CN101708991A - Method for preparing barium ferrite with low coercive force temperature coefficient - Google Patents
Method for preparing barium ferrite with low coercive force temperature coefficient Download PDFInfo
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- CN101708991A CN101708991A CN200910219803A CN200910219803A CN101708991A CN 101708991 A CN101708991 A CN 101708991A CN 200910219803 A CN200910219803 A CN 200910219803A CN 200910219803 A CN200910219803 A CN 200910219803A CN 101708991 A CN101708991 A CN 101708991A
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- barium ferrite
- coercive force
- temperature coefficient
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- force temperature
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Abstract
The invention provides a method for preparing barium ferrite with a low coercive force temperature coefficient. To solve the contradiction existing in the application of the traditional barium ferrite material that the coercive force temperature coefficient is too big, namely the coercive force is of drastic variation with temperature, the invention utilizes the coprecipitation-molten-salt growth method and substitutes the ternary combination of Co2+, Zn2+ and Sn4+ or Co2+, Mn2+ and Sn4+ for Fe3+ to adjust the coercive force temperature coefficient and the coercive force. In the method, just by adjusting the mixing amount, the coercive force temperature coefficient of the barium ferrite can be effectively lowered, and the application potential of the barium ferrite can be widened; simultaneously, due to the adoption of the coprecipitation-molten-salt growth method in which molten potassium chloride is used as a solvent, the reaction temperature is lowered, the reaction time is shortened, the probability of hard agglomeration of products is reduced, and the Co2+, Zn2+ and Sn4+ or Co2+, Mn2+ and Sn4+ ternary combination substituted single phase barium ferrite is obtained; the obtained product is high in purity and good in crystalline phase; and the process is simple, steps are few, the operation is convenient, the energy is saved, and the industrialized production is realized, so that the method of the invention is a good method for preparing the barium ferrite with the low coercive force temperature coefficient.
Description
Technical field:
The present invention relates to a kind of preparation method of technical field of magnetic materials, a kind of specifically preparation method with low coercive force temperature coefficient barium ferrite.
Background technology
Barium ferrite is a hard ferrite, has six side's magnetoplumbite structures, belongs to P6
3/ mmc spacer.Since its high saturation and magnetic intensity, high-coercive force, high magnetocrystalline anisotropy and chemical stability, and barium ferrite and doped barium ferrite thereof can be made chip and be used as microwave material.As permanent magnet material, magnetic recording material, barium ferrite and doped barium ferrite thereof have caused the interest of Science and Technology research widely.
Advanced barium ferrite and doped barium Ferrite Material thereof provide high signal to noise ratio, support the high-density canned data.Because the information retention time is relevant with remanent magnetism, magnetic recording requires to have high coercive force.Regulate the magnetic performance of barium ferrite by mixing, can make it to adapt to needs of different applications.Too high coercive force can make magnetic head saturated, and therefore available adulterated method reduces the magnetocrystalline anisotropy of barium ferrite.Information is preserved by barium ferrite and the steady state of ferritic Jie of doped barium thereof.The steady state that is situated between changes in time.The variation that is situated between between the steady state needs heat energy to activate.
Cation doping is a cutting barium ferrite magnetic performance, so that it satisfies the requirement of different application.Different aerial Fe
3+Replaced by different positively charged ions, magnetic performance will be different.4f in the magnetoplumbite structure
IVAnd 4f
VIEmpty by Fe
3+Occupy.At 4f
IVAnd 4f
VIAerial Fe
3+Empty with other as 12K, 2a, the aerial Fe of 2b
3+Spin direction is opposite.Different positively charged ions tends to occupy different skies.Co
2+And Sn
4+Tend to occupy 2b, 4f
VIAnd 12k sky.2b, 4f
VIThere is material impact the position to the magnetocrystalline anisotropy of barium ferrite.Co-Sn enters 2b, 4f in the barium ferrite that Co-Sn replaces
VISky obviously reduces the magnetocrystalline anisotropy of barium ferrite.Zn
2+Be non magnetic ion, if replace the Fe of 2a and 12k position
3+To reduce magnetic saturation intensity, but replace 4f
IVAnd 4f
VIThe Fe of position
3+Magnetic saturation intensity is increased.Zn tends to replace 4f
IVFe in the position
3+Thereby, the magnetic saturation intensity of increase barium ferrite.Sn
4+Be substituted with and help change coercive force temperature coefficient.Cr
3+Occupy 2a, 4f
VI, and the 12k position magnetic saturation intensity is significantly reduced, but coercive force is increased.Except replacing Fe
3+In addition, positively charged ion enters the magnetic that other sky also can influence barium ferrite.Dopant ion can also change Fe
3+Thereby between hyperconjugation change the magnetic of barium ferrite.Except single component and two-component doped, also have three components to mix, as synthetic BaFe
9.6Co
0.8Ti
0.8M
0.8O
19Report.Synthetic method, synthesis condition and trace impurity all have material impact to the coercive force and the magnetic saturation intensity of barium ferrite in addition.As seen having a lot of different approaches can be used for the magnetic of cutting barium ferrite makes it be applicable to different purposes.But existing barium ferrite material exists coercive force temperature coefficient excessive when using, and promptly coercive force varies with temperature big problem.More existing reduce trials of barium ferrite coercive force temperature coefficient with binary doped method, but coercive force temperature coefficient appoint can not be reduced to zero.
