CN113321208A - Preparation method of high-compactness graphene membrane - Google Patents
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Abstract
The invention discloses a preparation method of a high-compactness graphene film, which takes graphene oxide slurry A as a film-forming precursor and takes graphene oxide slurry B as an impregnant. Assembling a graphene film by a wet chemical method and carrying out thermal reduction, filling an impregnant into pores of reduced graphene oxide, repeating the steps for many times until a compact product is obtained, and finally completing graphitization treatment on the compact thermal reduction product. The graphene film obtained by the invention has fewer pores and high compactness, so that the graphene film has higher thermal conductivity. The temperature control device can be used in the fields of transverse temperature equalization of electronic equipment and the like.
Description
Technical Field
The invention belongs to the technical field of graphene film preparation, and particularly relates to a preparation method of a high-compactness graphene film.
Background
The rapid development of integrated circuits has made heat dissipation of electronic devices a common problem. Taking a smart phone as an example, the peak power consumption of the smart phone in the age of 5G can reach more than 10W. Heat accumulation is easily formed at high-power parts such as a Central Processing Unit (CPU), a baseband chip and the like. If heat is not removed from these areas by effective means, localized hot spots will be created, which in turn affect the performance and lifetime of the device. The plane heat conduction capability of graphite is extremely high, and the characteristic is very beneficial to transverse temperature equalization of local heat, so that the artificial graphite film is widely used as a heat dissipation material in electronic products such as smart phones and the like. The technical principle is that the graphite film diffuses local heat to the whole large plane in a heat conduction mode, so that the heat flow density is reduced, and local hot spots are eliminated. The heat diffusion capacity of the graphite film in the process is directly related to the thermal conductivity of the artificial graphite film.
The graphene is a graphite crystal with a hexagonal honeycomb structure, and the theoretical thermal conductivity of the graphene can reach more than 3000W/mK. Once the graphene is assembled into a graphene film with a certain thickness, the graphene film can be used as a new-generation heat dissipation material. Mainstream preparation methods of graphene include vapor deposition, graphene oxide and other technical routes. The graphene oxide is prepared by using graphene oxide slurry as a precursor, assembling graphene oxide into a GO thin film, and then obtaining the heat-conducting graphene film by high-temperature reduction and other technologies.
The heat dissipation capability of a graphene film is directly related to its thermal conductivity (λ). It is therefore common knowledge of many engineers to develop graphene films of high thermal conductivity. Graphene films are prepared through a graphene oxide technology route, and most of the graphene oxide films are subjected to reduction technology to remove non-carbon atoms. The high-temperature thermal reduction can remove oxygen atoms in the graphene oxide and repair a hexagonal carbon atom surface net, and is an important technical route for preparing the graphene film. The removal of these non-carbon atoms necessarily leaves defects in the graphene film, especially in the high-temperature thermal reduction technology, and the evolved gas is very likely to form pores in the film under the action of high temperature. The oxygen content in the graphene oxide is about 40%, so that the volume density of the graphene film formed by high-temperature thermal reduction is low (lower than 0.5 g/cm) in the actual production process3). The thermal conductivity of a solid material is directly related to the bulk density. If the bulk density is too low, it means that pores are contained inside the solid. These pores are poor conductors of heat. Therefore, the improvement of the densification degree of the graphene film has a positive effect on obtaining the graphene film with high thermal conductivity.
Graphene oxide undergoes a series of chemical and physical changes during thermal reduction and high-temperature heat treatment: in the thermal reduction process, oxygen atoms and other non-carbon elements are removed, the plane size shrinks, and the thickness direction shrinks; during the further high temperature heat treatment, the evolved gas causes a thickness-wise expansion under the effect of the high temperature. This complex physical change makes densification to produce graphene films a difficult point in the industry. Chinese patent CN107010618A discloses a method for preparing a graphene oxide film with high thermal conductivity, which comprises processing the graphene oxide film by low-temperature hot pressing and then high-temperature hot reduction. Chinese patent CN107140619A further uses a high-temperature hot-pressing process to process the graphene oxide film, and converts the graphene oxide film into a graphene film with high thermal conductivity under the combined action of high temperature and pressure. Most of these inventions relate to low/medium/high temperature hot pressing processes, and it is necessary to point out that these processes have two disadvantages: one is that, as described above, graphene oxide undergoes both shrinkage (in the plane direction) and expansion (in the thickness direction) during thermal reduction and high-temperature heat treatment. This complex dimensional change presents manufacturing challenges. The principle of hot press molding is to apply mechanical pressure to a sample through upper and lower working surfaces, and therefore hot press processing is effective to restrain expansion in the thickness direction. For such complicated dimensional change of graphene oxide, it is not appropriate to use only the hot press process. For example: and the sample is subjected to pressure treatment in the shrinkage stage, so that the shrinkage of the sample is limited, and cracks are easily generated. Secondly, the cost of the hot pressing equipment is higher, and the size of the product is limited by the working face of the hot press.
