CN113717702A - Graphene composite radiating fin and preparation method thereof - Google Patents
Graphene composite radiating fin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene composite radiating fin and a preparation method thereof, relates to the technical field of radiating materials, and aims to solve the problems of high cost and insufficient radiating performance of the existing graphene film preparation method; the invention comprises the raw materials of 60-90 parts of graphene, 1-10 parts of graphene oxide, 1-10 parts of a carbon forming agent, 0.1-5 parts of an anti-aggregation filler, 0.1-5 parts of a codeposition agent and 0.1-5 parts of a dispersing agent by weight; adding graphene, graphene oxide, an anti-aggregation filler and a dispersing agent into dispersing equipment, pouring deionized water, transferring the dispersed mixture into a reaction container, stirring, adding a co-deposition agent, heating to react completely, and standing until solid is settled; removing part of the supernatant, adding a carbon forming agent, stirring, spreading on a filter cloth, uniformly scraping and drying; separating the filter cloth from the intermediate product, pressing to form a film, sintering at high temperature, and finally rolling to form a finished radiating fin product; the invention has the advantages of economy, environmental protection, simple process, easy industrial production and excellent transverse and longitudinal heat dispersion of products.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to a graphene composite heat dissipation fin and a preparation method thereof.
Background
Graphene is a two-dimensional nano material with a hexagonal honeycomb structure consisting of carbon atoms in sp2 hybridized orbitals, and the special monoatomic layer structure of graphene determines that graphene has rich and novel physical properties. The nano-composite material has extremely large specific surface area, ultrahigh electrical conductivity and thermal conductivity and excellent mechanical property, and has extremely wide application prospect in the fields of nano-electronic devices, solar cells, photoelectric detection materials, lithium batteries, hydrogen storage materials, composite materials and the like.
The performance of the existing 3C electronic products is continuously improved, and the power consumption and the heat collection effect are more and more serious, so how to effectively eliminate and reduce the adverse effects caused by waste heat is one of the major research directions of electronic components. In recent years, graphite gradually replaces metal heat conducting materials, but the preparation cost is high.
The invention patent with the publication number of CN103080005B and the name of a graphite film and a manufacturing method of the graphite film discloses an artificial graphite film prepared by high-temperature carbonization and high-temperature graphitization of a polyimide film, wherein the film thickness of the heat-conducting film can be designed to be as thin as 5 mu m, the heat-radiating effect is still good, and the recorded thermal diffusivity is about 8.5cm2The thermal conductivity is about 400-600W/m.K, the density is small, and the requirement of lightness and thinness of electronic products can be well met, but the manufacturing cost of the artificial graphite film is high, the temperature is high and the time is long in the carbonization and graphitization processes in the manufacturing process, so that the energy consumption is high, and the heat dissipation performance of the product needs to be improved.
The publication number is CN104973592B, the name is a patent of invention of a preparation method of graphene film with high electric conductivity and high thermal conductivity by liquid phase method orientation, wherein, the invention discloses a method for preparing graphene film by carrying out vacuum suction filtration after graphene oxide is subjected to vacuum temperature control orientation deposition, then carrying out chemical vapor deposition reduction, and finally carrying out high pressure shaping, the graphene film prepared by the method obtains the performance of high electric conductivity and high thermal conductivity, wherein the thermal conductivity can reach 915W/m.K, and meanwhile, the specification of the patent also describes that the thermal conductivity of the graphene film obtained by disordered deposition and oriented physical deposition is about 500W/m.K; however, the step of vacuum temperature control directional deposition is controlled finely, the requirements on equipment and the loss are higher, the cost cannot be controlled, and the method is difficult to popularize for mass production in practical application.
