CN103496693A - Method for preparing Fe3O4 nanoparticle/graphene composite material by sol electrostatic self-assembly process and application thereof - Google Patents
Method for preparing Fe3O4 nanoparticle/graphene composite material by sol electrostatic self-assembly process and application thereof Download PDFInfo
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- CN103496693A CN103496693A CN201310433900.0A CN201310433900A CN103496693A CN 103496693 A CN103496693 A CN 103496693A CN 201310433900 A CN201310433900 A CN 201310433900A CN 103496693 A CN103496693 A CN 103496693A
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Abstract
The invention discloses a method for preparing a Fe3O4 nanoparticle/graphene composite material by a sol electrostatic self-assembly process, which comprises the following steps: (1) preparing a Fe(OH)3 sol solution of which the surface is positively charged; (2) preparing a graphene oxide sol of which the surface is negatively charged; and (3) mixing the graphene oxide sol and the Fe(OH)3 sol, magnetically stirring to generate a brownish black precipitate, separating, pouring out the supernate to obtain a Fe(OH)3/graphene oxide composite, and reducing the composite at 300-800 DEG C in a nitrogen atmosphere to obtain the Fe3O4/graphene nano composite material. The composite of the Fe(OH)3 colloidal particles and graphene oxide is performed in the water solution, and thus, the method has the advantages of low cost, energy saving, environment friendliness and simple technique, and can easily implement industrial mass production; and the preparation process of the Fe(OH)3 colloidal particle/graphene oxide composite material has obvious solution variation, and the solution becomes turbid from clear and finally precipitates, so that the supernate can be directly poured out.
Description
Technical field
The present invention relates to a kind of colloidal sol electrostatic self-assembled method and prepare Fe
3o
4the method of nano particle and graphene composite material and purposes.
Background technology
As the Graphene of two-dimensional sheet structured material and the matrix material of the compound generation of metal oxide nanoparticles, there is unique texture and character and be subject to paying close attention to widely.The main method that obtains at present graphene-based matrix material has: mechanically mixing and the material composition matrix material of directly growing other on graphene film by chemical process.Although but the mechanical blending method matrix material homogeneity for preparing of causing because the Graphene phase is different with metal oxide particle density simple to operate is bad; On graphene film, the composition of the chemical preparation process of growth the second material require complexity and matrix material is handling bad.
Summary of the invention
The objective of the invention is the customer service the deficiencies in the prior art, provide a kind of colloidal sol electrostatic self-assembled to prepare Fe
3o
4the method of nano particle and graphene composite material and purposes.
Technical scheme of the present invention is: a kind of colloidal sol electrostatic self-assembled method prepares Fe
3o
4the method of nano particle/graphene composite material, its step is as follows:
(1) under room temperature, the FeCl that configuration quality concentration is 15-30%
3the aqueous solution, in the situation that magnetic agitation, by FeCl
3the aqueous solution is added dropwise in the water of boiling, FeCl
3the mass ratio of water-soluble drop and water is 1:1-5, boils 1-5 minute after dropwising again, and obtains presenting brick-red transparence solution, and this kind of solution is the Fe (OH) of surface with positive charge
3sol solution;
(2) adopt the Hummers method to prepare graphene oxide, graphene oxide is distributed to water under ultrasound condition, the mass volume ratio of graphene oxide and water is 1:10-20, obtain the surperficial graphene oxide colloidal sol with negative charge;
(3) by graphene oxide colloidal sol and Fe (OH)
3colloidal sol mixes, graphene oxide colloidal sol and Fe (OH)
3the mass ratio of colloidal sol is 1:1-1:50, occurs the brownish black precipitation under magnetic agitation, separates, and outwells supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture is reduced under 300-800 ℃, nitrogen atmosphere, prepare Fe
3o
4/ graphene nanocomposite material.
Colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to adsorb the dyestuff rhodamine B in waste water.
Colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to electrode material for super capacitor.
Colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to lithium ion battery negative material.
The invention has the beneficial effects as follows: Fe (OH)
3the mixture of colloidal solid and graphene oxide carries out in the aqueous solution, with low cost and energy-conserving and environment-protective, and technique is simple, is easy to industrial volume production; Fe (OH)
3in the preparation process of colloidal solid and graphene oxide composite material, have obvious solution to change, solution colour becomes muddy to last appearance precipitation from clarification, directly outwells supernatant liquor and gets final product; Fe
3o
4generation and the reduction of Graphene can concentrate on same heat treatment step; Fe
3o
4the composition conveniently regulating and controlling of nano particle and graphene composite material.
Method of the present invention is eco-friendly, and simple and flexible utilizes the electrostatic self-assembled method to prepare uniform Fe
3o
4the matrix material of nano particle and Graphene stratiform structure.Assemble method simple possible in the aqueous solution under this room temperature, the requirement of producing applicable to the industrialization big area, reduction when in reduction step, realizing two components, energy saving economy is environmental protection again.
