CN101786601B - Preparation method of compound nano particle with Fe3O4/CoO core shell structure - Google Patents

Preparation method of compound nano particle with Fe3O4/CoO core shell structure Download PDF

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CN101786601B
CN101786601B CN 201010130172 CN201010130172A CN101786601B CN 101786601 B CN101786601 B CN 101786601B CN 201010130172 CN201010130172 CN 201010130172 CN 201010130172 A CN201010130172 A CN 201010130172A CN 101786601 B CN101786601 B CN 101786601B
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coo
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composite nanoparticle
nucleocapsid structure
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CN101786601A (en
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刘福田
孙莉
陈秀秀
杨萍
姜庆辉
张爱玉
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University of Jinan
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Abstract

The invention belongs to the technical field of nano material preparation, in particular to a preparation method of a compound nano particle with a Fe3O4/CoO core shell structure. The invention has the technical scheme that the preparation method of the compound nano particle with the Fe3O4/CoO core shell structure comprises the following steps of: preparing a Fe3O4 particle and preparing a Fe3O4/CoO compound nano particle. In the invention, a core shell is prepared in one step by adopting a solvent thermal method; the method has simple operation and is easy to realize; moreover, residual solutions of reaction are alcohol and water respectively, and therefore, the residual solutions do not have toxin or pollution, and the performances of the magnetism aspect, the stability aspect and the like of the particle are improved. The compound nano particle shows higher stability and good magnetic property, and can be used as a magnetic drug carrier to be applied to the field of biomedicines.

Description

Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle
Technical field
The invention belongs to the nano material preparing technical field, relate in particular to Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle.
Background technology
Nanometer Fe 3O 4Be a kind of important spinel type ferrite, have the advantages such as preparation technology is simple, price is low, nontoxic, pollution-free, and it have widely purposes in actual applications.For example it has quick, the magnetic sensitive characteristic of superior air humidity, has broad application prospects in fields such as the contrast imaging of air humidity dependent sensor spare, high density magnetic recording material, nuclear magnetic resonance and medicine control releases; Have good magnetic responsiveness, decide the aspects such as enzyme, immunodiagnosis and neoplasm targeted therapy, DNA separation and nucleic acid hybridization in cell separation, curing and also have a wide range of applications; In addition, magnetic Nano Fe 3O 4As functional material, also demonstrate many specific functions at aspects such as the stock of magnetic recording material, special catalyst raw material, magnetic fluid and magnetic materials.But these are used great majority and require magnetic particle to have the particle size of chemical stability, homogeneous and good dispersiveness in liquid phase.Thereby because having the anisotropic dipole moment effect of high-specific surface area, high-ratio surface energy and particle, magnetic nano-particle is easy to reunite some magnetic particle such as Fe, Fe 3O 4Be easy to be oxidized to γ-Fe 2O 3Thereby, cause particle to occur to assemble and precipitation, can not form stable dispersion, its application in biomedicine is restricted.
Although the magnetic Nano material of physics or chemical method preparation can reach nano-scale, but its distribution of sizes is wider, and surface exposure, chemical property is active, easily oxidation in air, easily assemble, make magnetic material lose single domain magnetic pole, dispersibility or lose the distinctive character of nano material.Usually in order to make nano particle can be good at being scattered in the carrier fluid, need that particle is carried out surface modification and make particle surface absorption one layer of polymeric, thereby produce sterically hindered repulsion and overcome interparticle gravitation, by can improve the contact angles and wetting of these particles and other medium to the surface modification of particle, improve the dispersiveness of particulate in carrier fluid simultaneously.Therefore, to exposed nanocrystalline the protection, be vital with chemical method.Can reduce its surface energy by the finishing to magnetic nano-particle, improve the oxidation resistance of particle, obtain the nano-complex particle of good dispersion; Simultaneously, suitable finishing can be regulated compatibility and the response characteristic of magnetic nano-particle and other materials.Therefore, the finishing for magnetic nano-particle also is the focus of studying both at home and abroad at present [1-4]Nano particle after the finishing can improve the aerial stability of nano particle and biocompatibility to a great extent, is applied to widely the fields such as biological medicine, targeting vector, catalysis.
