CN112520731B - Preparation method and production line of graphene heat-conducting film - Google Patents
Preparation method and production line of graphene heat-conducting film Download PDFInfo
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Abstract
The invention discloses a preparation method and a production line of a graphene heat-conducting film, and relates to the field of preparation of heat-conducting devices. A preparation method of a graphene heat conduction film comprises the following steps: s1: uniformly stirring and mixing a carbon source and a heat conduction reinforcing agent; s2: performing discharge machining on the mixed carbon source and the heat conduction reinforcing agent to obtain a doped graphene sheet; s3: screening the doped graphene sheets to obtain graphene rough sheets; s4: cleaning and drying the graphene rough sheet; s5: mixing the cleaned and dried graphene coarse sheets with an N-methyl pyrrolidone solution to obtain carbon dense slurry; s6: coating the carbon thick slurry into a graphene film in a blade mode; s7: and carrying out discharge hot-pressing treatment on the graphene film to obtain the graphene heat-conducting film. The method is used for processing and preparing the heat-conducting film by using a wide carbon source, provides a solution for solving the heat dissipation problem of the next generation of electronic devices, and meets the industrial requirements of easy operation, high efficiency and low cost.
Description
Technical Field
The invention relates to the field of preparation of heat-conducting devices, in particular to a preparation method and a production line of a graphene heat-conducting film.
Background
With the problem of large heat generation caused by the increasing functionalization and miniaturization of electronic components, the accumulation of heat has a serious impact on the service life of electronic equipment, and especially with the arrival of the 5G era, higher requirements are put forward on the heat dissipation management performance in communication. Conventional thermal management materials are mainly copper-based, aluminum-based and silver-based metal materials, which have the advantages of good thermal conductivity and easy processing, however, since metal materials have higher density values, non-metallic thermal conductive materials are more suitable in some applications requiring a small weight. In recent years, non-metallic heat conductive materials have been increasingly enriched with intensive research, especially carbon-based materials such as diamond thin films, highly oriented pyrolytic graphene, graphitized polyimide, and the like. Graphene as a typical representative of the carbon material is sp2A dense stack of monolayers of hybridized carbon atoms. The graphene has ultrahigh inherent thermal conductivity of 3500-5300W/m.K and 2630m2The graphene-based material has the advantages of large specific surface area per gram, low atomic mass, flexibility and firm bonding force, so that the graphene-based material can be used for developing a heat conducting film, is expected to meet the heat dissipation requirements of new-generation electronic equipment, and is easy for industrial production.
Chinese patent CN111252759A discloses a method for preparing graphene oxide by peeling graphene/amorphous carbon in liquid phase by light irradiation, and the yield of graphene oxide is affected by the preparation of electrolyte. Chinese patent CN110256981A discloses a preparation and structure of graphene thermal conductive film, which has a complex structure, needs to improve the structural integrity, and is not easy to be produced in mass.
Therefore, the development of the mass production method of the graphene-based heat-conducting film can provide a solution for solving the heat dissipation problem of the next-generation electronic device, and is an application approach for widening graphene materials, and meanwhile, the production cost is reduced.
Disclosure of Invention
In view of the above defects, the present invention provides a method and a production line for manufacturing a graphene thermal conductive film, so as to process a wide range of carbon sources and manufacture a thermal conductive film, to provide a solution for solving the heat dissipation problem of the next generation of electronic devices, and to meet the industrial requirements of easy operation, high efficiency and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a preparation method of a graphene heat-conducting film, which comprises the following steps:
s1: uniformly stirring and mixing a carbon source and a heat conduction reinforcing agent;
s2: performing discharge machining on the mixed carbon source and the heat conduction reinforcing agent to obtain a doped graphene sheet;
s3: screening the doped graphene sheets to obtain graphene rough sheets;
s4: cleaning and drying the graphene rough sheet;
s5: mixing the cleaned and dried graphene coarse sheets with an N-methyl pyrrolidone solution to obtain carbon dense slurry;
s6: coating the carbon thick slurry into a graphene film in a blade mode;
s7: and carrying out discharge hot-pressing treatment on the graphene film to obtain the graphene heat-conducting film.
Further, the method of performing the electrical discharge machining on the mixed carbon source and the thermal conductivity enhancer in the step S2 is: and (3) loading the mixed carbon source and heat conduction reinforcing agent into a plurality of heat insulation bottles, and sequentially carrying out alternating current electric discharge machining on the plurality of heat insulation bottles to convert the carbon source and the heat conduction reinforcing agent into doped graphene sheets.
Further, the method for cleaning the graphene rough sheet in the step S4 is as follows: firstly, diluted hydrochloric acid with the concentration of 10-20% is used for cleaning, and then N-methyl pyrrolidone is used for cleaning.
