CN113717702B - Graphene composite cooling fin and preparation method thereof - Google Patents
Graphene composite cooling fin and preparation method thereof Download PDFInfo
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- CN113717702B CN113717702B CN202111017795.3A CN202111017795A CN113717702B CN 113717702 B CN113717702 B CN 113717702B CN 202111017795 A CN202111017795 A CN 202111017795A CN 113717702 B CN113717702 B CN 113717702B
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Abstract
The invention discloses a graphene composite cooling fin and a preparation method thereof, relates to the technical field of cooling materials, and aims to solve the problems of high cost and poor cooling performance of the existing graphene film preparation method; the invention comprises raw materials of 60-90 parts by weight of graphene, 1-10 parts by weight of graphene oxide, 1-10 parts by weight of carbon forming agent, 0.1-5 parts by weight of anti-aggregation filler, 0.1-5 parts by weight of co-deposition agent and 0.1-5 parts by weight of dispersing agent; adding graphene, graphene oxide, an anti-aggregation filler and a dispersing agent into dispersing equipment, pouring deionized water, dispersing, transferring into a reaction vessel, stirring, adding a codeposition agent, heating to react completely, and standing until solids settle; removing part of supernatant, adding carbon forming agent, stirring, spreading on filter cloth, and oven drying; separating the filter cloth from the intermediate product, pressing the filter cloth into a film, sintering the film at a high temperature, and finally rolling the film into a cooling fin finished product; the invention is economical and environment-friendly, has simple process, is easy for industrial production, and has excellent transverse and longitudinal heat dissipation performance.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to a graphene composite heat dissipation sheet and a preparation method thereof.
Background
Graphene is a two-dimensional nanomaterial with a hexagonal honeycomb structure composed of carbon atoms in sp2 hybridized orbitals, and the special monoatomic layer structure determines that the graphene has rich and novel physical properties. The material has extremely large specific surface area, ultrahigh electrical conductivity and heat conductivity and excellent mechanical properties, 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, the energy consumption and the heat aggregation effect are more and more serious, and how to effectively remove and reduce the adverse effects caused by waste heat is always one of the key research directions of electronic components. In recent years, graphite gradually replaces metal heat conduction materials, but the preparation cost is higher.
The invention patent with publication No. CN103080005B, entitled graphite film and method for producing graphite film, wherein an artificial graphite film prepared by high temperature carbonization and high temperature graphitization of polyimide film is disclosed, the thickness of the heat conducting film material can be designed to be as thin as 5 μm, the heat dissipation effect is still good, and the recorded thermal diffusivity is about 8.5cm 2 The thermal conductivity is about 400-600W/m.K, the density is smaller, the requirements of light and thin electronic products can be better 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, the energy consumption is high, and the heat dissipation performance of the product is required to be improved.
The invention discloses a method for preparing a graphene film by carrying out vacuum temperature-controlled directional deposition on graphene oxide, vacuum suction filtration, chemical vapor deposition reduction and high-pressure shaping, wherein the graphene film prepared by the method has high electric conductivity and high heat conductivity, the heat conductivity can reach 915W/m.K, and meanwhile, the specification of the patent also records that the heat conductivity of the graphene film obtained by disordered deposition and directional physical deposition is about 500W/m.K; however, the vacuum temperature-control directional deposition has fine control, higher equipment requirement and loss, and the cost cannot be controlled, so that the method is difficult to popularize in mass production in practical application.
The invention patent application with publication number of CN112457625A and name of graphene composite material and graphene composite heat-conducting plastic discloses that after being mixed with heat-conducting material and pre-oriented, the aminated graphene is mixed with resin powder and subjected to secondary orientation treatment to prepare graphene composite material, and finally the graphene composite heat-conducting plastic is prepared by stirring and melt extrusion with fiber filler, wherein the transverse heat conductivity is 400W/m.K at most, the longitudinal heat conductivity is better and can reach 20W/m.K, but the preparation process steps are more, the steps comprise dispersing, rolling, shearing, re-rolling, granulating and the like are more complex, the required equipment types are more, and the heat dissipation performance of the product is still not good.
