CN108929521B - High-thermal-conductivity and high-electric-conductivity graphene-based composite material and preparation method thereof - Google Patents
High-thermal-conductivity and high-electric-conductivity graphene-based composite material and preparation method thereof Download PDFInfo
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- CN108929521B CN108929521B CN201810728632.8A CN201810728632A CN108929521B CN 108929521 B CN108929521 B CN 108929521B CN 201810728632 A CN201810728632 A CN 201810728632A CN 108929521 B CN108929521 B CN 108929521B
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Abstract
The invention discloses a high-thermal-conductivity and high-electric-conductivity graphene-based composite material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) adding a reducing agent into the graphene oxide dispersion liquid, stirring uniformly, then immersing commercial sponge into the mixture, sealing, heating for reaction, and drying to obtain graphene-based sponge; (2) and (3) pouring a polymer material into the graphene sponge, and curing to obtain the graphene-based composite material. According to the invention, the using amount of graphene is greatly reduced, the production cost is reduced, and the heat conductivity and the electric conductivity of the prepared composite material are greatly improved. And the preparation method is simple and easy to implement, low in cost and easy for large-scale production.
Description
Technical Field
The invention relates to a composite material and a preparation method thereof, in particular to a high-thermal-conductivity and high-electric-conductivity graphene-based composite material and a preparation method thereof.
Background
For electronic and optoelectronic devices, excellent thermal conduction and dissipation properties of materials are critical to their long-life high performance (s.int.j.heat Mass Transfer 2006, 49, 1658-. Polymer materials are widely used in these devices, but all have the problem of poor heat conduction and dissipation, so recently, researchers have paid extensive attention to how to improve the heat conduction and dissipation performance of these polymers. The graphene has great attention due to the ultrahigh thermal conductivity, large specific surface area and excellent mechanical property, and has great potential in improving the thermal conductivity of the polymer. The traditional preparation method of the graphene-based composite material mainly comprises the steps of dispersing graphene powder in a polymer (chem.Phys.Lett.2012, 531, 6-10; composite.Sci.Technol.2012, 70, 2176-. However, the method needs a large amount of graphene (> 0.5 wt%), which not only increases the cost of the composite material, but also causes the mechanical property of the composite material to be reduced, and the thermal conductivity of the obtained composite material is not more than 5.5W/mK at most (Nano Lett.2012, 12, 861-867).
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems in the prior art, the invention provides a graphene-based composite material with high thermal conductivity and high electric conductivity.
The invention also aims to provide a preparation method of the graphene-based composite material with high thermal conductivity and high electric conductivity.
The technical scheme is as follows: the preparation method of the high-thermal-conductivity and high-electric-conductivity graphene-based composite material comprises the following steps:
(1) adding a reducing agent into the graphene oxide dispersion liquid, stirring uniformly, then immersing commercial sponge into the mixture, sealing, heating for reaction, and drying to obtain graphene-based sponge;
(2) and (3) pouring a polymer material into the graphene sponge, and curing to obtain the graphene-based composite material.
In the step (1), the graphene oxide dispersion liquid is composed of graphene oxide and water. The graphite oxide can be stripped in water by ultrasonic wave. The concentration of the graphene oxide in the graphene oxide dispersion liquid is 0.3-3mg/ml, preferably 1-3 mg/ml.
In the step (1), the reducing agent is hydrazine hydrate or vitamin C,
when the reducing agent is hydrazine hydrate, the mass ratio of the hydrazine hydrate to the graphene oxide is (1-3) to 7, the reaction temperature is 70-95 ℃, preferably 90-95 ℃, and the reaction time is 0.5-5 h, preferably 0.5-2 h;
when the reducing agent is vitamin C, the mass ratio of the vitamin C to the graphene oxide is (1-5) to 1, preferably 1 to 1. The reaction temperature is 60-90 ℃, and the reaction time is 3-8 h.
In the step (1), the commercial sponge is melamine sponge, polyurethane sponge or polyvinyl alcohol sponge.
In the step (2), the polymer material is epoxy resin, polyvinyl chloride, polyethylene, polypropylene, polystyrene, ABS resin, polymethyl methacrylate, polyamide, polycarbonate, phenolic resin, urea resin, melamine formaldehyde resin, polyvinylidene rubber or polydimethylsiloxane. The amount of the polymer material is only required to be completely filled with the graphene-based sponge.
In step (2), the polymer material assumes a flow state upon infusion.
The graphene-based composite material with high thermal conductivity and high electric conductivity is prepared by the method.
The content of graphene in the graphene-based composite material is 0.02-0.09 wt%, and preferably 0.04-0.09 wt%.
The thermal conductivity of the graphene-based composite material is 5-45W/mK, preferably 23-45W/mK, and the electrical conductivity is 1-10S/m, preferably 4.5-10S/m.
The high-thermal-conductivity and high-electric-conductivity graphene-based composite material disclosed by the invention is applied to preparation of electronic devices or photoelectric devices.
