CN105752970A - Method for preparing carbon nanotube/graphene compound - Google Patents
Method for preparing carbon nanotube/graphene compound Download PDFInfo
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- CN105752970A CN105752970A CN201610188685.6A CN201610188685A CN105752970A CN 105752970 A CN105752970 A CN 105752970A CN 201610188685 A CN201610188685 A CN 201610188685A CN 105752970 A CN105752970 A CN 105752970A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a method for preparing a carbon nanotube/graphene compound.Carbon nanotubes, an additive and a surfactant are weighed and mixed according to the mass ratio of 100:(1-100):(0.01-1), then a solvent with the mass being 1-10 times that of the mixture is added into the mixture and evenly stirred and mixed, the solvent is distilled, then the product is placed in an oven to be dried, and then the carbon nanotube/graphene compound is prepared through the carbonization and pickling technology.By the adoption of in-situ one-step method, graphene does not need to be prepared in advance, the prepared carbon nanotube/graphene compound is high in specific surface area and good in electric performance, specific capacitance ranges from 100 F/g to 350 F/g, the specific surface area ranges from 150 m<2>/g to 400 m<2>/g, and the graphitization degree ranges from 30% to 70%.The method is rich in raw material, low in price and capable of achieving industrialization easily.
Description
Technical field
The invention belongs to nano-carbon material preparation field, the preparation method relating generally to a kind of carbon nano tube/graphene complex.
Background technology
Graphene, since successfully being prepared, has just become the focus of research both at home and abroad in the short time.As a kind of excellent Two-dimensional Carbon material, unique electronic structure makes it have the excellent physical and chemical performance such as high conductivity, high-transmittance, high-specific surface area, high intensity, mechanical performance and good electrical and thermal conductivity performance, has good application prospect in various electrode of electrochemical device materials, catalyst carrier, sensing material and energy storage etc..And CNT (CNTs) is as a kind of One-dimensional Quantum material, except the hollow-core construction with uniqueness, its radial dimension is nanometer scale, axial dimension is micron dimension, pipe two ends are substantially all sealing, and this makes it have the premium properties such as significantly high intensity, pliability, is all widely used in fields such as solaode, catalysis and the new industries of biotechnology, it has necessarily similar character to Graphene, and SWCN is seen as the graphene film of a drum.But owing to Graphene is different from the structure of CNT, in performance and application aspect, then there is some difference for they.In order to make full use of both advantages and overcome the deficiency existing for bi-material itself, Graphene and CNTs are generally carried out the compound carbon nano tube/graphene complex with prepared tridimensional network by people, by the cooperative effect between them, the performance of complex can be substantially improved, it is made to show the performance more excellent than any one homogenous material, obtain the characteristics such as better isotropism heat conductivity, isotropic conductivity, thus having good application prospect in ultracapacitor, solaode, display, biological detection, fuel cell etc..
The main method preparing carbon nano tube/graphene complex at present has mechanical mixing, chemical vapour deposition technique (CVD) and LBL self-assembly method (LBL).Mechanical mixing is Graphene and CNT simply to be mixed, then it is carried out subsequent treatment obtains graphene/carbon nano-tube complex, is usually present the phenomenon that dispersion is uneven, and is difficult to play the cooperative effect in the two performance；CVD is then deposited graphite alkene thin film in the substrates such as Copper Foil, graphene film is coated with catalyst, layer CNT is deposited again at catalyst surface, finally remove substrate and obtain carbon nano tube/graphene laminated film, but have that PROCESS FOR TREATMENT temperature is high, sedimentation rate is low, and the impacts such as harmful gas can be produced in course of reaction；And LBL method relies primarily on the interaction between molecule or ion, at substrate surface alternating deposit Graphene and CNT, obtain multilayered film material, but the raw material used is generally with active function groups, in use, easily there is irreversible redox reaction in free functional group, thus having a strong impact on overall performance.Mostly there is certain problem in existing technology, generally need pre-synthesis Graphene, and in building-up process, impurity can be introduced unavoidably, technique is loaded down with trivial details, subsequent treatment is complicated, cost is high, environmental pollution and be difficult to industrialized production etc., greatly limit the application of Graphene/CNTs and popularization.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of carbon nano tube/graphene complex, the specific surface area of obtained carbon nano tube/graphene complex is high, good electrical property, is 100～350F/g than electric capacity, and specific surface area is 150～400m2/ g, graphite alkylene degree reaches 30%～70%, and also abundant raw material, cheap, easily realize industrialization.
