CN103738953B - A kind of preparation method of carbon nano tube-graphene composite foam - Google Patents
A kind of preparation method of carbon nano tube-graphene composite foam Download PDFInfo
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- CN103738953B CN103738953B CN201310713369.2A CN201310713369A CN103738953B CN 103738953 B CN103738953 B CN 103738953B CN 201310713369 A CN201310713369 A CN 201310713369A CN 103738953 B CN103738953 B CN 103738953B
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Abstract
The invention belongs to the preparation method of nano composite material, particularly relate to the microwave preparation technical field of graphene-based matrix material.A kind of preparation method of carbon nano tube-graphene composite foam, first by ferrocene load on grapheme foam, the grapheme foam of ferrocene is had to carry out microwave treatment to load subsequently, the high temperature produced instantaneously makes ferrocene decompose on grapheme foam, produce catalyzer and carbon source simultaneously, realize carbon nanotube growth in situ, obtain carbon nano tube-graphene composite foam.In this matrix material, the vertical orientated growth of carbon nanotube is on grapheme foam hole wall surface, show the surface chemistry of super-hydrophobic super-oleophylic, have broad application prospects in absorption, oily water separation etc., and the method has easy and simple to handle, inexpensive, easily suitability for industrialized production feature, is a kind of important nano carbon material preparation method for material.
Description
Technical field
The invention belongs to the preparation method of nano composite material, particularly relate to the microwave preparation technical field of graphene-based matrix material.
Background technology
Grapheme foam is the novel three-dimension integrally functional materials of a class.This kind of material has flourishing pore texture, the specific surface area of super large and the conductive characteristic of excellence, has broad application prospects at numerous areas such as energy storage, environment protection and catalysis.The method preparing grapheme foam of current report comprises the multiple methods such as hydrothermal reduction method, chemical reduction method and chemical Vapor deposition process.Although grapheme foam shows the performance of a series of excellence, particularly hydrophobic performance is not ideal enough for the character of some aspect, and the hydrophobic performance how effectively improving grapheme foam becomes an important challenge.
Improving one of important channel of material hydrophobic performance is the roughness increasing material surface.As a kind of material typically with high length-diameter ratio, the particularly vertical orientated carbon nano pipe array of carbon nanotube is used for improving the hydrophobic property on surface, initiative super hydrophobic surface widely.Utilize the grapheme foam of chemical vapour deposition as substrate, after catalyst deposit, again carry out the preparation that chemical vapor deposition processes successfully achieves super-hydrophobic carbon nanotube-grapheme foam, but the loaded down with trivial details process of the method and extremely low productive rate significantly limit the possibility of this foam practical application.And by introducing carbon nanotube in the process of chemical preparation grapheme foam, can efficiently, low cost obtain graphene-carbon nano tube foam, but in this foam, carbon nanotube is often coated by graphene nanometer sheet institute, not obvious to the improvement of material hydrophobic.How to introduce vertical orientated carbon nano pipe array at grapheme foam hole wall surface and be still a difficult problem.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of preparation method of carbon nano tube-graphene composite foam, ferrocene is dispersed in the surface of grapheme foam by the method, and have the grapheme foam of ferrocene to carry out microwave treatment to load, induce ferrocene cracking and catalysis Formed nanotube, rapidly and efficiently obtain carbon nano tube-graphene composite foam.
The technical solution adopted in the present invention is as follows: a kind of preparation method of carbon nano tube-graphene composite foam, and this preparation method carries out in accordance with the following steps:
(1) be dispersed in lower boiling organic solvent by ferrocene and obtain ferrocene solution, the concentration range of ferrocene solution is 5 ~ 20mg/mL;
(2) grapheme foam is inserted in above-mentioned ferrocene solution, fully flood;
(3) by the grapheme foam taking-up after dipping, drying, the grapheme foam that load has ferrocene is obtained;
(4) grapheme foam of ferrocene load is had to be placed in microwave reactor; microwave treatment is carried out after utilizing non-oxide protective gas to purge; the high temperature that grapheme foam and microwave action produce makes ferrocene decompose carbon nano-tube, and naturally cooling obtains carbon nanotube-Graphene composite foam after being down to room temperature.
