CN110885079A - Preparation method of novel graphene-carbon nanotube composite material - Google Patents
Preparation method of novel graphene-carbon nanotube composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a novel graphene-carbon nanotube composite material, which comprises the steps of carrying out in-situ stripping on 40-50 layers of multi-walled carbon nanotubes to obtain a carbon nanotube solution with dozens of layers, adding graphene to prepare a graphene-multi-walled carbon nanotube mixed aqueous solution, then carrying out hydrothermal treatment to realize self-assembly to obtain the graphene-carbon nanotube composite material, providing a novel method for preparing a carbon functional material, and widening the application range of the carbon composite material.
Description
Technical Field
The invention belongs to the field of carbon functional composite materials, and particularly relates to a preparation method of a novel graphene-carbon nanotube composite material.
Background
Carbon Nanotubes (CNTs) and Graphene (Graphene) were discovered in 1991 and 2004, respectively, and have been of interest since the day they were discovered. Despite the numerous enthusiasms raised, it is still the focus of developers in many fields, and graphene and carbon nanotubes have been widely used in many fields due to their many unique and excellent characteristics. Carbon nanotubes and graphene are excellent one-dimensional and two-dimensional carbon materials, respectively, which exhibit one-dimensional and two-dimensional anisotropy, such as electrical conductivity, mechanical properties, thermal conductivity, and the like. In order to combine the advantages of both, graphene and carbon nanotubes have been used together in composite materials. The graphene and carbon nanotube composite material forms a three-dimensional network structure, and the graphene and carbon nanotube composite material shows more excellent performance than any single material, such as better isotropic thermal conductivity, isotropic electrical conductivity, three-dimensional space microporous network and the like, through a synergistic effect between the graphene and carbon nanotube composite material. Based on the properties, the graphene/carbon nanotube composite material has good application prospects in the aspects of super capacitors, solar cells, displays, biological detection, fuel cells and the like. Therefore, the graphene/carbon nanotube composite material is more and more applied by people, and the preparation and application of the graphene/carbon nanotube composite material are more widely concerned.
Graphene is a honeycomb two-dimensional crystal composed of single-layer hexagonal primitive carbon atoms, and is a basic unit for constructing other-dimension carbonaceous materials (such as 0D fullerene, 1D fullerene and 3D graphite). The theoretical specific surface area can reach 2600 m2/g, and the conductive performance and the mechanical performance are outstanding at room temperature, and the electron mobility is high. Compared with two-dimensional crystal graphene, the three-dimensional graphene has higher specific surface area and activity than the two-dimensional graphene, so that the three-dimensional graphene has important application value in the fields of catalysis, sensing, environmental protection, energy storage and the like, and more attracts people's extensive attention. Therefore, the prepared graphene-carbon nanotube composite material has wide potential application, and has good effect in both the battery aspect and the mechanical property aspect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a novel graphene-carbon nanotube composite material, the obtained three-dimensional graphene-carbon nanotube network structure composite material has good mechanical properties, a new method is provided for preparing a carbon functional material, and the application range of the carbon composite material is widened.
The technical purpose of the invention is realized by the following technical scheme.
A preparation method of a novel graphene-carbon nanotube composite material comprises the following steps:
step 1, in-situ stripping of carbon nanotubes
Placing the multi-walled carbon nanotube in concentrated nitric acid, performing reflux treatment at 80-100 ℃ to peel the multi-walled carbon nanotube into carbon nanotubes with less than 20 layers, naturally cooling to room temperature of 20-25 ℃ after the reflux treatment is finished, washing the solid with hydrochloric acid, and performing dialysis drying to obtain the carbon nanotube peeled in situ;
in the step 1, the mass percent of the concentrated nitric acid is 65-68 wt%.
In the step 1, the multi-walled carbon nanotubes comprise 40-50 layers of multi-walled carbon nanotubes.
In the step 1, after cooling to room temperature, washing with dilute hydrochloric acid, dialyzing the obtained solid with deionized water, washing to remove impurities on the surface, washing to neutrality, and then placing in an oven with the temperature of 80-100 ℃ for drying treatment for 8-12 h to obtain the in-situ stripped carbon nano tube.
