CN101837971A - Method for preparing graphene/Fe3O4 composite powder by alcohol thermal method - Google Patents
Method for preparing graphene/Fe3O4 composite powder by alcohol thermal method Download PDFInfo
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- CN101837971A CN101837971A CN201010174907A CN201010174907A CN101837971A CN 101837971 A CN101837971 A CN 101837971A CN 201010174907 A CN201010174907 A CN 201010174907A CN 201010174907 A CN201010174907 A CN 201010174907A CN 101837971 A CN101837971 A CN 101837971A
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Abstract
The invention relates to a method for preparing graphene/Fe3O4 composite powder by an alcohol thermal method, which comprises the following steps of: (1) weighing oxidated graphite and ferric salt at room temperature, dispersing into a glycol solution, adding polyethylene glycol after dissolving completely, then adding anhydrous sodium acetate, stirring and forming reaction liquid; (2) putting into a reaction kettle, heating to the temperature of 180 to 220 DEG C and reacting for 8 to 16h; and (3) cooling to the room temperature, collecting a product by using a magnet, washing the product by deionized water and drying so as to obtain the graphene/Fe3O4 composite powder. In the invention, the preparation method is simple and is easy for industrialized production; and Fe3O4 in the prepared graphene/Fe3O4 composite powder has pure crystalline phase, little possibility of agglomeration, favorable compounding with graphene and good dispersibility at the surface of the graphene and in the layer of the graphene, and the composite powder has small resistivity and high magnetization intensity.
Description
Technical field
The invention belongs to Graphene/Fe
3O
4The preparation field of composite granule particularly relates to the standby Graphene/Fe of the hot legal system of a kind of alcohol
3O
4The method of composite granule.
Background technology
Graphene is found a kind of novel two dimensional surface carbon nanomaterial in 2004, the monoatomic layer structures shape that it is special it have abundant and novel physicals.In the past few years, Graphene has become the research focus that gets most of the attention.Studies show that characteristics such as Graphene has ultra-thin, super firm and superpower conductivity are expected to obtain widespread use in fields such as nano electron device, matrix material, energy storage and biomedicines.
Recent study person finds, graphene-based matrix material can significantly improve performances such as the hardness, specific conductivity of mixture.G.Williams etc. have reported on ACS Nano 2 (2008) 1487-1491 and have utilized TiO
2Photocatalysis reduction-oxidation graphite prepare Graphene/TiO
2Mixture, the TiO of 2.6～4nm
2Particle is attached on the graphene film that approximately 2.2nm is thick.Y.J.Kin etc. have reported on Applied Physics Letters 95 (2009) 213101-1-213101-3 and have utilized vapour phase epitaxy method to make ZnO nanometer rod vertical-growth on the Graphene surface.Y.Fan etc. have reported at Carbon 48 (2010) 1743-1749 and have adopted the standby Graphene/Al that obtains of mechanical ball milling legal system
2O
3Composite powder is with Al
2O
3Electrical conductivity improved 13～16 orders of magnitude.
In addition and since the ferrite excellent magnetism can with and at application potential biological, medicine and other fields, Graphene and ferritic mixture also receive much attention gradually.H.P.Cong etc. Small 6 (2) (2010) 169-173 reported the graphite oxide thermal reduction prepared Graphene after again with Fe
3O
4Carry out compound preparation Graphene/Fe
3O
4The method of compound.
Yet prepare at present Graphene/Fe
3O
4Mainly there is following defective in the method for compound: processing step is more, cost is higher, and prepared Fe
3O
4Crystallization is incomplete.Therefore seek Graphene/Fe that one-step method prepares advantages of good crystallization, is difficult for reuniting, the intensity of magnetization is higher
3O
4Compound becomes the focus of research.Have no at present and adopt the standby Graphene/Fe of pure hot legal system
3O
4The report of composite granule.
Summary of the invention
Technical problem to be solved by this invention provides the standby Graphene/Fe of the hot legal system of a kind of alcohol
3O
4The method of composite granule, this preparation method is simple, is easy to suitability for industrialized production; Prepared Graphene/Fe
3O
4Fe in the composite granule
3O
4Crystalline phase is pure, be difficult for reuniting, with Graphene compound good, in Graphene surface and layer good dispersion, composite granule resistivity is little, the intensity of magnetization is high.