Summary of the invention
Exist coercive force temperature coefficient excessive in order to solve existing barium ferrite material when using, promptly coercive force varies with temperature big problem, and a kind of preparation method with low coercive force temperature coefficient barium ferrite is provided, and this method is utilized Co
2+, Zn
2+, Sn
4+Or Co
2+, Mn
2+, Sn
4+Ternary is united and is replaced Fe
3+Regulate the size of coercive force temperature coefficient.With the anhydrous sodium carbonate is precipitation agent, and gained throw out suction filtration is washed to no Cl-, 80 ℃ of oven dry.Is solvent with co-precipitation-molten-salt growth method with fusion Repone K, take by weighing the acclimatization thing, and by weight 1: 1 ratio and solid potassium chloride grinding mixing, with the temperature rise rate of 15 ℃/min, heat-treated 2 hours being warming up to 450 ℃, be warming up to 950 ℃ and heat-treated 4 hours.The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry can obtain the single-phase barium ferrite product B of ternary doping aFe
12-2xCo
X/2Zn
X/2Sn
xO
19(x=0.1～2.0) and BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19(x=0.1～0.6).Products therefrom BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19(x=0.1～2.0) and BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19The coercive force temperature coefficient of (x=0.1～0.6) reduces with the increase of doping x.BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19When x=0.4, become negative value, BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19When x=0.6, become negative value.
This patent characteristic feature of an invention and beneficial effect: metal ion is to the Ba in the barium ferrite
2+Or Fe
3+Carry out monobasic or binary and replace the magnetic property that can effectively adjust barium ferrite, but to the influential report of coercive force temperature coefficient seldom.Utilize Co
2+, Zn
2+, Sn
4+Or Co
2+, Mn
2+, Sn
4+Ternary is united and is replaced Fe
3+Can regulate the barium ferrite coercive force temperature coefficient by the controlled doping amount, enlarge the barium ferrite application potential.Utilizing co-precipitation-molten-salt growth method is solvent with fusion Repone K, can reduce temperature of reaction, shortens the reaction times, reduces the chance of product hard aggregation, the product purity height that obtains, and crystalline phase is good.Present method just can reduce the barium ferrite coercive force temperature coefficient as long as regulate doping, and technology is simple, and step is few, and is easy to operate, and save energy can realize suitability for industrialized production, is the good method of preparation low coercive force temperature coefficient barium ferrite.
Description of drawings:
Figure 1B aFe
10.0Co
0.5Zn
0.5Sn
1.0O
19The XRD spectra of sample
Fig. 2 BaFe
10.0Co
0.5Zn
0.5Sn
1.0O
19The sem photograph of sample
Fig. 3 substitutes amount x to BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19The influence of magnetic coercive force temperature coefficient value
Fig. 4 BaFe
11.6Co
0.1Mn
0.1Sn
0.2O
19The XRD spectra of sample
Fig. 5 BaFe
11.6Co
0.1Mn
0.1Sn
0.2O
19The sem photograph of sample
Fig. 6 substitutes amount x to BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19The influence of magnetic coercive force temperature coefficient value
Embodiment:
A kind of preparation method with low coercive force temperature coefficient barium ferrite, doping can change barium ferrite magnetic performance and temperature, time relation, it is a kind of useful especially magnetic performance that coercive force does not vary with temperature, and therefore preparing the low coercive force temperature coefficient barium ferrite has the important use meaning.This patent is with Zn
2+, Co
2+, Sn
4+Be dopant ion, three components are united and are replaced Fe
3+Ion, wherein Co
2+: Zn
2+: Sn
4+Mol ratio be 1: 1: 2, Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) mol ratio be 1: 11, gained doped barium ferrite BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19The coercive force temperature coefficient of (x=0.1～2.0) reduces with the increase of doping x; BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19When x=0.4, become negative value; Used synthetic method is co-precipitation/molten-salt growth method: taking by weighing muriate by the product molecular formula and be dissolved in an amount of distilled water, is that precipitation agent generates precipitation with the sodium carbonate solution, and suction filtration is washed to no Cl
-, 80 ℃ of oven dry; Take by weighing the 2g throw out, and,, be warming up to 450 ℃ and heat-treated 2 hours, be warming up to 950 ℃ and heat-treated 4 hours with the temperature rise rate of 15 ℃/min by weight 1: 1 ratio and solid potassium chloride grinding mixing; The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry promptly get target product.With co-precipitation/molten-salt growth method synthetic doped barium ferrite BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19(x=0.1～2.0) are single-phase sexangle barium ferrite.