In step 1, the reflux treatment is carried out at 60 to 80 ℃ for 10 to 20 hours, preferably 12 to 16 hours.
In step 1, the mass percent of the dilute hydrochloric acid is 5-8 wt%.
In step 1, the carbon nanotubes are exfoliated in situ in 10-16 layers.
Step 2, placing the in-situ peeled carbon nano tube obtained in the step 1 in a graphene dispersion solution, and uniformly dispersing the carbon nano tube and graphene in the solution to form a graphene-carbon nano tube mixed solution;
in step 2, the solvent of the mixed solution is water.
In step 2, the graphene is graphene oxide, reduced graphene oxide, or graphene.
In the step 2, the carbon nano tube and the graphene are uniformly dispersed in the solution by adopting a mode of firstly stirring and then ultrasonically dispersing, wherein the stirring speed is 300-500 revolutions per minute, the stirring time is 6-12 hours, the ultrasonic power is 500-800 w, and the ultrasonic time is 1-5 hours.
In step 2, the mass ratio of the in-situ exfoliated carbon nanotubes obtained in step 1 to graphene is (1-3): (1.5-4), preferably in an equal mass ratio.
And 3, carrying out hydrothermal reaction on the mixed solution of the graphene and the carbon nano tube obtained in the step 2 to carry out hydrothermal self-assembly on the graphene and the carbon nano tube to form graphene-carbon nano tube gel, cleaning the gel with deionized water, and then carrying out freeze drying to obtain the graphene-carbon nano tube composite material.
In the step 3, a reaction kettle with a polytetrafluoroethylene lining is selected as a reaction device.
In the step 3, the technological parameters for carrying out the hydrothermal reaction are that the temperature is raised to 80-90 ℃ from the room temperature of 20-25 ℃ at the temperature raising speed of 1-5 ℃ per minute and the reaction is carried out for 1-5 hours with heat preservation, then the temperature is raised to 150-180 ℃ at the temperature raising speed of 1-5 ℃ per minute and the reaction is carried out for 10-15 hours with heat preservation, and after the reaction is finished, the temperature is naturally cooled to the room temperature of 20-25 ℃ to generate the graphene-carbon nanotube gel.
In the step 3, the technological parameters for carrying out the hydrothermal reaction are that the temperature is raised to 80-85 ℃ from the room temperature of 20-25 ℃ at the temperature raising speed of 1-3 ℃ per minute and the reaction is carried out for 1-3 hours in a heat preservation way, then the temperature is raised to 160-180 ℃ at the temperature raising speed of 3-5 ℃ per minute and the reaction is carried out for 12-15 hours in a heat preservation way, and after the reaction is finished, the temperature is naturally cooled to the room temperature of 20-25 ℃ to generate the graphene-carbon nanotube gel.
In step 3, the freeze-drying time is 20 to 24 hours.
The invention provides a novel preparation method of a composite carbon material, which realizes in-situ stripping of multi-walled carbon nanotubes, is uniformly mixed with graphene, and then is subjected to hydrothermal treatment to realize self-assembly, so that the graphene coats the carbon nanotubes, and the graphene-carbon nanotube composite material is obtained.
Drawings
FIG. 1 is a scanning electron microscope image of a carbon nanotube used in the present invention before exfoliation.
FIG. 2 is a scanning electron microscope (1) of the carbon nanotube used in the present invention after exfoliation.
FIG. 3 is a scanning electron microscope (2) of the carbon nanotube used in the present invention after exfoliation.
Fig. 4 is a scanning electron microscope picture of the graphene-carbon nanotube composite material prepared by the present invention.
Detailed Description
The following is a further description of the invention and is not intended to limit the scope of the invention. The mass percentage of the selected concentrated nitric acid is 65-68 wt%. The mass percentage of the dilute hydrochloric acid is 5 wt%. Preparing a graphene oxide solution by adopting a Hummers method, wherein water is used as a solvent, and the concentration of graphene oxide is 50 mg/ml; the control speed is 500 revolutions per minute, and the ultrasonic power is 600 w.