Further, the method for blending carbon dense slurry in step S5 is: mixing the graphene crude sheet and the N-methyl pyrrolidone solution in a mass ratio of 5-10: 1, and stirring in a stirrer for 2-5 h.
Further, the graphene film is subjected to the discharge heating and pressing treatment in step S7 by using joule heat to heat, wherein the hot pressing voltage is set to 10V to 100V, the hot pressing capacitance is set to 10mF to 200mF, the hot pressing pressure is set to 20 to 30Mpa, and the processing time is 1h to 3 h.
Further, in the step S1, the resistance of the mixed carbon source and the thermal conductivity enhancer is 1 to 100 Ω.
The invention also discloses a production line of the graphene heat-conducting film, which is applied to the preparation method of the graphene heat-conducting film, and the production line comprises a first conveyor belt, a second conveyor belt, a heat-insulating bottle, a computer, and an electric discharge machining mechanism, a sorting mechanism, a cleaning mechanism, a drying mechanism, a thick slurry blending mechanism, a blade coating mechanism and an electric discharge hot-pressing mechanism which are sequentially arranged; the heat insulation bottle is used for storing the mixed carbon source and the heat conduction reinforcing agent; the first conveyor belt is used for conveying the heat insulation bottles; the electric discharge machining mechanism is used for carrying out electric discharge machining on the heat insulation bottle on the first conveyor belt to obtain doped graphene sheets; the second conveyor belt is used for conveying the doped graphene sheets poured out of the heat insulation bottle; the sorting mechanism is used for screening out graphene rough sheets from the doped graphene sheets on the second conveyor belt; the cleaning mechanism is used for cleaning and drying the graphene rough sheet; the thick slurry preparing mechanism is used for preparing thick carbon slurry; the blade coating mechanism is used for blade coating the carbon dense slurry into a graphene film; the discharge hot-pressing mechanism is used for performing discharge hot-pressing treatment on the graphene film to prepare a graphene heat-conducting film; and the computer is used for carrying out production cycle control on the electric discharge machining mechanism and the electric discharge hot-pressing mechanism.
Furthermore, two ends of the heat insulation bottle are respectively provided with a metal electrode, a first electrical interface and a fixing ring, and the first electrical interfaces at the two ends are respectively electrically connected with the metal electrodes at the same end; the electric discharge machining mechanism comprises a temperature sensing module and a first electric cabinet; the temperature sensing module is used for detecting the temperature of the heat insulation bottle; the first electrical cabinet is provided with a first flourishing discharge capacitor group and a first high-voltage power supply, the first flourishing discharge capacitor group is provided with a second electrical interface, and the first high-voltage power supply is electrically connected with the first flourishing capacitor group; the temperature sensing module and the first high-voltage power supply are respectively in communication connection with the computer; the two first conveyor belts are arranged side by side; the heat insulation bottles are sequentially arranged on the first conveying belt, and fixing rings of the heat insulation bottles are fixedly connected with the first conveying belt on the same side respectively; the plurality of first electrical cabinets are sequentially arranged beside the first conveyor belt, and the second electrical interfaces of the first container groups are electrically connected with the first electrical interfaces of the corresponding heat insulation bottles respectively; the charge-discharge capacitor groups sequentially carry out alternate discharge; and if the computer detects that the temperature peak value of a certain heat insulation bottle is lower than 3000K, the computer controls the first capacitor containing group corresponding to the heat insulation bottle to discharge again until the heat insulation bottle reaches the temperature peak value of 3000K.
Further, the sorting mechanism comprises a blower, an ultrasonic transducer, a distributor and an ultrasonic generator; the blower is arranged on one side of the second conveyor belt, and the plurality of ultrasonic transducers are arranged on the other side of the second conveyor belt opposite to the blower; the air blower is provided with a plurality of air outlets, and the air outlets are arranged towards the opposite side of the second conveyor belt; the ultrasonic generator distributes ultrasonic waves into a plurality of ultrasonic transducers through a distributor.
Further, the discharge hot-pressing mechanism comprises a hot-pressing upper die, a hot-pressing lower die, a vacuum cavity and a second electrical cabinet; the second electrical cabinet is provided with a second full discharge capacitor group and a second high-voltage power supply; the hot-pressing upper die and the hot-pressing lower die are arranged in the vacuum cavity in an up-down opposite manner; the second container group is electrically connected with the hot pressing upper die and the hot pressing lower die respectively; the second high-voltage power supply is electrically connected with the second holding capacitor group; the second high-voltage power supply is in communication connection with the computer.
