CN102276246A - Method for preparing cobalt ferrite nanometer granules by mechanical force chemical method - Google Patents
Method for preparing cobalt ferrite nanometer granules by mechanical force chemical method Download PDFInfo
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- CN102276246A CN102276246A CN201110203198XA CN201110203198A CN102276246A CN 102276246 A CN102276246 A CN 102276246A CN 201110203198X A CN201110203198X A CN 201110203198XA CN 201110203198 A CN201110203198 A CN 201110203198A CN 102276246 A CN102276246 A CN 102276246A
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- cobalt ferrite
- cobalt
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Abstract
The invention relates to a method for preparing spinel magnetic cobalt ferrite nanometer granules by mechanical force chemistry. The method comprises the following steps of: weighing a proper amount of cobalt salt, ferric salt and citric acid in a certain molar ratio; adding the mixture into a proper amount of absolute ethanol, mixing uniformly, and adding zirconium balls to ensure that a mass ratio of the balls to the materials is 2:1; loading the prepared ball materials into a high-energy planetary mill jar, and grinding at the speed of between 200 and 600 revolutions/minute to obtain wet gel under the action of grinding mechanical force for 5 to 10 hours; and drying the wet gel at the temperature of 100 DEG C, putting into a high-temperature furnace, and calcining at the temperature of 500 DEG C for 4 hours to obtain the spinel magnetic cobalt ferrite nanometer granules. A chemical formula of cobalt ferrite is CoxFeyO4, wherein the sum of x and y is equal to 3, the average crystallite dimension is between 40 and 100 nanometers, the cobalt ferrite is in a spherical shape or a regular tetrahedral shape or a regular octahedral shape, and the saturation magnetization intensity is between 25 and 60 electromagnetic units/gram. The method has the advantages of simple process, and low energy consumption; production links are easy to control and industrial production is easy to realize; and the problems of high cost and energy consumption, complex process and the like in the prior art are solved.
Description
Technical field
The invention belongs to the magnetic Nano material field, be specifically related to magnetic cobalt ferrite nanoparticles of a kind of spinel type and preparation method thereof.
Background technology
The magnetic vectolite of spinel structure is the soft magnetic materials of excellent property, has unique physical property, chemical property and magnetic property.Often they are used as magnetic recording material, stealthy absorbing material, magnetic cooling key problem in technology material and biomedical material etc., all have a wide range of applications in fields such as aviation, electronics, metallurgy, chemical industry, biology, medical science and environmental protection.At present, prepare ferritic method and mainly contain sol-gel method, chemical coprecipitation, hydrothermal method, solid reaction process etc., patent CN101486492A discloses a kind of method for preparing spinel type ferrite with chemical coprecipitation, by the sodium hydroxide precipitate metal ion, carry out hydrothermal treatment consists then and realize producing; Patent CN1837141A is manganese nodule or cobalt-bearing crust ore and fusing assistant mixed grinding, dewaters then, processing such as oven dry, high-temperature calcination, chemical subtraction, thereby obtains spinel type ferrite.Among these preparation methods, the subject matter of existence is that production process complexity, cost height, productive rate are low etc., can't satisfy industrial production requirement.
Summary of the invention
The objective of the invention is to overcome the shortcoming and the weak point of prior art, provide that a kind of production process is simple, productive rate is high, the magnetic cobalt ferrite nanoparticles preparation method of pollution-free, the spinel structure that is easy to realize suitability for industrialized production.
The molecular formula of the magnetic vectolite of a kind of spinel structure provided by the present invention is: Co
xFe
yO
4, x+y=3, the mean sizes of crystal grain is: 40～100nm, granular size is the hundreds of nanometer, has the shape characteristic of sphere, positive tetrahedron, regular octahedron.
The preparation method of the magnetic cobalt ferrite nanoparticles of spinel structure provided by the invention may further comprise the steps:
(1) takes by weighing an amount of cobalt, iron and citric acid by certain molar ratio, mix as cobalt chloride, iron nitrate and citric acid;
(2) mixture in the step (1) is added in an amount of dehydrated alcohol, adds the zirconium ball of certain mass, make that the mass ratio of ball material is 2: 1;
(3) the ball material for preparing is packed in the high-energy planetary mill mill jar, and the planetary mills revolution is 200r/min～600r/min, and milling time is 5h～10h, material is subjected to the grinding of mechanical force to issue biochemical reaction in the mill jar, pour out slurry then,, obtain xerogel with 100 ℃ of oven dry;
(4) xerogel is put into High Temperature Furnaces Heating Apparatus, calcine 4h under 500 ℃ the condition, can obtain the magnetic vectolite nanoparticle of spinel type.
