CN107814507B - Graphene-based heat-conducting composite material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a graphene-based heat-conducting composite material which is characterized in that: the composite material comprises graphene, palladium or platinum, copper nanoparticles and a resin high polymer material; the composite material comprises 40-90% of graphene, 0.1-10% of palladium or platinum, 9-50% of copper nanoparticles and 1-20% of resin macromolecules by mass. The graphene-based heat-conducting composite material has the characteristics of good heat conductivity and low price.
Description
Technical Field
The invention belongs to the field of preparation and application of nano materials, and particularly relates to a graphene-based heat-conducting composite material and preparation and application thereof.
Background
Graphene is a two-dimensional carbon material and has many excellent characteristics, such as high strength, high light transmittance, high electrical conductivity, and high thermal conductivity. Graphene has received great attention as a heat conductive material because of its good heat conductivity. The graphene heat-conducting film can be applied to electronic devices for heat dissipation of electronic elements, and has a wide application prospect. However, the high thermal conductivity of graphene is mainly measured in a single-layer graphene film, and a multilayer graphene film assembled by graphene can only obtain poor thermal conductivity. The main reason is that the graphene sheet layers are not consistent in direction in the assembling process, and the heat transfer performance of the graphene sheet layers is greatly different from the theoretical value due to the heat transfer defect caused by the inconsistent direction. In another approach for preparing the graphene heat-conducting film, a polyimide film is used as a raw material, and a multi-step carbonization process is carried out to obtain the graphene-like film material. The graphene film obtained by using graphene as a raw material or polyimide film as a raw material is not only flexible, but also brittle and easy to break, and generally low in strength, which is very unfavorable for the use of the graphene-based heat-conducting film. The high-temperature carbonization process using polyimide consumes a large amount of energy, has very high cost, and is not suitable for wide popularization and application. The graphene is adopted as a raw material, so that the preparation difficulty is high, and the defects of the graphene become the bottleneck and the main problems of the graphene as a heat conduction material.
Graphene is used as a main component of the heat conduction material, and an additive material is selected to improve the heat conduction performance and strength of the graphene film. Graphene obtained by physical or chemical vapor deposition methods is not only low in yield but also very high in cost. Graphite is used as a raw material, graphene oxide obtained by chemical stripping is subjected to a reduction step, and the method is low in cost and easy for batch production. Among metal materials, copper materials have good heat-conducting properties, so that the copper materials are very ideal additives. In addition, the copper material is easy to oxidize, and the copper is difficult to oxidize by coating with the graphene. Whereas, in order to increase the strength of the graphene film, a high toughness additive is indispensable. In order to improve the heat conductivity of graphene-based heat conductive materials, graphene heat conductive materials of novel compositions must be developed.
Disclosure of Invention
One of the purposes of the present invention is to overcome the above disadvantages and provide a graphene-based heat conductive composite material with good heat conductivity and low cost.
The invention also aims to provide a preparation method of the graphene-based heat-conducting composite material with good heat conductivity and low cost.
The invention further aims to provide the application of the graphene-based heat-conducting composite material with good heat conductivity and low cost.
The technical scheme adopted by the invention for solving the problems is as follows: a graphene-based heat-conducting composite material comprises graphene, metal palladium or platinum, copper nanoparticles and a resin high polymer material; the composite material comprises 40-90% of graphene, 0.1-10% of metal palladium or platinum, 8.9-50% of copper nanoparticles and 1-20% of resin macromolecules.
Preferably, the percentage of the graphene is 50-80%, the percentage of the metal palladium or platinum is 0.5-5%, the percentage of the copper nanoparticles is 10-30%, and the percentage of the resin polymer is 5-15%;
the resin macromolecules comprise epoxy resin, alkyd resin, polyacrylic resin, phenolic resin and ABS resin.