In described (1), lower boiling organic solvent is selected from one or more mixing in acetone, ethanol, gasoline, sherwood oil, benzene, ether, hexanaphthene and ethyl acetate.
Described raw graphite alkene foam is the standby grapheme foam of the grapheme foam of chemical preparation or hydrothermal reduction legal system.
Described chemical preparation grapheme foam adopts the reduction of reductive agent quadrol, sodium bisulfite, xitix, sodium sulphite, hydrogen iodide or Resorcinol to prepare gained; It is that additional reducing agent hydrothermal treatment consists does not prepare gained that described hydrothermal reduction prepares grapheme foam, or extra reductive agent hydrazine hydrate, sodium bisulfite, xitix or the sodium sulphite hydrothermal reduction of adding prepares gained.
One or more being selected from nitrogen, argon gas, helium, hydrogen and the low-carbon (LC) such as methane, ethene hydrocarbon gas of protective gas in described (4) without oxidisability mix.
Described microwave treatment power is 800W, and the treatment time is 5 ~ 600 seconds.
The vertical orientated growth of described carbon nanotube, on grapheme foam hole wall, has good super-hydrophobic super-oleophylic characteristic, has broad application prospects in absorption, oily water separation etc.
Compared with prior art, the present invention has following remarkable advantage:
1. technique is simple, and raw material is cheap and easy to get;
2., under microwave exposure, ferrocene is at grapheme foam hole wall surface original position pyrolysis Formed nanotube;
3. generated in-situ carbon nanotube vertical-growth is on Graphene hole wall, effectively can improve the wettability of original graphite alkene foam;
4. under microwave exposure, carbon nanotube has very high growth efficiency, and only the microwave treatment of 5s just can realize the growth of carbon nanotube.
Accompanying drawing explanation
Fig. 1 is carbon nano tube-graphene composite foam preparation flow figure;
Fig. 2 is the digital photograph of carbon nano tube-graphene composite foam, and the ferrocene strength of solution used is 15mg/mL, and microwave treatment time is 1 minute;
The electron scanning micrograph that Fig. 3 is carbon nano tube-graphene composite foam, the ferrocene strength of solution used is 15mg/mL, and microwave treatment time is 1 minute;
Fig. 4 is that carbon nano tube-graphene composite foam is to selective adsorption process that is oily and water;
Fig. 5 is the electron scanning micrograph of carbon nano tube-graphene composite foam, and the ferrocene strength of solution used is 15mg/mL, and microwave treatment time was 5 seconds;
Fig. 6 is the electron scanning micrograph of carbon nano tube-graphene composite foam, and the ferrocene strength of solution used is 20mg/mL, and microwave treatment time was 30 seconds.
Embodiment
Fig. 1 is the preparation flow schematic diagram of carbon nano tube-graphene composite foam in the present invention, and concrete preparation process is as described below:
(1) in lower boiling organic solvent, disperse ferrocene to obtain ferrocene solution, the concentration range of ferrocene solution is 5 ~ 20mg/mL; Low boiling point organic solvent used comprises one or more mixing in acetone, ethanol, gasoline, sherwood oil, benzene, ether, hexanaphthene, ethyl acetate;
(2) grapheme foam is inserted in above-mentioned ferrocene solution, fully flood; The grapheme foam used comprises the grapheme foam of chemical preparation and the standby grapheme foam of hydrothermal reduction legal system; The reductive agent of chemical preparation grapheme foam can be quadrol, sodium bisulfite, xitix, sodium sulphite, hydrogen iodide and Resorcinol etc.; Hydrothermal reduction additionally can add reductive agent as hydrazine hydrate, sodium bisulfite, xitix, sodium sulphite etc. when preparing grapheme foam, also can not additional reducing agent;
(3) by the grapheme foam taking-up after dipping, drying, the grapheme foam that load has ferrocene is obtained;
(4) grapheme foam of ferrocene load is had to be placed in microwave reactor; microwave treatment is carried out after utilizing protective gas to purge; the high temperature that grapheme foam and microwave action produce makes ferrocene decompose carbon nano-tube, and naturally cooling obtains carbon nanotube-Graphene composite foam after being down to room temperature.The protective gas used is non-oxidizing gas, comprises one or more mixing in nitrogen, argon gas, helium, hydrogen and the low-carbon (LC) such as methane, ethene hydrocarbon gas; Microwave treatment power is 800W, and the time is 5 ~ 600 seconds.
