CN101219891B - Solvent-thermal production method of self-assembling submicron sphere of magnetic vectolite - Google Patents
Solvent-thermal production method of self-assembling submicron sphere of magnetic vectolite Download PDFInfo
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- CN101219891B CN101219891B CN2008100069444A CN200810006944A CN101219891B CN 101219891 B CN101219891 B CN 101219891B CN 2008100069444 A CN2008100069444 A CN 2008100069444A CN 200810006944 A CN200810006944 A CN 200810006944A CN 101219891 B CN101219891 B CN 101219891B
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Abstract
The invention belongs to a technical field of preparation process of nanometer magnetic material, which provides a solvent thermal preparation method of magnetic self-assembly submicron spheres of cobalt ferrite, which comprises the following processes: trivalent ferric salts of 5 to 15 weight portions and bivalent cobalt salts of 5 to 15 weight portions are mixed; either of sodium acetate or sodium hydroxide of 15 to 30 weight portions is added; oleic acid of 150 to 200 weight portions is added; polyol of 150 to 200 weight portions is added; transparent liquid is obtained through magnetic stirring; the solution is filled in a high-pressure reaction vessel and sealed for reaction for 8 to 20 hours under 180 to 200 DEG C; after washed with water and ethanol in turn, the product is centrifugally separated and dried, and the magnetic self-assembly submicron sphere powders of CoFe2O4 are obtained. The method provided by the invention has low reaction temperature, and the obtained product has single phase; the method can prepare cobalt ferrite micron spheres of directional self-assembly nanometer particles and is suitable for industrial production of large output.
Description
Technical field
The invention belongs to magnetic Nano material fabricating technology field, particularly relate to a kind of solvothermal preparation method of magnetic vectolite self-assembly sub-micron ball.
Background technology
Vectolite (CoFe
2O
4) have high saturation magnetization, remanence intensity, bigger coercive force, and have favorable mechanical performance and chemical stability, these character that vectolite is used widely in fields such as magnetic recording, senser element, magnetic fluids.
At present synthetic high-quality magnetic Nano material the most extensive employing be liquid-phase synthesis process, wherein be divided into synthetic two kinds of organic synthesis and water again.The organic synthesis method is pyrolytic decomposition metal organic precursor body in the presence of the stablizer in organic solvent normally, its speed of response is fast, the magnetic nano crystal crystallization degree of gained is good, the size homogeneous, but this method condition harshness, the solvent that uses and stablizer expensive, and poisonous, operating environment is had relatively high expectations and easily physical environment is polluted; And aqueous phase synthesis method is a kind of method of the most ancient synthesizing magnetic material; usually utilize ferric iron and divalent cobalt ion under basic solution and 60～70 ℃, to carry out the co-precipitation gained by stoichiometric ratio; aqueous phase synthesis method mild condition close friend; simple to operate and be easy to scale preparation; but the factor that building-up process need be controlled is more, as water temperature, iron concentration, pH value etc.With above-mentioned organic synthesis method ratio, the deficiency of its maximum is that the water synthetic product is polydisperse, the distribution of sizes broad, and the state of aggregation of degree of crystallinity and nanoparticle is relatively poor, and the state of aggregation of nanoparticle and size are the principal elements that influences its character.
Summary of the invention
In view of above defective, the invention provides a kind of solvothermal preparation method of magnetic vectolite self-assembly sub-micron ball, adopt the vectolite self-assembly sub-micron ball diameter of the magnetic of this method acquisition to be about nanometer more than 100, form by directed self-assembly by the little vectolite nanoparticle about a large amount of 10 nanometers, and this method temperature of reaction is lower, the products therefrom thing is mutually single, is suitable for the bigger industrial production of output.
