℃ is low, phenomenon with the poor stability of variation of temperature rate, when the addition of CoO surpasses this scope as can be seen in addition, initial permeability in the time of 23 ℃ takes place significantly to descend, and-20～150 ℃ rate of change also bigger fluctuation can take place.
Embodiment 2
According to the prescription of following table 2 high-purity Fe
2O
3, Mn
3O
4, ZnO carries out proportioning, gives the burning condition and still adopts push type to give to burn stove and gave burning in 950 ℃ * 2 hours, adopts 20 minutes pulverizing equally;
Add alloy SiO
2: 0.005wt%), CaO:0.04wt%, Nb
2O
5: 0.02wt% and V
2O
5: 0.05wt%, alloy wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Also add alloy CoO:0.3wt%, CoOwt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Add additive: deionization pure water: 40～50wt%, binding agent: 0.5～1.5wt%, dispersant: 0.1～0.5wt% and defoamer: 0.1wt% with interior and value greater than zero; Carry out sand milling, additive wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
Carry out drying-granulating about 100 ℃ with the mist projection granulating tower.Form, in the control partial pressure of oxygen, carry out sintering with prepared raw material, obtain external diameter and be 22mm, internal diameter and be 14mm, highly be the annular sample of 8mm with 1300 ℃ * 5 hours heat-retaining condition.Same method is estimated, and charges to the rate of change saturation flux density and time peak temperature of initial permeability, initial permeability in table 2.Temperature characterisitic makes curve chart 2.
Table 2:
The explanation of embodiment 2: being suitable for example 4,5,6,7 is the example of different main formulas with comparative example 3,4, and different main formulas cause time peak temperature difference, and what promptly table 2 was explained is because the characteristic variations that the main formula difference causes.
Wherein be suitable for Fe in the example 4,5,6,7
2O
3, MnO and ZnO within the scope of the present invention, Fe in the comparative example 3,4
2O
3, MnO and ZnO not within the scope of the present invention.
From table 2 and Fig. 2 as can be seen, the inferior peak temperature that is suitable for example 4～7 is in 10～50 ℃ scope, and initial permeability is more than 3000 can obtain 23 ℃ the time, initial permeability is a benchmark during simultaneously with 23 ℃, in-20～150 ℃ scope the rate of change of initial permeability 15% with the electric property of saturation flux density more than 540mT interior, 23 ℃ the time, initial permeability when exceeding 23 ℃ of the prescriptions of the scope of application is low, and magnetic permeability is big with the variation of temperature rate.
By to the use amount of alloy and the abundant self-criticism of main formula, when inferior peak temperature exceeds 10～50 ℃ scope, bigger fluctuation will take place in temperature variation curve, the rate of change that the initial permeability that makes 23 ℃ is low, wide temperature range is interior also changes thereupon, so the present invention is set in the secondary peak temperature range in 10～50 ℃ the scope, in this scope, can satisfy the room temperature magnetic permeability greater than the rate of change of initial permeability in 3000 ,-20～150 ℃ the scope 15% with the performance requirement of saturation flux density more than 540mT interior, 23 ℃ the time.Be that its main formula scope is Fe
2O
3: 53.7～54.4mol%, MnO:36～38mol% and ZnO:8～10mol%.
On the basis of above-mentioned main formula, added certain SiO simultaneously
2, CaO, Nb
2O
5, V
2O
5, alloy such as CoO.Wherein, SiO
2Make grain boundary layer produce higher impedance layer, reduce eddy current loss with common interpolation of CaO; Nb
2O
5With SiO
2, CaO precipitate into grain boundary layer simultaneously, except reducing also can to reduce remanent magnetism the loss; V
2O
5Can suppress owing to adopt Nb
2O
5The generation of intragranular pore that causes and unusual crystallization to promote saturation flux density, reduces remanent magnetism.The use of CoO can make the characteristic variations rate in the wide temperature range reduce.
Production technology of the present invention is simple, can promote the degree height, and the material property of being produced is good and stable, meets the demand of industry development.
Binding agent described in this example is generally polyvinyl alcohol.
Present embodiment 1 described wt% is meant with respect to Fe
2O
3, Mn
3O
4Total weight ratio with ZnO.
The consumption of deionization pure water, binding agent, dispersant and each additive of using during sand milling of defoamer is a same domain technical staff common practise again.
Claims (5)
1. a Mn-Zn series soft magnetic ferrite is characterized in that: mainly by Fe
2O
3, Mn
3O
4Form with ZnO, wherein Mn
3O
4Calculate with MnO, its proportion is: Fe
2O
3: 53.7～54.4mol%, MnO:36～38mol% and ZnO:8～10mol%.
2. Mn-Zn series soft magnetic ferrite according to claim 1 is characterized in that: also add alloy SiO simultaneously
2, CaO, Nb
2O
5, and V
2O
5, its suitable doping scope is: SiO
2: 0.005～0.01wt%, CaO:0.03～0.06wt%, Nb
2O
5: 0.01～0.03wt% and V
2O
5: 0.01～0.06wt%; Wt% is meant the total weight ratio with respect to Fe203, Mn304 and ZnO.
