CN112280540A - Preparation method of high-thermal-conductivity graphene-metal particle composite material - Google Patents
Preparation method of high-thermal-conductivity graphene-metal particle composite material Download PDFInfo
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- CN112280540A CN112280540A CN201910662546.6A CN201910662546A CN112280540A CN 112280540 A CN112280540 A CN 112280540A CN 201910662546 A CN201910662546 A CN 201910662546A CN 112280540 A CN112280540 A CN 112280540A
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Abstract
The invention discloses a preparation method of a high-thermal-conductivity graphene-metal particle composite material, which comprises the steps of utilizing the high thermal conductivity of graphene along the in-plane direction and the isotropic thermal conductivity of metal, mixing and filtering a graphene layer and metal nanoparticles in a liquid phase to form a membrane, utilizing the metal coordination effect of the metal particles and graphene sheet layers to connect the graphene sheet layers, and finally fusing the metal nanoparticles between the graphene sheet layers through high-temperature compression treatment to prepare the high-thermal-conductivity carbon-based composite material. According to the invention, the high heat conduction of metal is utilized, and the high-efficiency heat conduction channel is built between the graphene layers, 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 relates to a preparation method of a graphene/metal particle 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, people have higher and higher power requirements and smaller sizes on electronic equipment, so that waste heat generated by the electronic equipment during operation is more and more concentrated, and further the heat management is more and more difficult, and therefore greater requirements are provided for the heat conduction performance and the heat dissipation performance of the equipment. 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 carbon material is an excellent material with high heat conductivity, low density, low thermal expansion, excellent mechanical property and chemical stability, and is also a heat conduction material with development prospect in recent years, so that the carbon material has wide application prospect in the fields of energy, communication, electronics and the like. Among them, graphene is the most representative carbon material with high thermal conductivity and high mechanical strength, and is widely used in various products. The theoretical thermal conductivity coefficient of the graphene is as high as 3080-5300W/(m.K), and the graphene is a filler with excellent thermoelectric property, which is commonly used in the preparation of a thermal conductive composite material at present. However, graphene as a two-dimensional material has high thermal conductivity only along a horizontal plane, and thermal conductivity perpendicular to a graphene layer shows a very low thermal conductivity coefficient, generally not exceeding 10W/(m · K), due to lack of an effective thermal conductivity channel, and thus application of graphene in thermal management is severely limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a preparation method of a graphene-based 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 material has high thermal conductivity (more than 1000W/(m.K)) in the graphene plane and has too low thermal conductivity (less than 10W/(m.K)) in the thickness direction perpendicular to the horizontal plane. The prepared composite material has a thermal conductivity coefficient along a plane of more than 800W/(m.K), and a thermal conductivity along the thickness direction of more than 56W/(m.K).
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of a high-thermal-conductivity graphene-metal particle composite material comprises the steps of uniformly dispersing metal nanoparticles and graphene in a solvent, carrying out suction filtration or sedimentation to enable the metal nanoparticles and the graphene to form a composite film, and carrying out heat treatment to enable the metal nanoparticles to be subjected to hot melting between graphene sheet layers so as to realize the connection of a graphene sheet layer structure in the thickness direction.
In the above technical solution, the graphene is two-dimensional sheet graphene, such as functionalized graphene sheet (with functional groups such as hydroxyl group and carboxyl group).
In the technical scheme, the metal nanoparticles are commercialized metal nanoparticles such as gold, silver and copper, and the metal nanoparticles have the microscopic appearances of nanospheres, nanorods and nanosheets and have the sizes of 10-50 nm.
In the above technical scheme, water is used as a solvent.
In the above technical scheme, the metal nanoparticles and the graphene are uniformly dispersed under the action of ultrasound, for example, the ultrasound action is continued for 1 to 5 hours under 80 to 150w, preferably for 2 to 3 hours under 100 to 150w, and a functional group existing in the graphene lamellar structure is combined with the metal nanoparticles through metal coordination, so that the adhesion between the graphene and the metal nanoparticles can be enhanced, and the uniform dispersion of the metal nanoparticles in the graphene lamellar structure is facilitated.
In the technical scheme, the composite membrane is formed by vacuum filtration or free settling. In the process of preparing the graphene/metal particle membrane, a membrane material is obtained by standing for 20-40 hours to enable a graphene lamellar structure and metal nanoparticles to freely settle to form a membrane or by a vacuum filtration method, the graphene can form a layer-by-layer stacked structure due to a two-dimensional structure of the graphene, the metal particles can be dispersed in a distributed manner among graphene layers due to the extremely small size of the graphene, and meanwhile, the coordination between the graphene and the metal particles is also beneficial to the dispersion of the metal particles; in particular, the existence of metal coordination can enhance the bonding between graphene and metal particles and prevent the material from dispersing after the solvent is removed.