The publication number is CN112457625A, the name is a graphene composite material and a graphene composite heat-conducting plastic, and the patent application discloses that aminated graphene is mixed with a heat-conducting material and subjected to pre-orientation treatment, then the mixture is mixed with resin powder and subjected to secondary orientation treatment to prepare a graphene composite material, and finally the graphene composite heat-conducting plastic is stirred, melted and extruded with fiber fillers to prepare the graphene composite heat-conducting plastic, wherein the transverse heat conductivity of the graphene composite heat-conducting plastic is 400W/m.K at most, the longitudinal heat conductivity of the graphene composite heat-conducting plastic is excellent and can reach 20W/m.K, but the preparation process steps of the graphene composite heat-conducting plastic are multiple, the steps of the preparation process comprise dispersion, rolling, shearing, re-rolling, granulation and the like are complex, the types of required equipment are multiple, and the heat-radiating performance of the product is still not good enough.
In view of the above, a graphene composite heat sink and a method for manufacturing the same are needed to solve the problems.
Disclosure of Invention
The invention aims to provide a graphene composite radiating fin and a preparation method thereof, and aims to solve the problems that the existing graphene film preparation method is high in cost and poor in radiating performance.
In order to achieve the purpose, the invention provides the following technical scheme: a graphene composite radiating fin comprises the following raw materials in parts by weight: 60-90 parts of graphene, 1-10 parts of graphene oxide, 1-10 parts of a carbon forming agent, 0.1-5 parts of an anti-aggregation filler, 0.1-5 parts of a co-deposition agent and 0.1-5 parts of a dispersing agent.
In a preferred scheme, the graphene is prepared by a physical method, the number of layers is less than 10, and the sheet diameter is 5-100 μm.
In a preferred scheme, the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 μm.
In a preferred embodiment, the carbon former is an organometallic compound or a metal oxide.
In the scheme, the carbon forming agent is preferably one or more of zinc acetate, magnesium acetate, aluminum acetate, nickel acetate, magnesium carbonate, zinc oxide, magnesium oxide and nickel oxide.
In a preferred scheme, the anti-aggregation filler is one or two of montmorillonite and hydrotalcite.
In a preferred embodiment, the co-deposition agent is one or more of cetyltrimethylammonium bromide, octadecylamine, triethanolamine, polyoxyethyleneoctadecylamine, KH 550.
In a preferred embodiment, the dispersant is one or more of dodecylbenzene sulfonic acid, dodecylsulfonic acid, polyvinylpyrrolidone and cellulose.
The other technical scheme provided by the invention is as follows: a preparation method of a graphene composite radiating fin comprises the following specific steps:
s1, weighing raw materials, wherein the raw materials comprise, by weight, 60-90 parts of graphene, 1-10 parts of graphene oxide, 1-10 parts of a carbon forming agent, 0.1-5 parts of an anti-aggregation filler, 0.1-5 parts of a co-deposition agent and 0.1-5 parts of a dispersing agent;
s2, adding the weighed graphene, graphene oxide, anti-aggregation filler and dispersant into a dispersing device, pouring a proper amount of deionized water, transferring the product into a reaction container after full dispersion, stirring, adding a co-deposition agent, heating, stopping stirring after complete reaction, and standing until solid is settled;
s3, removing part of supernatant in the reaction vessel, adding a carbon forming agent into the reaction vessel, uniformly stirring, pouring out a product in the reaction vessel, spreading the product on a filter cloth, uniformly scraping and drying;
and S4, separating the filter cloth from the intermediate product, pressing into a film, sintering at high temperature, and rolling the sintered product into a finished radiating fin product.
In a preferred scheme, the dispersing equipment is a basket type sand mill, the full dispersing time is 30min, the reaction vessel is a glass reaction kettle, the temperature is increased to 80 ℃, and the reaction time is 30 min; the amount of the removed supernatant is 80 percent of the total amount, and the drying temperature is 90 ℃; the high-temperature sintering process is that the membrane separated from the filter cloth is placed in a muffle furnace under nitrogen atmosphere, the temperature rise rate is 20 ℃/min, the temperature is raised to 1000-2000 ℃, and the temperature is reduced to room temperature after being kept for 1 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the graphene composite radiating fin and the preparation method thereof, the graphene prepared by adopting a physical method with excellent heat dissipation performance is used as a main material, the complete crystal form of the graphene is reserved, and the graphene composite radiating fin has good transverse heat conduction performance.
