CN101320607A - Preparation method of ferroferric oxide/multi-wall carbon nano-tube magnetic nanometer composite material - Google Patents
Preparation method of ferroferric oxide/multi-wall carbon nano-tube magnetic nanometer composite material Download PDFInfo
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- CN101320607A CN101320607A CNA2008100351500A CN200810035150A CN101320607A CN 101320607 A CN101320607 A CN 101320607A CN A2008100351500 A CNA2008100351500 A CN A2008100351500A CN 200810035150 A CN200810035150 A CN 200810035150A CN 101320607 A CN101320607 A CN 101320607A
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Abstract
The invention relates to a preparation method of the magnetic nanometer composite material of ferroferric oxide and multi-walled carbon nanometer tube. The method utilizes MWCNTs, ethylene glycol, ferricchloride and sodium acetate as the starting material, adopts the polyethylenimine of the cationic surfactant to process the surface modification of MWCNTs, adds polyethylene glycol and polyvinylpyrrolidone of dispersant, adopts the alcohol-thermal method to prepare Fe3O4/MWCNTs magnetic nanometer composite material. By changing the proportion of MWCNTs and ferricchloride, the Fe3O4/MWCNTs magnetic nanometer composite material with different compositions can be obtained. The prepared Fe3O4/MWCNTs magnetic nanometer composite material has the advantages of excellent magnetic performance and conductive performance, simple synthetic process and production equipment, and easily achieving the industrial production.
Description
Technical field
The invention belongs to the nano composite material preparation field, particularly relate to a kind of tri-iron tetroxide (Fe
3O
4The preparation method of)/multi-walled carbon nano-tubes (MWCNTs) magnetic nanometer composite material.
Background technology
Magnetic nano-particle has physical effects such as skin effect, small-size effect, quantum size effect and macroscopic quantum tunneling effect because of it, the characteristic of novelties such as the superparamagnetism that is produced, highfield irreversibility and high saturation magnetic field makes magnetic Nano material be widely used in industrial production fields such as magnetic recording, instrument, magnetic resonance video picture as a kind of special functional material, and in high-tech areas such as biological targeting material, bio-separation, immobilised enzymes wide application prospect is arranged also.
Carbon nano-tube (Carbon nanotubes, CNTs) have performances such as particular structure, electricity, mechanics, Chu Qing because of it, so in many frontiers such as nano electron device, superpower composite material, hydrogen storage material, catalyst carrier prospect that has a very wide range of applications.Carbon nano-tube is a kind of monodimension nanometer material of hollow structure, has higher draw ratio, therefore assemble the magnetic metal oxide/carbon nano tube compound material of 1-dimention nano level, make its excellent specific property that possesses carbon nano-tube and nano magnetic material simultaneously, become one of research focus.Reports such as Cheng Jipeng make iron ion be adsorbed on [journal of Zhejiang university (engineering version), 676,40, [4], (2006)] on the oxidized carbon nano-tube by liquid phase method, after 600 ℃ of annealing, make Fe then in nitrogen atmosphere
3O
4/ CNTs composite material; Reports such as Wan Miao adopt the liquid phase oxidation method of reducing to prepare MnO
2/ CNTs composite material [Materials Science and Engineering journal, 601,23, [5], (2005)]; Liu etc. have reported with the solvent-thermal method in-situ preparing NiFe
2O
4/ CNTs composite material [Carbon, 47,43, (2005)]; Reports such as Cao are by the synthetic Ni that makes of hydro-thermal
0.75Zn
0.25Fe
2O
4/ CNTs magnetic composite [Journal of Macromolecular Science, Part B:Physics, 541,45, (2006)]; Reports such as Yu Huarong adopt liquid-phase chemistry deposition technique to prepare Fe
2O
3/ CNTs composite material [Chinese Journal of Inorganic Chemistry, 1651,21, [11], (2005)].This shows that carbon nano-tube magnetic nanometer composite material is gathered around in industry and high-tech area because of the various performances of its uniqueness and had broad application prospects.Yet because carbon nano tube surface does not have functional groups, it is earlier carbon nano-tube to be carried out acidifying with high concentration strong acid or nitration mixture that conventional method prepares this type of nano composite material, thereby makes it contain that electronegative functional groups such as carboxyl is realized and magnetic nano-particle compound.But in the acidization of carbon nano-tube, the structure of nanotube and unique electricity mechanical property thereof can be by heavy damages, and therefore how destroying carbon nanometer tube particular structure and electricity mechanical property do not have to be solved always in preparation carbon nano-tube magnetic nanometer composite material process.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material, to solve prior art defective such as the structure of destroying carbon nanometer tube and electricity mechanical property easily in preparation carbon nano-tube magnetic nanometer composite material process.It is raw material that this method adopts MWCNTs and high iron chloride, to carrying out surface modification, synthesizes Fe by pure thermal synthesis method preparation by polymine
3O
4/ MWCNTs magnetic nanometer composite material, preparation method's technology is simple, is easy to suitability for industrialized production, and the magnetic nanometer composite material that obtains has good magnetic performance, and characteristics such as conduct electricity very well.