For achieving the above object, the present invention adopts the following technical scheme that
(1) mixing of raw material
Weigh CNT, additive and surfactant, CNT, additive and surfactant are 1 ~ 100:100:0.01 ~ 1 mixing in mass ratio, add after the stirring solvent mix homogeneously of 1 ~ 10 times of quality subsequently in mixture and distilling off solvent, be subsequently placed in baking oven and be dried；Whipping temp is 25～150 DEG C, and mixing time is 1～5h；Baking temperature is 35～100 DEG C, and drying time is 1 ~ 12h；
The CNT adopted is the mixing of one or more of SWCN, double-walled carbon nano-tube, multi-walled carbon nano-tubes, functionalization multi-walled carbon nano-tubes, short MWCNTs, industrialization multi-walled carbon nano-tubes, graphitization multi-walled carbon nano-tubes, large diameter thin wall carbon nano-tube and carbon nano-tube fibre；
The additive adopted is aluminum chloride, aluminum sulfate, aluminium carbonate, aluminum acetate, aluminum nitrate, aluminium hydroxide, sodium metaaluminate, aluminum phosphate, aluminium silicate, aluminium carbide, ten sulfate dihydrate aluminum ammoniums, metasilicic acid aluminum, trifluoromethanesulfonic acid aluminum, trialkylaluminium, dialkylaluminum chloride, one alkyl al dichloride, trialkyl tri-chlorination two aluminum, aluminum isopropylate., butyl aluminum, aluminium acetate, aluminium triformate, oxalic acid aluminum, propanoic acid aluminum, polyaluminium chloride, aluminium silicate, fluoric acid aluminum, aluminium secondary butylate, praseodynium aluminum, triisobutyl aluminium, oxine aluminum, aluminum perchlorate, aluminum monostearate, aluminium distearate, aluminum hydroxyacetate, ethyl aluminum dichloride, AL-PHOSETHYL aluminum tris(ethyl phosphite), aluminium acetylacetonate, aluminium dihydrogen phosphate, aluminum oleate, aluminium bromide, silver iodide, aluminum ethylate., aluctyl., one in isooctyl acid aluminum and trioctylaluminum；
The surfactant adopted is the one of dodecyl sodium sulfate, poly-methyl pyrrole alkanone, polyvinylpyrrolidone, fatty alcohol-polyoxyethylene ether, sodium lauryl sulphate, sodium hexadecyl sulfate, sodium stearyl sulfate, hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, Dodecyl trimethyl ammonium chloride, octyl sodium sulfonate and octyl sodium sulfate；
The solvent adopted be water, ethanol, dichloromethane, acetone, chloroform, methanol, oxolane, carbon tetrachloride, hexamethylene, isopropanol, 1,2-trichloroethane, triethylamine, toluene, pyridine, ethylenediamine, butanol, acetic acid, chlorobenzene, dimethylbenzene, N, dinethylformamide, Ketohexamethylene, Hexalin, N, N-dimethyl acetylamide, N-METHYLFORMAMIDE, phenol, dimethyl sulfoxide, ethylene glycol, N-Methyl pyrrolidone, the one in Methanamide, sulfolane and glycerol；
(2) carbonization
The raw material that step (1) mixes is put in atmosphere furnace, is incubated after then heating to predetermined temperature, be cooled to room temperature and take out；Charring process parameter is:
Heating rate: 1 DEG C/min～50 DEG C/min
Predetermined temperature: 1100 DEG C～2000 DEG C
Temperature retention time: 0.1h～10h
Protective atmosphere: N2Or Ar2
Gas flow: 25mL/min～300mL/min；
(3) pickling
Being placed in by step (2) gained carbonizing production in acid solution and stir, deionized water fully washs to neutrality, is then placed in 35～100 DEG C of vacuum drying ovens and is dried 1 ~ 12h, and vacuum is 1.0 × 10-1~1.0×105Pa；Acid cleaning process parameter is:
Acid solution: the one in hydrochloric acid, oxalic acid and sulphuric acid
Acid solution molar concentration: 0.05mol/L～6mol/L
Mixing time: 1～5h
Mixing speed: 25～200 revs/min.
