CN110872193B - Preparation method of high-thermal-conductivity graphene/chopped carbon fiber composite material - Google Patents
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- CN110872193B CN110872193B CN201811028241.1A CN201811028241A CN110872193B CN 110872193 B CN110872193 B CN 110872193B CN 201811028241 A CN201811028241 A CN 201811028241A CN 110872193 B CN110872193 B CN 110872193B
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Abstract
The invention discloses a preparation method of a high-thermal-conductivity graphene/chopped carbon fiber composite material, which comprises the steps of depositing and molding a graphene layer and chopped carbon fibers in a liquid phase by utilizing the high thermal conductivity of graphene along the in-plane direction and the high thermal conductivity of the carbon fibers along the axial direction, connecting the carbon fibers and the graphene by utilizing the bonding action of polyimide, and finally converting the polyimide into graphene through carbonization and graphitization treatment to prepare the full-carbon high-thermal-conductivity composite material. Traditional graphite alkene material, because the two-dimensional structure of graphite alkene makes it have super high heat conductivility along the horizontal plane, and owing to lack the heat conduction passageway along thickness direction, heat conductivility is relatively poor. According to the invention, the high-efficiency heat conduction channel is built between graphene layers by utilizing the axial high heat conduction of the chopped carbon fibers, so that the high heat performance of the material in the thickness direction is effectively improved, the defect of poor heat conduction in the thickness direction is overcome, and the high-performance heat conduction material is prepared.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a graphene/chopped carbon fiber composite material with high thermal conductivity, in particular to a preparation method of a carbon-based composite material with high thermal conductivity in the thickness direction and the horizontal direction.
Background
With the rapid development of scientific technologies in the fields of computers, communication, aerospace and the like, the power of electronic products is continuously increased, the size of the electronic products is smaller and smaller, and the heat management is more and more difficult, so that greater requirements on the heat conduction performance and the heat dissipation performance of materials are provided. For example, microelectronic die surface temperatures must be maintained at relatively low temperatures (e.g., silicon device < 100 ℃) to ensure high performance operation, which can easily lead to premature aging or damage if adequate thermal management is not provided. Therefore, the development of a high thermal conductivity scattering material capable of effectively channeling heat becomes a key issue for thermal management. The traditional metal heat conduction materials (such as aluminum, copper and the like) have the limitations of high density, high thermal expansion coefficient, easy oxidation, chemical corrosion resistance and the like, so that the ever-increasing heat dissipation requirements are difficult to meet.
Carbon is one of the most closely related and important elements existing in nature and having diverse electron orbital characteristics (sp, sp)2、sp3Hybridization), and further sp2The anisotropy of (b) causes anisotropy of crystals and anisotropy of arrangement thereof, and thus carbon materials having carbon element as a sole constituent element have various properties. Carbon (C)The material has high heat conduction, low density, low thermal expansion, excellent mechanical property and chemical stability, is a heat conduction material with the most development prospect in recent years, and has wide application prospect in the fields of energy, communication, electronics and the like. The carbon fiber and the graphene are two carbon materials with high heat conductivity and high mechanical strength, and are widely applied to various products. The theoretical thermal conductivity of graphene is as high as 3080-5300W/mK, but as a two-dimensional material, the graphene has high thermal conductivity only along the horizontal plane, and the thermal conductivity perpendicular to the graphene layer is short of an effective thermal conduction channel, so that the thermal conductivity of the graphene-based material along the thickness direction is very low and generally does not exceed 10W/mK, and the application of the graphene in thermal management is severely limited. The carbon fiber is a novel carbon material consisting of graphite highly oriented along the axial direction, has ultrahigh heat conductivity along the axial direction besides high strength, and has a heat conductivity coefficient along the axial direction of the fiber as high as 700W/mK.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a preparation method of a graphene/base carbon composite material with high thermal conductivity in the horizontal direction and the thickness direction aiming at the defect that the existing graphene material has obvious anisotropic thermal conductivity, namely the graphene/base carbon composite material has high thermal conductivity (more than 1000W/mK) only in the graphene plane and has too low thermal conductivity (less than 10W/mK) in the thickness direction vertical to the horizontal plane. The prepared composite material has a thermal conductivity coefficient along a plane of more than 800W/mK, and the thermal conductivity along the thickness direction reaches 56W/mK.