According to the preparation method of the graphene heat-conducting film, provided by the invention, an electric field is utilized to carry out a chemical carbonization process and a physical stripping process, the binding force of a graphite layer is overcome, and carbonized graphite carbon is successfully stripped into a sheet layer, so that the preparation method can be applied to almost all carbon-containing carbon sources. Meanwhile, the method utilizes discharge machining and heat conduction enhancer for auxiliary catalysis, so that carbon source carbonization and stripping are controllably completed, the method is suitable for a large part of non-carbonized carbon-containing carbon sources, the high heat conduction of graphene film products is guaranteed, the variety of the carbon sources for machining is expanded, the requirements of environmental protection, low cost, high efficiency, sustainable development and the like are further met, and an effective solution is provided for the large-scale preparation of high-quality high-efficiency graphene. Furthermore, the method has high process feasibility and continuity, can realize automation for most parts, is easy to integrate in the existing production line, greatly saves labor cost and ensures the safety of industrial production.
According to the production line of the graphene heat-conducting film, provided by the invention, the first conveyor belt, the second conveyor belt, the heat-insulating bottle, the computer, the sequential electric discharge machining mechanism, the sorting mechanism, the cleaning mechanism, the drying mechanism, the thick slurry blending mechanism, the blade coating mechanism and the electric discharge hot pressing mechanism are integrated, the automation degree is high, the labor cost is greatly saved, and the industrial production safety is ensured. The production rhythm control is carried out on the electric discharge machining mechanism and the electric discharge hot-pressing mechanism through the computer, voltage control and current control are achieved, the circuit stability of the production line is greatly improved, and the machining quality is optimized.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a graphene thermal conductive film according to the present invention;
fig. 2 is a schematic structural diagram of a production line of a graphene thermal conductive film according to the present invention;
FIG. 3 is a schematic structural view of an electric discharge machining mechanism in an embodiment of the present invention;
FIG. 4 is a schematic diagram of the configuration of the sorting mechanism in one embodiment of the present invention;
fig. 5 is a schematic structural diagram of an electric discharge hot press mechanism in an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention. Furthermore, features defined as "first" and "second" may explicitly or implicitly include one or more of the features for distinguishing between descriptive features, non-sequential, non-trivial and non-trivial.
Referring to fig. 1, the invention discloses a preparation method of a graphene heat-conducting film, which comprises the following steps:
s1: uniformly stirring and mixing a carbon source and a heat conduction reinforcing agent;
s2: performing discharge machining on the mixed carbon source and the heat conduction reinforcing agent to obtain a doped graphene sheet;
s3: screening the doped graphene sheets to obtain graphene rough sheets;
s4: cleaning and drying the graphene rough sheet;
s5: mixing the cleaned and dried graphene coarse sheets with an N-methyl pyrrolidone solution to obtain carbon dense slurry;
s6: coating the carbon thick slurry into a graphene film in a blade mode;
s7: and carrying out discharge hot-pressing treatment on the graphene film to obtain the graphene heat-conducting film.
It should be noted that, in the embodiment of the present invention, the carbon source may be any one or more of biomass carbon material, hydrocarbon material, carbon material refined by processing, and plastic powder. The heat conduction enhancer can be formed by mixing any one or more of metal nitride, inorganic non-metallic material, metal simple substance and metal oxide. Wherein the biomass carbon material is selected from lignin, pine wood powder, straw powder, etc.; hydrocarbon materials such as coke, coal, anthracite, and the like; processed and refined carbon materials such as ketjen black, carbon black, etc.; plastic powders such as polypropylene, polystyrene, etc. Metal nitrides such as boron nitride, silicon nitride, aluminum nitride; inorganic non-metallic materials such as graphite, silicon carbide, carbon fiber, carbon nanotube; simple metal such as copper powder and aluminum powder; metal oxides such as aluminum oxide, zinc oxide.
According to the preparation method of the graphene heat-conducting film, provided by the invention, an electric field is utilized to carry out a chemical carbonization process and a physical stripping process, the binding force of a graphite layer is overcome, and carbonized graphite carbon is successfully stripped into a sheet layer, so that the preparation method can be applied to almost all carbon-containing carbon sources. Meanwhile, the method utilizes discharge machining and heat conduction enhancer for auxiliary catalysis, so that carbon source carbonization and stripping are controllably completed, the method is suitable for a large part of non-carbonized carbon-containing carbon sources, the high heat conduction of graphene film products is guaranteed, the variety of the carbon sources for machining is expanded, the requirements of environmental protection, low cost, high efficiency, sustainable development and the like are further met, and an effective solution is provided for the large-scale preparation of high-quality high-efficiency graphene. Furthermore, the method has high process feasibility and continuity, can realize automation for most parts, is easy to integrate in the existing production line, greatly saves labor cost and ensures the safety of industrial production.