A preparation method of a graphene-based heat-conducting composite material comprises the following steps:
(1) preparation of graphene oxide
Graphite is used as a raw material, concentrated sulfuric acid is used as a solvent, potassium permanganate is used as an oxidant, the obtained graphene oxide is treated by hydrogen peroxide, and then is washed by hydrochloric acid and water and then dispersed for later use;
(2) copper nanoparticle preparation
Taking a metal copper salt as a raw material, taking a macromolecule as a protective agent, taking ethylene glycol as a reducing agent and a solvent, reacting at 120-160 ℃ under the protection of inert gas to obtain copper nanoparticle sol, washing, separating to obtain a copper nanoparticle dispersion liquid for later use
(3) Preparation of graphene-copper nano material-resin high polymer material compound
Uniformly mixing the graphene oxide dispersion liquid, palladium chloride or chloroplatinic acid, copper nanoparticle dispersion liquid and a resin high polymer material in proportion, heating to volatilize a solvent to obtain a composite material precursor, and heating or reducing by using a reducing agent to obtain the graphene-copper nano material-resin high polymer material composite.
Wherein the reducing agent can be one or more of hydrazine hydrate, sodium borohydride or hydrogen.
The application of the graphene-based heat-conducting composite material can be used for heat dissipation of electronic products.
Compared with the prior art, the invention has the advantages that:
according to the invention, a chemical stripping method is adopted to obtain graphene oxide, a liquid-phase reduction method is adopted to obtain copper nanoparticles, commercial resin is adopted as the resin, and platinum or palladium is used as a catalyst for reduction of the graphene oxide, so that the improvement of the heat conductivity is facilitated. The innovation point of the invention is that the combination of the four components can solve the problems of high cost and poor heat-conducting property of the graphene film.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) Preparation of graphene oxide
Dispersing 10 g of graphite in 200 ml of concentrated sulfuric acid, reducing the temperature to 0 ℃, adding 1.5 g of potassium permanganate under the stirring condition, stirring for 30 minutes, adding 30 g of potassium permanganate, heating to 40 ℃, reacting for 2 hours to obtain a viscous sample, slowly dripping water, adding 30 ml of 30% hydrogen peroxide, filtering to obtain a graphene oxide filter cake, washing with hydrochloric acid, washing with water, and finally dispersing in 10 l of water for later use;
(2) preparation of copper nanoparticles
Dissolving 17g of green copper dihydrate in 1000ml of ethylene glycol, simultaneously adding 30 g of PVP, dissolving in the solution, dropwise adding 0.5M NaOH ethylene glycol solution, adjusting the pH to be more than 10, stirring for 30min, heating to 160 ℃ under the protection of nitrogen, and heating for 3 hours to obtain a reddish brown solution. Cooling, adding acetone to obtain a precipitate, and washing with water to obtain a copper nanoparticle dispersion liquid for later use;
(3) preparation of graphene-copper nano material-resin high polymer material compound
Taking 6 liters of graphene oxide dispersion liquid, 0.83 g of palladium chloride, 2.5 g of copper nanoparticles and 1 g of epoxy resin, uniformly mixing, heating and drying after coating to obtain a composite film, and reducing the composite film by using hydrazine hydrate as a reducing agent to obtain the graphene-palladium-copper nano material-resin high polymer material composite.
Example 2
(1) Preparation of graphene oxide
Dispersing 10 g of graphite in 200 ml of concentrated sulfuric acid, reducing the temperature to 0 ℃, adding 1.5 g of potassium permanganate under the stirring condition, stirring for 30 minutes, adding 30 g of potassium permanganate, heating to 40 ℃, reacting for 2 hours to obtain a viscous sample, slowly dripping water, adding 30 ml of 30% hydrogen peroxide, filtering to obtain a graphene oxide filter cake, washing with hydrochloric acid, washing with water, and finally dispersing in 10 l of water for later use;
(2) preparation of copper nanoparticles
Dissolving 17g of green copper dihydrate in 1000ml of ethylene glycol, simultaneously adding 20 g of PVP, dissolving in the solution, dropwise adding 0.5M NaOH ethylene glycol solution, adjusting the pH to be more than 10, stirring for 30min, heating to 160 ℃ under the protection of nitrogen, and heating for 3 hours to obtain a reddish brown solution. Cooling, adding acetone to obtain a precipitate, and washing with water to obtain a copper nanoparticle dispersion liquid for later use;
(3) preparation of graphene-copper nano material-resin high polymer material compound
And (2) uniformly mixing 9 liters of graphene oxide dispersion liquid, 0.027 g of chloroplatinic acid hexahydrate, 0.89 g of copper nanoparticles and 0.1 g of alkyd resin, heating and drying after film coating to obtain a composite film, heating to 500 ℃ in a tubular furnace under a nitrogen atmosphere, and treating for 3 hours to obtain the graphene-platinum-copper nanomaterial-resin high polymer material composite.