The preparation method of a kind of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material of the present invention may further comprise the steps:
(1) surface modification of multi-walled carbon nano-tubes (MWCNTs)
Getting the cationic surfactant polymine is dissolved in the methanol solution, be mixed with the polymine methanol solution, add MWCNTs then, ultrasonic dispersion 20～60min, magnetic agitation 12～18h, wherein, the mass ratio of polymine and multi-walled carbon nano-tubes is 1: 1～3: 1, polymine is adsorbed on the MWCNTs surface, MWCNTs is carried out surface modification, make the MWCNTs surface have a large amount of positive charges;
(2) the synthetic Fe of pure hot method
3O
4/ MWCNTs magnetic nanometer composite material
At room temperature, the MWCNTs after the modification is added in the reactor, add high iron chloride (FeCl again
36H
2O), anhydrous sodium acetate, ethylene glycol, polyethylene glycol, polyvinylpyrrolidone, 300～500 rev/mins are stirred 20～40min down it are dissolved fully, and above-mentioned mixed solution is poured in the reactor, are warming up to 180～220 ℃, reaction 8～12h; Reaction finishes the back and uses the magnet collecting reaction product, and uses the deionized water wash product, at 50～80 ℃ of following vacuumize 20～28h, obtains nanometer Fe subsequently
3O
4/ MWCNTs composite material.
Methanol solution in the described step (1) is the methanol aqueous solution of 98～99.9wt%.
Polymine concentration of methanol solution in the described step (1) is 10～25wt%.
High iron chloride consumption in the described step (2) is 100～200% of a MWCNTs quality, the anhydrous sodium acetate consumption is 240～300% of a high iron chloride quality, the ethylene glycol consumption is 1/2～3/4 of a reactor volume, the polyethylene glycol consumption is 1/50～1/20 of an ethylene glycol volume, and the polyvinylpyrrolidone consumption is 0.07～3% of a MWCNTs quality.
Described nanometer Fe
3O
4Particle diameter is 20～200nm.
Method of the present invention makes that the excellent specific property of carbon nano-tube is kept fully.Polymine has effect unique as a kind of water soluble polymer cationic surfactant aspect the modified carbon nano-tube.In methanol solution, polymine is easy to be adsorbed on carbon nano tube surface, makes carbon nano tube surface have a large amount of positive charges.Ethylene glycol is the reproducibility organic solvent, can make part Fe
3+Be reduced into Fe
2+, while polymine and Fe
2+, Fe
3+Produce complexing, Fe
2+, Fe
3+Be adsorbed on the MWCNTs, and generate Fe with the at high temperature pure thermal response of the carbanion of anhydrous sodium acetate
3O
4Nano particle; The Fe that generates
3O
4It is electronegative that great amount of hydroxy group is contained on the surface, thereby a large amount of Fe
3O
4Nano particle is adsorbed on the MWCNTs by electrostatic attraction, prepares magnetic carbon-nano tube composite material, and adding dispensed in small quantity agent polyethylene glycol and polyvinylpyrrolidone prevent nanometer Fe in this external building-up process
3O
4Particle agglomeration.Not only exclusive structure and the electricity mechanical property of MWCNTs kept fully in this process, and the electrical property of composite material can have further raising.Beneficial effect of the present invention:
(1) uses cationic surfactant, to the acidification of MWCNTs, make the unique texture of MWCNTs and excellent properties not wreck in the abandoning tradition technology;
(2), can obtain the different nanometer Fe of forming by changing the ratio of MWCNTs and high iron chloride
3O
4/ MWCNTs magnetic nanometer composite material;
(3) prepared nanometer Fe
3O
4The magnetic property of/MWCNTs magnetic nanometer composite material and electric conductivity excellence;
(4) and synthesis technique and required production equipment simple, be easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is Fe
3O
4The X-ray diffractogram of/MWCNTs magnetic nanometer composite material.