Disclosure of Invention
Aiming at the technical defects in the prior art, the invention provides a densification method of a high-densification graphene film according to the chemical and physical changes of graphene oxide in the heat treatment process. Namely, the graphene slurry for film formation and the graphene slurry for impregnation are prepared according to the size relationship between graphene particles. The former is used for suction filtration and coating film formation, and after the graphene oxide film is thermally reduced, the pores of the former are filled with the impregnated graphene slurry. Carrying out thermal reduction on the impregnated product, and repeating the thermal reduction-impregnation-thermal reduction for multiple times to finally obtain the high compactness (the volume density is higher than 1.6 g/cm)3) The graphene film of (1).
In order to achieve the technical purpose, the invention specifically adopts the following technical scheme:
a preparation method of a high-compactness graphene membrane comprises the following steps:
1) preparing a graphene oxide film by taking the graphene oxide slurry A as a precursor in a suction filtration or slurry coating mode;
2) thermally reducing the graphene oxide film in vacuum or inert atmosphere to remove non-carbon atoms;
3) immersing the reduced graphene oxide film into the graphene oxide slurry B, and vacuumizing to 10Kpa to finish the immersion process;
4) repeating steps 2) and 3) until the weight and volume density of the reduced graphene oxide film are no longer increased;
5) and heating the graphene film subjected to the dipping treatment under a protective atmosphere to complete graphitization treatment, and finally forming a compact graphene film.
The mass concentration of the graphene oxide in the graphene oxide slurry A is 1-6 wt.%, and the sheet diameter is 2-100 micrometers.
The mass concentration of the graphene oxide in the graphene oxide slurry B is 0.2-6 wt.%, and the sheet diameter is 20-500 nm.
The graphene oxide slurry A is assembled into a graphene oxide film with the thickness of 10-400 microns in a suction filtration, coating and other modes.
The graphene oxide film is thermally reduced to be heated to 200-900 ℃ at the speed of 1 ℃/min.
The graphitization is that the reduced graphene oxide film is heated to 2200-3100 ℃ at a speed of 5 ℃/min under a protective atmosphere to form a compact graphene film.
The invention has the beneficial effects that:
according to the invention, the impregnated graphene slurry is used for filling the thermally reduced graphene oxide film, non-carbon atoms of the large-size graphene oxide film are removed in the thermal reduction process to leave pores, and the graphene oxide film is filled with small-size graphene oxide, so that the density of the graphene film is gradually improved in the repeated impregnation-thermal reduction process, the pores in the graphene film are correspondingly reduced, and the thermal conductivity of the solid material is improved.
Drawings
FIG. 1 is a process flow for preparing a high-density graphene oxide membrane according to the present invention;
FIG. 2 is a scanning electron micrograph of a dense graphene film of the present invention after repeated infiltration and thermal reduction;
fig. 3 is an X-ray diffraction pattern of the high-density graphene film in example 5 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The graphene oxide film is assembled by a wet chemical method by taking the graphene oxide as a precursor. And carrying out high-temperature thermal reduction to obtain the graphene film. This process is accompanied by the removal of a large number of non-carbon atoms and the formation of evolved gases. Therefore, the prepared graphene film is often porous and difficult to compact, and the electric conduction and heat conduction performance of the graphene film is further influenced. The invention selects proper graphene oxide slurry as a film forming component (A) and a dipping component (B) respectively, firstly assembles the graphene oxide into a film, and then thermally reduces the film to remove non-carbon atoms. The reduced product is then impregnated with graphene oxide slurry B, and the product is then thermally reduced. This process is repeated several times until no further weight gain occurs, and the product is subsequently graphitized. The graphene oxide film is converted into high compactness (the volume density is more than or equal to 1.6 g/cm) by the technology3) The graphene film of (1).
