CN112280541A - Preparation method of high-thermal-conductivity composite material based on graphitized poly-dopamine-coated metal particles - Google Patents
Preparation method of high-thermal-conductivity composite material based on graphitized poly-dopamine-coated metal particles Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-thermal-conductivity composite material based on graphitized polydopamine-coated metal particles, which comprises the steps of utilizing graphene to achieve high thermal conductivity along the in-plane direction, the isotropic thermal conductivity of metal and the adhesiveness of polydopamine, blending the metal particles coated with a layer of polydopamine with controllable thickness with a carbon-based filler, utilizing the adhesiveness of the polydopamine to connect graphene sheet layers, and finally performing high-temperature compression treatment to graphitize the polydopamine and melt the metal particles so as to prepare the high-thermal-conductivity composite material. According to the invention, high heat conduction of metal and graphitized polydopamine is utilized, and a high-efficiency heat conduction channel is built between 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
Along with the miniaturization and the increase of the density degree of the electronic appliance, the requirements of related components on the heat conduction performance and the electrical performance are higher and higher. For example, in the currently common tablet personal computers, the electronic appliances are increasingly diversified in function while the size is continuously reduced. The problem that the electronic device generates a large amount of heat in the high-speed operation process, the heat accumulation of the electronic product is obviously generated by long-time use, and further the accelerated aging of the internal device and the shell of the electronic product is caused, so that the use reliability of the electronic device is greatly influenced, and the service life of the electronic device is even reduced. Therefore, the development of a high thermal conductivity scattering material capable of effectively channeling heat becomes a key issue for thermal management.
Carbon element is one of the most closely related and important elements existing in nature and having diverse electron orbital characteristics, and sp2The anisotropy of (b) causes anisotropy of crystals and anisotropy of arrangement thereof, and thus carbon materials having carbon element as a sole constituent element have various properties. The carbon material has high heat conductivity, low density, low thermal expansion, excellent mechanical property and chemical stability, is a heat conduction material with the greatest development prospect in recent years, and has wide application prospect in the fields of energy, communication, electronics and the like. Wherein the graphene is a two-dimensional planar crystal with a honeycomb hexagonal structure, and the carrier mobility of the graphene is extremely high (15000 cm)2V · s) to provide a channel for the rapid migration of electrons and holes, which will greatly improve the performance of existing semiconductor materials and devices; graphene has the highest thermal conductivity (5300W/(m · K)) of all materials, which is bound to provide a completely new idea for the heat dissipation design of electronic devices. However, the two-dimensional structure of the graphene has high thermal conductivity only along the horizontal plane, and the thermal conductivity coefficient in the direction vertical to the graphene layer is very low and generally does not exceed 10W/(m.K), strictlyWhich limits its application in thermal management.
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 along the horizontal direction and the thickness direction aiming at the defect that the existing graphene material has obvious anisotropic thermal conductivity, namely the graphene-based composite material has high thermal conductivity along the plane of graphene (more than 1000W/(m.K)) and has too low thermal conductivity (less than 10W/(m.K)) in the thickness direction vertical to the horizontal plane, wherein the thermal conductivity of the prepared composite material along the plane is as high as more than 800W/(m.K), and the thermal conductivity along the thickness direction is more than 80W/(m.K).
The technical purpose of the invention is realized by the following technical scheme.
A preparation method of a high-thermal-conductivity composite material based on graphitized polydopamine-coated metal particles comprises the steps of uniformly dispersing polydopamine-coated metal nanoparticles and graphene in a solvent, forming a composite film by the polydopamine-coated metal nanoparticles and the graphene through suction filtration or sedimentation, and then carrying out thermal treatment to enable the polydopamine-coated metal nanoparticles to be subjected to hot melting and carbonization between graphene sheet layers, so that a graphene sheet layer structure is connected 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 40-80 nm.
In the above technical scheme, water is used as a solvent.