The technical purpose of the invention is realized by the following technical scheme.
A preparation method of a high-thermal-conductivity graphene/chopped carbon fiber composite material comprises the following steps:
step 1, uniformly dispersing graphene and carbon fibers in an N, N-dimethylacetamide solution of polyamic acid, performing vacuum filtration or free settling to enable the graphene and the carbon fibers to be freely stacked to form a composite membrane material, replacing a solvent N, N-dimethylacetamide by ethanol impregnation, and performing supercritical drying to obtain a graphene/carbon fiber/polyamic acid composite material;
in step 1, the graphene is a graphene sheet, preferably graphene oxide, or reduced graphene oxide, and the morphology has a lamellar structure, i.e., a graphene oxide sheet, or a reduced graphene oxide sheet.
In step 1, the carbon fibers are chopped carbon fibers, the diameter of the carbon fibers is 5-7 um, and the length of the carbon fibers is 2-5 um.
In step 1, the graphene and the carbon fiber are in an equal mass ratio.
In step 1, the mass percent of the polyamic acid in the N, N-dimethylacetamide solution of the polyamic acid is 1-5 wt%.
In step 1, graphene and carbon fibers are uniformly dispersed by ultrasound.
And 2, placing the graphene/carbon fiber/polyamide acid composite material obtained in the step 1 in a graphite mold, applying pressure and carrying out thermal amination treatment at 300-400 ℃ to obtain the graphene/carbon fiber/polyimide composite material, maintaining the applied pressure unchanged, sequentially carrying out carbonization at 1000-1200 ℃, and carrying out graphitization treatment at 2600-3000 ℃ to obtain the graphene/carbon fiber heat-conducting composite material.
In step 2, the applied pressure is 0.5 to 5MPa, preferably 1 to 3 MPa.
In the step 2, thermal amination treatment is carried out for 10-60 min at the temperature of 300-400 ℃, carbonization is carried out under the atmosphere of inert protective gas, and the inert protective gas is nitrogen, helium or argon, and the thermal amination treatment is carried out in a graphite mold.
In the step 2, carbonization is carried out for 1 to 5 hours at the temperature of 1000 to 1200 ℃, carbonization is carried out under the atmosphere of inert protective gas, and the inert protective gas is nitrogen, helium or argon, and carbonization is carried out in a tubular furnace.
In the step 2, graphitization treatment is carried out for 0.5 to 3 hours at 2600 to 3000 ℃, carbonization is carried out under the atmosphere of inert protective gas, and the inert protective gas is nitrogen, helium or argon, and the graphitization treatment is carried out in a graphite mold.
The technical scheme of the invention is specifically explained as follows:
(1) dissolving polyamide acid in DMAC (dimethylacetamide) to prepare a dilute solution of polyamide acid, then placing graphene sheets and chopped carbon fibers in the solution, and dispersing under ultrasound to obtain the graphene/carbon fiber dispersion solution.
(2) In the process of preparing the graphene/carbon fiber/polyamide acid film, the graphene (sheet) and the carbon fiber can be freely settled to form a film by standing for 24 hours, or a material is obtained by a vacuum filtration method, the graphene (sheet) can form a layer-by-layer stacked structure due to the two-dimensional structure of the graphene, and the chopped carbon fiber can be vertically arranged between graphene layers due to the extremely small thickness of the chopped carbon fiber. And polyamic acid is evenly coated on the surfaces of graphene and carbon fiber, so that the function of an adhesive is achieved, the adhesion between graphene and carbon fiber is enhanced, the material is prevented from being scattered after the solvent is removed, and finally the solvent is removed through supercritical drying, so that the material can be prevented from being contracted and deformed due to the internal stress in the solvent evaporation process.