Specifically, the method of performing the electrical discharge machining on the mixed carbon source and the thermal conductivity enhancer in the step S2 is: and (3) loading the mixed carbon source and heat conduction reinforcing agent into a plurality of heat insulation bottles A300, and sequentially carrying out alternating current electric discharge machining on the plurality of heat insulation bottles A300 to convert the carbon source and the heat conduction reinforcing agent into doped graphene sheets. In the machining process, the discharge voltage is preferably 100V-300V, and the discharge capacitance is preferably 40 mF-200 mF. In the invention, the mixed carbon source and the heat conduction reinforcing agent are arranged in a plurality of heat insulation bottles A300, so that voltage control and current control can be favorably carried out on the mixed carbon source and the heat conduction reinforcing agent, the circuit stability is improved, and the processing quality is optimized. The mixed carbon source and the heat conduction reinforcing agent are processed by using alternating current, so that the carbon source and the heat conduction reinforcing agent move in two directions, the carbonization effect and the stripping effect are greatly enhanced, and the carbon source is more fully carbonized and converted into graphene sheets.
Further, the method for cleaning the graphene rough sheet in the step S4 is as follows: firstly, diluted hydrochloric acid with the concentration of 10-20% is used for cleaning, and then N-methyl pyrrolidone is used for cleaning. Therefore, metal and inorganic ions in the graphene crude sheet are washed away by dilute hydrochloric acid, the graphene crude sheet is fully dispersed and stripped into small-sheet-layer graphene nanosheets by N-methyl pyrrolidone, the N-methyl pyrrolidone can absorb water among graphene sheet layers, and simultaneously thick slurry with good consistency is conveniently prepared for subsequent coating to prepare a uniform graphene film.
Specifically, the method for blending carbon dense slurry in step S5 includes: mixing the graphene crude sheet and the N-methyl pyrrolidone solution in a mass ratio of 5-10: 1, and stirring in a stirrer for 2-5 h. The graphene crude sheets and the N-methyl pyrrolidone solution are mixed according to the mass ratio of 5-10: 1, so that the concentration of the carbon dense slurry is ensured, and waste caused by excessive amount of the graphene crude sheets is avoided. In addition, the graphene coarse sheets are stirred for 2-5 hours by the stirrer, so that the graphene coarse sheets and the N-methyl pyrrolidone solution are fully mixed and contacted, the dissolution of the graphene coarse sheets in the N-methyl pyrrolidone solution is accelerated, and the efficiency of blending the carbon dense slurry is improved.
Specifically, the method of blade coating the carbon dense slurry to form the film in step S6 is: uniformly coating the carbon thick slurry on a copper foil substrate by using a scraper, and placing the copper foil substrate in a vacuum drying oven for accelerated drying, wherein the drying temperature is set to be 60-90 ℃, and the drying time is 2 h.
Specifically, the graphene film is subjected to the discharge heating and pressing treatment in step S7 by using joule heat to heat, wherein the hot pressing voltage is set to 10V to 100V, the hot pressing capacitance is set to 10mF to 200mF, the hot pressing pressure is set to 20 to 30Mpa, and the processing time is 1h to 3 h. In this manner, the conjugated skeleton in the defective graphene block can be substantially restored in a very short time by joule heat induced by current, and thus the microstructure and the flake arrangement can be finely controlled by voltage and capacitance, and the operation is easy.
Preferably, in the step S1, the resistance of the mixed carbon source and the thermal conductivity enhancer is 1 to 100 Ω. If the carbon source and the thermal conductivity enhancer after mixing are less than 1 ohm, a short circuit effect is caused, the current of the circuit is infinite, and the circuit is damaged. According to the joule heat formula Q ═ U2t/R, under a constant voltage, joule heat is inversely proportional to the square value of resistance, and therefore, if the mixed carbon source and heat conductivity enhancer are higher than 100 ohms, joule heat deficiency occurs, so that the mixed carbon source and heat conductivity enhancer cannot be completely converted into doped graphene sheets, resulting in low production efficiency. Therefore, the embodiment that the resistance of the mixed carbon source and the heat conduction reinforcing agent is 1-100 omega is preferable, the circuit can be protected, the conversion rate of the mixed carbon source and the mixed heat conduction reinforcing agent is high, and the production efficiency is improved.
