CN108962424B - Graphene conductive film and preparation method thereof - Google Patents
Graphene conductive film and preparation method thereof Download PDFInfo
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- CN108962424B CN108962424B CN201810818935.9A CN201810818935A CN108962424B CN 108962424 B CN108962424 B CN 108962424B CN 201810818935 A CN201810818935 A CN 201810818935A CN 108962424 B CN108962424 B CN 108962424B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention relates to a graphene conductive film and a preparation method thereof, wherein graphene particles are dispersed in a polyaryletherketone matrix to prepare the graphene film with excellent performance, graphene is uniformly dispersed in a solvent under the action of a dispersing agent to prepare the graphene film with high content, and the obtained film has good electrical performance.
Description
Technical Field
The invention relates to a graphene conductive film and a preparation method thereof, belonging to the technical field of polymer composite materials.
Background
As a novel nano material, compared with materials such as carbon nanotubes and the like, the graphene has a stable lattice structure and extremely high current carriers, so that the graphene shows excellent electrical properties, and meanwhile, the graphene material also has good thermal stability and chemical stability, and is an excellent substitute of a high-performance conductive film. The current preparation method of the graphene conductive film mainly comprises a vacuum filtration method, a spin coating method, a self-assembly method, an epitaxial production method and the like, and the raw material component of the graphene conductive film is usually graphene oxide or graphene. The pure graphene film prepared by the method has high graphene content, can give full play to the excellent electrical properties of the graphene material, but the film prepared by the pure graphene has low mechanical strength and cannot meet the process use requirements. In order to improve the mechanical property of the graphene conductive film, the polymer modified graphene conductive film is a better solution: the graphene material and the polymer are mixed to form the film, so that the advantages of excellent electrical property of the graphene and excellent mechanical property of the polymer film can be fully exerted, and the conductive film with excellent comprehensive performance is prepared. But the method is limited by the defects that the graphene material is easy to agglomerate and oxidize and the like, and the problem that the conductivity of the film cannot reach the expected effect due to low graphene content widely exists in the existing graphene polymer film.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a graphene conductive film and a preparation method thereof.
In order to realize the invention, the following technical scheme is adopted:
the graphene conductive film is characterized by comprising the following components in parts by weight:
40-99 parts of polyaryletherketone resin
1-80 parts of graphene
0.1-10 parts of a dispersing agent.
Further, the graphene is subjected to surface treatment by adopting mixed acid of concentrated sulfuric acid and concentrated nitric acid, so that functional groups are generated on the surface of the graphene, and the graphene is washed and dried for later use.
Further, the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 5:1;
furthermore, the dispersing agent is an amphiphilic substance with two end groups of maleimide group and amino group respectively, straight-chain alkane in the middle and 2-10 carbon atoms.
The method for preparing the graphene conductive film is characterized by comprising the following steps: the method comprises the following steps:
(1) dispersing graphene in mixed acid of concentrated sulfuric acid and concentrated nitric acid, wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 5:1, and performing ultrasonic treatment for 12-48h at normal temperature; after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the mixed acid solution, continuously stirring while dropwise adding, washing graphene until filtrate is neutral, and drying for later use;
(2) weighing polyaryletherketone and the graphene obtained in the step (1) according to a ratio, adding the polyaryletherketone and the graphene into a reaction vessel, then adding a trichloromethane solvent, adding a dispersing agent according to a ratio, carrying out ultrasonic treatment until the polyaryletherketone is completely dissolved, and stirring at a high speed for 10-30 minutes until the graphene is uniformly dispersed to obtain a graphene/polyaryletherketone compound;
(3) and flattening the obtained graphene/polyaryletherketone compound into a composite film with uniform thickness, and vacuumizing and drying the composite film in a vacuum oven at 80 ℃ for 8-12 hours to obtain the graphene conductive film.
The innovation point and the technical effect of the invention are as follows:
(1) the polyaryletherketone is added into the graphene conductive film, and has the characteristics of high temperature resistance, cold resistance, excellent mechanical property and the like, so that the toughness of the graphene conductive film is improved;
(2) according to the invention, the graphene is modified by the mixed acid of concentrated sulfuric acid and concentrated nitric acid, and then modified graphene particles are dispersed in the polyaryletherketone matrix to prepare the graphene film with excellent performance, the graphene can be more uniformly dispersed in a solvent under the action of a dispersing agent to prepare the high-content graphene film, and the obtained film has good electrical property;
(3) the invention provides reasonable raw material proportion and process conditions, and ensures the conductivity and mechanical property of the prepared graphene conductive film;
(4) the graphene conductive film provided by the invention has the characteristics of high conductivity, light weight, high temperature resistance, easiness in processing, good mechanical property, capability of adjusting resistivity in a larger range and the like, and has wide application in the fields of aerospace, electronic information and high and new technology.
Detailed Description
The graphene conductive film and the method for manufacturing the same according to the present invention are further described below with reference to specific examples and descriptions, but the present invention is not limited to the following examples.
Example 1
A graphene conductive film comprises the following components in parts by weight:
polyaryletherketone 80 parts
Vacuum-dried graphene 20 parts
1 part of dispersant
The dispersant is straight-chain alkane with two end groups of maleimide group and amino group and the middle of 5 carbon atoms.