Compared with prior art, characteristics of the present invention are: do raw material with soluble metal salt and citric acid, make xerogel by the mechanical force and chemical effect, calcining at a lower temperature, prepared the magnetic cobalt ferrite nanoparticles of spinel type, average grain size has the shape characteristic of sphere, positive tetrahedron, regular octahedron at 40～100nm, and saturation magnetization is controlled to be 25～60emu/g.Preparation method of the present invention is simple, safety, low, the less energy consumption of cost, is fit to suitability for industrialized production, and the magnetic vectolite particle of the spinel structure that is obtained can be applied in fields such as medical, biological, civilian and military projects.
Description of drawings
Fig. 1 is the XRD spectra of product
Fig. 2 is products C o
2FeO
4SEM figure
Fig. 3 is products C oFe
2O
4SEM figure
Fig. 4 is products C o
1.5Fe
1.5O
4SEM figure
Fig. 5 is products C o
2FeO
4Magnetic hysteresis loop
Fig. 6 is products C oFe
2O
4Magnetic hysteresis loop
Fig. 7 is products C o
1.5Fe
1.5O
4Magnetic hysteresis loop
Embodiment
The XRD of all products adopts the Y500 type x-ray diffractometer test of Chinese Dandong ray instrument company among the listed embodiment of the present invention, SEM adopts the high and low vacuum sem test of the U.S. Quanta-200 of Fei company type, and magnetic property adopts the MPMS-XL-7 type superconductive quantum interference magnetic measurement system testing of U.S. Quantum Design company.
(1) be to take by weighing cobalt chloride 11.904g, iron nitrate 10.213g and citric acid 21.206g at 1: 2 by the molar ratio of iron and cobalt;
(2) pour an amount of dehydrated alcohol into, add the zirconium ball of certain mass then, make that the mass ratio of ball material is 2: 1;
(3) the planetary mills revolution being set is 200r/min, and grinding 5h in planetary mills, material by mechanical force generation chemical reaction, take out slurry then in planetary mills, 100 ℃ of oven dry, obtains xerogel;
(4) xerogel is put into High Temperature Furnaces Heating Apparatus, calcine 4h under 500 ℃ the condition, can obtain the magnetic nano-particle Co of spinel type
2Fe0
4, as shown in Figure 2, product is a regular octahedron shape, and grain-size is about 47.6nm, and Fig. 5 is the magnetic hysteresis loop of this product, and saturation magnetization is 26.9emu/g.
Embodiment 2
(1) be to take by weighing cobalt chloride 5.965g, iron nitrate 20.188g and citric acid 21.320g at 2: 1 by the molar ratio of iron and cobalt;
(2) pour an amount of dehydrated alcohol into, add the zirconium ball of certain mass then, make that the mass ratio of ball material is 2: 1;
(3) the planetary mills revolution being set is 400r/min, and grinding 8h in planetary mills, material by mechanical force generation chemical reaction, take out slurry then in planetary mills, 100 ℃ of oven dry, obtains xerogel;
(4) xerogel is put into High Temperature Furnaces Heating Apparatus, calcine 4h under 500 ℃ the condition, can obtain the magnetic nano-particle CoFe of spinel type
2O
4, as shown in Figure 3, product is spherical, and grain-size is about 57nm, and Fig. 6 is the magnetic hysteresis loop of this product, and saturation magnetization is 51.3emu/g.
Embodiment 3
(1) be to take by weighing cobalt chloride 11.904g, iron nitrate 20.185g and citric acid 21.324g at 1: 1 by the molar ratio of iron and cobalt;
(2) pour an amount of dehydrated alcohol into, add the zirconium ball of certain mass then, make that the mass ratio of ball material is 2: 1;
(3) the planetary mills revolution being set is 600r/min, and grinding 10h in planetary mills, material by mechanical force generation chemical reaction, take out slurry then in planetary mills, 100 ℃ of oven dry, obtains xerogel;
(4) xerogel is put into High Temperature Furnaces Heating Apparatus, calcine 4h under 500 ℃ the condition, can obtain the magnetic nano-particle Co of spinel type
1.5Fe
1.5O
4, as shown in Figure 4, product is a positive tetrahedron shape, and grain-size is about 84.5nm, and Fig. 7 is the magnetic hysteresis loop of this product, and saturation magnetization is 57.8emu/g.