(3) Polyamic acid is subjected to a thermal amination treatment to be converted into polyimide, which is used as a raw material for industrially producing graphite paper, and the polyimide can be converted into graphene by being subjected to carbonization and graphitization treatments. In the process of carbonization and graphitization which is carried out after thermal amination is performed, the graphite mold applies compressive stress to the material, so that the material can be prevented from being deformed, and the crystal orientation of the polyimide is facilitated, and the performance of the material is influenced. And finally, the lattice defects of the graphene and the carbon fibers can be repaired through graphitization treatment, so that the impurity content is reduced, and the heat conduction performance is improved.
According to the technical scheme, the graphene/carbon fiber/polyimide is subjected to compression molding through the steps, so that the integrity and compactness of the material are improved. The horizontal stacking of graphene gives high horizontal plane thermal conductivity to the material; the axial heat conduction of the chopped carbon fibers provides a channel for heat conduction in the thickness direction of the material; and the graphene produced by polyimide pyrolysis plays a role in connecting carbon fibers and the graphene. Through the structural design, the control of the anisotropic heat conductivity of the carbon-based composite material is realized, and the high-heat-conductivity carbon composite material with the heat conductivity larger than 800W/(m.K) along the plane direction and larger than 56W/(m.K) along the thickness direction is obtained.
Compared with the prior art, the matrix raw materials of the graphene and the carbon fiber are cheap and easy to obtain, and the process is simple. According to the invention, the microstructure ordering of graphene and carbon fiber, the densification and graphitization of the material can be efficiently completed, the graphene/carbon fiber carbon-based composite material with high heat conductivity coefficient along the plane and thickness direction can be obtained, and the comprehensive heat conductivity of the graphene/carbon fiber carbon-based composite material is far superior to that of the traditional graphene and graphite-based composite material.
Drawings
Fig. 1 is a flow chart of a preparation process of the high thermal conductivity graphene/carbon fiber composite material of the present invention.
Detailed Description
The following 6 examples of the present invention are given to further illustrate the present invention and not to limit the scope of the present invention. The supercritical drying can be realized by using commercially available supercritical drying equipment, such as Tousimis supercritical drying device in USA. The size of the short carbon fiber is 5-7 um in diameter and 2-5 um in length, and the short carbon fiber is obtained by adopting commercially available carbon fiber for short cutting. The heat conductivity coefficient was measured using a relaxation resistant LFA467 flash method thermal conductivity meter.
Example 1
The polyamic acid was diluted in DMAC to obtain a polyamic acid solution with a concentration of 2%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers were weighed and dispersed in the polyamic acid solution, respectively. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And (3) placing the obtained composite material in a graphite mold, applying a pressure of 0.5MPa, and performing thermal amination treatment at 350 ℃ for 30min to obtain the graphene/carbon fiber/polyimide composite material. Then the polyimide is thermally treated for 1h at 1000 ℃ in a tubular furnace under the condition of inert gas, so that the polyimide is carbonized into a carbon film. And finally, placing the composite material in a graphite mold, carrying out graphitization treatment for 0.5h at 2600 ℃, and converting the carbon film into a graphene structure to obtain the graphene/carbon fiber composite material. The thermal conductivity of the test material was 805W/(m.K) in the planar direction and 56W/(m.K) in the thickness direction.
Example 2
Polyamide acid is diluted in DMAC to obtain a polyamide acid solution with the concentration of 1%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers are respectively weighed and dispersed in the polyamide acid solution. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And (3) placing the obtained composite material in a graphite mold, applying a pressure of 1MPa, and performing thermal amination treatment at 350 ℃ for 40min to obtain the graphene/carbon fiber/polyimide composite material. Then, the polyimide was carbonized into a carbon film by heat treatment at 1000 ℃ for 4 hours in a tube furnace under an inert gas condition. And finally, placing the composite material in a graphite mold, and carrying out graphitization treatment for 2h at 2800 ℃ to convert the carbon film into a graphene structure, thereby obtaining the graphene/carbon fiber composite material. The thermal conductivity of the test material was 875W/(m.K) in the planar direction and 69W/(m.K) in the thickness direction.