Specifically, as shown in fig. 1, the invention provides a method for preparing a high-density graphene film, which comprises the following steps:
1) preparing a graphene oxide film of 10-400 micrometers by taking graphene oxide slurry A with the mass concentration of 0.2-6 wt.% as a precursor through suction filtration or slurry coating, wherein the sheet diameter of the graphene oxide is 2-100 micrometers;
2) heating to 200-900 ℃ at the speed of 1 ℃/min in vacuum or inert atmosphere to carry out thermal reduction on the graphene oxide film, and removing non-carbon atoms;
3) immersing the reduced graphene oxide film into graphene oxide slurry B with the mass concentration of 0.2-6 wt.%, and vacuumizing to finish the impregnation process, wherein the graphene oxide sheet diameter in the graphene oxide slurry B is 20-500 nanometers;
4) repeating steps 2) and 3) until the weight and bulk density of the reduced graphene oxide film no longer increase (fig. 2);
5) and heating the graphene film subjected to the dipping treatment to 2200-3100 ℃ at a speed of 5 ℃/min under a protective atmosphere to complete the graphitization treatment, and finally forming a compact graphene film.
Example 1
1) Graphene oxide slurry A with the average sheet diameter of 2 microns and the mass concentration of 1.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 10 microns is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 1 graphene oxide film is loaded into a graphite mold, and then the temperature is raised to 200 ℃ at a speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 20nm and the mass concentration of 0.2 wt.%. And vacuumizing the two parts to 10Kpa in a vacuum oven, and finishing the impregnation process under the action of negative pressure.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 200 ℃ at a speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
6) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 2200 ℃ at the speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.6g/cm3The thermal conductivity was 733W/mK.
Example 2
1) Graphene oxide slurry A with the average sheet diameter of 10 micrometers and the mass concentration of 2.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 20 micrometers is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 2 graphene oxide films were loaded into a graphite mold and then heated to 400 ℃ at a rate of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 50nm and the mass concentration of 0.5 wt.%. And vacuumizing the two parts to 10Kpa in a vacuum oven, and finishing the impregnation process under the action of negative pressure.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 400 ℃ at a speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes. The thermally reduced composite was again impregnated with graphene oxide slurry B and reduced again at a temperature of 400 ℃ for 30 minutes.
6) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the film, putting the film into a graphite mold, and heating the film to 2300 ℃ at the speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.65g/cm3The thermal conductivity was 751W/mK.
Example 3
1) Graphene oxide slurry A with the average sheet diameter of 20 micrometers and the mass concentration of 2.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 50 micrometers is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 2 graphene oxide films were loaded into a graphite mold and then heated to 600 ℃ at a rate of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 100nm and the mass concentration of 1.0 wt.%. And vacuumizing the two parts to 10Kpa in a vacuum oven, and finishing the impregnation process under the action of negative pressure.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 600 ℃ at the speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes. And impregnating the thermally reduced compound with the graphene oxide slurry B again, and reducing the compound at the temperature of 600 ℃ for 30 minutes again, namely repeating the impregnation-thermal reduction process for 2 times.
6) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 2400 ℃ at a speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.71g/cm3The thermal conductivity is 779W/mK.
Example 4
1) Graphene oxide slurry A with the average sheet diameter of 50 microns and the mass concentration of 3.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 100 microns is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 3 graphene oxide films were loaded into a graphite mold and then heated to 800 ℃ at a rate of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 200nm and the mass concentration of 2.0 wt.%. And vacuumizing the two parts to 10Kpa in a vacuum oven, and finishing the impregnation process under the action of negative pressure.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 800 ℃ at the speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes. And impregnating the thermally reduced compound with the graphene oxide slurry B again, and reducing the compound at the temperature of 800 ℃ for 30 minutes again, namely repeating the impregnation-thermal reduction process for 2 times.
6) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 2500 ℃ at a speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.79g/cm3The thermal conductivity was 811W/mK.
Example 5
1) Graphene oxide slurry A with the average sheet diameter of 100 micrometers and the mass concentration of 5.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 200 micrometers is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 3 graphene oxide films were loaded into a graphite mold and then heated to 900 ℃ at a rate of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 500nm and the mass concentration of 3.0 wt.%. And vacuumizing the two parts to 10Kpa in a vacuum oven, and finishing the impregnation process under the action of negative pressure.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 900 ℃ at the speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes. Impregnating the compound subjected to thermal reduction again with the graphene oxide slurry B, and reducing the compound at the temperature of 900 ℃ for 30 minutes again, namely repeating the impregnation-thermal reduction process for 2 times
6) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 2600 ℃ at a speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.85g/cm3The thermal conductivity was 835W/mK.