Claims (4)
1. a spinel type magnetic nano-particle is characterized in that, the chemical formula of described vectolite is: Co
xFe
yO
4, wherein, x+y=3, the mean sizes of crystal grain is: 40～100nm.
2. spinel type magnetic cobalt ferrite nanoparticles according to claim 1 is characterized in that the pattern that particle shows is sphere, positive tetrahedron shape and regular octahedron shape, and saturation magnetization is 25～60emu/g.
3. according to claim 1, described spinel type magnetic vectolite nanometer particle process method is characterized in that may further comprise the steps:
(1) takes by weighing an amount of cobalt salt, molysite and citric acid according to certain molar ratio, mix, add an amount of dehydrated alcohol then, add the zirconium ball of certain mass again, make that the mass ratio of ball material is 2: 1;
(2) the ball material for preparing in the step (1) is packed in the high-energy planetary mill mill jar, planetary mills is with the speed rotation of 200r/min～600r/min, grinding machinery power effect 5h～10h makes it that wet gel that chemical reaction obtains take place, and then wet gel is dried into xerogel at 100 ℃;
(3) xerogel that obtains in the step (2) is calcined 4h under 500 ℃ condition, can obtain the magnetic vectolite of spinel type of the present invention.
4. preparation method according to claim 3 is characterized in that, the metal-salt described in the step (1) is the cobalt salt and the molysite of solubility, comprises hydrochloride, nitrate or the vitriol of cobalt or iron.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731078A (en) * | 2012-06-26 | 2012-10-17 | 武汉理工大学 | Octahedral porous cobalt ferrite material and its preparation method |
| CN103771538A (en) * | 2014-01-27 | 2014-05-07 | 石家庄铁道大学 | Low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder |
| CN104496456A (en) * | 2014-12-02 | 2015-04-08 | 北京科技大学 | Preparation method of cobalt ferrite magnetostrictive material |
| CN108102427A (en) * | 2017-12-29 | 2018-06-01 | 华南协同创新研究院 | A kind of sub-micron ceramic pigment color containing cobalt black and its preparation method and application |
| CN112047381A (en) * | 2019-06-05 | 2020-12-08 | 中国科学院大连化学物理研究所 | Cathode with crystal face preferentially exposed for solid oxide fuel cell and preparation method and application thereof |
| CN114835169A (en) * | 2022-05-24 | 2022-08-02 | 沈阳理工大学 | Spinel type ferrite, preparation method thereof and wave-absorbing material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786668A (en) * | 2010-01-13 | 2010-07-28 | 桂林理工大学 | Low-temperature preparation method of Co ferrite Nano powder |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101786668A (en) * | 2010-01-13 | 2010-07-28 | 桂林理工大学 | Low-temperature preparation method of Co ferrite Nano powder |
Non-Patent Citations (3)
| Title |
|---|
| 《电子元件与材料》 20101130 席国喜等 低热固相-溶胶凝胶法制备钴铁氧体的研究 第48-51页 1-4 第29卷, 第11期 * |
| 席国喜等: "低热固相–溶胶凝胶法制备钴铁氧体的研究", 《电子元件与材料》 * |
| 肖利等: "纳米CoFe2O4的制备中前驱体热分解过程研究", 《湖南工业大学学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731078A (en) * | 2012-06-26 | 2012-10-17 | 武汉理工大学 | Octahedral porous cobalt ferrite material and its preparation method |
| CN103771538A (en) * | 2014-01-27 | 2014-05-07 | 石家庄铁道大学 | Low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder |
| CN104496456A (en) * | 2014-12-02 | 2015-04-08 | 北京科技大学 | Preparation method of cobalt ferrite magnetostrictive material |
| CN108102427A (en) * | 2017-12-29 | 2018-06-01 | 华南协同创新研究院 | A kind of sub-micron ceramic pigment color containing cobalt black and its preparation method and application |
| CN108102427B (en) * | 2017-12-29 | 2020-10-09 | 华南协同创新研究院 | Submicron cobalt-containing black ceramic pigment and preparation method and application thereof |
| CN112047381A (en) * | 2019-06-05 | 2020-12-08 | 中国科学院大连化学物理研究所 | Cathode with crystal face preferentially exposed for solid oxide fuel cell and preparation method and application thereof |
| CN112047381B (en) * | 2019-06-05 | 2021-09-24 | 中国科学院大连化学物理研究所 | Cathode with crystal face preferentially exposed for solid oxide fuel cell and preparation method and application thereof |
| CN114835169A (en) * | 2022-05-24 | 2022-08-02 | 沈阳理工大学 | Spinel type ferrite, preparation method thereof and wave-absorbing material |
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