In view of the foregoing, there is a need for a graphene composite heat sink and a method for preparing the same to solve these problems.
Disclosure of Invention
The invention aims to provide a graphene composite cooling fin and a preparation method thereof, which are used for solving the problems of high cost and poor heat dissipation performance of the existing graphene film preparation method.
In order to achieve the above purpose, the present invention provides the following technical solutions: the graphene composite cooling 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 mu m.
In a preferred scheme, the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m.
In a preferred embodiment, the carbon former is an organometallic compound or 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 embodiment, the anti-aggregation filler is one or both of montmorillonite and hydrotalcite.
In a preferred embodiment, the co-deposition agent is one or more of cetyltrimethylammonium bromide, octadecylamine, triethanolamine, polyoxyethylene octadecylamine, KH 550.
In a preferred embodiment, the dispersant is one or more of dodecylbenzene sulfonic acid, dodecylsulfonic acid, polyvinylpyrrolidone, cellulose.
The other technical scheme provided by the invention is as follows: the preparation method of the graphene composite cooling 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 carbonizing 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 weighed graphene, graphene oxide, anti-aggregation filler and dispersing agent into dispersing equipment, pouring a proper amount of deionized water, fully dispersing, transferring the product into a reaction container, stirring, adding a codeposition agent into the reaction container, heating, stopping stirring after the reaction is completed, and standing until solids settle;
s3, after 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 on filter cloth, uniformly scraping and drying;
s4, separating the filter cloth from the intermediate product, pressing the filter cloth into a film, sintering the film at a high temperature, and rolling the sintered product into a cooling fin finished 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 raised to 80 ℃, and the reaction time is 30min; the amount of supernatant removed is 80% of the total amount, and the drying temperature is 90 ℃; the high-temperature sintering process is to place the membrane separated from the filter cloth in a muffle furnace under nitrogen atmosphere, and the temperature rising rate is 20 ℃/min, the temperature is raised to 1000-2000 ℃, and the temperature is reduced to room temperature after the temperature is kept for 1 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the graphene composite cooling fin and the preparation method thereof, graphene prepared by a physical method with excellent cooling performance is used as a main material, the complete crystal form of the graphene is reserved, and the graphene composite cooling fin has good transverse heat conducting performance.
2. According to the graphene composite cooling fin and the preparation method thereof, graphene oxide with small sheet diameter and graphene with large sheet diameter are used as raw materials for compounding, and gaps among graphene sheets prepared by a physical method are filled in the high-temperature sintering process of the graphene oxide, so that the transverse heat conduction performance of the graphene is further improved.
3. According to the graphene composite cooling fin and the preparation method thereof, the anti-aggregation filler is utilized to jointly disperse graphene and graphene oxide through pi-pi superposition, and under the action of the co-deposition agent, the co-deposition agent reacts with the anti-aggregation filler, so that the graphene, the graphene oxide and the anti-aggregation filler are jointly deposited, slurry and water are effectively separated, drying efficiency is indirectly improved, and energy consumption is reduced.
4. According to the graphene composite radiating fin and the preparation method thereof, substances with high temperature for promoting the carbon formation of organic compounds are also used, namely the carbon forming agent, and in the high-temperature sintering process, the substances and the graphene and the anti-aggregation filler are used for promoting the co-deposition agent, the dispersing agent and other decomposable components in a system together to form spherical carbon materials, so that carbon lap joint among the materials is realized, the formation of defects is avoided, and meanwhile, longitudinal carbon lap joint is generated in a flat layer structure, so that the longitudinal heat conducting performance of a product is improved.