Referring to fig. 2 to 5, the invention further provides a production line of the graphene thermal conductive film, which is applied to the preparation method of the graphene thermal conductive film. The production line comprises a first conveyor belt A100, a second conveyor belt A200, a heat insulation bottle A300, a computer A400, and an electric discharge machining mechanism B100, a sorting mechanism B200, a cleaning mechanism B300, a drying mechanism B400, a thick slurry blending mechanism B500, a blade coating mechanism B600 and an electric discharge hot-pressing mechanism B700 which are sequentially arranged. The heat insulation bottle A300 is used for storing the mixed carbon source and the heat conduction reinforcing agent. The first conveyor a100 is used to convey the heat-insulated bottle a 300. The electric discharge machining mechanism B100 is used for carrying out electric discharge machining on the heat insulation bottle A300 on the first conveyor belt A100 to obtain doped graphene sheets. The second conveyor belt a200 is used to convey the doped graphene sheets poured out of the insulated bottle a 300. The sorting mechanism B200 is used for screening out graphene rough sheets from the doped graphene sheets on the second conveyor belt A200. The cleaning mechanism B300 is used for cleaning and drying the graphene rough sheets. The thick slurry preparing mechanism B500 is used for preparing the carbon thick slurry. The blade coating mechanism B600 is used for blade coating the carbon concentrated slurry into a graphene film. The discharge hot-pressing mechanism B700 is used for performing discharge hot-pressing treatment on the graphene film to prepare the graphene heat-conducting film. The computer a400 is configured to perform tact control on the electric discharge machining mechanism B100 and the electric discharge hot press mechanism B700.
According to the production line of the graphene heat-conducting film, the first conveyor belt A100, the second conveyor belt A200, the heat-insulating bottle A300, the computer A400, the discharge machining mechanism B100, the sorting mechanism B200, the cleaning mechanism B300, the drying mechanism B400, the thick slurry blending mechanism B500, the blade coating mechanism B600 and the discharge hot-pressing mechanism B700 are integrated in sequence, the degree of automation is high, the labor cost is greatly saved, and the industrial production safety is guaranteed. The computer A400 is used for controlling the production rhythm of the discharge machining mechanism B100 and the discharge hot-pressing mechanism B700, so that voltage control and current control are realized, the circuit stability of the production line is greatly improved, and the machining quality is optimized.
It should be noted that, two ends of the heat-insulating bottle a300 are respectively provided with a metal electrode a310, a first electrical interface a320 and a fixing ring (not shown in the figure), and the first electrical interfaces a320 at the two ends are respectively electrically connected with the metal electrode a310 at the same end; the metal electrodes A310 at the two ends are used for conducting current, so that the current is mixed with the carbon source and the heat conduction reinforcing agent, and the carbon source and the heat conduction reinforcing agent are converted into the doped graphene sheet. The electric discharge machining mechanism B100 includes a temperature sensing module B110 and a first electrical cabinet B120. The temperature sensing module B110 is used for detecting the temperature of the heat insulation bottle A300. Specifically, the temperature sensing module B110 may be a high-resolution spectrometer equipped with a filter, and the real-time temperature peak is obtained by fitting the collected light wave intensity to a black body radiation equation and performing back-stepping; the maximum light intensity of a sample area can be obtained by combining image processing of a high-speed camera provided with a filter, and then a real-time temperature peak value is obtained by Planck distribution reverse-deduction.
The first electrical cabinet B120 has a first holding capacitor group B121 and a first high-voltage power supply B122, the first holding capacitor group B121 has a second electrical interface B123, and the first high-voltage power supply B122 is electrically connected with the first holding capacitor group B121; so as to charge the first capacitor bank by the first high-voltage power supply B122. The temperature sensing module B110 and the first high-voltage power supply B122 are respectively in communication connection with the computer A400; the temperature peak value of the heat insulation bottle A300 in the machining process is obtained by the computer A400, the first capacitor containing group B121 in the first electrical cabinet B120 is controlled to be charged and discharged, and the production rhythm control of the electric discharge machining mechanism B100 is further realized.
The two first conveyor belts a100 are arranged side by side; the heat insulation bottles A300 are sequentially arranged on the first conveyor belt A100, and fixing rings of the heat insulation bottles A300 are fixedly connected with the first conveyor belt on the same side respectively; the plurality of first electrical cabinets B120 are sequentially arranged beside the first conveyor belt a100, and the second electrical interfaces B123 of the first capacitor holding groups B121 are electrically connected to the first electrical interfaces a320 of the corresponding heat-insulating bottles a300 respectively; the charge-discharge capacitor groups sequentially carry out alternate discharge; if the computer a400 detects that the temperature peak of a certain heat-insulating bottle a300 is lower than 3000K, the computer a400 controls the first capacitor bank B121 corresponding to the heat-insulating bottle a300 to discharge again until the heat-insulating bottle a300 reaches the temperature peak of 3000K.
