CN100336732C - Microwave synthetic method for water soluble magnetic cobalt-ferrite CoFe2O4 nano crystal - Google Patents
Microwave synthetic method for water soluble magnetic cobalt-ferrite CoFe2O4 nano crystal Download PDFInfo
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- CN100336732C CN100336732C CNB2006100256634A CN200610025663A CN100336732C CN 100336732 C CN100336732 C CN 100336732C CN B2006100256634 A CNB2006100256634 A CN B2006100256634A CN 200610025663 A CN200610025663 A CN 200610025663A CN 100336732 C CN100336732 C CN 100336732C
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Abstract
The present invention relates to a microwave synthetic method for water soluble magnetic cobalt ferrite CoFe2O4 nanocrystal. Water is used as solvent; bivalent cobalt salt and trivalent ferric salt are dissolved in the water; water soluble polyatomic alcohol is added as stabilizing agents; the pH value of a solution is adjusted to manufacture an alkaline reaction precursor solution; then, the precursor solution is filled in a hermetic polytetrafluoroethene tank; the precursor solution reacts in a microwave reactor with controllable temperature and controllable pressure to quickly synthesize the cobalt ferrite CoFe2O4 nanocrystal. The method of the present invention has the advantages of simple operation, mild condition and low cost; the cobalt ferrite CoFe2O4 nanocrystal of the synthetic product has the characteristics of good water solubility, high stability, strong magnetism, uniform size distribution, adjustable size, easy connection with biological macromolecules, etc.
Description
Technical field
The present invention relates to a kind of water-soluble magnetic vectolite CoFe
2O
4The microwave synthesis method of nanocrystal is a raw material with ferric iron and divalent cobalt, utilizes temperature control, pressure control microwave-assisted synthesis to prepare vectolite CoFe
2O
4Magnetic nano crystal belongs to the nano material preparation technical field.
Background technology
Vectolite CoFe
2O
4Body phase material is a kind of ferromagnetic compound.As nanometer vectolite CoFe
2O
4When particle diameter is about the 3-10 nanometer,, promptly in the presence of magnetic field, have magnetic, when magnetic field disappears, show as non magnetic because yardstick quantum effect and dielectric confinement effect make them show superparamagnetism matter.The material of this property is at Magnetic resonance imaging, and targeted drug is treated, biomolecules and cellular segregation, and clinical diagnosis is widely used.
Synthetic high-quality magnetic Nano material is (as Fe
3O
4, Fe
2O
3, MFe
2O
4, M=Co, Mn, Ni) 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 high temperature (200 ℃～300 ℃) decomposing metal organism presoma in the presence of the stablizer in organic solvent normally, as FeCup
3Cup:C
6H
5N (NO) O-, iron carbonyl Fe (CO)
5, Fe (acac)
3Ferric acetyl acetonade or with 2: 1 the mixture of mol ratio of corresponding cobalt, nickel, manganese organism presoma) (1.J.Am.Chem.Soc.1999,121,11595; 2.J.Am.Chem.Soc.2002,124,8204; 3.J.Am.Chem.Soc.2001,123,12798.), its speed of response is fast, and 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.The more important thing is that the nanocrystal surface that the organic synthesis method obtains adsorbs a large amount of hydrophobic nature stablizers, make it be insoluble in water, can not be directly used in biomarker.Must adopt the method for ligand exchange and coating, the surface of nanocrystal is modified to increase its wetting ability.Aqueous phase synthesis method is a kind of method of the most ancient synthesizing magnetic material, utilizes ferric iron and divalent cobalt ion to carry out the co-precipitation gained by stoichiometric ratio under basic solution and 60-70 ℃ usually.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, and iron concentration, pH value etc.With organic synthesis method ratio, the deficiency of its maximum is that water method synthetic product is polydisperse, the distribution of sizes broad, and degree of crystallinity is poor.This will have a strong impact on it and use, special application at biomedical sector.The development of nano biological medical technology, more and more higher to the requirement of magnetic nanoparticle, wish that it not only has good magnetic and also wishes to have good water-solubility, biocompatibility and dimensional homogeneity.But the at present traditional organic phase and the product of water phase synthesis method all can't satisfy these requirements.
Summary of the invention
The objective of the invention is to defective, a kind of water-soluble magnetic vectolite CoFe is provided at present water and organic synthesis method
2O
4The microwave synthesis method of nanocrystal, aqueous phase synthesizes high quality vectolite CoFe
2O
4Magnetic nano crystal has that resultant velocity is fast, a product good water solubility, advantage that monodispersity is good.