In the above technical solution, after the composite film is formed, the solvent is removed by supercritical drying to prevent the material from being contracted and deformed by internal stress during the evaporation of the solvent.
In the technical scheme, when the heat treatment is carried out, the composite film is subjected to pressure of 0.5-5 MPa, metal nano particles are melted at the temperature of 1000-2000 ℃ (the treatment time is 20-40 min), and the melted metal is connected with a graphene lamellar structure in the thickness direction to obtain the graphene/metal particle heat-conducting composite material; and placing the composite film in a graphite mold for heat treatment. In the heat treatment process of the graphene/metal particle membrane material, the graphite mold applies compressive stress to the graphene/metal particle membrane material, so that the deformation of the material can be prevented, and the deformation of the metal particles after hot melting is facilitated, thereby affecting the performance of the material. In the heat treatment process, functional groups on the graphene sheets can fall off, so that lattice defects on the structure of the graphene sheets are perfected, the impurity content is reduced, and the heat conductivity is improved.
In the technical scheme, before heat treatment, the composite membrane is subjected to pressure application of 0.5-5 MPa, preheating treatment is carried out for 1-2 h at 800-850 ℃, inert gas is nitrogen, helium or argon, the composite membrane is placed in a graphite mold to apply pressure, and pretreatment is carried out in a tubular furnace under the condition of the inert gas.
The hot-pressing molding of the graphene/metal particles through the steps improves the integrity and compactness of the material. The horizontal stacking of graphene gives high horizontal plane thermal conductivity to the material; the isotropic heat conduction performance of the metal particles formed between the graphene sheet layer structures after melting provides a channel for heat conduction in the thickness direction of the material; meanwhile, the function of connecting graphene is achieved. Through the design of the structure, 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.
As a traditional excellent heat and electricity conducting material, besides high heat conductivity coefficient (500- & ltSUB & gt 700W/(m & K)), different metal materials also show good ductility and can be used as optional fillers for preparing heat conducting composite materials. Compared with the prior art, the invention has the following beneficial effects: the matrix raw materials of the graphene and the metal particles are simple in process. According to the invention, the microstructure ordering of graphene and metal particles, the densification and graphitization of the material can be efficiently completed, the graphene-based composite material with high heat conductivity coefficient along the plane and thickness directions can be obtained, the comprehensive heat conductivity of the graphene-based composite material is far superior to that of the traditional graphene and graphene-based composite material, particularly, the heat conductivity along the thickness direction is greatly improved, namely, the application of metal nanoparticles in increasing the heat conductivity in the thickness direction of the graphene-based composite material is realized.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the composite material of the present invention.
Fig. 2 is a transmission electron micrograph of graphene oxide used in the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples. According to the literature: yu H, Zhang B, Bulin C, et al, high-efficiency synthesis of graphene oxide based on improved hummers method, scientific reports,2016,6:36143. The specific size of the metal nanoparticles is related to the trade mark, for example, the size of the gold nanoparticles of Nanjing Xiancheng nanomaterial Technical Co., Ltd is 50nm, and the size is 10-50 nm. When dispersion is to be carried out, 100w of ultrasound is selected for 2 hours. The inert gas in the heat treatment is nitrogen.
Example 1
0.5g of functionalized graphene and 0.1g of gold nanorods are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the gold nanorods into the graphene dispersion liquid which is continuously stirred, so that the gold nanorods and the functionalized graphene sheets have sufficient coordination combination. And (3) carrying out vacuum filtration on the dispersion liquid to remove the hydrosolvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/gold nanorod composite material.
Placing the obtained composite material in a graphite mold, applying a pressure of 0.5MPa, preheating for 2h at 800 ℃ in a tubular furnace under the condition of inert gas, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out fusion treatment on metal particles for 0.5h at 1500 ℃, converting gold nanorods into liquid metal, and dispersing the liquid metal among graphene lamellar structures to obtain the graphene/gold particle 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
0.5g of functionalized graphene and 0.1g of silver nanorods are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the silver nanorods into the graphene dispersion liquid which is continuously stirred, so that the gold nanorods and the functionalized graphene sheets have sufficient coordination combination. And (3) carrying out vacuum filtration on the dispersion liquid to remove the hydrosolvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/silver nanorod composite material.