Perhaps with Mn
2+, Co
2+, Sn
4+Described dopant ion, three components are united and are replaced Fe
3+Ion, wherein Co
2+: Mn
2+: Sn
4+Mol ratio be 1: 1: 2, Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) mol ratio be 1: 11, gained doped barium ferrite BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19The coercive force temperature coefficient of (x=0.1～0.6) reduces with the increase of doping x; BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19When x=0.6, become negative value.With co-precipitation/molten-salt growth method synthetic doped barium ferrite BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19(x=0.1～0.6) is single-phase sexangle barium ferrite.
Concrete experiment is raw materials used: iron trichloride, bariumchloride, zinc chloride, cobalt chloride, manganous chloride, tindichloride and anhydrous sodium carbonate are analytical pure.Press BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19(x=0.1～2.0) or BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19(x=0.1～0.6) molecular formula, wherein Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) or Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) mol ratio be 1: 11.Take by weighing iron trichloride, bariumchloride, zinc chloride, cobalt chloride, manganous chloride, tindichloride and be dissolved in and stir under 70 ℃ of water-baths in the distilled water, form mixing solutions.Other gets excessive 60% anhydrous sodium carbonate and is dissolved in an amount of distilled water, stirs under 70 ℃ of water-baths.Above-mentioned mixing solutions is poured into rapidly in the sodium carbonate solution that continues to stir, continued to stir 1 hour, cooling and aging, suction filtration is washed to no Cl
-, 80 ℃ of oven dry.Take by weighing the acclimatization thing, and,, be warming up to 450 ℃ and heat-treated 2 hours, be warming up to 950 ℃ and heat-treated 4 hours with the temperature rise rate of 15 ℃/min by weight 1: 1 ratio and solid potassium chloride grinding mixing; The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry promptly get target product.
Embodiment 1:
Referring to Fig. 1-Fig. 2, press BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19Molecular formula takes by weighing 1 * 10
-2Mol BaCl
22H
2O, 9.17 * 10
-2Mol FeCl
36H
2O, 4.58 * 10
-3Mol ZnCl
2, 4.58 * 10
-3Mol CoCl
26H
2O, 9.17 * 10
-3Mol SnCl
22H
2O is dissolved in and stirs under 70 ℃ of water-baths in the distilled water, forms mixing solutions.Other gets 2.83 * 10
-1The mol anhydrous sodium carbonate is dissolved in an amount of distilled water, stirs under 70 ℃ of water-baths.Above-mentioned mixing solutions is poured into rapidly in the sodium carbonate solution that continues to stir, continued to stir 1 hour, cooling and aging, suction filtration is washed to no Cl
-, 80 ℃ of oven dry.Take by weighing the 2g throw out, and,, be warming up to 450 ℃ and heat-treated 2 hours, be warming up to 950 ℃ and heat-treated 4 hours with the temperature rise rate of 15 ℃/min by weight 1: 1 ratio and solid potassium chloride grinding mixing; The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry promptly get target product BaFe
10.0Co
0.5Zn
0.5Sn
1.0O
19Fig. 3 shows that alternative amount x is to BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19The influence curve of magnetic coercive force temperature coefficient value.