For achieving the above object, the present invention is solvent with water, divalent cobalt and trivalent iron salt is water-soluble, add water miscible polyvalent alcohol as stablizer, regulator solution pH value makes the alkali reaction precursor solution, then this precursor solution is placed airtight polytetrafluoroethyltank tank, but reacts in the microwave reactor of temperature controllable and pressure control, rapidly synthetic high quality (water-soluble, size homogeneous) 2nm～50nm vectolite CoFe
2O
4Magnetic nano crystal, its size distribution are at 10%-20%, and saturated magnetic intensity reaches 60emu/g-120emu/g.
Method of the present invention specifically comprises the steps:
1, reacting precursor formulations prepared from solutions:
With mol ratio is that 1: 2 divalent cobalt and trivalent iron salt is soluble in water, and iron salt concentration is controlled at the 0.001-1.0 mol.Add water miscible polyvalent alcohol as stablizer, the volume ratio of polyvalent alcohol and water was controlled at 1: 10 to 10: 1.Regulator solution pH value obtains precursor solution to 5-12.
2, the synthetic vectolite CoFe of microwave
2O
4Nanocrystal:
Above-mentioned precursor solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate vectolite CoFe
2O
4Nanocrystal.Microwave heating condition is: microwave oscillation frequency 300MHZ～3000MHZ, microwave power 50W～1000W, 1 minute～10 hours heat-up time, 50～250 degrees centigrade of Heating temperatures.
Trivalent iron salt of the present invention comprises iron nitrate, Iron triperchlorate, iron(ic) chloride, iron acetate, ferric sulfate etc.
Divalent cobalt of the present invention comprises Xiao Suangu, cobaltous perchlorate, Cobaltous diacetate, rose vitriol, cobalt chloride etc.
Water miscible polyvalent alcohol of the present invention comprises ethylene glycol, polyoxyethylene glycol, glycerol, 1,2-propylene glycol etc.
Method of the present invention is simple to operate, mild condition, and cost is low.Synthetic product vectolite CoFe
2O
4Nanocrystal has water-soluble and good stability, and magnetic property is strong, and uniform in size distribution is easily with characteristics such as biomacromolecule are connected.
Embodiment
Below by several specific embodiments technical scheme of the present invention is further described.Following examples do not constitute limitation of the invention.
Embodiment 1
1, reacting precursor formulations prepared from solutions:
With mol ratio is that 1: 2 cobalt chloride (divalence) and iron(ic) chloride is soluble in water, and concentration of iron is 0.01 mol, adds glycerol as stablizer, and the volume ratio of glycerol and water was controlled at 1: 1.Regulator solution pH value to 12.
2, the synthetic vectolite CoFe of microwave
2O
4Nanocrystal:
Above-mentioned precursor solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate vectolite CoFe
2O
4Nanocrystal.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ,
Microwave power: 400W,
Heat-up time: 4 hours,
Heating temperature: 140 degrees centigrade.
Embodiment 2
1, reacting precursor formulations prepared from solutions:
With mol ratio is that 1: 2 rose vitriol and ferric sulfate is soluble in water, and concentration of iron is 0.04 mol, adds ethylene glycol as stablizer, and the volume ratio of ethylene glycol and water was controlled at 1: 2.Regulator solution pH value to 8 obtains precursor solution.
2, the synthetic vectolite CoFe of microwave
2O
4Nanocrystal:
Above-mentioned precursor solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate vectolite CoFe
2O
4Nanocrystal.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ,
Microwave power: 600W,
Heat-up time: 30 minutes,
Heating temperature: 160 degrees centigrade.
Embodiment 3
1, reacting precursor formulations prepared from solutions:
With mol ratio is that 1: 2 nitric acid cobalt salt and nitric acid molysite is soluble in water, and iron salt concentration is 0.1 mol, adds polyoxyethylene glycol as stablizer, and polyoxyethylene glycol and water volume ratio were controlled at 1: 4.Regulator solution pH value to 10 obtains precursor solution.
2, the synthetic vectolite CoFe of microwave
2O
4Nanocrystal:
Above-mentioned precursor solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate vectolite CoFe
2O
4Nanocrystal.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ,
Microwave power: 100W,
Heat-up time: 2 hours,
Heating temperature: 200 degrees centigrade.