According to the invention, graphene is firstly self-assembled on a commercial sponge framework to form a conductive path, and then the conductive path is compounded with a polymer material, so that the conductive path can be realized by using the least graphene, and the heat conductivity and the electric conductivity of the obtained composite material are basically unchanged or are greatly improved while the using amount of the graphene is greatly reduced.
Has the advantages that:
1. in the prior art, the minimum use amount of graphene is 0.5 wt%, the use amount of graphene is greatly reduced, the production cost is reduced, and the obtained composite material has good mechanical property.
2. According to the invention, the self-assembly of graphene is realized by means of the skeleton of the commercial sponge to form a heat conduction and electric conduction path, so that the graphene-based sponge can be produced in large scale, and then the polymer material is poured into the graphene-based sponge, so that the large-size graphene-based composite material can be easily prepared and can be produced in large scale;
3. the method provided by the invention is simple and easy to implement, low in cost, green and environment-friendly, and suitable for large-scale production.
Drawings
FIG. 1 is a graphene-based sponge;
fig. 2 shows a graphene/epoxy resin composite material obtained after epoxy resin is poured into graphene-based sponge and cured.
Detailed Description
The present invention will be described in detail with reference to the following examples.
The following examples graphene content, electrical conductivity, thermal conductivity test methods:
calculating the content of graphene: [ (graphene sponge mass-commercial sponge mass)/graphene composite mass ]. 100%
And (3) conductivity test: the resistivity is measured by a standard four-probe method (ST 2253digital four-point probe, Suzhou junction electronic Co. Ltd. China), and then the reciprocal is taken
And (3) testing thermal conductivity: thermal conductivity tester (NETZSCH LFA447 Nanofllash (Germany))
Example 1:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 14mg of hydrazine hydrate, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 2 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge as shown in figure 1;
4. mixing the two components of the epoxy resin according to a general proportion, and then pouring the mixture into the graphene-based sponge;
5. and after the pouring, putting the obtained product into an oven, maintaining the temperature at 60 ℃ for 1h, maintaining the temperature at 90 ℃ for 1h, and maintaining the temperature at 120 ℃ for 1h to obtain the required graphene/epoxy resin composite material, wherein the obtained product is shown in figure 2.
The graphene content of this example was measured to be about 0.05 wt%, conductivity: 6S/m, thermal conductivity: 27W/mK.
Example 2:
1. weighing 30mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 0.3mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 8.5mg of hydrazine hydrate, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 70 ℃ for 5 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. the two components of dow corning 184: mixing the prepolymer A and the cross-linking agent B according to the mass ratio of 10: 1, and then pouring the mixture into the graphene-based sponge;
5. after the pouring, the obtained product is put into an oven and maintained at 120 ℃ for 2 hours, and the required graphene/polydimethylsiloxane composite material can be obtained, similarly as shown in fig. 2.
The graphene content of this example was measured to be about 0.02 wt%, conductivity: 1S/m, thermal conductivity: 5W/mK
Example 3:
1. weighing 300mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 3mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, adding 128mg of hydrazine hydrate, and uniformly stirring;
2. placing polyurethane sponge in the solution, sealing the beaker, and placing the beaker in an oven at 95 ℃ for 0.5 h;
3. taking out the polyurethane sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. adding polyvinyl chloride into the graphene-based sponge, melting at 170 ℃, and pouring the melted polyvinyl chloride into the graphene-based sponge;
5. and after the pouring, naturally cooling to obtain the required graphene/polyvinyl chloride composite material, which is similar to that shown in figure 2.
The graphene content of this example was measured to be about 0.09 wt%, conductivity: 10S/m, thermal conductivity: 45W/mK
Example 4:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 60 ℃ for 8 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. heating polyethylene to the melting point (105-135 ℃) of the polyethylene, and pouring the polyethylene into the graphene-based sponge after the polyethylene is melted;
5. after the pouring, the graphene/polyethylene composite material is obtained by natural cooling, which is similar to that shown in fig. 2.
The graphene content of this example was measured to be about 0.06 wt%, conductivity: 6.5S/m, thermal conductivity: 29W/mK
Example 5:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 70 ℃ for 5 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. heating polypropylene to the melting point (160 ℃) of the polypropylene to be melted, and then pouring the polypropylene into the graphene-based sponge;
5. after the pouring, the graphene/polypropylene composite material is naturally cooled, and the required graphene/polypropylene composite material can be obtained, similarly as shown in fig. 2.
The graphene content of this example was measured to be about 0.07 wt%, conductivity: 7S/m, thermal conductivity: 33W/mK
Example 6:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. heating polystyrene to the melting point (150-180 ℃) of the polystyrene, and pouring the polystyrene into the graphene-based sponge after the polystyrene is melted;
5. after the pouring, the graphene/polystyrene composite material is obtained by natural cooling, which is similar to that shown in fig. 2.
The graphene content of this example was measured to be about 0.04 wt%, conductivity: 4.5S/m, thermal conductivity: 23W/mK
Example 7:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing polyurethane sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the polyurethane sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. infusing molten ABS resin into the graphene-based sponge;
5. after the pouring, the graphene/ABS resin composite material is obtained by natural cooling, which is similar to that shown in FIG. 2.
