CN110734055A - three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite material and preparation method thereof - Google Patents
three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite materials and a preparation method thereof, wherein the materials are single-walled carbon nanotube reinforced three-dimensional porous graphene flexible skeletons prepared by steps of chemical vapor deposition by taking a mixture of copper powder and single-walled carbon nanotubes which are uniformly mixed by a ball milling method as a template, the method can simply and controllably adjust the content of the single-walled carbon nanotubes in the composite and inhibit the agglomeration of the single-walled carbon nanotubes and graphene sheet layers, the carbon nanotubes and graphene in the composite structure are connected, supported and reinforced, and the composite structure has good mechanical strength and flexibility and can be widely used as flexible electronic materials at .
Description
Technical Field
The invention relates to a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite material and a preparation method thereof, belonging to the field of new energy nano materials.
Background
Three-dimensional porous graphene frameworks, such as graphene foams, water/aerogels, graphene sponges and the like, are of flexible electronic materials which are most concerned in recent years, and are formed by stacking micrometer-scale graphene sheets with different macroscopic orientations, and the three-dimensional porous graphene frameworks still maintain delocalized pi-bond conjugated structures of graphene sheets on a microscopic scale, so that the three-dimensional porous graphene frameworks are beneficial to transmission of electrons, and simultaneously greatly reduce contact electron and solid-liquid interface resistance generally encountered by two-dimensional materials.
Drieschner et al report a graphene foam preparation method, which is obtained by a chemical vapor deposition method using copper/nickel powder as a template, wherein the pore diameter (0.5-1 μm) of the graphene foam obtained by the method is far smaller than that of a three-dimensional porous graphene skeleton obtained by chemical vapor deposition using commercial nickel/copper foam as a template, so that the graphene foam has a higher specific surface area, and the specific capacitance of the graphene foam for an electric double layer supercapacitor electrode is obtained due to the fact that the specific capacitance of the graphene is actually represented (100F g)-1) And theoretical specific capacitance of graphene (-550F g)-1) The reason for this is thatThe large diameter of the copper particles and the loose form of the template result in a material with still large pore sizes, which provides a limited increase in the surface area. In addition, since the pore size is large but the pore walls are thin, the foam is easily broken when pressed or bent, and the flexibility and mechanical strength are insufficient.
The problems of low specific surface area, insufficient flexibility and insufficient mechanical strength of the material can be greatly improved by combining the three-dimensional porous graphene framework and the carbon nano tubes, because the carbon nano tubes have excellent flexibility, unique tubular structures, abundant mesopores and easy chemical modification, and the properties can bring more choices for improving the performance of the composite material, but a simple, efficient and controllable method for preparing the three-dimensional porous graphene framework-carbon nano tube composite is lacked at present, the carbon nano tubes are easy to wind into bundles at so as to reduce the effective area and the charge transmission efficiency, the carbon nano tubes are difficult to be uniformly distributed in the graphene framework at , and the preparation methods of reported at present are relatively complex and uncontrollable, such as a liquid phase composite method (a hydrothermal/solvothermal method and the like), a chemical vapor deposition method adopting commercial templates (copper foil, copper foam/nickel) and a binder-assisted synthesis method and the like.
Therefore, the preparation method of simple, controllable and efficient prepared three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite materials is researched, and the preparation method has great significance for the application of the graphene-carbon nanotube composite flexible materials in the field of wearable electronics.
Disclosure of Invention
The invention aims to provide three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite materials and a preparation method thereof.
The material is characterized in that a carbon nano tube and graphene are connected, supported and reinforced with each other, the material is a flexible composite material with a hierarchical porous structure, the flexible composite material is prepared by -step chemical vapor deposition, a template of the chemical vapor deposition is obtained by uniformly mixing copper powder and single-walled carbon nano tubes by using a ball milling method and tabletting, the single-walled carbon nano tubes are preassembled into the copper powder template by using ball milling in advance, so that the solid-solid physical mixing method is simple to operate, the content of the carbon nano tubes in the graphene-single-walled carbon nano tube composite can be controllably adjusted by adjusting the amount of the carbon nano tubes added into the copper powder (ball milling process), the graphene-copper powder tabletting is used for reducing gaps in the copper powder-single-walled carbon nano tube mixture, and the water/gas gel material which is higher in specific surface area, mechanical strength and flexibility than foamed graphene is obtained after the chemical vapor deposition has the advantages of no binder, low cost, simplicity and convenience in operation, simple equipment, suitability for .