At Fe 3O 4Surface coating iron, cobalt oxide, nickel oxide, iron oxide prepare the existing more report of composite nanoparticle.Present Fe 3O 4/ CoO composite nanoparticle is mainly with pulse laser deposition method, sol-gal process preparation.C.A.kleint etc. (1998, J.APPL.PHYS) adopt the pulse laser deposition method at Fe 3O 4The surface has prepared CoO magnetic shell, and has inquired into Fe 3O 4The heat treatment of each crystal face of/CoO nucleocapsid structure, pulse laser deposition method need special instrument, and nano ferriferrous oxide is not easy to be uniformly dispersed in gas phase, easily so that the compound particle particle is larger.The sol-gal process complex process needs generation and the calcining of colloidal sol, and generating the higher and reaction of temperature needs hydrogen reducing usually, and power consumption is large.Have not yet to see with solvent-thermal method and prepare Fe 3O 4The report of/CoO.
Summary of the invention
The object of the invention is to, overcome the deficiencies in the prior art, provide a kind of preparation process simple, efficient is high, and magnetic property better, stability, dispersiveness Fe preferably 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle.It is higher at first to prepare magnetic property with solvent-thermal method, and dispersiveness is the nano ferriferrous oxide particle preferably; Then adopt equally solvent-thermal method to prepare that magnetic property is good, stability is higher, monodispersed Fe 3O 4/ CoO composite nanoparticle.
For solving the problems of the technologies described above, technical scheme of the present invention is:
Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle, described preparation method comprises the steps:
1) preparation nanometer Fe 3O 4Particle:
The preparation of a, predecessor is arranged on 65 ℃ and keep constant temperature with the water-bath water temperature, with FeCl 36H 2O and FeSO 47H 2O is dissolved in respectively in the mixed liquor solution of 50ml water and ethylene glycol; make respectively the solution that concentration is 0.15-0.4mol/L and 0.1-0.2mol/L; wherein the volume ratio of water and ethylene glycol is 1: 1-1: 3; with above-mentioned two kinds of solution in water-bath, mix and rapid stirring even; be added drop-wise to fast NaOH solution in the mixed liquor and simultaneously stirring; to pH value of solution be 6.5; slowly drip again NaOH to pH value be 7-9; add the surfactant enuatrol and the neopelex that account for reactant quality 1%-3%; static 30min after fully stirring under nitrogen protection makes nanometer Fe 3O 4The predecessor of particle;
B, magnetic particle prepare nanometer Fe 3O 4The predecessor of particle is transferred in the hydrothermal reaction kettle, at 150 ℃ of-180 ℃ of 6-8h of lower reaction time, after reaction is finished product is taken out, stir and ultrasonic dispersion 5-10min, then use distilled water and absolute ethyl alcohol cross washing, product at 50 ℃ of lower vacuum drying 10h, is namely got dry Fe 3O 4Magnetic nanoparticle;
Step 1) mol ratio of enuatrol and neopelex is 1: 2 among a.The purity of ethylene glycol is 99%.
2) preparation Fe 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, makes Co (CH 3COO) 24H 2O solution is got step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 3COO) 24H 2In the O solution, the washing drying obtains Fe after the reaction 3O 4/ CoO composite nanoparticle.
Step 2) absolute ethyl alcohol purity is 99.7% in.
Fe of the present invention 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle, step 2) described preparation Fe 3O 4/ CoO composite nanoparticle: with Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.03-0.05mol/L 3COO) 24H 2O solution is got 0.001-0.004mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, and the adding mass fraction is the ultrasonic Co (CH that is scattered in 100mL of polyvinylpyrrolidone of 1%-3% 3COO) 24H 2In the O solution, mixed liquor changed over to react 4-6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Fe of the present invention 3O 4/ CoO nucleocapsid structure is compound receives the preparation method of water particle, step 2) described preparation Fe 3O 4/ CoO composite nanoparticle: with Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.03-0.05mol/L 3COO) 24H 2O solution is got 0.001-0.004mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, adding simultaneously mass percent is the Co (CH of the ultrasonic 100mL of being scattered in of surfactant of 1%-3% 3COO) 24H 2In the O solution, mixed liquor changed over to react 4-6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.Surfactant is polyvinylpyrrolidone, enuatrol or neopelex.