Carbon nano tube-graphene composite foam prepared by aforesaid method, carbon nanotube is vertical orientated on grapheme foam hole wall, and the material obtained has good ultra-hydrophobicity.The method is simple to operate, easily amplifies.Below will the invention will be further described by several specific embodiment:
embodiment 1:
By 0.6g ferrocene ultrasonic disperse in the acetone of 40mL, obtain the ferrocene acetone soln that concentration is 15mg/mL.The grapheme foam that quadrol assisted Reduction prepares is inserted in the acetone soln of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare puts seasoning, after acetone volatilization completely, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in argon replaces reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 1min, obtains carbon nano tube-graphene composite foam.Thermogravimetric analysis shows that the content of carbon nanotube in composite foam is 32wt%.Figure 2 shows that the composite foam digital photograph obtained, Figure 3 shows that the electron scanning micrograph of composite foam, as can be seen from the figure a large amount of vertical orientated carbon nanotube of both sides uniform loading of grapheme foam hole wall, the length of carbon nanotube is at about 5 μm.Fig. 4 illustrates gained carbon nano tube-graphene composite foam to selective adsorption capacity that is oily and water, water droplet can present spherical state and rest on the surface of foam for a long time, and the moment that oil droplet is touching foam just penetrates in the space of foam completely, reflect super-hydrophobic, the super oil-wetted surface characteristic of this composite foam.
embodiment 2:
By 0.75g ferrocene ultrasonic disperse in the acetone of 50mL, obtain the ferrocene acetone soln that concentration is 15mg/mL.The grapheme foam that quadrol assisted Reduction prepares is inserted in the acetone soln of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare puts seasoning, after acetone volatilization completely, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in argon replaces reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 5s, obtains carbon nano tube-graphene composite foam.Thermogravimetric analysis shows that the content of carbon nanotube in mixture is 8wt%.Figure 5 shows that the electron scanning micrograph of the composite foam obtained, the length of carbon nanotube as can be seen from the figure grown in this embodiment is shorter, is hundreds of nanometer.
embodiment 3:
By 0.6g ferrocene ultrasonic disperse in the gasoline of 30mL, obtain the ferrocene gasoline solution that concentration is 20mg/mL.The grapheme foam that xitix assisted Reduction prepares is inserted in the solution of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare puts seasoning, after gasoline volatilization is complete, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in nitrogen replacement reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 30s, obtains carbon nano tube-graphene composite foam.In mixture, the content of carbon nanotube is 42wt%.
embodiment 4:
By 0.4g ferrocene ultrasonic disperse in the ethanol of 40mL, obtain the ferrocene ethanolic soln that concentration is 10mg/mL.The grapheme foam that hydro-thermal assisted Reduction prepares is inserted in the solution of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare is put in stink cupboard dry, after ethanol volatilization completely, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in hydrogen exchange reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 15s, obtains carbon nano tube-graphene composite foam.In mixture, the content of carbon nanotube is 23wt.%
embodiment 5:
By 0.2g ferrocene ultrasonic disperse in the acetone of 40mL, obtain the ferrocene acetone soln that concentration is 5mg/mL.The grapheme foam prepared that reduced by quadrol is inserted in the solution of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare is put in stink cupboard dry, after acetone volatilization completely, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in hydrogen/argon gas gas mixture metathesis reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 40s, obtains carbon nano tube-graphene composite foam.In mixture, the content of carbon nanotube is 17wt%.Figure 6 shows that the electron scanning micrograph of the composite foam obtained.