Fig. 2 is Fe
3O
4/ MWCNTs magnetic nanometer composite material transmission electron microscope photo.
Fig. 3 is Fe
3O
4The volt-ampere curve figure that/MWCNTs magnetic nanometer composite material electric performance test is drawn.
Fig. 4 is Fe
3O
4/ MWCNTs magnetic nanometer composite material magnetic hysteresis loop figure.
Fig. 5 is Fe
3O
4/ MWCNTs magnetic nanometer composite material magnetism testing photo.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing the 2g polymine and be dissolved in 18g methanol aqueous solution (99.5wt%), be mixed with 10wt% polymine methanol solution, take by weighing 1g MWCNTs again and add above-mentioned solution, ultrasonic dispersion 30min, magnetic agitation 12h at room temperature then, reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs of modification.The MWCNTs of above-mentioned modification is added three-neck flask, add 50ml ethylene glycol, the high iron chloride of 1.35g, 3.6g water sodium acetate, 1ml polyethylene glycol, 0.01g polyvinylpyrrolidone again, at revolution is to stir 30min under the 350r/min, high iron chloride and anhydrous sodium acetate are dissolved fully, again above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 12h.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 24h, obtain Fe
3O
4/ MWCNTs magnetic nanometer composite material.
Fig. 1 is the Fe that present embodiment became
3O
4The X-ray diffractogram of/MWCNTs magnetic nanometer composite material can be seen Fe
3O
4With the diffraction maximum of MWCNTs, show that this composite material is Fe
3O
4/ MWCNTs nano composite material.
Fig. 2 is Fe
3O
4/ MWCNTs magnetic nanometer composite material transmission electron microscope photo, as can be seen: lot of F e
3O
4Nano particle is adsorbed on the carbon nano-tube, and particle diameter is in 20～200nm scope.
Fig. 3 is Fe
3O
4The volt-ampere curve figure that/MWCNTs magnetic nanometer composite material and MWCNTs are drawn behind electric performance test, as can be seen: Fe
3O
4The conductivity of/MWCNTs magnetic nanometer composite material is significantly improved than the conductivity of carbon nano-tube.
Fig. 4 is Fe
3O
4The magnetic hysteresis loop figure of/MWCNTs nano composite material, as can be seen: the magnetization of nano composite material is very high, and coercive force is bigger.
Fig. 5 is Fe
3O
4/ MWCNTs magnetic nanometer composite material magnetism testing photo, the magnetic induction sensitivity of nano composite material is very strong as can be seen.
Embodiment 2
Take by weighing the 1.5g polymine and be dissolved in 13.5g methanol aqueous solution (99.5wt%), be mixed with 10wt% polymine methanol solution, take by weighing 1.5g MWCNTs again and add above-mentioned solution, ultrasonic dispersion 30min, magnetic agitation 15h at room temperature then, reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs of modification.The MWCNTs of above-mentioned modification is added three-neck flask, add 55ml ethylene glycol, the high iron chloride of 2g, 5.4g anhydrous sodium acetate, 2ml polyethylene glycol, 0.015g polyvinylpyrrolidone again, at revolution is mechanical agitation 30min under the 450r/min, high iron chloride and anhydrous sodium acetate are dissolved fully, again above-mentioned solution is poured in the reactor, be warming up to 220 ℃, reaction 9h.Question response finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 24h, obtain Fe
3O
4/ MWCNTs magnetic nanometer composite material.
The X ray test result shows that this composite material is Fe
3O
4/ MWCNTs nano magnetic composite materials.Transmission electron microscope observing shows lot of F e
3O
4Nano particle is adsorbed on the carbon nano-tube.Conductivity test shows Fe
3O
4The conductivity of/MWCNTs magnetic composite is significantly improved than the conductivity of carbon nano-tube.The magnetic hysteresis loop figure of this nano composite material shows that the magnetization of composite material is very high, and coercive force is bigger.
Embodiment 3
Take by weighing the 3g polymine and be dissolved in 27g methanol aqueous solution (99.5wt%), be mixed with 10wt% polymine methanol solution, take by weighing 2gMWCNTs again and add above-mentioned solution, ultrasonic dispersion 30min, magnetic agitation 15h at room temperature then, reaction finishes the back carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs of modification.The MWCNTs of above-mentioned modification is added three-neck flask, add 45ml ethylene glycol, the high iron chloride of 2.7g, 7.2g water sodium acetate, 1.5ml polyethylene glycol, 0.015g polyvinylpyrrolidone again, at revolution is to stir 30min under the 400r/min high iron chloride and anhydrous sodium acetate are dissolved fully, again above-mentioned solution is poured in the reactor, be warming up to 210 ℃, reaction 10h.Question response finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 24h, obtain Fe
3O
4/ MWCNTs magnetic nanometer composite material.