In order to reach above purpose, the solvothermal preparation method of this kind magnetic vectolite self-assembly sub-micron ball provided by the invention may further comprise the steps:
A. at first getting the trivalent iron salt of 5-15 parts by weight and the divalent cobalt of 5-15 parts by weight mixes, and then add the sodium-acetate of 15-30 parts by weight or in the sodium hydroxide any one, the oleic acid that adds the 150-200 parts by weight, add the polyvalent alcohol of 150-200 parts by weight, become transparent liquid through magnetic agitation;
B. above-mentioned gained solution is packed in the autoclave, airtight, 180-200 ℃ reaction 8-20 hour, product is after water and ethanol wash successively, and centrifugation, drying promptly get magnetic CoFe
2O
4Self-assembly sub-micron ball powder.
Wherein, above-mentioned trivalent iron salt can be iron trichloride, ferric sulfate, iron nitrate etc.;
Above-mentioned trivalent iron salt is preferably 1: 1 weight ratio with divalent cobalt to be mixed;
Above-mentioned divalent cobalt can be cobaltous acetate, cobalt chloride, rose vitriol, Xiao Suangu etc.;
Above-mentioned polyvalent alcohol can be ethylene glycol, glycerol etc.;
The purity of mentioned reagent is preferably analytical pure.
Described solvent-thermal method is meant in special closed reactor high pressure autoclave, adopts organic solvent as reaction system, by to the reaction system heating, produces the environment of a High Temperature High Pressure and a kind of effective means of carrying out material preparation in reaction system.In solvent-thermal method, solvent can play two effects: the medium agent of pressure and the medium of chemical reaction owing to be in high-temperature high-pressure state in reaction.Under high pressure, most reactants all fully (or part) be dissolved in organic solvent, can make to be reflected near carrying out in the homogeneous phase, thereby add the carrying out of fast response.Specific to this synthetic route, this is reflected in the high voltage bearing autoclave and carries out because reaction system is airtight, when temperature of reaction be higher than when adding the boiling point of organic solvent, will build a kind of reaction environment of High Temperature High Pressure.The reaction environment of this High Temperature High Pressure helps improving the solubleness of reactant in solvent, accelerate speed of reaction, improve the degree of crystallinity of product.
Oleic adding is also for the directed self-assembly decisive role of nanoparticle among the present invention.In the methods of the invention, oleic acid is as a kind of tensio-active agent, and a hydrophilic end of its molecule is adsorbed on the cobalt ferrite nanoparticle, and hydrophobic one end then points to the periphery.Under the solvent thermal condition, because just the surface energy of the cobalt ferrite nanoparticle that forms is very high,, stablize self in order to reduce surface energy, the cobalt ferrite nanoparticle that these oleic acid moleculars are wrapped in can flock together.If there is not the guide effect of oleic acid molecular, this gathering will be at random, direction-free.Hydrophilic end just because of oleic acid molecular is adsorbed on the cobalt ferrite nanoparticle, and hydrophobic one end then points to the periphery, and this just makes that the gathering of cobalt ferrite nanoparticle can not be random, but a kind of directed self-assembly under the assistance of oleic acid molecular is assembled.
In sum, the solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball provided by the invention, this method temperature of reaction is lower, and the products therefrom thing is mutually single, can make the cobalt ferrite microballoon of directed self-assembled nanometer particle, be suitable for the bigger industrial production of output.
Description of drawings
Fig. 1 is the transmission electron microscope photo of products obtained therefrom in the specific embodiment 1 of solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball provided by the invention;
Fig. 2 is the selected area electron diffraction style of products obtained therefrom in the specific embodiment 1 of solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball provided by the invention.