Example 3
Polyamide acid is diluted in DMAC to obtain a polyamide acid solution with the concentration of 5%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers are respectively weighed and dispersed in the polyamide acid solution. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And (3) placing the obtained composite material in a graphite mold, applying a pressure of 3MPa, and performing thermal amination treatment at 400 ℃ for 15min to obtain the graphene/carbon fiber/polyimide composite material. Then the polyimide is thermally treated for 1h at 1000 ℃ in a tubular furnace under the condition of inert gas, so that the polyimide is carbonized into a carbon film. And finally, placing the composite material in a graphite mold, carrying out graphitization treatment for 0.5h at 3000 ℃, and converting the carbon film into a graphene structure to obtain the graphene/carbon fiber composite material. The thermal conductivity of the test material was 915W/(m.K) in the planar direction and 63W/(m.K) in the thickness direction.
Example 4
Polyamide acid is diluted in DMAC to obtain a polyamide acid solution with the concentration of 3%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers are respectively weighed and dispersed in the polyamide acid solution. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And (3) placing the obtained composite material in a graphite mold, applying a pressure of 3MPa, and performing thermal amination treatment at 300 ℃ for 60min to obtain the graphene/carbon fiber/polyimide composite material. Then the polyimide is thermally treated for 5 hours at 1000 ℃ in a tubular furnace under the condition of inert gas, so that the polyimide is carbonized into a carbon film. And finally, placing the composite material in a graphite mold, carrying out graphitization treatment for 1h at 3000 ℃, and converting the carbon film into a graphene structure to obtain the graphene/carbon fiber composite material. The thermal conductivity of the test material was 890W/(m.K) in the planar direction and 73W/(m.K) in the thickness direction.
Example 5
Polyamide acid is diluted in DMAC to obtain a polyamide acid solution with the concentration of 1%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers are respectively weighed and dispersed in the polyamide acid solution. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And (3) placing the obtained composite material in a graphite mold, applying a pressure of 1MPa, and performing thermal amination treatment at 360 ℃ for 20min to obtain the graphene/carbon fiber/polyimide composite material. Then the polyimide is thermally treated for 3 hours at 1000 ℃ in a tubular furnace under the condition of inert gas, so that the polyimide is carbonized into a carbon film. And finally, placing the composite material in a graphite mold, carrying out graphitization treatment for 3h at 2600 ℃, and converting the carbon film into a graphene structure to obtain the graphene/carbon fiber composite material. The thermal conductivity of the test material was 811W/(mK) in the planar direction and 57W/(mK) in the thickness direction.
Example 6
Polyamide acid is diluted in DMAC to obtain a polyamide acid solution with the concentration of 5%, and then 0.5g of reduced graphene oxide (rGO) and 0.5g of chopped carbon fibers are respectively weighed and dispersed in the polyamide acid solution. Placing the mixture in an ultrasonic disperser, and performing ultrasonic treatment for 2 hours to obtain uniform dispersion liquid. Standing the dispersion liquid for 24 hours to enable the rGO and the carbon fibers to freely settle, removing the upper-layer liquid, replacing a solvent DMAC by ethanol immersion, and then carrying out supercritical drying on the composite material to obtain the graphene/carbon fiber/polyamide acid composite material.
And placing the obtained composite material in a graphite mold, applying a pressure of 2MPa, and performing thermal amination treatment at 360 ℃ for 10min to obtain the graphene/carbon fiber/polyimide composite material. Then the polyimide is thermally treated for 2 hours at 1000 ℃ in a tubular furnace under the condition of inert gas, so that the polyimide is carbonized into a carbon film. And finally, placing the composite material in a graphite mold, carrying out graphitization treatment for 2h at 3000 ℃, and converting the carbon film into a graphene structure to obtain the graphene/carbon fiber composite material. The thermal conductivity of the test material was 901W/(m.K) in the planar direction and 72W/(m.K) in the thickness direction.