To illustrate the advantages of adding noble metals palladium or platinum to graphene-based thermal conductive film materials, we performed reference experiments on the basis of examples 1 and 2. In contrast to examples 1 and 2, no noble metals palladium or platinum were added to the reference samples. Through the measurement of the thermal conductivity of the obtained sample, the thermal conductivity of the sample obtained in example 1 is 2200W/m/K, and the thermal conductivity of the reference sample is 1600W/m/K; similarly, the sample obtained in example 2 was found to have a thermal conductivity of 1900W/m/K, while the reference sample had a thermal conductivity of 1200W/m/K. Therefore, the experimental result shows that the heat-conducting property can be greatly improved by adding the noble metal.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (4)
1. A graphene-based heat-conducting composite material is characterized in that: the composite material comprises graphene, palladium or platinum, copper nanoparticles and a resin high polymer material; the composite material comprises 40-90% of graphene, 0.1-10% of palladium or platinum, 9-50% of copper nanoparticles and 1-20% of resin macromolecules by mass;
the graphene-based heat-conducting composite material is prepared by the following preparation method:
(1) preparation of graphene oxide
Graphite is used as a raw material, concentrated sulfuric acid is used as a solvent, potassium permanganate is used as an oxidant, the obtained graphene oxide is treated by hydrogen peroxide, and then is washed by hydrochloric acid and water and then dispersed for later use;
(2) copper nanoparticle preparation
Taking a metal copper salt as a raw material, taking a macromolecule as a protective agent, taking ethylene glycol as a reducing agent and a solvent, reacting at 120-160 ℃ under the protection of inert gas to obtain copper nanoparticle sol, washing, and separating to obtain a copper nanoparticle dispersion liquid for later use;
(3) preparation of graphene-copper nano material-resin high polymer material compound
Uniformly mixing the graphene oxide dispersion liquid, palladium chloride or chloroplatinic acid, copper nanoparticle dispersion liquid and a resin high polymer material in proportion, heating to volatilize a solvent to obtain a composite material precursor, and heating or reducing by using a reducing agent to obtain the graphene-copper nano material-resin high polymer material composite.
2. The graphene-based thermally conductive composite of claim 1, wherein: the percentage of the graphene is 50-80%, the percentage of palladium or platinum is 0.5-5%, the percentage of copper nanoparticles is 10-30%, and the percentage of resin macromolecules is 5-15%.
3. The graphene-based thermally conductive composite of claim 1 or 2, wherein: the resin macromolecules comprise epoxy resin, alkyd resin, polyacrylic resin, phenolic resin and ABS resin.
4. The application of the graphene-based heat-conducting composite material is characterized in that: the graphene-based thermally conductive composite material according to claim 1 or 2 is applied to heat dissipation of electronic products.
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| CN109135686B (en) * | 2018-08-10 | 2020-01-21 | 中国矿业大学 | Graphene-based modified nano fluid heat transfer working medium and preparation method thereof |
| CN109181175A (en) * | 2018-09-12 | 2019-01-11 | 芦露华 | A kind of fever composite material and preparation method of graphene and bimetal nano line |
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| CN103193978B (en) * | 2013-04-24 | 2015-07-08 | 黑龙江大学 | Preparation method for polyaniline/graphene/nano-copper composite material |
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