Embodiment
Below in conjunction with the drawings and the specific embodiments technical scheme of the present invention is further specified, but the qualification of the present invention of not opposing:
Embodiment 1
By weight 15: 15: 30: take by weighing iron trichloride at 150: 200, cobaltous acetate, sodium-acetate, oleic acid, ethylene glycol, mix after magnetic agitation becomes the orange transparent liquid, then this solution is packed in the autoclave, airtight, reaction is 10 hours under 180 ℃ of conditions, product is after water and ethanol wash successively, centrifugation, dry, products obtained therefrom is through powder x-ray diffraction (XRD), transmission electron microscope (as shown in Figure 1) is characterized by uniform vectolite self-assembly sub-micron ball, in addition, the selected area electron diffraction style of gained vectolite self-assembly sub-micron ball as shown in Figure 2.
Embodiment 2
By weight 10: 14: 20: take by weighing iron nitrate, cobaltous acetate, sodium-acetate, oleic acid, ethylene glycol at 150: 180, mix after magnetic agitation becomes the orange transparent liquid, then this solution is packed in the autoclave, airtight, reaction is 20 hours under 180 ℃ of conditions, product after water and ethanol wash successively, centrifugation, drying, products obtained therefrom is characterized by uniform vectolite self-assembly sub-micron ball through powder x-ray diffraction (XRD), transmission electron microscope (TEM).
Embodiment 3
By weight 5: 5.5: 30: take by weighing iron trichloride, cobaltous acetate, sodium hydroxide, oleic acid, ethylene glycol at 150: 200, mix after magnetic agitation becomes the orange transparent liquid, then this solution is packed in the autoclave, airtight, reaction is 8 hours under 200 ℃ of conditions, product after water and ethanol wash successively, centrifugation, drying, products obtained therefrom is characterized by uniform vectolite self-assembly sub-micron ball through powder x-ray diffraction (XRD), transmission electron microscope (TEM).
Claims (4)
1. the solvothermal preparation method of a magnetic vectolite self-assembly sub-micron ball is characterized in that, may further comprise the steps:
A. at first getting the trivalent iron salt of 5-15 parts by weight and the divalent cobalt of 5-15 parts by weight mixes, and then add the sodium-acetate of 15-30 parts by weight or in the sodium hydroxide any one, the oleic acid that adds the 150-200 parts by weight, the polyvalent alcohol that adds the 150-200 parts by weight, become transparent liquid through magnetic agitation, wherein, described trivalent iron salt is any one in iron trichloride, ferric sulfate, the iron nitrate, and described divalent cobalt is any one in cobaltous acetate, cobalt chloride, rose vitriol, the Xiao Suangu;
B. above-mentioned gained solution is packed in the autoclave, airtight, 180-200 ℃ reaction 8-20 hour, product is after water and ethanol wash successively, and centrifugation, drying promptly get magnetic CoFe
2O
4Self-assembly sub-micron ball powder.
2. the solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball according to claim 1 is characterized in that described polyvalent alcohol is any one in ethylene glycol, the glycerol.
3. the solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball according to claim 1 and 2 is characterized in that the purity of described reagent is analytical pure.
4. the solvothermal preparation method of a kind of magnetic vectolite self-assembly sub-micron ball according to claim 1 is characterized in that, the trivalent iron salt among the described step a is that 1: 1 weight ratio is mixed with divalent cobalt.
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| CN2008100069444A CN101219891B (en) | 2008-01-25 | 2008-01-25 | Solvent-thermal production method of self-assembling submicron sphere of magnetic vectolite |
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| CN2008100069444A CN101219891B (en) | 2008-01-25 | 2008-01-25 | Solvent-thermal production method of self-assembling submicron sphere of magnetic vectolite |
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| CN101219891A CN101219891A (en) | 2008-07-16 |
| CN101219891B true CN101219891B (en) | 2010-09-15 |
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| CN102583567B (en) * | 2012-01-09 | 2013-11-27 | 中国科学院金属研究所 | Superfine high-dispersion super-paramagnetism ferrate nano particles and preparation method thereof |
| CN106219610B (en) * | 2016-07-02 | 2017-09-01 | 烟台鑫洋电子有限公司 | A kind of preparation method of Conjugate ferrite nano magnetic material |
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