The preparation process parameters are adjusted according to the content of the invention, the preparation of the graphene/chopped carbon fiber composite material can be realized, the performance basically consistent with the invention is shown, the heat conductivity coefficient of the prepared composite material along the plane can reach 800-900W/mK, and the heat conductivity along the thickness direction can reach 56-75W/mK. 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. The preparation method of the high-thermal-conductivity graphene/chopped carbon fiber composite material is characterized by comprising the following steps of:
step 1, uniformly dispersing graphene and carbon fibers in an N, N-dimethylacetamide solution of polyamic acid, performing vacuum filtration or free settling to enable the graphene and the carbon fibers to be freely stacked to form a composite membrane material, replacing a solvent N, N-dimethylacetamide by ethanol impregnation, and performing supercritical drying to obtain a graphene/carbon fiber/polyamic acid composite material; the carbon fibers are chopped carbon fibers, the diameter of the carbon fibers is 5-7 mu m, and the length of the carbon fibers is 2-5 mu m;
and 2, placing the graphene/carbon fiber/polyamide acid composite material obtained in the step 1 in a graphite mold, applying pressure and carrying out thermal amination treatment at 300-400 ℃ to obtain the graphene/carbon fiber/polyimide composite material, maintaining the applied pressure unchanged, sequentially carrying out carbonization at 1000-1200 ℃, and carrying out graphitization treatment at 2600-3000 ℃ to obtain the graphene/carbon fiber heat-conducting composite material.
2. The preparation method of the high thermal conductivity graphene/chopped carbon fiber composite material according to claim 1, wherein in step 1, the graphene is graphene oxide sheets or graphene oxide sheets are reduced.
3. The preparation method of the high thermal conductivity graphene/chopped carbon fiber composite material according to claim 1, wherein in the step 1, the mass ratio of the graphene to the carbon fiber is equal.
4. The preparation method of the high thermal conductivity graphene/chopped carbon fiber composite material according to claim 1, wherein in the step 1, the mass percentage of the polyamic acid in the N, N-dimethylacetamide solution of the polyamic acid is 1-5 wt%.
5. The preparation method of the high-thermal-conductivity graphene/chopped carbon fiber composite material according to claim 1, wherein in the step 2, the applied pressure is 0.5-5 MPa.
6. The method for preparing the graphene/chopped carbon fiber composite material with high thermal conductivity according to claim 1, wherein in the step 2, the applied pressure is 1-3 MPa.
7. The method for preparing a graphene/chopped carbon fiber composite material with high thermal conductivity according to claim 1, wherein in step 2, thermal amination treatment is performed at 300-400 ℃ for 10-60 min, carbonization is performed under an inert protective gas atmosphere, the inert protective gas is nitrogen, helium or argon, and thermal amination treatment is performed in a graphite mold.
8. The method for preparing the graphene/chopped carbon fiber composite material with high thermal conductivity according to claim 1, wherein in the step 2, the graphene/chopped carbon fiber composite material is carbonized at 1000-1200 ℃ for 1-5 hours under an inert protective gas atmosphere, the inert protective gas is nitrogen, helium or argon, and the carbonization is selectively performed in a tube furnace.
9. The method for preparing a graphene/chopped carbon fiber composite material with high thermal conductivity according to claim 1, wherein in step 2, graphitization treatment is performed at 2600-3000 ℃ for 0.5-3 hours, carbonization is performed under an inert shielding gas atmosphere, and the inert shielding gas is nitrogen, helium or argon, and graphitization treatment is performed in a graphite mold.
10. The preparation method of the high-thermal-conductivity graphene/chopped carbon fiber composite material as claimed in claim 1, wherein the thermal conductivity of the graphene/chopped carbon fiber composite material along a plane can reach 800-900W/mK, and the thermal conductivity along the thickness direction can reach 56-75W/mK.
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