In the technical scheme, the metal nanoparticles coated with the polydopamine are uniformly mixed with the dopamine, the trihydroxymethyl aminomethane is added to initiate dopamine to polymerize on the surfaces of the metal nanoparticles, and the polydopamine-coated metal particles are obtained through centrifugation. Dispersing metal nano particles into an aqueous solution containing dopamine hydrochloride by ultrasonic action (such as 100W for 30 minutes), and then adding a trihydroxymethyl aminomethane buffer solvent to make the pH value of the solution alkaline (such as pH 7-8) to initiate dopamine autopolymerization; after the reaction is completed, the metal nano particles coated with the polydopamine are obtained by a centrifugal separation method.
In the technical scheme, the poly-dopamine-coated metal nanoparticles and graphene are uniformly dispersed under the action of ultrasound, for example, the ultrasound action is continued for 1-5 hours under 80-150 w, preferably for 2-3 hours under 100-150 w, functional groups existing in the graphene lamellar structure are combined with poly-dopamine layers on the surfaces of the poly-dopamine-coated metal nanoparticles through multiple interaction, and then the modified metal particle/graphene composite dispersion liquid is obtained.
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 graphene lamellar structure and polydopamine-coated metal nanoparticles are allowed to freely settle to form a membrane by standing for 20-40 hours, or a membrane material is obtained by a vacuum filtration method, the graphene can form a layer-by-layer stacked structure due to the two-dimensional structure of the graphene, the polydopamine-coated metal particles can be dispersed in a distributed manner among graphene layers due to the extremely small size, and the interaction between the graphene and the polydopamine-coated metal particles is also beneficial to the dispersion of the polydopamine-coated metal particles; in particular, the existence of polydopamine 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 pressure is applied to the composite film at 0.5-5 MPa, the carbonization coated by the polydopamine and the melting of the metal nanoparticles are carried out at the temperature of 1000-2000 ℃ (the treatment time is 0.5-2 h), and the melted metal is connected with the 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 polydopamine-coated metal particles after hot melting is facilitated, so that the performance of the material is influenced. 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; meanwhile, polydopamine can be graphitized to be filled between metal and graphene, so that interface thermal resistance is reduced, and the heat conductivity of the composite material 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 graphene/polydopamine coated metal particles are subjected to hot pressing molding through the steps, so that the integrity and compactness of the material are improved. 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; the graphitized polydopamine layer also plays a role in connecting the graphene and the metal. Through the design of the structure, the adjustment and control of the anisotropic heat conductivity of the carbon-based composite material are realized, and the high-heat-conductivity carbon composite material with the heat conductivity of more than 800W/(m.K) along the plane direction and more than 80W/(m.K) along the thickness direction is obtained, compared with the Chinese invention patent application of the prior applicant subject group (a preparation method of the high-heat-conductivity graphene-metal particle composite material, application No. 2019106625466, application No. 2019, 7-month and 22-day), the improvement is obvious, the application is based on the Chinese invention patent application, the metal melting and the poly-dopamine carbonization act together through the technical means of the poly-dopamine-coated metal particles, the heat conductivity of the composite material in the thickness direction is further enhanced, and experimental actual tests prove that the application belongs to the patent application of the technical scheme obtained under the same subject, the act of applying an abnormal application that is not a simple replacement or assembly of multiple patent applications for different materials, components, proportions, parts, etc.
As a traditional excellent heat conduction material, besides having a high heat conduction coefficient (500- & ltSUB & gt 700W/(m & ltSUB & gt K)), different metal materials also show good ductility, and the metal materials can be considered to be combined with carbon materials as intercalation layers so as to improve the relevant performance. Compared with the prior art, the invention has the following beneficial effects: the matrix raw material graphene and the modified metal particles are simple in process, and the graphitized polyphenyl polymer is compounded with metal so as to well improve the heat conduction efficiency of the composite material. According to the invention, the microstructure ordering of the graphene and the modified 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 direction can be obtained, and the comprehensive heat conductivity of the graphene-based composite material is far superior to that of the traditional graphene and graphene-based composite material, namely the application of the polydopamine-coated metal nanoparticles in increasing the heat conductivity of the graphene-based composite material in the thickness direction 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 science and technology Limited is 50nm, and the size of the silver nanoparticles is 60-80 nm. When dispersion is carried out, 100w of ultrasonic stirring is selected for 2 hours. The inert gas in the heat treatment is nitrogen.