Specifically, in an embodiment of the present invention, referring to fig. 3, the first electrical cabinet B120 is set to 3 groups, and when the first conveyor a100 conveys three thermal insulation bottles a300, the first group of the first holding capacitor group B121 performs electric discharge machining on the first thermal insulation bottle a300, and the first group of the first holding capacitor group B121 performs charging immediately after the machining is completed. After the first group is discharged, the second group of the first capacitor bank B121 is discharged to the second heat insulation bottle a300, and the second group of the first capacitor bank B121 is charged immediately after being processed. After the second group finishes discharging, the first capacitor group B121 in the first electrical cabinet B120 of the third group discharges the third thermal insulation bottle a300, and the first capacitor group B121 of the third group immediately charges after finishing discharging. Because the discharge processing temperature is directly related to the quality of graphene, generally, it is considered that high-quality few-layer graphene can be obtained only when the temperature reaches more than 3000K, therefore, after the third heat-insulating bottle a300 is processed, the computer a400 detects and judges whether the temperature peak value in the heating process of the 3 heat-insulating bottles a300 is lower than 3000K, if the temperature peak value of a certain heat-insulating bottle a300 is detected to be lower than 3000K, the computer a400 controls the first containing capacitor group B121 corresponding to the heat-insulating bottle a300 to discharge again until the heat-insulating bottle a300 is detected to reach the temperature peak value of 3000K; if the temperature peak values of the 3 heat-insulating bottles a300 reach 3000K, the first conveyor belt a100 sends out the three heat-insulating bottles a300 which are processed, and transports the three heat-insulating bottles a300 to be processed to corresponding positions, and the first holding capacitors of the 3 groups of first electrical cabinets B120 discharge in turn again according to the sequence. In this embodiment, the computer a400 controls the first holding capacitor groups B121 in each group of the first electrical cabinets B120 to alternately charge and discharge, so as to fully utilize the efficiency of the electric wires, reduce the idle time of the equipment, improve the production efficiency of the graphene to the maximum, and ensure the quality of the graphene.
It is further worth noting that, referring to fig. 4, the sorting mechanism B200 includes a blower B210, an ultrasonic transducer B220, a distributor B230, and an ultrasonic generator B240; the blower B210 is disposed at one side of the second conveyor belt a200, and a plurality of the ultrasonic transducers B220 are disposed at the other side of the second conveyor belt a200 opposite to the blower B210; the air blower B210 is provided with a plurality of air outlets B211, and the air outlets B211 are arranged towards the opposite side of the second conveyor belt a 200; the ultrasonic generator B240 distributes the ultrasonic waves into the several ultrasonic transducers B220 through the distributor B230. Therefore, when the doped graphene sheets are conveyed to the sorting mechanism B200 by the second conveyor belt A200, under the combined action of the ultrasonic field and the wind field, the doped graphene sheets realize that the graphene coarse sheets are sorted at the upper air inlet, and the graphene fine sheets are sorted at the lower air inlet, so that the graphene coarse sheets are sorted.
Specifically, the discharge hot-pressing mechanism B700 includes an upper hot-pressing mold B710, a lower hot-pressing mold B720, a vacuum chamber B730, and a second electrical cabinet B740; the second electrical cabinet B740 has a second holding capacitor bank B741 and a second high-voltage power supply B742; the hot pressing upper die B710 and the hot pressing lower die B720 are disposed in the vacuum chamber B730 in an up-down opposite manner; effectively avoiding the oxidation of the graphene film in the discharge hot-pressing process so as to ensure the quality of the graphene heat-conducting film. The second capacitor containing group B741 is electrically connected to the hot-pressing upper die B710 and the hot-pressing lower die B720, respectively; so as to realize the power supply and heating of the hot-pressing upper die B710 and the hot-pressing lower die B720. The second high-voltage power supply B742 is electrically connected to the second holding capacitor group B741; to enable the second high voltage power supply B742 to charge the second hold capacitor. The second high voltage power supply B742 is communicatively connected to the computer a 400. So that the computer A400 controls the second holding capacitor group B741 to discharge and charge, and further realizes the production cycle control of the discharge hot-pressing mechanism B700. In this way, the conjugated skeleton in the defective graphene block can be substantially restored within a very short time by joule heat induced by current, and thus voltage and capacitance are finely controlled by the computer a400, thereby realizing control of microstructure and sheet arrangement, and handling is easy.
Specifically, the washing mechanism B300 includes a washing tank (not shown) for washing away impurities attached to the graphene platelets.
Specifically, the drying mechanism includes a drying box (not shown), and the drying box is used for drying the graphene rough sheets.
Specifically, the thick slurry preparing mechanism B500 includes a preparing tank (not shown) for mixing the graphene crude sheets with the N-methylpyrrolidone solution, and a stirrer (not shown) for stirring the mixed graphene crude sheets with the N-methylpyrrolidone solution.