The beneficial effects of the present invention is:
(1) specific surface area of the carbon nano tube/graphene complex that the present invention prepares is high, good electrical property, is 100～350F/g than electric capacity, and specific surface area is 150～400m2/ g, graphite alkylene degree reaches 30%～70%；
(2) solve carbon nano tube/graphene mixing inequality, can be realized by situ study, it is not necessary to Graphene is as raw material, and technique is simple, operates safety；
(3) abundant raw material, cheap, easily realize industrialization.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture of the carbon nano tube/graphene complex adopting embodiment 1 technique to prepare；
Fig. 2 is the scanning electron microscopic picture of the carbon nano tube/graphene complex adopting embodiment 2 technique to prepare；
Fig. 3 is the scanning electron microscopic picture of the carbon nano tube/graphene complex adopting embodiment 3 technique to prepare；
Fig. 4 is the scanning electron microscopic picture of the carbon nano tube/graphene complex adopting embodiment 4 technique to prepare.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
SWCN, aluminum sulfate and poly-methyl pyrrole alkanone being weighed according to mass ratio 50:100:0.05 and mix, employing ethanol is solvent, and the mass ratio of mixture and solvent is 1:4.By mechanical agitation by both mix homogeneously, whipping temp is 80 DEG C, and mixing time is 2h.To be mixed uniformly after, reduce pressure distilling off solvent, is positioned over 80 DEG C of vacuum drying ovens (1.0 × 10-1Pa) dry 8 hours, it is cooled to room temperature.Drying sample is positioned in atmosphere furnace, passes into nitrogen (nitrogen flow is 100mL/min), be warming up to 2000 DEG C with 10 DEG C/min, be incubated 0.5h, be cooled to room temperature and take out.Being positioned over by carbonizing production in hydrochloric acid solution (acid solution molar concentration is 2mol/L), stir 1.5h, mixing speed is 80 revs/min, is washed till neutrality with deionized water after isolated by filtration.It is positioned over vacuum drying oven (1.0 × 10-1Pa) in, dry 80 DEG C dry 12 hours, namely obtain carbon nano tube/graphene complex.
Prepared carbon nano tube/graphene composite properties is as follows: be 350F/g than electric capacity, and specific surface area is 400m2/ g, graphite alkylene degree is 70%.
Embodiment 2
Industrialization multi-walled carbon nano-tubes, aluminum nitrate and dodecyl sodium sulfate being weighed according to mass ratio 100:100:0.1 and mix, employing N-METHYLFORMAMIDE is solvent, and the mass ratio of mixture and solvent is 1:10.By mechanical agitation by both mix homogeneously, whipping temp is 100 DEG C, and mixing time is 3h.To be mixed uniformly after, reduce pressure distilling off solvent, is positioned over 70 DEG C of vacuum drying ovens (1.0 × 102Pa) dry 6 hours, it is cooled to room temperature.Drying sample is positioned in atmosphere furnace, passes into argon (argon flow amount is 200mL/min), be warming up to 1800 DEG C with 15 DEG C/min, be incubated 4h, be cooled to room temperature and take out.Being positioned over by carbonizing production in hydrochloric acid solution (acid solution molar concentration is 4mol/L), stir 3h, mixing speed is 90 revs/min, is washed till neutrality with deionized water after isolated by filtration.It is positioned over vacuum drying oven (1.0 × 10-1Pa) in, dry 60 DEG C dry 12 hours, namely obtain carbon nano tube/graphene complex.
Prepared carbon nano tube/graphene composite properties is as follows: be 200F/g than electric capacity, and specific surface area is 250m2/ g, graphite alkylene degree is 50%.