The technical scheme of the invention is as follows:
the three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite material is flexible composite materials with hierarchical porous structures, the matrix of the composite material is a three-dimensional porous graphene skeleton obtained by chemical vapor deposition with copper powder as a template, single-walled carbon nanotubes embedded in the skeleton are pre-assembled in the copper powder template by ball milling in advance, and the content of the carbon nanotubes in the composite can be controllably adjusted by simply adjusting the amount of the carbon nanotubes added into the copper powder (ball milling process).
The preparation principle is that nano copper powder with a fixed particle size and single-walled carbon nanotubes are uniformly mixed according to a mass ratio of by a ball milling method, and then are pressed into copper powder-single-walled carbon nanotube self-supporting square blocks by a powder tablet press, wherein the content of the carbon nanotubes in the graphene-single-walled carbon nanotube composite can be controllably adjusted by adjusting the amount of the carbon nanotubes added into the copper powder (ball milling process).
The preparation process of the invention comprises the following steps:
(1) preparing a nanometer copper powder-single-walled carbon nanotube composite template: adding 3-6 g of nano copper powder (with the diameter of 200-2000 nm) and 0.5-10 mg of single-walled carbon nanotube powder into a 50ml closed agate tank filled with inert gas (nitrogen or argon), fixing the tank in a ball mill, ball-milling for 4-10 h at the rotating speed of 400-800 rpm, placing the ball-milled single-walled carbon nanotube-nano copper powder composite in a square mold (2 x 2cm), pressing the powder into a self-supporting square block (2 x 2cm) at the pressure of 10-20 MPa by using a powder tablet press, and taking the block as a template for chemical vapor deposition.
(2) Preparing a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible compound: directly placing the self-supporting square block obtained in the step (1) into a quartz tube furnace, keeping the pressure in the tube at 500-8000 Pa, raising the temperature to 850-1050 ℃ at the speed of 10-30 ℃/min under the protection of high-purity argon (50-200 sccm), preserving the temperature for 20-60 min, fully annealing the square template, then performing chemical vapor deposition by taking methane as a carbon source, and then placing the self-supporting square block deposited with the graphene framework into a quartz tube furnace with the concentration of 1-3 mol L-1FeSO of (2)4Placing the solution at 60-100 ℃ for 6-48 hours, taking out the solution until the sample floats on the surface of the solution, repeatedly cleaning the solution by using dilute hydrochloric acid (1-3M), concentrated nitric acid and deionized water respectively, and freeze-drying the solution; putting the dried three-dimensional single-walled carbon nanotube-graphene skeleton into a quartz tube furnace, and heating for 30-60 minutes at 400-500 ℃ under the protection of high-purity argon (10-100 sccm); and pressing the obtained aerogel into a tablet by using a powder tablet press, and fixing the aerogel onto a flexible conductive film by using conductive silver paste to serve as a flexible electrode.
The composite material has the advantages that the composite material has a hierarchical porous structure and good flexibility, the carbon nano tubes are added into a graphene framework to achieve the effects of connecting, supporting and reinforcing the framework, the mechanical strength of the framework is increased, the flexibility of the framework structure is greatly enhanced due to the excellent flexibility of the carbon nano tubes, the composite material is prepared by a conventional -step chemical vapor deposition method, a template for chemical vapor deposition is obtained by uniformly mixing copper powder and single-walled carbon nano tubes by a ball milling method and tabletting, the single-walled carbon nano tubes are pre-assembled into the copper powder template by ball milling in advance, the solid-solid physical mixing method is simple to operate, the content of the carbon nano tubes in the graphene-single-walled carbon nano tube composite can be controllably adjusted by adjusting the amount of the added copper powder (ball milling process), the graphene-copper powder tabletting is used for reducing gaps in the mixture of the copper powder-single-walled carbon nano tubes, and the water/gas gel material which is higher in specific surface area, mechanical strength and flexibility than foamed graphene after chemical vapor deposition is obtained.
Drawings
Fig. 1 is a macroscopic digital photograph of the three-dimensional porous graphene framework-single-walled carbon nanotube flexible electrode prepared in example 1;
fig. 2 is a scanning electron microscope photograph of the three-dimensional porous graphene framework-single-walled carbon nanotube composite material prepared in example 1.