Specifically, the blade coating mechanism B600 includes a scraper (not shown in the figure), a copper foil substrate (not shown in the figure), and a vacuum drying oven (not shown in the figure), wherein the blade coating mechanism B600 uniformly coats the carbon dense slurry on the copper foil substrate through the scraper, and the vacuum drying oven is used for drying the prepared graphene film.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (2)
1. A preparation method of a graphene heat conduction film is characterized by comprising the following steps:
s1: uniformly stirring and mixing a carbon source and a heat conduction reinforcing agent, wherein the resistance of the mixed carbon source and heat conduction reinforcing agent is 1-100 omega;
s2: the mixed carbon source and the heat conduction reinforcing agent are arranged in a heat insulation bottle for electric discharge machining, and doped graphene is obtained; wherein, the method of performing the electrical discharge machining on the mixed carbon source and the thermal conductivity enhancer in the step S2 is: the mixed carbon source and the heat conduction reinforcing agent are arranged in a plurality of heat insulation bottles, and alternating current electric discharge machining is sequentially carried out on the plurality of heat insulation bottles, wherein the discharge voltage is 100-300V, and the discharge capacitance is 40-200 mF, so that the carbon source and the heat conduction reinforcing agent are converted into doped graphene sheets;
s3: screening the doped graphene sheets to obtain graphene rough sheets;
s4: cleaning and drying the graphene rough sheet; the method for cleaning the graphene rough sheet in the step S4 includes: firstly, cleaning with dilute hydrochloric acid with the concentration of 10-20%, and then cleaning with N-methyl pyrrolidone;
s5: mixing the cleaned and dried graphene coarse sheets with an N-methyl pyrrolidone solution to obtain carbon dense slurry; the method for blending the carbon dense slurry in the step S5 includes: mixing the graphene crude sheets and the N-methyl pyrrolidone solution in a mass ratio of 5-10: 1, and stirring in a stirrer for 2-5 hours;
s6: coating the carbon thick slurry into a graphene film in a blade mode;
s7: carrying out discharge hot pressing treatment on the graphene film to obtain a graphene heat conducting film; in the step S7, the graphene film is subjected to the discharge heating and pressing treatment by joule heat, the hot pressing voltage is set to 10V to 100V, the hot pressing capacitance is set to 10mF to 200mF, the hot pressing pressure is set to 20 to 30Mpa, and the processing time is 1h to 3 h.
2. The production line of the graphene heat-conducting film is applied to the preparation method of the graphene heat-conducting film as claimed in claim 1, and is characterized in that: the production line comprises a first conveyor belt, a second conveyor belt, a heat insulation bottle, a computer, and an electric discharge machining mechanism, a sorting mechanism, a cleaning mechanism, a drying mechanism, a thick slurry blending mechanism, a blade coating mechanism and an electric discharge hot-pressing mechanism which are sequentially arranged;
the heat insulation bottle is used for storing the mixed carbon source and the heat conduction reinforcing agent;
the first conveyor belt is used for conveying the heat insulation bottles;
the electric discharge machining mechanism is used for carrying out electric discharge machining on the heat insulation bottle on the first conveyor belt to obtain doped graphene sheets;
the second conveyor belt is used for conveying the doped graphene sheets poured out of the heat insulation bottle;
the sorting mechanism is used for screening out graphene rough sheets from the doped graphene sheets on the second conveyor belt;
the cleaning mechanism is used for cleaning and drying the graphene rough sheet;
the thick slurry preparing mechanism is used for preparing thick carbon slurry;
the blade coating mechanism is used for blade coating the carbon dense slurry into a graphene film;
the discharge hot-pressing mechanism is used for performing discharge hot-pressing treatment on the graphene film to prepare a graphene heat-conducting film;
the computer is used for controlling the production takt time of the electric discharge machining mechanism and the electric discharge hot-pressing mechanism;
the two ends of the heat insulation bottle are respectively provided with a metal electrode, a first electrical interface and a fixing ring, and the first electrical interfaces at the two ends are respectively electrically connected with the metal electrodes at the same end;
the electric discharge machining mechanism comprises a temperature sensing module and a first electric cabinet;
the temperature sensing module is used for detecting the temperature of the heat insulation bottle;
the first electrical cabinet is provided with a first flourishing discharge capacitor group and a first high-voltage power supply, the first flourishing discharge capacitor group is provided with a second electrical interface, and the first high-voltage power supply is electrically connected with the first flourishing capacitor group;