Example 1
1) In-situ stripping of carbon nanotubes: 4g of 40 to 50-layer multi-walled carbon nanotubes were immersed in 80ml of concentrated nitric acid, refluxed at 80 ℃ for 16 hours, filtered, cooled to room temperature, and washed with 5 wt% dilute hydrochloric acid. Dialyzing the obtained solid with deionized water, washing off impurities on the surface, washing the solid to be neutral, finally drying the solid in a drying oven at 100 ℃, and drying for 12 hours to obtain the in-situ stripped carbon nano tube, wherein the number of layers is 13-16;
2) adding 1g of in-situ stripped few-layer carbon nano tubes into 30ml of graphene oxide solution, stirring for 12h, and then carrying out ultrasonic dispersion for 2h to well disperse the carbon nano tubes in the graphene solution to form graphene-carbon nano tube mixed aqueous solution;
3) transferring 15ml of the prepared graphene-carbon nanotube aqueous solution into a reaction kettle with a polytetrafluoroethylene lining, heating to 80 ℃ from room temperature of 25 ℃ at a heating rate of 5 ℃ per minute, carrying out heat preservation reaction for 1 hour, heating to 160 ℃ at a heating rate of 5 ℃ per minute, and carrying out heat preservation reaction for 12 hours. And after the reaction is finished, taking out the reaction kettle, naturally cooling to room temperature, pouring out the generated graphene-carbon nanotube gel, repeatedly washing with deionized water, and freeze-drying for 20 hours to obtain the graphene-carbon nanotube composite material.
Example 2
1) In-situ stripping of carbon nanotubes: 5g of 40 to 50-layer multi-walled carbon nanotubes were immersed in 100ml of concentrated nitric acid, refluxed at 80 ℃ for 20 hours, filtered, cooled to room temperature, and washed with 5 wt% dilute hydrochloric acid. Dialyzing the obtained solid with deionized water, washing off impurities on the surface, washing the solid to be neutral, finally drying the solid in a drying oven at 100 ℃, and drying for 8 hours to obtain the in-situ stripped carbon nano tube, wherein the number of layers is 10-15;
2) adding 2.5g of in-situ stripped few-layer carbon nanotubes into 75ml of graphene oxide solution, stirring for 6 hours, and then carrying out ultrasonic dispersion for 5 hours to well disperse the carbon nanotubes in the graphene solution to form graphene-carbon nanotube mixed aqueous solution;
3) and (2) transferring 50ml of the prepared graphene-carbon nanotube aqueous solution into a reaction kettle with a polytetrafluoroethylene lining, heating to 90 ℃ from the room temperature of 20 ℃ at the heating rate of 3 ℃ per minute, carrying out heat preservation reaction for 3 hours, heating to 180 ℃ at the heating rate of 5 ℃ per minute, and carrying out heat preservation reaction for 10 hours. And after the reaction is finished, taking out the reaction kettle, naturally cooling to room temperature, pouring out the generated graphene-carbon nanotube gel, repeatedly washing with deionized water, and freeze-drying for 20 hours to obtain the graphene-carbon nanotube composite material.
Example 3
1) In-situ stripping of carbon nanotubes: 4g of 40 to 50-layer multi-walled carbon nanotubes were immersed in 100ml of concentrated nitric acid, refluxed at 100 ℃ for 12 hours, filtered, cooled to room temperature, and washed with 5 wt% dilute hydrochloric acid. Dialyzing the obtained solid with deionized water, washing off impurities on the surface, washing the solid to be neutral, finally drying the solid in a drying oven at 100 ℃, and drying for 12 hours to obtain the in-situ stripped carbon nano tube with 10-14 layers;
2) adding 2g of in-situ stripped few-layer carbon nanotubes into 50ml of graphene oxide solution, stirring for 10 hours, and then carrying out ultrasonic dispersion for 1 hour to well disperse the carbon nanotubes in the graphene solution to form graphene-carbon nanotube mixed aqueous solution;
3) and (3) moving 30ml of the prepared graphene-carbon nanotube aqueous solution into a reaction kettle with a polytetrafluoroethylene lining, heating to 85 ℃ from the room temperature of 20 ℃ at the heating rate of 5 ℃ per minute, carrying out heat preservation reaction for 5 hours, heating to 150 ℃ at the heating rate of 3 ℃ per minute, and carrying out heat preservation reaction for 15 hours. And after the reaction is finished, taking out the reaction kettle, naturally cooling to room temperature, pouring out the generated graphene-carbon nanotube gel, repeatedly washing with deionized water, and freeze-drying for 24 hours to obtain the graphene-carbon nanotube composite material.