The graphene content of this example was measured to be about 0.045 wt%, conductivity: 5S/m, thermal conductivity: 25W/mK
Example 8:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing polyvinyl alcohol sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the polyvinyl alcohol sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. pouring molten polymethyl methacrylate into the graphene-based sponge;
5. after the pouring, the graphene/polymethyl methacrylate composite material can be obtained by natural cooling, which is similar to that shown in fig. 2.
The graphene content of this example was measured to be about 0.055 wt%, conductivity: 6.5S/m, thermal conductivity: 29W/mK
Example 9:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing polyvinyl alcohol sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the polyvinyl alcohol sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. pouring molten polyamide into the graphene-based sponge;
5. after the pouring, the graphene/polyamide composite material is naturally cooled, and the required graphene/polyamide composite material can be obtained, similarly as shown in fig. 2.
The graphene content of this example was measured to be about 0.058 wt%, conductivity: 7.2S/m, thermal conductivity: 31W/mK
Example 10:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing polyvinyl alcohol sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the polyvinyl alcohol sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. pouring molten polycarbonate into the graphene-based sponge;
5. after the pouring, the graphene/polycarbonate composite material is obtained by natural cooling, which is similar to that shown in fig. 2.
The graphene content of this example was measured to be about 0.061 wt%, conductivity: 7.8S/m, thermal conductivity: 29W/mK
Example 11:
1. weighing 100mg of graphite oxide, putting the graphite oxide into 100ml of water, then ultrasonically dispersing for 1h to prepare 1mg/ml of graphene oxide dispersion liquid, taking 100ml out, putting the graphene oxide dispersion liquid into a beaker, then adding 100mg of vitamin C, and uniformly stirring;
2. placing melamine sponge in the solution, sealing the beaker, and placing the beaker in an oven at 90 ℃ for 3 hours;
3. taking out the melamine sponge and drying to obtain the graphene-based sponge, which is similar to the graphene-based sponge shown in figure 1;
4. pouring a thermosetting phenolic resin precursor into the graphene-based sponge;
5. after the pouring, the obtained product is placed in an oven and maintained at 150 ℃ for 2 hours, and the required graphene/phenolic resin composite material can be obtained, similarly as shown in fig. 2.
The graphene content of this example was measured to be about 0.047 wt%, conductivity: 5.9S/m, thermal conductivity: 26.8W/mK.
Claims (10)
1. The preparation method of the graphene-based composite material with high thermal conductivity and high electric conductivity is characterized by comprising the following steps:
(1) adding a reducing agent into the graphene oxide dispersion liquid, stirring uniformly, then immersing commercial sponge into the mixture, sealing, heating for reaction, and drying to obtain graphene-based sponge;
(2) pouring a polymer material into the graphene sponge, and curing to obtain the graphene-based composite material;
the graphene-based composite material contains 0.02-0.09 wt% of graphene.
2. The method according to claim 1, wherein in the step (1), the graphene oxide dispersion liquid is composed of graphene oxide and water, wherein the concentration of the graphene oxide is 0.3-3 mg/ml.
3. The method according to claim 1, wherein in step (1), the reducing agent is hydrazine hydrate or vitamin C,
when the reducing agent is hydrazine hydrate, the mass ratio of the hydrazine hydrate to the graphene oxide is (1-3) to 7, the reaction temperature is 70-95 ℃, and the reaction time is 0.5-5 h;
when the reducing agent is vitamin C, the mass ratio of the vitamin C to the graphene oxide is (1-5) to 1, the reaction temperature is 60-90 ℃, and the reaction time is 3-8 h.
4. The method of claim 1, wherein in step (1), the commercial sponge is a melamine sponge, a polyurethane sponge, or a polyvinyl alcohol sponge.
5. The method according to claim 1, wherein in the step (2), the polymer material is epoxy resin, polyvinyl chloride, polyethylene, polypropylene, polystyrene, ABS resin, polymethyl methacrylate, polyamide, polycarbonate, phenol resin, urea resin, melamine formaldehyde resin, polyvinylidene rubber, or polydimethylsiloxane.
6. The method of claim 1, wherein in step (2), the polymeric material assumes a flow state upon infusion.
7. The graphene-based composite material with high thermal and electrical conductivity prepared by the method of any one of claims 1 to 6.
8. The material according to claim 7, wherein the graphene content in the graphene-based composite material is 0.02-0.09 wt%.
9. The material according to claim 7, wherein the graphene-based composite material has a thermal conductivity of 5 to 45W/mK and an electrical conductivity of 1 to 10S/m.
10. The use of the graphene-based composite material with high thermal conductivity and high electrical conductivity of claim 7 in the preparation of electronic devices or optoelectronic devices.
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| CN105694433A (en) * | 2016-03-30 | 2016-06-22 | 天津大学 | Preparation method of polymer foam/graphene composite material integrating high heat conductivity and high flexibility |
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| CN105694433A (en) * | 2016-03-30 | 2016-06-22 | 天津大学 | Preparation method of polymer foam/graphene composite material integrating high heat conductivity and high flexibility |
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