2. According to the graphene composite radiating fin and the preparation method thereof, the small-sheet-diameter graphene oxide and the large-sheet-diameter graphene are compounded as raw materials, and the graphene oxide fills gaps between graphene sheets prepared by a physical method in a high-temperature sintering process, so that the transverse heat-conducting property of the graphene is further improved.
3. According to the graphene composite radiating fin and the preparation method thereof, the anti-aggregation filler is dispersed together with graphene and graphene oxide through pi-pi superposition, and the co-deposition agent reacts with the anti-aggregation filler under the action of the co-deposition agent, so that the graphene, the graphene oxide and the anti-aggregation filler are deposited together, the slurry is separated from water efficiently, the drying efficiency is indirectly improved, and the energy consumption is reduced.
4. According to the graphene composite radiating fin and the preparation method thereof, a substance which can promote organic compounds to form carbon at high temperature, namely a carbon forming agent, is used, and in the high-temperature sintering process, the carbon forming agent, the co-deposition agent, the dispersing agent and the like in a co-promotion system of graphene and anti-aggregation filler can be decomposed to form spherical carbon materials, so that carbon overlapping between materials is realized, defects are avoided, meanwhile, longitudinal carbon overlapping is generated in a flat layer structure, and the longitudinal heat conducting performance of a product is improved.
5. The graphene composite radiating fin and the preparation method thereof have the advantages of simple, rapid and efficient preparation steps, economic and environment-friendly process and low cost, the prepared graphene composite radiating fin product has excellent radiating performance, the transverse thermal conductivity can exceed 1600W/m.K, the longitudinal thermal conductivity can reach 25-46W/m.K, and the graphene composite radiating fin is suitable for industrial production.
Drawings
Fig. 1 is a graphene composite heat sink prepared in example 5 of the present invention;
fig. 2 is a cross-sectional SEM image of the graphene composite heat sink prepared in example 5 of the present invention;
fig. 3 is a cross-sectional SEM image of a sample before sintering of the graphene composite heat spreader prepared in example 5 of the present invention.
Detailed Description
Example 1
Weighing 80g of graphene, 5g of graphene oxide, 1g of montmorillonite, 1g of polyvinylpyrrolidone, 1g of hexadecyl trimethyl ammonium bromide and 3g of zinc acetate for later use, wherein the graphene is prepared by mechanically stripping graphite, the number of layers is less than 10, the sheet diameter is 5-100 mu m, and the graphene oxide is prepared by a chemical method and has the sheet diameter of 0.5-50 mu m;
fully dispersing graphene, graphene oxide, montmorillonite, polyvinylpyrrolidone and 3L of deionized water in a basket type sand mill for 30 minutes, pouring the product into a 5L glass reaction kettle for stirring, adding cetyl trimethyl ammonium bromide into the reaction kettle, raising the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant through a water pump with a filter element, adding zinc acetate, spreading on filter cloth after fully stirring for 10 minutes, uniformly scraping by adopting a scraper, and drying in a drying oven at 90 ℃. And after drying, separating the graphene film from the filter cloth, rolling on a double-roller machine, then placing the obtained film-shaped sample in a muffle furnace for sintering under the nitrogen atmosphere, wherein the heating rate is 20 ℃/min, heating to 1000 ℃, keeping for 1 hour, and then cooling to room temperature. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 100MPa to obtain the graphene composite radiating fin, wherein the thickness of the graphene composite radiating fin is 100 microns, and the transverse thermal conductivity coefficient is 980W/m.K and the longitudinal thermal conductivity coefficient is 32W/m.K.