Example 4
1) In-situ stripping of carbon nanotubes: 5g of 40 to 50-layer multi-walled carbon nanotubes were immersed in 100ml of concentrated nitric acid, refluxed at 100 ℃ for 10 hours, filtered, cooled to room temperature, and washed with 5 wt% dilute hydrochloric acid. Dialyzing the obtained solid with deionized water, washing off impurities on the surface, washing the solid to be neutral, finally drying the solid in an oven at 80 ℃ for 10 hours to obtain the in-situ stripped carbon nano tube, wherein the number of layers is 12-16;
2) adding 2.5g of in-situ stripped few-layer carbon nanotubes into 50ml of graphene oxide solution, stirring for 8 hours, and then carrying out ultrasonic dispersion for 3 hours to well disperse the carbon nanotubes in the graphene solution to form graphene-carbon nanotube mixed aqueous solution;
(3) transferring a small amount of the prepared graphene-carbon nanotube aqueous solution into a reaction kettle with a polytetrafluoroethylene lining, heating to 80 ℃ from room temperature of 20 ℃ at a heating rate of 5 ℃ per minute, carrying out heat preservation reaction for 3 hours, heating to 160 ℃ at a heating rate of 5 ℃ per minute, and carrying out heat preservation reaction for 15 hours. And after the reaction is finished, taking out the reaction kettle, naturally cooling to room temperature, pouring out the generated graphene-carbon nanotube gel, repeatedly washing with deionized water, and freeze-drying for 24 hours to obtain the graphene-carbon nanotube composite material.
As shown in fig. 1-4, the carbon nanotubes before and after in-situ peeling were compared in morphology, and it was found that in-situ peeling of carbon nanotubes, i.e., peeling of multi-walled carbon nanotubes, could be achieved by using the technical solution of the present invention; and after hydrothermal self-assembly and freeze drying, the preparation of the graphene coated carbon nanotube composite material is realized.
The preparation of the graphene-carbon nanotube composite material can be realized by adjusting the process parameters according to the content of the invention, and the graphene-carbon nanotube composite material has the performance basically consistent with that of the invention. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A preparation method of a novel graphene-carbon nanotube composite material is characterized by comprising the following steps:
step 1, in-situ stripping of carbon nanotubes
Placing the multi-walled carbon nanotube in concentrated nitric acid, performing reflux treatment at 80-100 ℃ to peel the multi-walled carbon nanotube into carbon nanotubes with less than 20 layers, naturally cooling to room temperature of 20-25 ℃ after the reflux treatment is finished, washing the solid with hydrochloric acid, and performing dialysis drying to obtain the carbon nanotube peeled in situ;
step 2, placing the in-situ exfoliated carbon nanotubes obtained in the step 1 in a graphene dispersion solution, and uniformly dispersing the carbon nanotubes and graphene in the solution to form a graphene-carbon nanotube mixed solution, wherein the graphene is graphene oxide, reduced graphene oxide or graphene, and the mass ratio of the in-situ exfoliated carbon nanotubes obtained in the step 1 to the graphene is (1-3): (1.5-4);
and 3, performing hydrothermal reaction on the graphene-carbon nanotube mixed solution obtained in the step 2 to perform hydrothermal self-assembly on graphene and carbon nanotubes to form graphene-carbon nanotube gel, cleaning the graphene-carbon nanotube gel with deionized water, and then performing freeze drying to obtain the graphene-carbon nanotube composite material, wherein the technological parameters of the hydrothermal reaction are that the temperature is raised to 80-90 ℃ from the room temperature of 20-25 ℃ at the temperature raising rate of 1-5 ℃ per minute and the temperature is kept for reaction for 1-5 hours, the temperature is raised to 150-180 ℃ at the temperature raising rate of 1-5 ℃ per minute and the temperature is kept for reaction for 10-15 hours, and after the reaction is finished, the graphene-carbon nanotube gel is generated by naturally cooling to the room temperature of 20-25 ℃.