The X ray test result shows that this composite material is Fe
3O
4/ MWCNTs composite material, electron microscopic observation show lot of F e
3O
4Nano particle is adsorbed on the carbon nano-tube, conductivity test shows Fe
3O
4The conductivity of/MWCNTs magnetic nanometer composite material is significantly improved than the conductivity of carbon nano-tube, and the magnetic field intensity of the magnetic hysteresis loop figure test shows nano composite material of this nano composite material is very high, and coercive force is bigger.
Take by weighing the 4g polymine and be dissolved in 36g methanol aqueous solution (99.5wt%), be mixed with 10wt% polymine methanol solution, take by weighing 2gMWCNTs again and add above-mentioned solution, ultrasonic dispersion 30min, magnetic agitation 12h at room temperature then, reaction finishes carbon pipe suspension is carried out suction filtration, washing, drying, obtains the MWCNTs of modification.MWCNTs after the above-mentioned modification is added three-neck flask, add 50ml ethylene glycol, the high iron chloride of 3.3g, 8.1g water sodium acetate, 1ml polyethylene glycol, 0.025g polyvinylpyrrolidone again, under revolution 500r/min, stir 30min, high iron chloride and anhydrous sodium acetate are dissolved fully, again above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 11h.Question response finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuumize 24h, obtain nanometer Fe
3O
4/ MWCNTs magnetic nanometer composite material.
The X ray test result shows that this composite material is Fe
3O
4/ MWCNTs composite material, transmission electron microscope observing show lot of F e
3O
4Nano particle is adsorbed on the carbon nano-tube, conductivity test shows Fe
3O
4The conductivity of/MWCNTs magnetic nanometer composite material is significantly improved than the conductivity of carbon nano-tube, and the magnetization of this nano composite material magnetic hysteresis loop figure test shows composite material is very high, and coercive force is bigger.
Claims (5)
1. the preparation method of a tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material may further comprise the steps:
(1) surface modification of multi-walled carbon nano-tubes MWCNTs
The cationic surfactant polymine is dissolved in the methanol solution, be made into the polymine methanol solution, add MWCNTs then, ultrasonic dispersion 20～60min, magnetic agitation 12～18h, wherein, the mass ratio of polymine and multi-walled carbon nano-tubes is 1: 1～3: 1, polymine is adsorbed on the MWCNTs surface, MWCNTs is carried out surface modification, make the MWCNTs surface have a large amount of positive charges;
(2) the synthetic Fe of pure hot method
3O
4/ MWCNTs magnetic nanometer composite material
At room temperature, MWCNTs after the modification is added in the reactor, add high iron chloride, anhydrous sodium acetate, ethylene glycol, polyethylene glycol, polyvinylpyrrolidone again, 300～500 rev/mins are stirred 20～40min down it are dissolved fully, above-mentioned mixed solution is poured in the reactor, be warming up to 180～220 ℃, reaction 8～12h;
Reaction finishes the back and uses the magnet collecting reaction product, and uses the deionized water wash product, at 50～80 ℃ of following vacuumize 20～28h, obtains nanometer Fe subsequently
3O
4/ MWCNTs composite material.
2. the preparation method of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material according to claim 1, it is characterized in that: the methanol solution in the described step (1) is the methanol aqueous solution of 98～99.9wt%.
3. the preparation method of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material according to claim 1, it is characterized in that: the polymine concentration of methanol solution in the described step (1) is 10～25wt%.
4. the preparation method of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material according to claim 1, it is characterized in that: the high iron chloride consumption in the described step (2) is 100～200% of a MWCNTs quality, the anhydrous sodium acetate consumption is 240～300% of a high iron chloride quality, the ethylene glycol consumption is 1/2～3/4 of a reactor volume, the polyethylene glycol consumption is 1/50～1/20 of an ethylene glycol volume, and the polyvinylpyrrolidone consumption is 0.07～3% of a MWCNTs quality.
5. the preparation method of tri-iron tetroxide/multi-wall carbon nano-tube magnetic nanometer composite material according to claim 1 is characterized in that: described nanometer Fe
3O
4Particle diameter is 20～200nm.
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