the temperature sensing module and the first high-voltage power supply are respectively in communication connection with the computer;
the two first conveyor belts are arranged side by side;
the heat insulation bottles are sequentially arranged on the first conveying belt, and fixing rings of the heat insulation bottles are fixedly connected with the first conveying belt on the same side respectively;
the plurality of first electrical cabinets are sequentially arranged beside the first conveyor belt, and the second electrical interfaces of the first container groups are electrically connected with the first electrical interfaces of the corresponding heat insulation bottles respectively; the charge-discharge capacitor groups sequentially carry out alternate discharge;
if the computer detects that the temperature peak value of a certain heat insulation bottle is lower than 3000K, the computer controls the first capacitor containing group corresponding to the heat insulation bottle to discharge again until the heat insulation bottle reaches the temperature peak value of 3000K;
the sorting mechanism comprises a blower, an ultrasonic transducer, a distributor and an ultrasonic generator;
the blower is arranged on one side of the second conveyor belt, and the plurality of ultrasonic transducers are arranged on the other side of the second conveyor belt opposite to the blower;
the air blower is provided with a plurality of air outlets, and the air outlets are arranged towards the opposite side of the second conveyor belt;
the ultrasonic generator distributes ultrasonic waves into a plurality of ultrasonic transducers through a distributor;
the discharge hot-pressing mechanism comprises a hot-pressing upper die, a hot-pressing lower die, a vacuum cavity and a second electrical cabinet;
the second electrical cabinet is provided with a second full discharge capacitor group and a second high-voltage power supply;
the hot-pressing upper die and the hot-pressing lower die are arranged in the vacuum cavity in an up-down opposite manner;
the second container group is electrically connected with the hot pressing upper die and the hot pressing lower die respectively;
the second high-voltage power supply is electrically connected with the second holding capacitor group;
the second high-voltage power supply is in communication connection with the computer.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103831733A (en) * | 2014-02-21 | 2014-06-04 | 山东大学 | Supersonic vibration assisted fluidifying fine grinding material feeding device |
| CN204276098U (en) * | 2014-12-04 | 2015-04-22 | 嘉善申嘉科技有限公司 | Powder screening system |
| CN105013705A (en) * | 2015-07-05 | 2015-11-04 | 上海朗亿功能材料有限公司 | Micro-nano powder removing equipment |
| CN105776185A (en) * | 2014-12-25 | 2016-07-20 | 江南石墨烯研究院 | Preparation method of graphene paper with high thermal conductivity and electrical conductivity |
| CN107337804A (en) * | 2017-08-04 | 2017-11-10 | 湖南国盛石墨科技有限公司 | A kind of PET/ micro crystal graphites alkene composite heat conducting film and preparation method thereof |
| WO2020051000A1 (en) * | 2018-09-05 | 2020-03-12 | William Marsh Rice University | Flash joule heating synthesis method and compositions thereof |
| CN111943180A (en) * | 2020-08-25 | 2020-11-17 | 天能帅福得能源股份有限公司 | Simple and efficient graphene preparation process |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206908B (en) * | 2018-09-12 | 2021-05-07 | 中国科学院山西煤炭化学研究所 | High-thermal-conductivity graphite/plastic composite material and preparation method thereof |
| CN110684510B (en) * | 2019-10-23 | 2021-10-26 | 广东工业大学 | Heat-conduction-enhanced heat-energy-storage shape-stabilized phase-change composite material and preparation method thereof |
-
2020
- 2020-12-24 CN CN202011554657.4A patent/CN112520731B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103831733A (en) * | 2014-02-21 | 2014-06-04 | 山东大学 | Supersonic vibration assisted fluidifying fine grinding material feeding device |
| CN204276098U (en) * | 2014-12-04 | 2015-04-22 | 嘉善申嘉科技有限公司 | Powder screening system |
| CN105776185A (en) * | 2014-12-25 | 2016-07-20 | 江南石墨烯研究院 | Preparation method of graphene paper with high thermal conductivity and electrical conductivity |
| CN105013705A (en) * | 2015-07-05 | 2015-11-04 | 上海朗亿功能材料有限公司 | Micro-nano powder removing equipment |
| CN107337804A (en) * | 2017-08-04 | 2017-11-10 | 湖南国盛石墨科技有限公司 | A kind of PET/ micro crystal graphites alkene composite heat conducting film and preparation method thereof |
| WO2020051000A1 (en) * | 2018-09-05 | 2020-03-12 | William Marsh Rice University | Flash joule heating synthesis method and compositions thereof |
| CN111943180A (en) * | 2020-08-25 | 2020-11-17 | 天能帅福得能源股份有限公司 | Simple and efficient graphene preparation process |
Non-Patent Citations (4)
| Title |
|---|
| Flash Graphene from plastic Waste;Duy Xuan Luong, et al;《ACS NANO》;20201029;第14卷(第11期);全文 * |
| Gram-scale bottom-up flash graphene synthesis;Tour, JM, et al;《Nature》;20200130;第577卷(第7792期);全文 * |
| Rapid roll-to-roll production of graphene films using intensive Joule heating;Liu, YJ, et al;《Carbon》;20191231;第155卷;全文 * |
| 石墨烯化学气相沉积法可控制备的催化反应体系研究;金燕等;《化工学报》;20200630;第71卷(第6期);全文 * |
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