Example 1
1. 100mg of metal nano particles (gold nanorods) are weighed, dispersed in 10ml of dopamine hydrochloride solution (1mg/ml), ultrasonically stirred for 30min, 12.1mg of trihydroxymethyl aminomethane is introduced to initiate dopamine polymerization, and after room temperature reaction, the polydopamine coated metal particles (modified gold nanorods) are obtained through centrifugal separation.
2. 0.5g of functionalized graphene and 0.1g of modified gold nanorods are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the modified gold nanorods into the graphene dispersion liquid which is continuously stirred, so that the modified gold nanorods and the functionalized graphene sheets are fully combined. 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.
3. Placing the obtained composite material in a graphite mold, applying a pressure of 0.5MPa, preheating for 1h at 800 ℃ in a tubular furnace under the condition of inert gas, then placing the composite material in the graphite mold, keeping the pressure unchanged, carrying out fusion treatment on metal particles and graphitization treatment on polydopamine for 1h at 1500 ℃, converting gold nanorods into liquid metal, dispersing, graphitizing the polydopamine, linking metal and graphene, and finally obtaining the graphene/gold particle composite material. The thermal conductivity of the test material was 815W/(mK) in the planar direction and 86W/(mK) in the thickness direction.
Example 2
1. Weighing 100mg of metal nano particles (gold nanoplates), dispersing the metal nano particles into 15ml of dopamine hydrochloride solution (1mg/ml), ultrasonically stirring for 30min, introducing 15.5mg of trihydroxymethyl aminomethane to initiate dopamine polymerization, reacting at room temperature, and centrifugally separating to obtain the polydopamine-coated metal particles (modified gold nanoplates).
2. 0.5g of functionalized graphene and 0.1g of modified gold nanoplatelets are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the modified gold nanoplatelets into the graphene dispersion under continuous stirring, so that the modified gold nanoplatelets and the functionalized graphene nanoplatelets are fully combined. 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/modified gold nanosheet composite material.
3. Placing the obtained composite material in a graphite mold, applying a pressure of 1MPa, preheating 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 of metal particles and graphitization of polydopamine for 2h at 1000 ℃, converting gold nano-sheets into a liquid metal dispersed and graphitized polydopamine linked metal and graphene sheet layer structure, and obtaining the graphene/gold particle composite material. The thermal conductivity of the test material was 865W/(m.K) in the planar direction and 95W/(m.K) in the thickness direction.
Example 3
1. 100mg of metal nano particles (silver nanorods) are weighed, dispersed in 10ml of dopamine hydrochloride solution (1mg/ml), ultrasonically stirred for 30min, 12.1mg of trihydroxymethyl aminomethane is introduced to initiate dopamine polymerization, and after room temperature reaction, the metal particles (modified silver nanorods) coated with polydopamine are obtained through centrifugal separation.
2. 0.5g of functionalized graphene and 0.1g of modified silver nanorods are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the modified silver nanorods into the graphene dispersion liquid which is continuously stirred, so that the modified silver nanorods and the functionalized graphene sheets are fully combined. 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/modified silver nanorod composite material.
3. 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 of metal particles and graphitization of polydopamine for 1h at 1800 ℃, converting silver nanorods into liquid metal for dispersion, graphitizing the polydopamine, linking the metal with a graphene sheet layer structure, and obtaining the graphene/silver particle composite material. The thermal conductivity of the test material was 893W/(m.K) in the planar direction and 90W/(m.K) in the thickness direction.
Example 4
1. 100mg of metal nano particles (copper nanorods) are weighed, dispersed in 10ml of dopamine hydrochloride solution (1mg/ml), ultrasonically stirred for 30min, 12.1mg of trihydroxymethyl aminomethane is introduced to initiate dopamine polymerization, and after the reaction at room temperature (20-25 ℃), the metal particles (modified copper nanorods) coated with polydopamine are obtained through centrifugal separation.