As shown in fig. 3, the characteristic size L of the inner graphite crystallite can be calculated to be 150nm by the scherrer equation.
Example 6
1) Graphene oxide slurry A with the average sheet diameter of 100 micrometers and the mass concentration of 6.0 wt.% is used as a precursor, and a graphene oxide film with the thickness of 400 micrometers is formed on a tetrafluoroethylene filter membrane through a vacuum filtration method.
2) The graphene oxide film was rolled out and cut into a square of 100X 100 mm. 3 graphene oxide films were loaded into a graphite mold and then heated to 900 ℃ at a rate of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes.
4) And taking out the reduced graphene oxide film subjected to thermal reduction treatment from the mold, and immersing the reduced graphene oxide film into graphene oxide slurry B with the average particle size of 500nm and the mass concentration of 6.0 wt.%. And putting the two into an autoclave to pressurize to 3MPa to complete the impregnation process.
5) And taking out the reduced graphene oxide film subjected to the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 900 ℃ at the speed of 1 ℃/min. After the target temperature was reached, the temperature was maintained for 30 minutes. Impregnating the compound subjected to thermal reduction again with the graphene oxide slurry B, and reducing the compound at the temperature of 900 ℃ for 30 minutes again, namely repeating the impregnation-thermal reduction process for 2 times
6) And taking out the reduced graphene oxide film after the dipping treatment, weighing the reduced graphene oxide film, putting the film into a graphite mold, and heating the film to 3100 ℃ at a speed of 5 ℃/min. And after the target temperature is reached, keeping the temperature for 30 minutes to finish the graphitization treatment. The volume density of the graphene film after graphitization treatment can reach 1.84g/cm3The thermal conductivity was 896W/mK.
The properties of the graphene films prepared in examples 1 to 6 of the present invention are shown in table 1.
TABLE 1 physical Properties of ultra-high thermal conductivity graphene films
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A preparation method of a high-compactness graphene membrane is characterized by comprising the following steps:
1) preparing a graphene oxide film by taking the graphene oxide slurry A as a precursor in a suction filtration or slurry coating mode;
2) thermally reducing the graphene oxide film in vacuum or inert atmosphere to remove non-carbon atoms;
3) immersing the reduced graphene oxide film into the graphene oxide slurry B, and vacuumizing to 10Kpa to finish the immersion process;
4) repeating steps 2) and 3) until the weight and volume density of the reduced graphene oxide film are no longer increased;
5) and heating the graphene film subjected to the dipping treatment under a protective atmosphere to complete graphitization treatment, and finally forming a compact graphene film.
2. The method for preparing a high-density graphene film according to claim 1, wherein the mass concentration of graphene oxide in the graphene oxide slurry A is 1-6 wt.%, and the sheet diameter is 2-100 μm.
3. The method for preparing a high-density graphene film according to claim 1, wherein the mass concentration of graphene oxide in the graphene oxide slurry B is 0.2-6 wt.%, and the sheet diameter is 20-500 nm.
4. The method for preparing the high-compactness graphene film according to claim 1, wherein the graphene oxide film is thermally reduced to be heated to 200-900 ℃ at a speed of 1 ℃/min.
5. The method for preparing the high-compactness graphene film according to claim 1, wherein the graphitization is to heat the reduced graphene oxide film to 2200-3100 ℃ at a speed of 5 ℃/min under a protective atmosphere.
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| CN115536018A (en) * | 2022-09-30 | 2022-12-30 | 深圳市贝特瑞新能源技术研究院有限公司 | Graphene oxide slurry, heat-conducting film and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115010119A (en) * | 2022-06-10 | 2022-09-06 | 中国航发北京航空材料研究院 | Graphene thick film and preparation method thereof |
| CN115010119B (en) * | 2022-06-10 | 2023-10-20 | 中国航发北京航空材料研究院 | Graphene thick film and preparation method thereof |
| CN115536018A (en) * | 2022-09-30 | 2022-12-30 | 深圳市贝特瑞新能源技术研究院有限公司 | Graphene oxide slurry, heat-conducting film and preparation method |
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