Fig. 3 is a transmission electron microscope photograph of the three-dimensional porous graphene framework-single-walled carbon nanotube composite material prepared in example 1.
Detailed Description
The invention will now be described in further detail with reference to the following figures and examples.
Example 1
Preparing a nanometer copper powder-single-walled carbon nanotube composite template: adding 5g of nano copper powder (with the diameter of 200-2000 nm) and 2mg of single-walled carbon nanotube powder into a 50ml closed agate tank filled with inert gas (nitrogen or argon), fixing the tank in a ball mill, carrying out ball milling for 6h at the rotating speed of 600rpm, placing the ball-milled single-walled carbon nanotube-nano copper powder composite in a square mold (2 x 2cm), pressing the powder into a self-supporting square block (2 x 2cm) at the pressure of 20MPa by using a powder tablet press, and taking the block as a template for chemical vapor deposition.
Preparing a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible compound: directly placing the self-supporting square block obtained in the step (1) into a quartz tube furnace, keeping the pressure in the tube at 1000Pa, raising the temperature to 1000 ℃ at the speed of 30 ℃/min under the protection of high-purity argon (200sccm), preserving the temperature for 30min, fully annealing the square template, then performing chemical vapor deposition by taking methane as a carbon source, and then placing the self-supporting square block deposited with the graphene framework into a quartz tube furnace with the concentration of 2mol L-1FeSO of (2)4In solution, after standing at 80 ℃ for 48 hours until the sample drifted in solutionTaking out the solution after the surface of the solution is finished, repeatedly washing the solution by using dilute hydrochloric acid (2M), concentrated nitric acid and deionized water respectively, and freeze-drying the solution; placing the dried three-dimensional single-walled carbon nanotube-graphene skeleton into a quartz tube furnace, and heating at 500 ℃ for 30 minutes under the protection of high-purity argon (500sccm), wherein macroscopic digital photographs of the prepared three-dimensional porous graphene skeleton-single-walled carbon nanotube aerogel under the conditions are respectively shown in fig. 1 a; and pressing the obtained aerogel into a tablet by using a powder tablet press, and fixing the aerogel onto a flexible conductive film by using conductive silver paste to serve as a flexible electrode. The macroscopic digital photograph, the scanning electron microscope photograph and the transmission electron microscope photograph of the three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite prepared under the condition are respectively shown in fig. 1b, fig. 2 and fig. 3.
Example 2
Preparing a nanometer copper powder-single-walled carbon nanotube composite template: adding 5g of nano copper powder (with the diameter of 200-2000 nm) and 4mg of single-walled carbon nanotube powder into a 50ml closed agate tank filled with inert gas (nitrogen or argon), fixing the tank in a ball mill, carrying out ball milling for 6h at the rotating speed of 600rpm, placing the ball-milled single-walled carbon nanotube-nano copper powder compound in a square mold (2 x 2cm), pressing the powder into a self-supporting square block (2 x 2cm) at the pressure of 20MPa by using a powder tablet press, and taking the block as a template for chemical vapor deposition.
Preparing a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible compound: directly placing the self-supporting square block obtained in the step (1) into a quartz tube furnace, keeping the pressure in the tube at 1000Pa, raising the temperature to 1000 ℃ at the speed of 30 ℃/min under the protection of high-purity argon (200sccm), preserving the temperature for 30min, fully annealing the square template, then performing chemical vapor deposition by taking methane as a carbon source, and then placing the self-supporting square block deposited with the graphene framework into a quartz tube furnace with the concentration of 2mol L-1FeSO of (2)4Placing the solution at 80 ℃ for 48 hours, taking out the solution until the sample floats on the surface of the solution, repeatedly washing the solution by using dilute hydrochloric acid (2M), concentrated nitric acid and deionized water respectively, and freeze-drying the solution; putting the dried three-dimensional single-walled carbon nanotube-graphene skeleton into a quartz tube furnace, and heating for 30 minutes at 500 ℃ under the protection of high-purity argon (500 sccm);and pressing the obtained aerogel into a tablet by using a powder tablet press, and fixing the aerogel onto a flexible conductive film by using conductive silver paste to serve as a flexible electrode.