2. 0.5g of functionalized graphene and 0.1g of modified copper particles were weighed and dispersed in 50ml of distilled water, respectively. And then gradually adding the aqueous dispersion of the modified copper nanorod into the graphene dispersion liquid which is continuously stirred, so that the modified copper nanorod and the functionalized graphene sheet are fully combined. 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/modified copper nanorod composite material.
3. Placing the obtained composite material in a graphite mold, applying 2MPa pressure, 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 of the modified copper nano rods and graphitization treatment of the polydopamine at 2000 ℃ for 30min, converting the copper nano rods into liquid metal for dispersion, and graphitizing the polydopamine linked metal and graphene sheet layer structure to obtain the graphene/copper particle composite material. The thermal conductivity of the test material was 870W/(m.K) in the planar direction and 92W/(m.K) in the thickness direction.
Example 5
1. 100mg of metal nano particles (gold nanospheres) are weighed, dispersed in 10ml of dopamine hydrochloride solution (1mg/ml), ultrasonically stirred for 30min, 12.1mg of trihydroxymethyl aminomethane is introduced to initiate dopamine polymerization, and after room temperature reaction, the polydopamine coated metal particles (modified gold nanospheres) are obtained through centrifugal separation.
2. 0.5g of functionalized graphene and 0.1g of modified gold nanospheres are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the modified gold nanospheres into the graphene dispersion liquid which is continuously stirred, so that the modified gold nanospheres and the functionalized graphene sheets are fully combined. 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/modified gold nanosphere composite material.
3. Placing the obtained composite material in a graphite mold, applying 2MPa pressure, carrying out preheating treatment for 2h at 800 ℃ in a tube furnace under the condition of inert gas, then placing the composite material in the graphite mold, keeping the pressure unchanged, carrying out melting of metal particles and graphitization treatment of polydopamine for 1.5h at 1500 ℃, converting gold nanospheres into a liquid metal, dispersing the liquid metal, graphitizing the polydopamine, linking the metal with a graphene sheet layer structure, and obtaining the graphene/gold particle composite material. The thermal conductivity of the test material was 820W/(m.K) in the planar direction and 83W/(m.K) in the thickness direction.
Example 6
1. 100mg of metal nano particles (silver nanospheres) are weighed and dispersed in 10ml of dopamine hydrochloride solution (1mg/ml), after ultrasonic stirring is carried out for 30min, 12.1mg of trihydroxymethyl aminomethane is introduced to initiate dopamine polymerization, and after room temperature reaction, centrifugal separation is carried out to obtain the polydopamine coated metal particles (modified silver nanospheres).
2. 0.5g of functionalized graphene and 0.1g of modified silver nanospheres are weighed and respectively dispersed in 50ml of distilled water. And then gradually adding the aqueous dispersion of the modified silver nanospheres into the graphene dispersion liquid which is continuously stirred, so that the modified 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/modified silver nanosphere composite material.
3. Placing the obtained composite material in a graphite mold, applying a pressure of 3MPa, preheating for 1h at 820 ℃ under the condition of inert gas in a tube furnace, then placing the composite material in the graphite mold, maintaining the pressure unchanged, carrying out melting of metal particles and graphitization of polydopamine for 1.5h at 1200 ℃, converting silver nanospheres into liquid metal for dispersion, graphitizing the polydopamine for linking the metal with a graphene sheet layer structure, and obtaining the graphene/silver particle composite material. The thermal conductivity of the test material was 860W/(m.K) in the planar direction and 84W/(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 composite material has a thermal conductivity coefficient of more than 800W/(m.K) along the plane direction, namely the performance of the original graphene is basically maintained, and the thermal conductivity coefficient along the thickness direction can reach 80-95W/(m.K), which is obviously better than the performance of the original graphene and the graphene-metal composite material. 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 composite material based on graphitized polydopamine-coated metal particles is characterized in that polydopamine-coated metal nanoparticles and graphene are uniformly dispersed in a solvent, a composite film is formed by the polydopamine-coated metal nanoparticles and the graphene through suction filtration or sedimentation, and then heat treatment is carried out to carbonize the polydopamine and melt the metal nanoparticles, so that a graphene sheet structure is connected in the thickness direction.