The preparation method comprises the following steps:
(1) dispersing graphene in mixed acid (volume ratio is 5: 1) of concentrated sulfuric acid and concentrated nitric acid, and carrying out ultrasonic reaction for 24 hours at normal temperature; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, washing the graphene filtrate to be neutral, and drying for later use;
(2) weighing 80 parts of polyaryletherketone and 20 parts of graphene which is subjected to vacuum drying according to a ratio, completely adding the weighed materials into a beaker, adding 500ml of chloroform serving as a solvent, adding 1 part of straight-chain alkane dispersant with two end groups of maleimide group and amino group and 5 carbon atoms in the middle, carrying out ultrasonic treatment until the polyaryletherketone is completely dissolved, stirring at a high speed for 30 minutes until the polyaryletherketone is uniformly dispersed, and stirring at a speed of 800r/min to obtain a graphene/polyaryletherketone solution;
(3) and pouring the obtained graphene/polyaryletherketone solution on a flat glass plate, flattening the solution to form a composite film with uniform thickness, and vacuumizing and drying the composite film in a vacuum oven at 80 ℃ for 8 hours to obtain the graphene conductive film.
Example 2
A graphene conductive film comprises the following components in parts by weight:
polyaryletherketone 60 parts
80 parts of graphene subjected to vacuum drying
10 portions of dispersant
The dispersant is straight-chain alkane with maleimide group and amino group as two end groups and 6 carbon atoms in the middle.
The preparation method comprises the following steps:
(1) dispersing graphene in mixed acid (volume ratio is 5: 1) of concentrated sulfuric acid and concentrated nitric acid, and carrying out ultrasonic reaction for 36h at normal temperature; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, washing the graphene filtrate to be neutral, and drying for later use;
(2) weighing 60 parts of polyaryletherketone and 80 parts of graphene subjected to vacuum drying according to a proportion, completely adding the weighed materials into a beaker, adding 500ml of chloroform serving as a solvent, adding 10 parts of straight-chain alkane dispersant with two end groups of maleimide group and amino group and 6 carbon atoms in the middle, carrying out ultrasonic treatment until the polyaryletherketone is completely dissolved, stirring at a high speed for 30 minutes until the dispersion is uniform, and stirring at a speed of 800r/min to obtain a graphene/polyaryletherketone solution;
(3) and pouring the obtained graphene/polyaryletherketone solution on a flat glass plate, flattening the solution to form a composite film with uniform thickness, and vacuumizing and drying the composite film in a vacuum oven at 80 ℃ for 8 hours to obtain the graphene conductive film.
Example 3
A graphene conductive film comprises the following components in parts by weight:
99 parts of polyaryletherketone
1 part of graphene subjected to vacuum drying
0.1 part of dispersant
The dispersant is straight-chain alkane with two end groups of maleimide group and amino group and the middle of 5 carbon atoms.
The preparation method comprises the following steps:
(1) dispersing graphene in mixed acid (volume ratio is 5: 1) of concentrated sulfuric acid and concentrated nitric acid, and carrying out ultrasonic reaction for 24 hours at normal temperature; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, washing the graphene filtrate to be neutral, and drying for later use;
(2) weighing 99 parts of polyaryletherketone and 1 part of graphene which is subjected to vacuum drying according to a ratio, completely adding the weighed materials into a beaker, adding 500ml of chloroform serving as a solvent, adding 0.1 part of straight-chain alkane dispersant with two end groups of maleimide group and amino group and 5 carbon atoms in the middle, carrying out ultrasonic treatment until the polyaryletherketone is completely dissolved, stirring at a high speed for 30 minutes until the polyaryletherketone is uniformly dispersed, and stirring at a speed of 800r/min to obtain a graphene/polyaryletherketone solution;
(3) and pouring the obtained graphene/polyaryletherketone solution on a flat glass plate, flattening the solution to form a composite film with uniform thickness, and vacuumizing and drying the composite film in a vacuum oven at 80 ℃ for 8 hours to obtain the graphene conductive film.
Claims (3)
1. A preparation method of a graphene conductive film is characterized by comprising the following steps: the graphene conductive film comprises the following components in parts by weight:
40-99 parts of polyaryletherketone resin
1-80 parts of graphene
0.1 to 10 portions of dispersant
The preparation method comprises the following steps:
(1) dispersing graphene in mixed acid of concentrated sulfuric acid and concentrated nitric acid, wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 5:1, and performing ultrasonic treatment for 12-48h at normal temperature; after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the mixed acid solution, continuously stirring while dropwise adding, washing graphene until filtrate is neutral, and drying for later use;
(2) weighing polyaryletherketone and the graphene obtained in the step (1) according to a ratio, adding the polyaryletherketone and the graphene into a reaction vessel, then adding a chloroform solvent, adding a dispersing agent according to a ratio, carrying out ultrasonic treatment until the polyaryletherketone is completely dissolved, and stirring at a high speed for 10-30 minutes until the graphene is uniformly dispersed to obtain a graphene/polyaryletherketone compound;
(3) and flattening the obtained graphene/polyaryletherketone compound into a composite film with uniform thickness, and vacuumizing and drying the composite film in a vacuum oven at 80 ℃ for 8-12 hours to obtain the graphene conductive film.
2. A graphene conductive film, which is prepared by the preparation method of claim 1.
3. The graphene conductive film according to claim 2, wherein the dispersant is an amphiphilic substance having terminal groups of maleimide group and amino group, a straight-chain alkane in the middle, and 2-10 carbon atoms.
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