Standby Graphene/the Fe of the hot legal system of a kind of alcohol of the present invention
3O
4The method of composite granule comprises:
(1) configuration of reaction solution
At room temperature, take by weighing mass ratio and be 1: 1～1: 100 graphite oxide, molysite, be distributed in the ethylene glycol solution that concentration is 98wt%～99.5wt%, be incorporated as the polyoxyethylene glycol of ethylene glycol volume 1/50～1/25 after treating to dissolve fully, add again with molysite in Fe
3+The ratio of mole number be 8: 1～12: 1 anhydrous sodium acetate, stir, make the above-mentioned substance dissolving, form reaction solution;
(2) solvent thermal reaction
Above-mentioned reaction solution is put into reactor, be warming up to 180～220 ℃, reaction 8～16h;
(3) Graphene/Fe
3O
4The collection of composite granule and washing
Be cooled to room temperature, collect product with magnet, the deionized water washed product is dried and be get final product.
Molysite in the described step (1) is Iron(III) chloride hexahydrate FeCl
36H
2O.
The molysite in the described step (1) and the mass volume ratio of ethylene glycol are 1g: 20～1000ml.
The molecular weight of the polyoxyethylene glycol in the described step (1) is 200～1000.
Stirring velocity in the described step (1) is 300～600 commentaries on classics/min, and the time is 20～40min.
Bake out temperature in the described step (3) is 40～80 ℃, and the time is 12～24h.
By regulating the ratio of graphite oxide, molysite, obtain the different Graphene/Fe that form
3O
4Composite granule.
This preparation method is with respect to common liquid phase method, and magnetic nanoparticle is more stable in organic phase, is difficult for generating impurity phase.Because in liquid phase, magnetic nano-particle is very easily reunited because of the effect that is subjected to the strong electrostatic attraction of solion, so this method selects electrostatic stabilization good anhydrous sodium acetate adds as alkaline reagent, to prevent Fe
3O
4Extensive reunion.
Beneficial effect
(1) preparation method of the present invention is simple, and is low to the production unit requirement, is easy to suitability for industrialized production;
(2) prepared Graphene/Fe
3O
4Fe in the composite granule
3O
4Crystalline phase is pure, be difficult for reuniting, with Graphene compound good, in Graphene surface and layer good dispersion, composite granule resistivity is little, the intensity of magnetization is high.
Description of drawings
Fig. 1 is the transmission electron microscope photo of synthetic powder;
Fig. 2 is the high-resolution-ration transmission electric-lens photo of synthetic powder;
Fig. 3 is the X-ray diffractogram of synthetic powder;
Fig. 4 is the hysteresis curve figure of synthetic powder.
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 high iron chloride of 500mg, 50mg graphite oxide, add three-neck flask, add again 50ml ethylene glycol, fully stir.Add 0.92g anhydrous sodium acetate, 1.5ml Macrogol 200 again, be 500 rev/mins of following mechanical stirring 30min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 12h at revolution.Reaction finishes, and collects product with magnet, and uses the deionized water washed product, with product dry 16h under 60 ℃, obtains Graphene/Fe then
3O
4Composite granule.Fig. 1 is the transmission electron microscope photo of present embodiment synthetic powder, can find out: Fe
3O
4The Nano microsphere particle diameter is at 100～200nm, Fe
3O
4Nano microsphere is attached to Graphene surface and interlayer equably, does not observe the Fe that is free on outside the Graphene
3O
4Particle.Fig. 2 is the high-resolution-ration transmission electric-lens photo of present embodiment synthetic powder, can find out: the Fe in this composite granule
3O
4Nano microsphere is by a plurality of Fe
3O
4The directed gathering of nanocrystal forms, and its grain size is about 5nm, and interplanar distance is about 0.25nm; Graphene film in this composite granule is made up of 5～20 layer graphenes, and the interlamellar spacing of Graphene is about 0.34nm.Fig. 3 is the X-ray diffractogram of present embodiment synthetic powder, and the diffraction maximum among the figure shows: the nano particle in this composite granule is Fe
3O
4Fig. 4 is the magnetic hysteresis loop figure of present embodiment synthetic powder, and as can be seen: the specific magnetising moment of this composite granule is higher, reaches 63.3emu/g.Resistivity measurement is the result show: the resistivity of this composite granule is 0.989 Ω/cm, and it has excellent conducting performance.