Claims (2)
1, a kind of water-soluble magnetic vectolite CoFe
2O
4The microwave synthesis method of nanocrystal is characterized in that comprising the steps:
1) reacting precursor formulations prepared from solutions: with mol ratio is that 1: 2 divalent cobalt and trivalent iron salt is soluble in water, iron salt concentration is controlled at the 0.001-1 mol, add water miscible polyvalent alcohol as stablizer, the volume ratio of polyvalent alcohol and water was controlled at 1: 10 to 10: 1, regulator solution pH value obtains precursor solution to 5-12;
2) the synthetic vectolite CoFe of microwave
2O
4Nanocrystal: above-mentioned precursor solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate vectolite CoFe
2O
4Nanocrystal; Wherein, microwave heating condition is: microwave oscillation frequency 300MHZ～3000MHZ, microwave power 50W～1000W, 1 minute～10 hours heat-up time, 50～250 degrees centigrade of Heating temperatures.
2, according to the water-soluble magnetic vectolite CoFe of claim 1
2O
4The microwave synthesis method of nanocrystal is characterized in that described trivalent iron salt is iron nitrate, Iron triperchlorate, iron(ic) chloride, iron acetate or ferric sulfate; Described divalent cobalt is Xiao Suangu, cobaltous perchlorate, Cobaltous diacetate, rose vitriol or cobalt chloride; Described water miscible polyvalent alcohol is ethylene glycol, polyoxyethylene glycol, glycerol or 1, the 2-propylene glycol.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173459B (en) * | 2011-01-28 | 2012-08-22 | 湖州师范学院 | Method for preparing yttrium ferrite nanometer powder by using microwaves |
| CN102531066A (en) * | 2011-02-24 | 2012-07-04 | 中国科学院福建物质结构研究所 | Spherical ferrate having hollow structure 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 |
| CN108723383B (en) * | 2017-04-13 | 2021-09-21 | 中国科学院金属研究所 | Controllable preparation method of multi-morphology iron-cobalt alloy magnetic nanoparticles with high saturation magnetic induction intensity |
| CN108383514A (en) * | 2018-03-13 | 2018-08-10 | 昆明理工大学 | A kind of preparation method of Nanosized Mn-Zn Ferrite powder |
| CN109021919B (en) * | 2018-07-09 | 2021-03-12 | 中南大学 | Preparation method and application of graphene/cobalt-nickel-manganese ferrite nanocomposite |
| CN114308047B (en) * | 2022-01-10 | 2022-11-01 | 濮阳市中汇新能源科技有限公司 | Light degradation material for organic wastewater |
Citations (4)
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| WO2000071465A1 (en) * | 1999-05-22 | 2000-11-30 | Henkel Kommanditgesellschaft Auf Aktien | Redispersable metal oxides and hydroxides with particle sizes in the nanometric size range |
| CN1378996A (en) * | 2002-05-17 | 2002-11-13 | 中国科学院上海硅酸盐研究所 | Process for synthesizing nano barium ferrite powder by microwave induction and low-temp combustion |
| JP2003277189A (en) * | 2002-03-20 | 2003-10-02 | Kazuyuki Taji | Fine particle powder of single crystal cobalt ferrite and method for producing the same |
| CN1657490A (en) * | 2005-02-07 | 2005-08-24 | 武汉理工大学 | Method for preparing cobalt ferrite by coprecipitation |
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Patent Citations (4)
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| WO2000071465A1 (en) * | 1999-05-22 | 2000-11-30 | Henkel Kommanditgesellschaft Auf Aktien | Redispersable metal oxides and hydroxides with particle sizes in the nanometric size range |
| JP2003277189A (en) * | 2002-03-20 | 2003-10-02 | Kazuyuki Taji | Fine particle powder of single crystal cobalt ferrite and method for producing the same |
| CN1378996A (en) * | 2002-05-17 | 2002-11-13 | 中国科学院上海硅酸盐研究所 | Process for synthesizing nano barium ferrite powder by microwave induction and low-temp combustion |
| CN1657490A (en) * | 2005-02-07 | 2005-08-24 | 武汉理工大学 | Method for preparing cobalt ferrite by coprecipitation |
Non-Patent Citations (3)
| Title |
|---|
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| 溶胶-凝胶法与微波燃烧法制备CoFe2O4纳米颗粒的比较研究 王丽等，磁性材料及器件，第36卷第6期 2005 * |
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