Example 2
Weighing 80g of graphene, 2g of graphene oxide, 0.1g of montmorillonite, 1g of polyvinylpyrrolidone, 1g of hexadecyl trimethyl ammonium bromide and 3g of zinc acetate for later use, wherein the graphene is prepared by mechanically stripping graphite, the number of layers is less than 10, the sheet diameter is 5-100 mu m, and the graphene oxide is prepared by a chemical method and has the sheet diameter of 0.5-50 mu m;
fully dispersing graphene, graphene oxide, montmorillonite, polyvinylpyrrolidone and 3L of deionized water in a basket type sand mill for 30 minutes, pouring the product into a 5L glass reaction kettle for stirring, adding cetyl trimethyl ammonium bromide into the reaction kettle, raising the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant through a water pump with a filter element, adding zinc acetate, spreading on filter cloth after fully stirring for 10 minutes, uniformly scraping by adopting a scraper, and drying in a drying oven at 90 ℃. And after drying, separating the graphene film from the filter cloth, rolling on a double-roller machine, then placing the obtained film-shaped sample in a muffle furnace for sintering under the nitrogen atmosphere, wherein the heating rate is 20 ℃/min, heating to 1000 ℃, keeping for 1 hour, and then cooling to room temperature. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 20MPa to obtain the graphene composite radiating fin, wherein the thickness of the graphene composite radiating fin is 100 microns, and the transverse thermal conductivity coefficient is 1120W/m.K, and the longitudinal thermal conductivity coefficient is 46W/m.K.
Example 3
In the same way as example 2, the sintering temperature was raised to 1500 ℃, and the transverse thermal conductivity and the longitudinal thermal conductivity of the obtained graphene composite heat sink were measured to be 1350W/m.K and 36W/m.K, respectively.
Example 4
Weighing 60g of graphene, 1g of graphene oxide, 5g of montmorillonite, 5g of cellulose, 5gKH550 and 10g of zinc oxide for later use, wherein the graphene is prepared by mechanically stripping graphite, the number of layers is 3-5, the sheet diameter is 5-100 mu m, and the graphene oxide is prepared by a chemical method and the sheet diameter is 0.5-50 mu m;
dispersing graphene, graphene oxide, montmorillonite, cellulose and 3L of deionized water in a basket type sand mill for 30 minutes, pouring a product into a 5L glass reaction kettle for stirring, adding KH550 into the reaction kettle, regulating the pH value of a system to be 4-5, raising the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant through a water pump with a filter element, adding zinc oxide, spreading on filter cloth after fully stirring for 10 minutes, uniformly scraping by using a scraper, and drying in a drying oven at 90 ℃. And after drying, separating the graphene film from the filter cloth, rolling on a double-roller machine, then placing the obtained film-shaped sample in a muffle furnace for sintering under the nitrogen atmosphere, wherein the heating rate is 20 ℃/min, heating to 2000 ℃, keeping for 1 hour, and then cooling to room temperature. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 50MPa to obtain the graphene composite radiating fin, wherein the thickness of the graphene composite radiating fin is 100 microns, and the transverse thermal conductivity coefficient is 1410W/m.K and the longitudinal thermal conductivity coefficient is 25W/m.K through measurement.
Example 5
Weighing 80g of graphene, 2g of graphene oxide, 0.1g of montmorillonite, 1g of cellulose, 1gKH550 and 3g of magnesium acetate for later use, wherein the graphene is prepared by mechanically stripping graphite, the number of layers is less than 10, the sheet diameter is 5-100 mu m, and the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m;
dispersing graphene, graphene oxide, montmorillonite, cellulose and 3L of deionized water in a basket type sand mill for 30 minutes, pouring a product into a 5L glass reaction kettle for stirring, adding KH550 into the reaction kettle, regulating the pH value of a system to be 4-5, raising the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant through a water pump with a filter element, adding magnesium acetate, spreading on a filter cloth after fully stirring for 10 minutes, uniformly scraping by using a scraper, and drying in a drying oven at 90 ℃. And after drying, separating the graphene film from the filter cloth, rolling on a double-roller machine, then placing the obtained film-shaped sample in a muffle furnace for sintering under the nitrogen atmosphere, wherein the heating rate is 20 ℃/min, heating to 2000 ℃, keeping for 1 hour, and then cooling to room temperature. And (3) placing the sintered sample on a double-roller machine, rolling under the pressure of 100MPa to obtain the graphene composite radiating fin, wherein the thickness of the graphene composite radiating fin is 100 microns, and the transverse thermal conductivity is 1620W/m.K and the longitudinal thermal conductivity is 26W/m.K through measurement.