5. The graphene composite cooling fin and the preparation method thereof have the advantages that the preparation steps are simple, quick and efficient, the process is economic and environment-friendly, the cost is low, the heat dissipation performance of the prepared graphene composite cooling fin product is excellent, the longitudinal thermal conductivity can reach 25-46W/m.K except that the transverse thermal conductivity can exceed 1600W/m.K, and the graphene composite cooling 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 a 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 sink 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, the graphene oxide is prepared by a chemical method, and the sheet diameter is 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, then pouring the product into a 5L glass reaction kettle for stirring, adding cetyltrimethylammonium bromide into the reaction kettle, heating to 80 ℃, fully reacting for 30 minutes, stopping stirring, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant by a water pump with a filter element, adding zinc acetate, fully stirring for 10 minutes, spreading on filter cloth, uniformly scraping by a scraper, and drying in a 90 ℃ drying box. And (3) separating the graphene film from the filter cloth after drying, rolling on a double-roller machine, placing the obtained film sample in a muffle furnace for sintering under a nitrogen atmosphere, heating to 1000 ℃ at a heating rate of 20 ℃/min, and cooling to room temperature after keeping for 1 hour. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 100MPa to obtain the graphene composite cooling fin, wherein the thickness of the graphene composite cooling fin is 100 mu m, and the transverse thermal conductivity is 980W/m.K and the longitudinal thermal conductivity is 32W/m.K through measurement.
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, the graphene oxide is prepared by a chemical method, and the sheet diameter is 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, then pouring the product into a 5L glass reaction kettle for stirring, adding cetyltrimethylammonium bromide into the reaction kettle, heating to 80 ℃, fully reacting for 30 minutes, stopping stirring, waiting for 10 minutes, gradually settling a solid sample, removing 80% of supernatant by a water pump with a filter element, adding zinc acetate, fully stirring for 10 minutes, spreading on filter cloth, uniformly scraping by a scraper, and drying in a 90 ℃ drying box. And (3) separating the graphene film from the filter cloth after drying, rolling on a double-roller machine, placing the obtained film sample in a muffle furnace for sintering under a nitrogen atmosphere, heating to 1000 ℃ at a heating rate of 20 ℃/min, and cooling to room temperature after keeping for 1 hour. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 20MPa to obtain the graphene composite cooling fin, wherein the thickness of the graphene composite cooling fin is 100 mu m, and the transverse thermal conductivity is 1120W/m.K and the longitudinal thermal conductivity is 46W/m.K through measurement.
Example 3
As in example 2, the sintering temperature was raised to 1500℃to obtain a graphene composite fin, and the lateral thermal conductivity was measured to 1350W/mK and the longitudinal thermal conductivity was measured to 36W/mK.
Example 4
Weighing 60g of graphene, 1g of graphene oxide, 5g of montmorillonite, 5g of cellulose, 5gKH g 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, the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m;
dispersing graphene, graphene oxide, montmorillonite and cellulose in 3L deionized water in a basket type sand mill for 30 minutes, pouring the product into a 5L glass reaction kettle for stirring, adding KH550 into the reaction kettle, regulating the pH value of the system to be between 4 and 5, heating the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, gradually settling a solid sample after waiting for 10 minutes, removing 80% of supernatant by a water pump with a filter element, adding zinc oxide, fully stirring for 10 minutes, spreading on filter cloth, uniformly scraping by a scraper, and drying in a drying box at 90 ℃. And (3) separating the graphene film from the filter cloth after drying, rolling on a double-roller machine, placing the obtained film sample in a muffle furnace for sintering under a nitrogen atmosphere, heating to 2000 ℃ at a heating rate of 20 ℃/min, and cooling to room temperature after keeping for 1 hour. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 50MPa to obtain the graphene composite cooling fin, wherein the thickness of the graphene composite cooling fin is 100 mu m, and the transverse thermal conductivity is 1410W/m.K and the longitudinal thermal conductivity is 25W/m.K through measurement.