Embodiment 2:
Referring to Fig. 4-Fig. 5, press BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19Molecular formula takes by weighing 1 * 10
-2Mol BaCl
22H
2O, 1.06 * 10
-1Mol FeCl
36H
2O, 9.14 * 10
-4Mol ZnCl
2, 9.14 * 10
-4Mol CoCl
26H
2O, 1.83 * 10
-3Mol SnCl
22H
2O is dissolved in and stirs under 70 ℃ of water-baths in the distilled water, forms mixing solutions.Other gets 2.83 * 10
-1The mol anhydrous sodium carbonate is dissolved in an amount of distilled water, stirs under 70 ℃ of water-baths.Above-mentioned mixing solutions is poured into rapidly in the sodium carbonate solution that continues to stir, continued to stir 1 hour, cooling and aging, suction filtration is washed to no Cl
-, 80 ℃ of oven dry.Take by weighing the 2g throw out, and,, under (450 ℃, 2h)+(950 ℃, 4h), heat-treat with the temperature rise rate of 15 ℃/min by weight 1: 1 ratio and solid potassium chloride grinding mixing.The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry promptly get target product BaFe
11.6Co
0.1Mn
0.1Sn
0.2O
19Fig. 6 shows that alternative amount x is to BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19The influence curve of magnetic coercive force temperature coefficient value.
Claims (4)
1. preparation method with low coercive force temperature coefficient barium ferrite is with Zn
2+, Co
2+, Sn
4+Be dopant ion, three components are united and are replaced Fe
3+Ion, wherein Co
2+: Zn
2+: Sn
4+Mol ratio be 1: 1: 2, Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) mol ratio be 1: 11, gained doped barium ferrite BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19The coercive force temperature coefficient of (x=0.1～2.0) reduces with the increase of doping x; BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19When x=0.4, become negative value; Used synthetic method is co-precipitation/molten-salt growth method: taking by weighing muriate by the product molecular formula and be dissolved in an amount of distilled water, is that precipitation agent generates precipitation with the sodium carbonate solution, and suction filtration is washed to no Cl
-, 80 ℃ of oven dry; Take by weighing the acclimatization thing, and,, be warming up to 450 ℃ and heat-treated 2 hours, be warming up to 950 ℃ and heat-treated 4 hours with the temperature rise rate of 15 ℃/min by weight 1: 1 ratio and solid potassium chloride grinding mixing; The thermal treatment product is washed to no Cl again
-, 80 ℃ of oven dry promptly get target product.
2. a kind of preparation method with low coercive force temperature coefficient barium ferrite according to claim 1 is characterized in that: described with co-precipitation/molten-salt growth method synthetic doped barium ferrite BaFe
12-2xCo
X/2Zn
X/2Sn
xO
19(x=0.1～2.0) are single-phase sexangle barium ferrite.
3. a kind of preparation method with low coercive force temperature coefficient barium ferrite according to claim 1 is characterized in that: described dopant ion is Mn
2+, Co
2+, Sn
4+, three components are united and are replaced Fe
3+Ion, wherein Co
2+: Mn
2+: Sn
4+Mol ratio be 1: 1: 2, Ba
2+: (Fe
3++ Co
2++ Zn
2++ Sn
4+) mol ratio be 1: 11, gained doped barium ferrite BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19The coercive force temperature coefficient of (x=0.1～0.6) reduces with the increase of doping x; BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19When x=0.6, become negative value.
4. a kind of preparation method with low coercive force temperature coefficient barium ferrite according to claim 3 is characterized in that: described with co-precipitation/molten-salt growth method synthetic doped barium ferrite BaFe
12-2xCo
X/2Mn
X/2Sn
xO
19(x=0.1～0.6) is single-phase sexangle barium ferrite.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587971A (en) * | 2016-12-15 | 2017-04-26 | 陕西科技大学 | Multiferroic composite ceramics with softened magnetic hysteresis loops and preparation method for multiferroic composite ceramics |
| CN111116193A (en) * | 2019-12-25 | 2020-05-08 | 深圳顺络电子股份有限公司 | Microwave ferrite material and preparation method and device thereof |
-
2009
- 2009-11-11 CN CN200910219803A patent/CN101708991A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106587971A (en) * | 2016-12-15 | 2017-04-26 | 陕西科技大学 | Multiferroic composite ceramics with softened magnetic hysteresis loops and preparation method for multiferroic composite ceramics |
| CN111116193A (en) * | 2019-12-25 | 2020-05-08 | 深圳顺络电子股份有限公司 | Microwave ferrite material and preparation method and device thereof |
| CN111116193B (en) * | 2019-12-25 | 2022-05-10 | 深圳顺络电子股份有限公司 | Microwave ferrite material and preparation method and device thereof |
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Open date: 20100519 |