2. The method for preparing a novel graphene-carbon nanotube composite material according to claim 1, wherein in step 1, the mass percent of the concentrated nitric acid is 65-68 wt%, and the mass percent of the dilute hydrochloric acid is 5-8 wt%.
3. The method of claim 1, wherein the step 1 is performed by performing a reflow process at 60-80 ℃ for 10-20 hours, preferably 12-16 hours.
4. The method of claim 1, wherein in step 1, the multi-walled carbon nanotubes comprise 40-50 layers of multi-walled carbon nanotubes, and the in-situ exfoliated carbon nanotubes comprise 10-16 layers.
5. The method for preparing a novel graphene-carbon nanotube composite material according to claim 1, wherein in step 1, after cooling to room temperature, diluted hydrochloric acid is used for washing, the obtained solid is dialyzed with deionized water, impurities on the surface are washed away, the solid is washed to be neutral, and then the solid is placed in an oven at 80-100 ℃ for drying treatment, wherein the drying time is 8-12 h, so that the in-situ exfoliated carbon nanotube is obtained.
6. The method of claim 1, wherein in step 2, the solvent of the mixed solution is water, and the mass ratio of the in-situ exfoliated carbon nanotubes obtained in step 1 to the graphene is equal.
7. The method for preparing a novel graphene-carbon nanotube composite material according to claim 1, wherein in step 2, the carbon nanotubes and the graphene are uniformly dispersed in the solution by stirring and then ultrasonic dispersion, wherein the stirring speed is 300-500 rpm, the stirring time is 6-12 hours, the ultrasonic power is 500-800 w, and the ultrasonic time is 1-5 hours.
8. The method for preparing a novel graphene-carbon nanotube composite material according to claim 1, wherein in step 3, a reaction vessel with a polytetrafluoroethylene lining is selected as a reaction device.
9. The method for preparing a novel graphene-carbon nanotube composite material according to claim 1, wherein in step 3, the hydrothermal reaction is carried out at a temperature of 80-85 ℃ from room temperature of 20-25 ℃ at a temperature rising rate of 1-3 ℃ per minute for 1-3 hours, and then the reaction is carried out at a temperature rising rate of 3-5 ℃ per minute for 12-15 hours, and after the reaction is completed, the graphene-carbon nanotube gel is formed by naturally cooling to room temperature of 20-25 ℃.
10. The method of claim 1, wherein the freeze-drying time in step 3 is 20 to 24 hours.
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| CN112210120A (en) * | 2020-10-10 | 2021-01-12 | 吉林大学 | Heat-conducting filler and preparation method thereof, and polyarylethersulfone heat-conducting composite material and preparation method thereof |
| CN113428851A (en) * | 2021-06-11 | 2021-09-24 | 江苏天奈科技股份有限公司 | Graphene-carbon nanotube composite material, preparation method thereof and prepared graphene-carbon nanotube composite slurry |
| CN114360917A (en) * | 2021-12-09 | 2022-04-15 | 中国科学院高能物理研究所 | Three-dimensional composite material of graphdiyne-carbon nano tube and preparation method and application thereof |
| CN114605667A (en) * | 2022-03-10 | 2022-06-10 | 西安理工大学 | Preparation method of tannic acid functionalized carbon nanotube/graphene composite hydrogel |
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| CN112210120B (en) * | 2020-10-10 | 2021-08-20 | 吉林大学 | Heat-conducting filler and preparation method thereof, and polyarylethersulfone heat-conducting composite material and preparation method thereof |
| CN113428851A (en) * | 2021-06-11 | 2021-09-24 | 江苏天奈科技股份有限公司 | Graphene-carbon nanotube composite material, preparation method thereof and prepared graphene-carbon nanotube composite slurry |
| CN114360917A (en) * | 2021-12-09 | 2022-04-15 | 中国科学院高能物理研究所 | Three-dimensional composite material of graphdiyne-carbon nano tube and preparation method and application thereof |
| CN114360917B (en) * | 2021-12-09 | 2023-09-29 | 中国科学院高能物理研究所 | Graphite alkyne-carbon nano tube three-dimensional composite material and preparation method and application thereof |
| CN114605667A (en) * | 2022-03-10 | 2022-06-10 | 西安理工大学 | Preparation method of tannic acid functionalized carbon nanotube/graphene composite hydrogel |
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