Example 5
Weighing 80g of graphene, 2g of graphene oxide, 0.1g of montmorillonite, 1g of cellulose, 1gKH g 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, the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m;
dispersing graphene, graphene oxide, montmorillonite and cellulose in 3L deionized water in a basket type sand mill for 30 minutes, pouring the product into a 5L glass reaction kettle for stirring, adding KH550 into the reaction kettle, regulating the pH value of the system to be between 4 and 5, heating the reaction temperature to 80 ℃, stopping stirring after fully reacting for 30 minutes, gradually settling a solid sample after waiting for 10 minutes, removing 80% of supernatant by a water pump with a filter element, adding magnesium acetate, fully stirring for 10 minutes, spreading on filter cloth, uniformly scraping by a scraper, and drying in a drying box at 90 ℃. And (3) separating the graphene film from the filter cloth after drying, rolling on a double-roller machine, placing the obtained film sample in a muffle furnace for sintering under a nitrogen atmosphere, heating to 2000 ℃ at a heating rate of 20 ℃/min, and cooling to room temperature after keeping for 1 hour. And (3) placing the sintered sample on a double-roller machine, and rolling under the pressure of 100MPa to obtain the graphene composite cooling fin, wherein the thickness of the graphene composite cooling fin is 100 mu m, and the transverse thermal conductivity is 1620W/m.K and the longitudinal thermal conductivity is 26W/m.K through measurement.
Comparative example:
adopting a method in the patent with the bulletin number of CN104973592B and the name of a preparation method for preparing the graphene film with high electric conductivity and high heat conductivity by a liquid phase method, taking 5g of graphene oxide to be dispersed in 2L of water, and carrying out ultrasonic dispersion for 5h; the obtained solid matter is directionally deposited for 4 hours in a vacuum drying oven at 80 ℃; vacuum filtering the deposited material for 5 hours; and (3) placing the pumped and filtered graphene into a muffle furnace, reducing the graphene in a nitrogen atmosphere at 1500 ℃, and rolling the graphene into a film under 100MPa by a double-roller machine, wherein the transverse thermal conductivity is 920W/m.K and the longitudinal thermal conductivity is 9W/m.K.
The above is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be covered by the present invention. Therefore, the protection scope of the present invention should be defined by the claims.
The present invention is not described in detail in the present application, and is well known to those skilled in the art.
Claims (1)
1. The preparation method of the graphene composite cooling fin is characterized by comprising the following specific steps of:
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 carbonizing 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 weighed graphene, graphene oxide, anti-aggregation filler and dispersing agent into dispersing equipment, pouring a proper amount of deionized water, fully dispersing, transferring the product into a reaction container, stirring, adding a codeposition agent into the reaction container, heating, stopping stirring after the reaction is completed, and standing until solids settle;
s3, after 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 on filter cloth, uniformly scraping and drying;
s4, separating the filter cloth from the intermediate product, pressing the filter cloth into a film, sintering the film at a high temperature, and rolling the sintered product into a cooling fin finished product;
the graphene is prepared by a physical method, the number of layers is smaller than 10, and the sheet diameter is 5-100 mu m;
the graphene oxide is prepared by a chemical method, and the sheet diameter is 0.5-50 mu m;
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;
the anti-aggregation filler is one or two of montmorillonite and hydrotalcite;
the codeposition agent is one or more of hexadecyl trimethyl ammonium bromide, octadecylamine, triethanolamine, polyoxyethylene octadecylamine and KH 550;
the dispersing agent is one or more of dodecylbenzene sulfonic acid, dodecylsulfonic acid, polyvinylpyrrolidone and cellulose;
in the step S2, dispersing equipment is a basket type sand mill, the full dispersing time is 30min, a reaction vessel is a glass reaction kettle, the temperature is raised to 80 ℃, and the reaction time is 30min; in the step S3, the amount of the supernatant liquid removed is 80% 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, heat up the membrane to 1000-2000 ℃ at a heating rate of 20 ℃/min, and cool the membrane to room temperature after keeping for 1 h.
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