embodiment 6:
By 0.5g ferrocene ultrasonic disperse in the sherwood oil of 50mL, obtain the ferrocene petroleum ether solution that concentration is 10mg/mL.The grapheme foam prepared that reduced by quadrol is inserted in the solution of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare is put in stink cupboard dry, after sherwood oil volatilization completely, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in argon gas gas mixture metathesis reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 600s, obtains carbon nano tube-graphene composite foam.In mixture, the content of carbon nanotube is 28wt%.
embodiment 7:
By 0.3g ferrocene ultrasonic disperse in the sherwood oil of 20mL and the mixing solutions of 20mL gasoline, obtain the ferrocene solution that concentration is 7.5mg/mL.The grapheme foam prepared that reduced by quadrol is inserted in the solution of above-mentioned ferrocene.Taken out by impregnated grapheme foam, ambient temperatare is put in stink cupboard dry, after solvent evaporates is complete, obtains the grapheme foam being supported with ferrocene.The grapheme foam being supported with ferrocene is placed in microwave reactor, passes into the air in nitrogen mixture metathesis reactor.Opened by microwave reactor, carry out microwave exposure process, the power of microwave reactor is 800W, and the treatment time is 30s, obtains carbon nano tube-graphene composite foam.In mixture, the content of carbon nanotube is 15wt.%.
Claims (4)
1. a preparation method for carbon nano tube-graphene composite foam, is characterized in that: this preparation method carries out in accordance with the following steps:
(1) ferrocene is dispersed in lower boiling organic solvent obtains ferrocene solution, the concentration range of ferrocene solution is 5 ~ 20mg/mL, and described lower boiling organic solvent is selected from one or more mixing in acetone, ethanol, gasoline, sherwood oil, benzene, ether, hexanaphthene and ethyl acetate;
(2) grapheme foam is inserted in above-mentioned ferrocene solution, fully flood;
(3) by the grapheme foam taking-up after dipping, drying, the grapheme foam that load has ferrocene is obtained;
(4) grapheme foam of ferrocene load is had to be placed in microwave reactor; microwave treatment is carried out after utilizing non-oxide protective gas to purge; the high temperature that grapheme foam and microwave action produce makes ferrocene decompose carbon nano-tube; naturally cooling obtains carbon nanotube-Graphene composite foam after being down to room temperature; wherein said microwave treatment power is 800W, and the time is 5 ~ 600 seconds.
2. the preparation method of a kind of carbon nano tube-graphene composite foam according to claim 1, is characterized in that: described raw graphite alkene foam is the standby grapheme foam of the grapheme foam of chemical preparation or hydrothermal reduction legal system.
3. the preparation method of a kind of carbon nano tube-graphene composite foam according to claim 2, is characterized in that: described chemical preparation grapheme foam adopts the reduction of reductive agent quadrol, sodium bisulfite, xitix, sodium sulphite, hydrogen iodide or Resorcinol to prepare gained; It is that additional reducing agent hydrothermal treatment consists does not prepare gained that described hydrothermal reduction prepares grapheme foam, or extra reductive agent hydrazine hydrate, sodium bisulfite, xitix or the sodium sulphite hydrothermal reduction of adding prepares gained.
4. the preparation method of a kind of carbon nano tube-graphene composite foam according to claim 1, is characterized in that: one or more being selected from nitrogen, argon gas, helium, hydrogen and methane, ethene of protective gas in described (4) without oxidisability mix.
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