Embodiment 3
Double-walled carbon nano-tube, aluminum chloride and poly-methyl pyrrole alkanone being weighed according to mass ratio 70:100:0.03, employing acetone is solvent, and the mass ratio of raw material and solvent is 1:6.By mechanical agitation by both mix homogeneously, whipping temp is 30 DEG C, and mixing time is 1.5h.To be mixed uniformly after, reduce pressure distilling off solvent, is positioned over 35 DEG C of vacuum drying ovens (1.0 × 10-1Pa) dry 2h, is cooled to room temperature.Drying sample is positioned in atmosphere furnace, passes into nitrogen (nitrogen flow is 80mL/min), be warming up to 1500 DEG C with 5 DEG C/min, be incubated 2h, be cooled to room temperature and take out.Being positioned over by carbonizing production in sulfuric acid solution (acid solution molar concentration is 1mol/L), stir 2h, mixing speed is 60 revs/min, is washed till neutrality with deionized water after isolated by filtration.It is positioned over vacuum drying oven (1.0 × 10-1Pa) dry 80 DEG C of dry 4h in, namely obtain carbon nano tube/graphene complex.
Prepared carbon nano tube/graphene composite properties is as follows: be 120F/g than electric capacity, and specific surface area is 200m2/ g, graphite alkylene degree is 30%.
Embodiment 4
SWCN and the mixture (SWCN is 1:2 with the mass ratio of double-walled carbon nano-tube) of double-walled carbon nano-tube, aluminium hydroxide and dodecyl sodium sulfate are weighed according to mass ratio 30:100:0.01 and mixes, employing toluene is solvent, and the mass ratio of mixture and solvent is 1:3.By mechanical agitation by both mix homogeneously, whipping temp is 80 DEG C, and mixing time is 4h.To be mixed uniformly after, reduce pressure distilling off solvent, is positioned over 60 DEG C of vacuum drying ovens (1.0 × 10-1Pa) dry 3h, is cooled to room temperature.Drying sample is positioned in atmosphere furnace, passes into nitrogen (nitrogen flow is 80mL/min), be warming up to 1300 DEG C with 4 DEG C/min, be incubated 3h, be cooled to room temperature and take out.Being positioned over by carbonizing production in hydrochloric acid solution (acid solution molar concentration is 0.5mol/L), stir 5h, mixing speed is 40 revs/min, is washed till neutrality with deionized water after isolated by filtration.It is positioned over vacuum drying oven (1.0 × 105Pa) dry 100 DEG C of dry 2h in, namely obtain carbon nano tube/graphene complex.
Prepared carbon nano tube/graphene composite properties is as follows: ratio electric capacity 100F/g, specific surface area 150m2/ g, graphite alkylene degree is 30%.
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.
Claims (6)
1. the preparation method of a carbon nano tube/graphene complex, it is characterised in that: described preparation method includes the mixing of raw material, carbonization and acid cleaning process, specifically comprises the following steps that
(1) mixing of raw material
Weigh CNT, additive and surfactant, CNT, additive and surfactant are 1 ~ 100:100:0.01 ~ 1 mixing in mass ratio, add after the stirring solvent mix homogeneously of 1 ~ 10 times of quality subsequently in mixture and distilling off solvent, be subsequently placed in baking oven and be dried；
(2) carbonization
The raw material that step (1) mixes is put in atmosphere furnace, is incubated after then heating to predetermined temperature, be cooled to room temperature and take out；Charring process parameter is:
Heating rate: 1 DEG C/min～50 DEG C/min
Predetermined temperature: 1100 DEG C～2000 DEG C
Temperature retention time: 0.1h～10h
Protective atmosphere: N2Or Ar2
Gas flow: 25mL/min～300mL/min；
(3) pickling
Being placed in by step (2) gained carbonizing production in acid solution and stir, deionized water fully washs to neutrality, is then placed in 35～100 DEG C of vacuum drying ovens and is dried 1 ~ 12h, and vacuum is 1.0 × 10-1~1.0×105Pa；Acid cleaning process parameter is:
Acid solution: the one in hydrochloric acid, oxalic acid and sulphuric acid
Acid solution molar concentration: 0.05mol/L～6mol/L
Mixing time: 1～5h
Mixing speed: 25～200 revs/min.