Example 3
Preparing a nanometer copper powder-single-walled carbon nanotube composite template: adding 5g of nano copper powder (with the diameter of 200-2000 nm) and 6mg of single-walled carbon nanotube powder into a 50ml closed agate tank filled with inert gas (nitrogen or argon), fixing the tank in a ball mill, carrying out ball milling for 6h at the rotating speed of 600rpm, placing the ball-milled single-walled carbon nanotube-nano copper powder compound in a square mold (2 x 2cm), pressing the powder into a self-supporting square block (2 x 2cm) at the pressure of 20MPa by using a powder tablet press, and taking the block as a template for chemical vapor deposition.
Preparing a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible compound: directly placing the self-supporting square block obtained in the step (1) into a quartz tube furnace, keeping the pressure in the tube at 1000Pa, raising the temperature to 1000 ℃ at the speed of 30 ℃/min under the protection of high-purity argon (200sccm), preserving the temperature for 30min, fully annealing the square template, then performing chemical vapor deposition by taking methane as a carbon source, and then placing the self-supporting square block deposited with the graphene framework into a quartz tube furnace with the concentration of 2mol L-1FeSO of (2)4Placing the solution at 80 ℃ for 48 hours, taking out the solution until the sample floats on the surface of the solution, repeatedly washing the solution by using dilute hydrochloric acid (2M), concentrated nitric acid and deionized water respectively, and freeze-drying the solution; putting the dried three-dimensional single-walled carbon nanotube-graphene skeleton into a quartz tube furnace, and heating for 30 minutes at 500 ℃ under the protection of high-purity argon (500 sccm); and pressing the obtained aerogel into a tablet by using a powder tablet press, and fixing the aerogel onto a flexible conductive film by using conductive silver paste to serve as a flexible electrode.
Claims (2)
- The three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible composite material is characterized by being a flexible self-supporting composite with a hierarchical porous structure, which is obtained by steps of chemical vapor deposition.
- 2. The preparation method of the three-dimensional porous graphene framework-single-walled carbon nanotube flexible composite material as claimed in claim 1, wherein the composite material is prepared by low-pressure chemical vapor deposition using methane as a carbon source, and is characterized in that a template for chemical vapor deposition is obtained by ball milling single-walled carbon nanotube powder and nano-copper powder, and the preparation method comprises the following specific steps:(1) preparing a nanometer copper powder-single-walled carbon nanotube composite template: adding 3-6 g of nano copper powder (with the diameter of 200-2000 nm) and 0.5-10 mg of single-walled carbon nanotube powder into a 50ml closed agate tank filled with inert gas (nitrogen or argon), fixing the tank in a ball mill, ball-milling for 4-10 h at the rotating speed of 400-800 rpm, and placing the ball-milled single-walled carbon nanotube-nano copper powder composite in a square mold (2 multiplied by 2cm and 2cm)2) In the method, powder is pressed into a self-supporting square block (2 multiplied by 0.2 cm) by a powder tablet press at the pressure of 10-20 MPa3) The block is used as a template for the subsequent chemical vapor deposition;(2) preparing a three-dimensional porous graphene skeleton-single-walled carbon nanotube flexible compound: directly placing the self-supporting square block obtained in the step (1) into a quartz tube furnace, keeping the pressure in the tube at 500-8000 Pa, raising the temperature to 850-1050 ℃ at the speed of 10-30 ℃/min under the protection of high-purity argon (50-200 sccm), preserving the temperature for 20-60 min, fully annealing the square template, performing chemical vapor deposition reaction for 10-60 min by using methane (4-10 sccm) as a carbon source and hydrogen (10-20 sccm) as a reducing gas, then reducing the temperature to room temperature at the fastest speed, taking out the self-supporting square block deposited with graphene, and placing the self-supporting square block in a quartz tube furnace with the concentration of 1-3 mol L-1FeSO of (2)4Placing the solution at 60-100 ℃ for 6-48 hours, taking out the solution until the sample floats on the surface of the solution, repeatedly cleaning the solution by using dilute hydrochloric acid (1-3M), concentrated nitric acid and deionized water respectively, and freeze-drying the solution; putting the dried three-dimensional single-walled carbon nanotube-graphene skeleton into a quartz tube furnace, and heating for 30-60 minutes at 400-500 ℃ under the protection of high-purity argon (10-100 sccm); and pressing the obtained aerogel into a tablet by using a powder tablet press, and fixing the aerogel onto a flexible conductive film by using conductive silver paste to serve as a flexible electrode.
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