Take by weighing the high iron chloride of 50mg, 50mg graphite oxide, add three-neck flask, add again 50ml ethylene glycol, fully stir.Add 80mg anhydrous sodium acetate, 1.0ml poly(oxyethylene glycol) 400 again, be 300 rev/mins of following mechanical stirring 40min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 220 ℃, reaction 8h at revolution.Reaction finishes, and collects product with magnet, and uses the deionized water washed product, with product dry 24h under 40 ℃, obtains Graphene/Fe then
3O
4Composite granule.Transmission electron microscope observing shows: Fe
3O
4The Nano microsphere particle diameter is at 100～200nm, and is compound good with Graphene.High-resolution-ration transmission electric-lens is observed and is shown: the Fe in this composite granule
3O
4Nano microsphere is by a plurality of Fe
3O
4The directed gathering of nanocrystal forms, and graphene film is made up of 5～20 layer graphenes.The XRD test result shows: the nano particle in this composite granule is Fe
3O
4Magnetic hysteresis loop figure test shows: this composite granule has good magnetic performance.Resistivity measurement is the result show: this composite granule has excellent conducting performance.
Embodiment 3
Take by weighing the high iron chloride of 2.5g, 25mg graphite oxide, add three-neck flask, add again 50ml ethylene glycol, fully stir.Add 9.0g anhydrous sodium acetate, 2.0ml cetomacrogol 1000 again, be 600 rev/mins of following mechanical stirring 20min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 180 ℃, reaction 16h at revolution.Reaction finishes, and collects product with magnet, and uses the deionized water washed product, with product dry 12h under 80 ℃, obtains Graphene/Fe then
3O
4Composite granule.Transmission electron microscope observing shows: Fe
3O
4The Nano microsphere particle diameter is at 100～200nm, and is compound good with Graphene.High-resolution-ration transmission electric-lens is observed and is shown: the Fe in this composite granule
3O
4Nano microsphere is by a plurality of Fe
3O
4The directed gathering of nanocrystal forms, and graphene film is made up of 5～20 layer graphenes.The XRD test result shows: the nano particle in this composite granule is Fe
3O
4Magnetic hysteresis loop figure test shows: this composite granule has good magnetic performance.Resistivity measurement is the result show: this composite granule has excellent conducting performance.
Claims (6)
1. the hot legal system of alcohol is for Graphene/Fe
3O
4The method of composite granule comprises:
(1) configuration of reaction solution
At room temperature, take by weighing mass ratio and be 1: 1～1: 100 graphite oxide, molysite, be distributed in the ethylene glycol solution that concentration is 98wt%～99.5wt%, be incorporated as the polyoxyethylene glycol of ethylene glycol volume 1/50～1/25 after treating to dissolve fully, add again with molysite in the ratio of mole number of Fe3+ be 8: 1～12: 1 anhydrous sodium acetate, stir, make the above-mentioned substance dissolving, form reaction solution;
(2) solvent thermal reaction
Above-mentioned reaction solution is put into reactor, be warming up to 180～220 ℃, reaction 8～16h;
(3) Graphene/Fe
3O
4The collection of composite granule and washing
Be cooled to room temperature, collect product with magnet, the deionized water washed product is dried and be get final product.
2. the hot legal system of a kind of alcohol according to claim 1 is for Graphene/Fe
3O
4The method of composite granule is characterized in that: the molysite in the described step (1) is Iron(III) chloride hexahydrate FeCl
36H
2O.
3. the hot legal system of a kind of alcohol according to claim 1 is for Graphene/Fe
3O
4The method of composite granule is characterized in that: the molysite in the described step (1) and the mass volume ratio of ethylene glycol are 1g: 20～1000ml.
4. the hot legal system of a kind of alcohol according to claim 1 is for Graphene/Fe
3O
4The method of composite granule is characterized in that: the molecular weight of the polyethylene glycol in the described step (1) is 200～1000.
5. the hot legal system of a kind of alcohol according to claim 1 is for Graphene/Fe
3O
4The method of composite granule is characterized in that: the mixing speed in the described step (1) is 300～600 to turn to/min, and the time is 20～40min.
6. the hot legal system of a kind of alcohol according to claim 1 is for Graphene/Fe
3O
4The method of composite granule is characterized in that: the bake out temperature in the described step (3) is 40～80 ℃, and the time is 12～24h.
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|---|---|---|---|
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| CN101837971B CN101837971B (en) | 2012-01-11 |
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