Accompanying drawing 1 is Fe 3O 4The XRD collection of illustrative plates of magnetic nanoparticle, as seen from Figure 1 Fe 3O 4Each peak value of magnetic nanoparticle coincide, and purity is higher;
Accompanying drawing 2 is Fe 3O 4The AGM collection of illustrative plates of magnetic nanoparticle is by finding out Fe among Fig. 2 3O 4The magnetic nanoparticle superparamagnetism is good, saturation magnetization is higher;
Accompanying drawing 3 is Fe 3O 4The XRD collection of illustrative plates of/CoO nucleocapsid structure composite nanoparticle is as seen from Figure 3 except Fe 3O 4Characteristic peak the characteristic peak of CoO has also appearred outward, coated CoO;
Accompanying drawing 6 is Fe 3O 4The SEM figure of/CoO nucleocapsid structure composite nanoparticle.Be Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 4 o'clock, and the reaction time is 4 hours Fe that make 3O 4/ CoO nucleocapsid structure composite nanoparticle, dispersion is more even as seen from the figure, about tens nanometers of particle.
The invention has the beneficial effects as follows: the present invention adopts solvent-thermal method, and shell prepares a step to be finished, and is simple to operate, be easy to realize, and the reaction residual solution is alcohol and water, and nontoxic pollution-free also improves the performance of the aspects such as magnetic, stability of particle.This composite nanoparticle presents that stability is higher, magnetic property good, can be used as a kind of magnetic medicine carrier and is applied to biomedicine field.
Description of drawings
Accompanying drawing 1 is Fe 3O 4The XRD collection of illustrative plates of magnetic nanoparticle.
Accompanying drawing 2 is Fe 3O 4The AGM collection of illustrative plates of magnetic nanoparticle.
Accompanying drawing 3 is Fe 3O 4The XRD collection of illustrative plates of/CoO nucleocapsid structure composite nanoparticle.
Accompanying drawing 4 is 6 hours for the reaction time, Fe 3O 4With Co (CH 3COO) 24H 2The different mol ratio of O does not add the Fe that makes under the surfactant 3O 4/ CoO nucleocapsid structure composite nanoparticle and Fe 3O 4The contrast AGM collection of illustrative plates of magnetic nanoparticle, among the figure:
A0 is pure Fe 3O 4Magnetic nanoparticle;
A1 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 4;
A2 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 2;
A3 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 3: 4.
Accompanying drawing 5 is 4 hours for the reaction time, Fe 3O 4With Co (CH 3COO) 24H 2The different mol ratio of O adds the Fe that makes under the surfactant 3O 4/ CoO nucleocapsid structure composite nanoparticle and Fe 3O 4The contrast AGM collection of illustrative plates of magnetic nanoparticle, among the figure:
A0 is pure Fe 3O 4Magnetic nanoparticle;
A1 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 4;
A2 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 2;
A3 is Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 3: 4.
Accompanying drawing 6 is Fe 3O 4The SEM figure of/CoO nucleocapsid structure composite nanoparticle.
Below in conjunction with the drawings and specific embodiments to the detailed description of the invention:
The specific embodiment
Embodiment 1
Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle,
At first prepare nanometer Fe 3O 4Particle:
The preparation of a, predecessor is arranged on 65 ℃ and keep constant temperature with the water-bath water temperature, and the mixed liquor solution of preparation water and ethylene glycol (volume ratio of water and ethylene glycol is 1: 1-1: 3), and with FeCl 36H 2O and FeSO 47H 2O is dissolved in respectively the above-mentioned mixed liquor of 50mL; make the solution that concentration is respectively 0.15mol/L and 0.1mol/L; mixing and rapid stirring are even in water-bath; be added drop-wise to fast NaOH solution in the mixed liquor and simultaneously stirring; to pH value of solution be 6.5; slowly drip again NaOH to pH value be 8; add the surfactant enuatrol and the neopelex that account for reactant quality 2%; the mol ratio of enuatrol and neopelex is 1: 2; static 30min after fully stirring under nitrogen protection makes nanometer Fe 3O 4The predecessor of particle;
B, magnetic particle prepare nanometer Fe 3O 4The predecessor of particle is transferred in the hydrothermal reaction kettle, at 160 ℃ of 6h of lower reaction time, after reaction is finished product is taken out, stir and ultrasonic dispersion 5min, then use distilled water and absolute ethyl alcohol cross washing, product at 50 ℃ of lower vacuum drying 10h, is namely got dry Fe 3O 4Magnetic nanoparticle.