2. The preparation method of the highly thermal conductive composite material based on the graphitized poly-dopamine coated metal particle as claimed in claim 1, wherein the poly-dopamine coated metal nanoparticle is prepared by uniformly blending metal nanoparticles and dopamine, adding tris (hydroxymethyl) aminomethane to initiate dopamine polymerization on the surface of the metal nanoparticles, and centrifuging to obtain the poly-dopamine coated metal particle, wherein the metal nanoparticles are commercialized metal nanoparticles such as gold, silver and copper, and have a microscopic morphology of nanospheres, nanorods and nanosheets, and a size of 40-80 nm.
3. The method for preparing a high thermal conductive composite material based on graphitized poly-dopamine coated metal particles according to claim 1, wherein graphene is two-dimensional sheet graphene, such as functionalized graphene sheet (with functional groups such as hydroxyl group and carboxyl group); water is used as a solvent.
4. The method for preparing a high thermal conductive composite material based on graphitized poly-dopamine coated metal particles according to claim 1, wherein the poly-dopamine coated metal nanoparticles and graphene are uniformly dispersed under the action of ultrasound, such as 80-150 w ultrasound for 1-5 hours, preferably 100-150 w ultrasound for 2-3 hours.
5. The preparation method of the high thermal conductivity composite material based on the graphitized polydopamine-coated metal particles as claimed in claim 1, wherein a composite membrane is formed by vacuum filtration or free settling, and during the preparation of the graphene/metal particle membrane, the graphene lamellar structure and the polydopamine-coated metal nanoparticles are allowed to freely settle for 20-40 hours to form a membrane, or the membrane material is obtained by vacuum filtration.
6. The method for preparing a high thermal conductive composite material based on graphitized poly-dopamine coated metal particles as claimed in claim 1, wherein after the composite film is formed, the solvent is removed by supercritical drying to prevent the material from shrinking and deforming due to internal stress during the solvent evaporation process.
7. The preparation method of the high thermal conductivity composite material based on the graphitized polydopamine coated metal particles as claimed in claim 1, wherein during the heat treatment, the pressure of 0.5-5 MPa is applied to the composite film, the carbonization coated with polydopamine and the melting of the metal nanoparticles are performed at 1000-2000 ℃ (the treatment time is 0.5-2 h), and the melted metal is connected with the graphene lamellar structure in the thickness direction, so as to obtain the graphene/metal particle thermal conductivity composite material; and placing the composite film in a graphite mold for heat treatment.
8. The preparation method of the high thermal conductivity composite material based on the graphitized poly-dopamine coated metal particles as claimed in claim 1, wherein before the heat treatment, the composite film is subjected to a pressure of 0.5 to 5MPa, and is subjected to a preheating treatment at 800 to 850 ℃ for 1 to 2 hours, wherein the inert gas is nitrogen, helium or argon, the composite film is selectively placed in a graphite mold to be subjected to a pressure application, and the pretreatment is performed in a tube furnace under the condition of the inert gas.
9. Highly thermally conductive composite materials based on graphitized polydopamine coated metal particles obtainable by the process according to any of claims 1 to 8, characterized by a thermal conductivity in the planar direction of more than 800W/(m.K) and in the thickness direction of more than 80W/(m.K), preferably a thermal conductivity in the thickness direction of 80 to 95W/(m.K).
10. The application of the polydopamine-coated metal nanoparticles in increasing the heat conductivity of the graphene-based composite material in the thickness direction.
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| CN114751404A (en) * | 2022-04-29 | 2022-07-15 | 上海大学 | High-thermal-conductivity graphene thick film and preparation method thereof |
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