2. the preparation method of a kind of carbon nano tube/graphene complex according to claim 1, it is characterised in that: the CNT adopted in step (1) is the mixing of one or more of SWCN, double-walled carbon nano-tube, multi-walled carbon nano-tubes, functionalization multi-walled carbon nano-tubes, short MWCNTs, industrialization multi-walled carbon nano-tubes, graphitization multi-walled carbon nano-tubes, large diameter thin wall carbon nano-tube and carbon nano-tube fibre.
null3. method according to claim 1，It is characterized in that: the additive adopted in step (1) is aluminum chloride、Aluminum sulfate、Aluminium carbonate、Aluminum acetate、Aluminum nitrate、Aluminium hydroxide、Sodium metaaluminate、Aluminium nitride、Aluminum phosphate、Aluminium silicate、Aluminium carbide、Ten sulfate dihydrate aluminum ammoniums、Metasilicic acid aluminum、Trifluoromethanesulfonic acid aluminum、Trialkylaluminium、Dialkylaluminum chloride、One alkyl al dichloride、Trialkyl tri-chlorination two aluminum、Aluminum isopropylate.、Butyl aluminum、Aluminium acetate、Aluminium triformate、Oxalic acid aluminum、Propanoic acid aluminum、Polyaluminium chloride、Aluminium silicate、Fluoric acid aluminum、Aluminium secondary butylate、Praseodynium aluminum、Triisobutyl aluminium、Oxine aluminum、Aluminum perchlorate、Aluminum monostearate、Aluminium distearate、Aluminum hydroxyacetate、Ethyl aluminum dichloride、AL-PHOSETHYL aluminum tris(ethyl phosphite)、Aluminium acetylacetonate、Aluminium dihydrogen phosphate、Aluminum oleate、Aluminium bromide、Silver iodide、Aluminum ethylate.、Aluctyl.、One in isooctyl acid aluminum and trioctylaluminum.
4. method according to claim 1, it is characterised in that: the surfactant adopted in step (1) is the one of dodecyl sodium sulfate, poly-methyl pyrrole alkanone, polyvinylpyrrolidone, fatty alcohol-polyoxyethylene ether, sodium lauryl sulphate, sodium hexadecyl sulfate, sodium stearyl sulfate, hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, Dodecyl trimethyl ammonium chloride, octyl sodium sulfonate and octyl sodium sulfate.
5. method according to claim 1, it is characterized in that: the solvent adopted in step (1) be water, ethanol, dichloromethane, acetone, chloroform, methanol, oxolane, carbon tetrachloride, hexamethylene, isopropanol, 1,2-trichloroethane, triethylamine, toluene, pyridine, ethylenediamine, butanol, acetic acid, chlorobenzene, dimethylbenzene, N, dinethylformamide, Ketohexamethylene, Hexalin, N, N-dimethyl acetylamide, N-METHYLFORMAMIDE, phenol, dimethyl sulfoxide, ethylene glycol, N-Methyl pyrrolidone, the one in Methanamide, sulfolane and glycerol.
6. method according to claim 1, it is characterised in that: in step (1), whipping temp is 25～150 DEG C, and mixing time is 1～5h；Baking temperature is 35～100 DEG C, and drying time is 1 ~ 12h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107640758A (en) * | 2017-10-30 | 2018-01-30 | 福州大学 | A kind of preparation method of mesoporous carbon/graphene oxide compound |
| CN108579771A (en) * | 2018-03-23 | 2018-09-28 | 福州大学 | A kind of Catalyzed by Modified Bentonite agent of synthesis of dimmer acid |
| CN109181492A (en) * | 2018-08-03 | 2019-01-11 | 无锡泰科纳米新材料有限公司 | A kind of graphene heat radiation coating for electronic component |
| CN112723339A (en) * | 2020-12-11 | 2021-04-30 | 深圳市德方纳米科技股份有限公司 | Array type doped multi-walled carbon nanotube, preparation method thereof and electrode material |
| CN114735676A (en) * | 2022-04-11 | 2022-07-12 | 暨南大学 | Method for preparing carbon nano tube by taking waste snack box as raw material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107640758A (en) * | 2017-10-30 | 2018-01-30 | 福州大学 | A kind of preparation method of mesoporous carbon/graphene oxide compound |
| CN108579771A (en) * | 2018-03-23 | 2018-09-28 | 福州大学 | A kind of Catalyzed by Modified Bentonite agent of synthesis of dimmer acid |
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| CN112723339A (en) * | 2020-12-11 | 2021-04-30 | 深圳市德方纳米科技股份有限公司 | Array type doped multi-walled carbon nanotube, preparation method thereof and electrode material |
| CN114735676A (en) * | 2022-04-11 | 2022-07-12 | 暨南大学 | Method for preparing carbon nano tube by taking waste snack box as raw material |
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