The accompanying drawing explanation:
Fig. 1 is the Fe made
3o
4nano particle/graphene composite material transmission electron microscope photo;
Fig. 2 is the Fe made
3o
4nano particle/graphene composite material Raman figure;
Fig. 3 is the Fe made
3o
4the schematic diagram of nano particle/graphene composite material absorbing dye;
Fig. 4 is the Fe made
3o
4nano particle/graphene composite material cyclic voltammogram.
Embodiment
Embodiment 1
Under room temperature, the FeCl that configuration 40mL concentration is 10%
3the aqueous solution; Get the beaker 200mL distilled water of packing into, by the FeCl configured
3the aqueous solution drip and to enter in the water of boiling, after dropwising, then boil 2 minutes, gained solution is bolarious transparent aqueous solution, solution presents steady state, is Fe (OH)
3water-sol system.Adopt the Hummers method to prepare graphene oxide, surface is with negative charge; Make the concentration of graphene oxide reach 0.1mg/mL ultrasonic being distributed in water of graphene oxide.Fe (OH) by surface with positive charge
3colloidal sol 10.7mL joins in graphene oxide colloidal sol, occurs the brownish black precipitation under magnetic agitation, separates, and removes supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture, at 500 ℃, is reduced under inert atmosphere, prepare Fe
3o
4/ graphene composite material.
In colloidal solid and graphene oxide recombination process, Fe (OH)
3colloidal sol is brick-red, and graphene oxide colloidal sol is golden yellow, after two kinds of colloidal sols mix, brown precipitation slowly occurs.In heat treatment process, Graphene and Fe
3o
4generate simultaneously.Whole change in process is obvious, simple to operate, is conducive to industrial applications.Preparation-obtained Fe
3o
4the transmission electron microscope of nano particle and graphene composite material as shown in Figure 1, shows that it forms uniform network structure; Fig. 2 is Fe
3o
4the X-ray diffractogram of nano particle and graphene composite material, show its really by Fe
3o
4the matrix material that nano particle and Graphene form; By Fe
3o
4nano particle and graphene composite material 50mg throw in and enter that to contain concentration be 10
-5the water of Mmol dyestuff rhodamine B is as sorbent material, and after 6 minutes, upper solution becomes transparently, obtains after tested Fig. 3, and mixture self has good magnetic, can separate and obtain by externally-applied magnetic field, convenient recovery and recycle; By Fe
3o
4nano particle and graphene composite material are for the electrochemistry cyclic voltammetry, obtain Fig. 4, the result demonstration, cyclic voltammetric has good rectangle, show that mixture is suitable as the electrode material activity thing, can be used as preparing the electrode of ultracapacitor and lithium ion battery.
Under room temperature, the FeCl that configuration 40mL concentration is 10%
3the aqueous solution; Get the beaker 200mL distilled water of packing into, by the FeCl configured
3the aqueous solution drip and to enter in the water of boiling, after dropwising, then boil 2 minutes, gained solution is bolarious transparent aqueous solution, presents steady state, is Fe (OH)
3water-sol system.Adopt the Hummers method to prepare graphene oxide, surface is with negative charge; Make the concentration of graphene oxide reach 0.1mg/mL ultrasonic being distributed in water of graphene oxide.Fe (OH) by surface with positive charge
3colloidal sol 5mL joins in Graphene colloidal sol, occurs the brownish black precipitation under magnetic agitation, and upper solution is faint yellow, separates, and removes supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture, at 500 ℃, is reduced under inert atmosphere, prepare Fe
3o
4/ graphene composite material.
Embodiment 3
Under room temperature, the FeCl that configuration 40mL concentration is 10%
3the aqueous solution; Get the beaker 200mL distilled water of packing into, by the FeCl configured
3the aqueous solution drip and to enter in the water of boiling, after dropwising, then boil 2 minutes, gained solution is bolarious transparent aqueous solution, presents steady state, is Fe (OH)
3water-sol system.Adopt the Hummers method prepare graphene oxide (W. S. Hummers and R. E. Offeman,
j. Am. Chem. Soc.,1958,80,1339.), surface is with negative charge; Make the concentration of graphene oxide reach 0.1mg/mL ultrasonic being distributed in water of graphene oxide.Fe (OH) by surface with positive charge
3sol solution 20mL joins in graphene dispersing solution, occurs the brownish black precipitation under magnetic agitation, and upper solution is light brick-red, separates, and removes supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture, at 500 ℃, is reduced under inert atmosphere, prepare Fe
3o
4/ graphene composite material.