Comparative example:
the method is characterized in that 5g of graphene oxide is dispersed in 2L of water and ultrasonically dispersed for 5 h; controlling the obtained solid substance to directionally deposit for 4 hours in a vacuum drying oven at the temperature of 80 ℃; carrying out vacuum filtration on the deposited substance for 5 hours; and (3) placing the filtered graphene into a muffle furnace, reducing the graphene in a nitrogen atmosphere at 1500 ℃, rolling the graphene into a film by a double-roller machine at 100MPa, and measuring that the transverse thermal conductivity is 920W/m.K and the longitudinal thermal conductivity is 9W/m.K.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (10)
1. The graphene composite radiating fin is characterized by comprising the following raw materials in parts by weight: 60-90 parts of graphene, 1-10 parts of graphene oxide, 1-10 parts of a carbon forming agent, 0.1-5 parts of an anti-aggregation filler, 0.1-5 parts of a co-deposition agent and 0.1-5 parts of a dispersing agent.
2. The graphene composite fin according to claim 1, wherein: the graphene is prepared by a physical method, the number of layers is less than 10, and the sheet diameter is 5-100 mu m.
3. The graphene composite fin according to claim 1, wherein: the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m.
4. The graphene composite fin according to claim 1, wherein: the carbon forming agent is an organic metal compound or a metal oxide.
5. The graphene composite fin according to claim 4, wherein: the carbon forming agent is one or more of zinc acetate, magnesium acetate, aluminum acetate, nickel acetate, magnesium carbonate, zinc oxide, magnesium oxide and nickel oxide.
6. The graphene composite fin according to claim 1, wherein: the anti-aggregation filler is one or two of montmorillonite and hydrotalcite.
7. The graphene composite fin according to claim 1, wherein: the codeposition agent is one or more of cetyl trimethyl ammonium bromide, octadecylamine, triethanolamine, polyoxyethylene octadecylamine and KH 550.
8. The graphene composite fin according to claim 1, wherein: the dispersing agent is one or more of dodecylbenzene sulfonic acid, dodecylsulfonic acid, polyvinylpyrrolidone and cellulose.
9. The preparation method of the graphene composite cooling fin according to any one of claims 1 to 9, characterized by comprising the following specific steps:
s1, weighing raw materials, wherein the raw materials comprise, by weight, 60-90 parts of graphene, 1-10 parts of graphene oxide, 1-10 parts of a carbon forming agent, 0.1-5 parts of an anti-aggregation filler, 0.1-5 parts of a co-deposition agent and 0.1-5 parts of a dispersing agent;
s2, adding the weighed graphene, graphene oxide, anti-aggregation filler and dispersant into a dispersing device, pouring a proper amount of deionized water, transferring the product into a reaction container after full dispersion, stirring, adding a co-deposition agent, heating, stopping stirring after complete reaction, and standing until solid is settled;
s3, removing part of supernatant in the reaction vessel, adding a carbon forming agent into the reaction vessel, uniformly stirring, pouring out a product in the reaction vessel, spreading the product on a filter cloth, uniformly scraping and drying;
and S4, separating the filter cloth from the intermediate product, pressing into a film, sintering at high temperature, and rolling the sintered product into a finished radiating fin product.
10. The method of claim 9, wherein: in the step S2, the dispersing equipment is a basket type sand mill, the time for full dispersion is 30min, the reaction vessel is a glass reaction kettle, the temperature is raised to 80 ℃, and the reaction time is 30 min; in the step S3, the amount of the removed supernatant is 80 percent of the total amount, and the drying temperature is 90 ℃; in the step S4, the high-temperature sintering process is to place the membrane separated from the filter cloth in a muffle furnace under nitrogen atmosphere, raise the temperature at a rate of 20 ℃/min to 1000-2000 ℃, maintain for 1h, and then lower the temperature to room temperature.
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