And placing the obtained composite material in a graphite mold, applying a pressure of 1MPa, carrying out preheating treatment for 1h at 850 ℃ in a tube furnace under the condition of inert gas, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out melting treatment on metal particles for 40min at 1000 ℃, converting the silver nanorods into liquid metal, and dispersing the liquid metal among graphene lamellar structures to obtain the graphene/gold particle 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
0.5g of functionalized graphene and 0.1g of copper nanorods are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the water dispersion liquid of the silver nanorods into the graphene dispersion liquid which is continuously stirred, so that the copper nanorods and the functionalized graphene sheets have sufficient coordination and combination. And (3) carrying out vacuum filtration on the dispersion liquid to remove the hydrosolvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/copper nanorod composite material.
Placing the obtained composite material in a graphite mold, applying a pressure of 5MPa, carrying out preheating treatment for 1.5h at 800 ℃ under the condition of inert gas in a tube furnace, then placing the composite material in the graphite mold, keeping the pressure unchanged, carrying out melting treatment on metal particles for 0.5h at 1800 ℃, converting copper nanorods into liquid metal, and dispersing the liquid metal among graphene lamellar structures to obtain the graphene/copper particle composite material. The thermal conductivity of the test material was 890W/(m.K) in the planar direction and 63W/(m.K) in the thickness direction.
Example 4
0.5g of functionalized graphene and 0.1g of gold particles were weighed and dispersed in 50ml of distilled water, respectively. And then gradually adding the aqueous dispersion of the gold particles into the graphene dispersion liquid which is continuously stirred, so that the gold particles and the functionalized graphene sheets have sufficient coordination combination. And (3) carrying out vacuum filtration on the dispersion liquid, removing a water solvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/gold particle composite material.
And placing the obtained composite material in a graphite mold, applying a pressure of 2MPa, carrying out preheating treatment for 2h at 850 ℃ in a tube furnace under the condition of inert gas, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out melting treatment on metal particles for 20min at 2000 ℃, converting the gold particles into liquid metal, and dispersing the liquid metal among graphene lamellar structures to obtain the graphene/gold particle composite material. The thermal conductivity of the test material was 820W/(m.K) in the planar direction and 58W/(m.K) in the thickness direction.
Example 5
0.5g of functionalized graphene and 0.1g of silver nanosheet are weighed and dispersed in 50ml of distilled water respectively. And then gradually adding the aqueous dispersion of the silver nanosheets into the graphene dispersion liquid which is continuously stirred, so that the silver nanosheets and the functionalized graphene sheets have sufficient coordination combination. And (3) carrying out vacuum filtration on the dispersion liquid to remove the hydrosolvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/silver nanosheet composite material.
Placing the obtained composite material in a graphite mold, applying a pressure of 2MPa, carrying out preheating treatment for 1h at 800 ℃ in a tube furnace under the condition of inert gas, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out melting treatment on metal particles for 40min at 1500 ℃, converting silver nanosheets into liquid metal, and dispersing the liquid metal among graphene lamellar structures to obtain the graphene/silver particle composite material. The thermal conductivity of the test material was 900W/(m.K) in the planar direction and 72W/(m.K) in the thickness direction.
Example 6
0.5g of functionalized graphene and 0.1g of silver nanospheres are weighed and dispersed in 50ml of distilled water respectively. And then gradually adding the aqueous dispersion of the silver nanospheres into the graphene dispersion liquid which is continuously stirred, so that the silver nanospheres and the functionalized graphene sheets have sufficient coordination combination. And (3) carrying out vacuum filtration on the dispersion liquid, removing the hydrosolvent to obtain a composite membrane material, and then carrying out supercritical drying on the composite material to obtain the graphene/silver nanosphere composite material.
Placing the obtained composite material in a graphite mold, applying a pressure of 3MPa, preheating for 1h at 820 ℃ in a tube furnace under the condition of inert gas, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out fusion treatment on metal particles for 0.5h at 1600 ℃, converting silver nanospheres into liquid metal and dispersing the liquid metal among graphene lamellar structures, thus obtaining the graphene/silver particle composite material. The thermal conductivity of the test material was 850W/(m.K) in the planar direction and 60W/(m.K) in the thickness direction.
The preparation of the composite material can be realized by adjusting the process parameters according to the content of the invention, and tests show that the thermal conductivity of the composite material along the plane direction is more than 800W/(m.K), namely the performance of the original graphene is basically maintained, and the thermal conductivity along the thickness direction can reach 56-75W/(m.K), which is obviously better than the performance of the original graphene. 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. A preparation method of a high-thermal-conductivity graphene-metal particle composite material is characterized by uniformly dispersing metal nanoparticles and graphene in a solvent, performing suction filtration or sedimentation to enable the metal nanoparticles and the graphene to form a composite film, and performing thermal treatment to enable the metal nanoparticles to be subjected to hot melting between graphene sheet layers so as to realize a graphene sheet layer structure connected in the thickness direction.