Embodiment 4
A kind of colloidal sol electrostatic self-assembled method prepares Fe
3o
4the method of nano particle/graphene composite material, its step is as follows:
(1) under room temperature, the FeCl that configuration quality concentration is 15%
3the aqueous solution, in the situation that magnetic agitation, by FeCl
3the aqueous solution is added dropwise in the water of boiling, FeCl
3the mass ratio of water-soluble drop and water is 1:1, after dropwising, boils 1 minute again, obtains the Fe (OH) of surface with positive charge
3colloidal sol;
(2) during graphene oxide is distributed to water under ultrasound condition, the mass volume ratio of graphene oxide and water is 1:10, obtains the graphene oxide colloidal sol of surface with negative charge;
(3) by graphene oxide colloidal sol and Fe (OH)
3colloidal sol mixes, graphene oxide colloidal sol and Fe (OH)
3the mass ratio of colloidal sol is 1:1, occurs the brownish black precipitation under magnetic agitation, separates, and outwells supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture is reduced under 300 ℃, nitrogen atmosphere, obtain Fe
3o
4/ graphene nanocomposite material.
Embodiment 5
A kind of colloidal sol electrostatic self-assembled method prepares Fe
3o
4the method of nano particle/graphene composite material, its step is as follows:
(1) under room temperature, the FeCl that configuration quality concentration is 30%
3the aqueous solution, in the situation that magnetic agitation, by FeCl
3the aqueous solution is added dropwise in the water of boiling, FeCl
3the mass ratio of water-soluble drop and water is 1:5, after dropwising, boils 5 minutes again, obtains the Fe (OH) of surface with positive charge
3colloidal sol;
(2) during graphene oxide is distributed to water under ultrasound condition, the mass volume ratio of graphene oxide and water is 1:20, obtains the graphene oxide colloidal sol of surface with negative charge;
(3) by graphene oxide colloidal sol and Fe (OH)
3colloidal sol mixes, graphene oxide colloidal sol and Fe (OH)
3the mass ratio of colloidal sol is 1:50, occurs the brownish black precipitation under magnetic agitation, separates, and outwells supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture is reduced under 800 ℃, nitrogen atmosphere, obtain Fe
3o
4/ graphene nanocomposite material.
Embodiment 6
A kind of colloidal sol electrostatic self-assembled method prepares Fe
3o
4the method of nano particle/graphene composite material, its step is as follows:
(1) under room temperature, the FeCl that configuration quality concentration is 20%
3the aqueous solution, in the situation that magnetic agitation, by FeCl
3the aqueous solution is added dropwise in the water of boiling, FeCl
3the mass ratio of water-soluble drop and water is 1:3, after dropwising, boils 3 minutes again, obtains the Fe (OH) of surface with positive charge
3colloidal sol;
(2) during graphene oxide is distributed to water under ultrasound condition, the mass volume ratio of graphene oxide and water is 1:15, obtains the graphene oxide colloidal sol of surface with negative charge;
(3) by graphene oxide colloidal sol and Fe (OH)
3colloidal sol mixes, graphene oxide colloidal sol and Fe (OH)
3the mass ratio of colloidal sol is 1:20, occurs the brownish black precipitation under magnetic agitation, separates, and outwells supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture is reduced under 500 ℃, nitrogen atmosphere, obtain Fe
3o
4/ graphene nanocomposite material.
Claims (4)
1. a colloidal sol electrostatic self-assembled method prepares Fe
3o
4the method of nano particle/graphene composite material is characterized in that its step is as follows:
(1) under room temperature, the FeCl that configuration quality concentration is 15-30%
3the aqueous solution, in the situation that magnetic agitation, by FeCl
3the aqueous solution is added dropwise in the water of boiling, FeCl
3the mass ratio of water-soluble drop and water is 1:1-5, boils 1-5 minute after dropwising again, and obtains the Fe (OH) of surface with positive charge
3colloidal sol;
(2) during graphene oxide is distributed to water under ultrasound condition, the mass volume ratio of graphene oxide and water is 1:10-20, obtains the graphene oxide colloidal sol of surface with negative charge;
(3) by graphene oxide colloidal sol and Fe (OH)
3colloidal sol mixes, graphene oxide colloidal sol and Fe (OH)
3the mass ratio of colloidal sol is 1:1-1:50, occurs the brownish black precipitation under magnetic agitation, separates, and outwells supernatant liquid, obtains Fe (OH)
3with the mixture of graphene oxide, mixture is reduced under 300-800 ℃, nitrogen atmosphere, obtain Fe
3o
4/ graphene nanocomposite material.
2. colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to adsorb the dyestuff rhodamine B in waste water.
3. colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to electrode material for super capacitor.
4. colloidal sol electrostatic self-assembled method prepares Fe
3o
4nano particle/graphene composite material is applied to lithium ion battery negative material.
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Patent Citations (2)
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| CN101837971A (en) * | 2010-05-14 | 2010-09-22 | 东华大学 | Method for preparing graphene/Fe3O4 composite powder by alcohol thermal method |
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