And then preparation Fe 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.001mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean adds mass fraction and is the Co (CH of 2% the ultrasonic 100mL of being scattered in of polyvinylpyrrolidone simultaneously 3COO) 24H 2In the O solution, change in the hydrothermal reaction kettle mixed liquor over to reaction 4 hours, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Embodiment 2
The preparation nanometer Fe 3O 4Particle prepares Fe according to method identical among the embodiment 1 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.002mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean adds mass percent and is the Co (CH of 2% the ultrasonic 100mL of being scattered in of polyvinylpyrrolidone simultaneously 3COO) 24H 2In the O solution, change in the hydrothermal reaction kettle mixed liquor over to reaction 4 hours, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Embodiment 3
The preparation nanometer Fe 3O 4Particle prepares Fe according to method identical among the embodiment 1 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.003mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean adds mass percent and is the Co (CH of 2% the ultrasonic 100mL of being scattered in of polyvinylpyrrolidone simultaneously 3COO) 24H 2In the O solution, change in the hydrothermal reaction kettle mixed liquor over to reaction 4 hours, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Accompanying drawing 5 is that embodiment 1,2 and 3 is at Fe 3O 4With Co (CH 3COO) 24H 2Add the Fe that surfactant makes under the different mol ratio of O 3O 4/ CoO nucleocapsid structure composite nanoparticle and Fe 3O 4The contrast AGM collection of illustrative plates of magnetic nanoparticle, among the figure:
A0 is pure Fe 3O 4Magnetic nanoparticle;
A1 is the Fe of embodiment 1 preparation 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure;
A2 is the Fe of embodiment 2 preparations 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure;
A3 is the Fe of embodiment 3 preparations 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure.
As can be seen from Figure 5, under the same reaction time conditions, Fe 3O 4With Co (CH 3COO) 24H 2The Fe that the different mol ratio of O makes 3O 4/ CoO nucleocapsid structure composite nanoparticle curve changes greatly by the contrast magnetic property, is converted into A1 better performances behind the specific saturation magnetization.
Embodiment 4
Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle,
At first prepare nanometer Fe 3O 4Particle:
The preparation of a, predecessor is arranged on 65 ℃ and keep constant temperature with the water-bath water temperature, and the mixed liquor solution of preparation water and ethylene glycol (volume ratio of water and ethylene glycol is 1: 1-1: 3), and with FeCl 36H 2O and FeSO 47H 2O is dissolved in respectively the above-mentioned mixed liquor of 50mL; make concentration and be respectively 0.4 and the solution of 0.2mol/L; mixing and rapid stirring are even in water-bath; NaOH solution is added drop-wise in the mixed liquor fast and stirs simultaneously, to pH value of solution be 6.5, slowly drip again NaOH to pH value be 8; add the surfactant enuatrol and the neopelex that account for reactant quality 2%; the mol ratio of enuatrol and neopelex is 1: 2, stirs 30min under nitrogen protection again, makes nanometer Fe 3O 4The predecessor of particle;
B, magnetic particle prepare nanometer Fe 3O 4The predecessor of particle is transferred in the hydrothermal reaction kettle, at 150 ℃ of-180 ℃ of 8h of lower reaction time, after reaction is finished product is taken out, stir and ultrasonic dispersion 10min, then use distilled water and absolute ethyl alcohol cross washing, product at 50 ℃ of lower vacuum drying 10h, is namely got dry Fe 3O 4Magnetic nanoparticle.
And then preparation Fe 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.001mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 100mL 3COO) 24H 2In the O solution, mixed liquor changed over to react 6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Embodiment 5
The preparation nanometer Fe 3O 4Particle prepares Fe according to method identical among the embodiment 4 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.002mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 100mL 3COO) 24H 2In the O solution, mixed liquor changed over to react 6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Embodiment 6
The preparation nanometer Fe 3O 4Particle prepares Fe according to method identical among the embodiment 4 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.04mol/L 3COO) 24H 2O solution is got 0.003mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 100mL 3COO) 24H 2In the O solution, mixed liquor changed over to react 6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
Accompanying drawing 4 is that embodiment 4,5 and 6 is at Fe 3O 4With Co (CH 3COO) 24H 2Do not add the Fe that makes under the surfactant under the different mol ratio of O 3O 4/ CoO nucleocapsid structure composite nanoparticle and Fe 3O 4The contrast AGM collection of illustrative plates of magnetic nanoparticle, among the figure:
A0 is pure Fe 3O 4Magnetic nanoparticle;
A1 is the Fe of embodiment 4 preparations 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure;
A2 is the Fe of embodiment 5 preparations 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure;
A3 is the Fe of embodiment 6 preparations 3O 4/ CoO nucleocapsid structure composite nanoparticle magnetization curve figure;
A1, A2, A3 are reaction 6h, do not add the differential responses thing proportioning Fe of surfactant 3O 4The AGM collection of illustrative plates of/CoO nucleocapsid structure composite nanoparticle, magnetic property changes greatly after coating by contrast, is converted into A1 better performances behind the specific saturation magnetization.The superparamagnetism of composite nanoparticle descends as seen from Figure 4, is the larger reason of particle that generates, and needs to add surfactant, changes Fe 3O 4, Co (CH 3COO) 24H 2The concentration of O is the reaction time when, to reach better magnetic performance and stability.