2. The method for preparing the graphene-metal particle composite material with high thermal conductivity according to claim 1, wherein the graphene is two-dimensional sheet graphene, such as functionalized graphene sheet; the metal nanoparticles are commercialized metal nanoparticles such as gold, silver and copper, and the metal nanoparticles have the microscopic appearances of nanospheres, nanorods and nanosheets and have the sizes of 10-50 nm; water is used as a solvent.
3. The method for preparing the graphene-metal particle composite material with high thermal conductivity according to claim 1, wherein the ultrasonic action is selected to achieve uniform dispersion of the metal nanoparticles and the graphene, such as 80-150 w ultrasonic action for 1-5 hours, preferably 100-150 w ultrasonic action for 2-3 hours.
4. The method for preparing the graphene-metal particle composite material with high thermal conductivity according to claim 1, wherein the graphene lamellar structure and the metal nanoparticles are allowed to freely settle to form a film by standing for 20 to 40 hours.
5. The preparation method of the graphene-metal particle composite material with high thermal conductivity according to claim 1, wherein the membrane material is obtained by a vacuum filtration method.
6. The method for preparing a highly thermally conductive graphene-metal particle composite material according to claim 1, wherein after the composite film is formed, the solvent is removed by supercritical drying to prevent the material from being shrunk and deformed by internal stress during the solvent evaporation process.
7. The preparation method of the graphene-metal particle composite material with high thermal conductivity according to claim 1, wherein before the heat treatment, the composite film is subjected to a pre-heating treatment at 800-850 ℃ for 1-2 h under a pressure of 0.5-5 MPa, and an inert gas is nitrogen, helium or argon, and the composite film is placed in a graphite mold to apply pressure, and is subjected to the pre-treatment in a tube furnace under the condition of the inert gas.
8. The preparation method of the graphene-metal particle composite material with high thermal conductivity as claimed in claim 1, wherein during the thermal treatment, the composite film is subjected to carbonization at 1000-2000 ℃ under a pressure of 0.5-5 MPa, and the metal nanoparticles are melted (the treatment time is 20-40 min), and the melted metal is connected with the graphene lamellar structure in the thickness direction, so as to obtain the graphene/metal particle thermal-conductive composite material; and placing the composite film in a graphite mold for heat treatment.
9. The graphene-metal particle composite material having high thermal conductivity obtained by the production method according to any one of claims 1 to 8, wherein the thermal conductivity is more than 800W/(m.K) in the planar direction and more than 56W/(m.K) in the thickness direction, and preferably the thermal conductivity in the thickness direction is 56 to 75W/(m.K).
10. The application of the metal nanoparticles in increasing the heat conduction capability of the graphene-based composite material in the thickness direction.
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| CN113416389A (en) * | 2021-07-28 | 2021-09-21 | 四川大学 | Ultrahigh isotropic heat conduction material of epoxy two-dimensional sheet metal nano filler and preparation method thereof |
| CN113755142A (en) * | 2021-09-09 | 2021-12-07 | 广西师范大学 | High-thermal-conductivity aniline functionalized graphene/copper composite material and preparation method thereof |
| CN113999657A (en) * | 2021-11-23 | 2022-02-01 | 安徽碳华新材料科技有限公司 | Processing technology of alkene-carbon composite material |
| CN115155482A (en) * | 2022-07-25 | 2022-10-11 | 江苏大学 | Device and method for preparing graphene loaded nano metal particles by pulse discharge flash |
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| CN107164647A (en) * | 2017-04-28 | 2017-09-15 | 哈尔滨赫兹新材料科技有限公司 | High heat conduction rigidity graphene/copper nano composite material fin and preparation method thereof |
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| CN113416389A (en) * | 2021-07-28 | 2021-09-21 | 四川大学 | Ultrahigh isotropic heat conduction material of epoxy two-dimensional sheet metal nano filler and preparation method thereof |
| CN113416389B (en) * | 2021-07-28 | 2022-05-13 | 四川大学 | Ultrahigh isotropic heat conduction material of epoxy two-dimensional sheet metal nano filler and preparation method thereof |
| CN113755142A (en) * | 2021-09-09 | 2021-12-07 | 广西师范大学 | High-thermal-conductivity aniline functionalized graphene/copper composite material and preparation method thereof |
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| CN115155482A (en) * | 2022-07-25 | 2022-10-11 | 江苏大学 | Device and method for preparing graphene loaded nano metal particles by pulse discharge flash |
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