3. Mn-Zn series soft magnetic ferrite according to claim 1 and 2, it is characterized in that: alloy also has CoO, and its suitable doping scope is: CoO:0.05～0.6wt%, wt% are meant the total weight ratio with respect to Fe2O3, Mn3O4 and ZnO.
4. the production method of a Mn-Zn series soft magnetic ferrite is characterized in that:
1), weighing: correctly weigh each raw-material weight by aforementioned proportion;
2), mix: the raw material after the weighing is put into the dry type vibratory ball mill successively, carry out mixing in 20～30 minutes, require to mix, do not have tangible aberration;
3), give burning: the raw material input push type that mixes is given firing, give the burning temperature and be set at 850～1100 ℃, it is 2～5 hours that high temperature gives the burning time;
4), pulverize: adopt vibrator to carry out 10～40 minutes pulverizing, make it comment equal particle directly to reach below the 2.5 μ m giving the powder that burns down;
5), sand milling: in sand mill, drop into an amount of powder, drop into the impurity that measures in advance, and drop into the sand milling that following additives deionization pure water, polyvinyl alcohol, dispersant and defoamer carry out meticulous pulverizing, by 40～80 minutes grindings averaged particles is directly reached below the 2.2 μ m;
6), granulation: adopt the spray granulating and drying tower to make the particulate material that out of roundness is good, mobile performance is good, the loose specific weight of raw material is at 1.20～1.40g/cm3 usually, and angle of repose is smaller or equal to 30 degree, and pellet moisture content is in 0.5wt%.
5. Mn-Zn series soft magnetic ferrite according to claim 1, it is characterized in that: magnetic core initial permeability in the time of 23 ℃ is more than 3000, initial permeability is a benchmark during simultaneously with 23 ℃, in-20～150 ℃ scope the rate of change of initial permeability 15% with interior, saturation flux density 23 ℃ the time more than 540mT.
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|---|---|---|---|
| CNA200710019719XA CN101241793A (en) | 2007-02-06 | 2007-02-06 | Mn-Zn soft magnetic ferrite and production method |
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|---|---|---|---|
| CNA200710019719XA CN101241793A (en) | 2007-02-06 | 2007-02-06 | Mn-Zn soft magnetic ferrite and production method |
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|---|---|
| CN101241793A true CN101241793A (en) | 2008-08-13 |
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| CN107001150A (en) * | 2014-12-25 | 2017-08-01 | 日立金属株式会社 | The manufacture method and MnZn based ferrites of MnZn based ferrites |
| CN107973598A (en) * | 2017-12-01 | 2018-05-01 | 常熟市三佳磁业有限公司 | A kind of manufacture method of manganese-zinc ferrite core |
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| CN107001150A (en) * | 2014-12-25 | 2017-08-01 | 日立金属株式会社 | The manufacture method and MnZn based ferrites of MnZn based ferrites |
| CN107001150B (en) * | 2014-12-25 | 2021-03-09 | 日立金属株式会社 | Method for producing MnZn ferrite, and MnZn ferrite |
| CN105712714A (en) * | 2015-03-31 | 2016-06-29 | 浙江安特磁材有限公司 | Rubber-plastic ferrite magnetic powder and preparation method thereof |
| CN109311763A (en) * | 2017-04-12 | 2019-02-05 | 杰富意化学株式会社 | Rod-shaped MnZn FERRITE CORE and its manufacturing method and antenna |
| CN107973598A (en) * | 2017-12-01 | 2018-05-01 | 常熟市三佳磁业有限公司 | A kind of manufacture method of manganese-zinc ferrite core |
| CN109705807A (en) * | 2018-12-17 | 2019-05-03 | 安徽华林磁电科技有限公司 | A kind of electromagnetic absorption composite material |
| CN112382456A (en) * | 2020-11-12 | 2021-02-19 | 南通三优佳磁业有限公司 | Preparation method of soft magnetic ferrite material for power converter of hybrid electric vehicle |
| CN112382456B (en) * | 2020-11-12 | 2022-02-22 | 南通三优佳磁业有限公司 | Preparation method of soft magnetic ferrite material for power converter of hybrid electric vehicle |
| CN112645702A (en) * | 2020-12-15 | 2021-04-13 | 越峰电子(广州)有限公司 | Wide-frequency wide-temperature high-permeability Mn-Zn ferrite material and preparation method and application thereof |
| CN112645702B (en) * | 2020-12-15 | 2023-12-08 | 越峰电子(广州)有限公司 | Mn-Zn ferrite material with wide frequency, wide temperature range and high magnetic conductivity as well as preparation method and application thereof |
| CN114959610A (en) * | 2022-05-30 | 2022-08-30 | 陕西工业职业技术学院 | Parallel arm type three-free cooperative driving type film glancing angle sputtering platform |
| CN114959610B (en) * | 2022-05-30 | 2023-08-22 | 陕西工业职业技术学院 | Parallel arm type three-freedom cooperative driving thin film glancing angle sputtering platform |
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