The superparamagnetism of finding out nucleocapsid structure from Fig. 4 and Fig. 5 is 4 hours good than the reaction time, and Fe 3O 4With Co (CH 3COO) 24H 2The mol ratio of O is 1: 4 o'clock, and saturation magnetization improves, than pure Fe 3O 4Saturation magnetization high.

Claims (7)

1.Fe 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: described preparation method comprises the steps:
1) preparation nanometer Fe 3O 4Particle:
The preparation of a, predecessor is arranged on 65 ℃ and keep constant temperature with the water-bath water temperature, with FeCl 36H 2O and FeSO 47H 2O is dissolved in respectively in the mixed liquor solution of 50ml water and ethylene glycol; make respectively the solution that concentration is 0.15-0.4mol/L and 0.1-0.2mol/L; wherein the volume ratio of water and ethylene glycol is 1: 1-1: 3; with above-mentioned two kinds of solution in water-bath, mix and rapid stirring even; be added drop-wise to fast NaOH solution in the mixed liquor and simultaneously stirring; to pH value of solution be 6.5; slowly drip again NaOH to pH value be 7-9; add the surfactant enuatrol and the neopelex that account for reactive material weight 1%-3%; under nitrogen protection, stir again 30min, make nanometer Fe 3O 4The predecessor of particle;
B, magnetic particle preparation are with nanometer Fe 3O 4The predecessor of particle is transferred in the hydrothermal reaction kettle, at 150 ℃ of-180 ℃ of 6-8h of lower reaction time, after reaction is finished product is taken out, stir and ultrasonic dispersion 5-10min, then use distilled water and absolute ethyl alcohol cross washing 6 times, product at 50 ℃ of lower vacuum drying 10h, is namely got dry Fe 3O 4Magnetic nanoparticle;
2) preparation Fe 3O 4/ CoO composite nanoparticle:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, makes Co (CH 3COO) 24H 2O solution is got step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 3COO) 24H 2In the O solution, the washing drying obtains Fe after the reaction 3O 4/ CoO composite nanoparticle.
2. Fe according to claim 1 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: step 2) described preparation Fe 3O 4/ CoO composite nanoparticle is specially:
With Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.03-0.05mol/L 3COO) 24H 2O solution is got 0.001-0.004mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, the ultrasonic Co (CH that is scattered in 100mL 3COO) 24H 2In the O solution, mixed liquor changed over to react 4-6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
3. Fe according to claim 1 and 2 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: step 2) described preparation Fe 3O 4/ CoO composite nanoparticle is specially: with Co (CH 3COO) 24H 2O is dissolved in the absolute ethyl alcohol, and making concentration is the Co (CH of 0.03-0.05mol/L 3COO) 24H 2O solution is got 0.001-0.004mol step 1) the middle Fe for preparing 3O 4The magnetic nanoparticle washes clean, adding simultaneously mass percent is the Co (CH of the ultrasonic 100mL of being scattered in of surfactant of 1%-3% 3COO) 24H 2In the O solution, mixed liquor changed over to react 4-6h in the hydrothermal reaction kettle, reactant is dry with absolute ethanol washing, obtain Fe 3O 4/ CoO nucleocapsid structure composite nanoparticle.
4. Fe according to claim 3 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: described surfactant is polyvinylpyrrolidone, enuatrol or neopelex.
5. Fe according to claim 1 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: step 1) mol ratio of enuatrol and neopelex is 1: 2 among a.
6. Fe according to claim 1 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: step 1) purity of ethylene glycol is 99% among a.
7. Fe according to claim 1 and 2 3O 4The preparation method of/CoO nucleocapsid structure composite nanoparticle is characterized in that: step 2) in absolute ethyl alcohol purity be 99.7%.
CN 201010130172 2010-03-23 2010-03-23 Preparation method of compound nano particle with Fe3O4/CoO core shell structure Expired - Fee Related CN101786601B (en)

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