CN113788476A - System and method for continuously preparing graphene film - Google Patents
System and method for continuously preparing graphene film Download PDFInfo
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- CN113788476A CN113788476A CN202111068737.3A CN202111068737A CN113788476A CN 113788476 A CN113788476 A CN 113788476A CN 202111068737 A CN202111068737 A CN 202111068737A CN 113788476 A CN113788476 A CN 113788476A
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Abstract
The invention discloses a system and a method for continuously preparing a graphene film, wherein the system comprises: the method comprises the following steps: the graphene container is used for accommodating a graphene solution and comprises a container opening; the suction filtration device is arranged above the graphene container and comprises a suction filtration port, the suction filtration port is arranged opposite to the container port up and down, the suction filtration port is provided with a plurality of suction filtration holes, and the suction filtration port can be in contact with or close to the liquid level of the graphene solution; the suction filtration substrate is a thin film containing pores; the transmission device comprises a plurality of transmission wheels, and is used for enabling the suction filtration substrate to pass through the space between the container opening and the suction filtration opening and move continuously, and in the moving process, graphene in the graphene solution is loaded on the surface of the suction filtration substrate under the action of the suction filtration device to form a graphene film; and the heating device is used for drying the graphene film coated on the suction filtration substrate. The system and the method provided by the invention are used for solving the problem that large-area and batch preparation is difficult to realize in the production process of the graphene film.
Description
Technical Field
The present invention relates to the field of graphene, and in particular, to a system and a method for continuously preparing a graphene film.
Background
The graphene film is a material with high thermal conductivity and high flexibility, and has wide usability in the fields of aerospace, mobile phones and computers. The preparation method of the graphene film mainly comprises the following steps: chemical vapor deposition, knife coating, spray coating, suction filtration, and the like. The film obtained by the chemical vapor deposition method has the best quality, but is limited by conditions and has higher cost, and the obtained graphene is a single-layer graphene film and has limited application scenes.
The blade coating method is the most common graphene film forming method, but the existing graphene film has the following problems in the blade coating production process: a: the existing graphene film is often produced, and the phenomenon of uneven graphene coverage on the surface of the film occurs, so that the quality of the graphene film is greatly influenced; b: the existing graphene film is always in a film covering state due to the existence and the dirt of the surface of the graphene film, so that a blind area appears when the graphene powder is covered, the film covering effect of the graphene powder is influenced, and the quality of the graphene film is reduced. For graphene preparation by a spraying method, as described in patent CN110813576B, in a production process of a current graphene heat dissipation film spraying device, a substrate is blown or deformed by high-pressure gas sprayed from a nozzle, so that the produced graphene heat dissipation film is unqualified, and dust on the substrate adheres to the substrate, which also affects the quality of the graphene heat dissipation film. The filtration method can obtain high-quality graphene film, but owing to receive process units's restriction, often stay in the laboratory stage, provide the flexible high conductive film of graphite alkene with sandwich structure and preparation method and application as CN110164590B, what adopted is that traditional laboratory buchner flask carries out the suction filtration, though obtained the higher graphene film of quality, unfortunately do not possess continuous production's ability.
Disclosure of Invention
The invention aims to provide a system and a method capable of continuously preparing a graphene film, so as to solve the problem that large-area and batch preparation is difficult to realize in the production process of the graphene film.
In one aspect, the present invention provides a system for continuously preparing a graphene film, including: the graphene container is used for accommodating a graphene solution and comprises a container opening; the suction filtration device is arranged above the graphene container and comprises a suction filtration port, the suction filtration port is arranged opposite to the container port up and down, the suction filtration port is provided with a plurality of suction filtration holes, and the suction filtration port can be in contact with or close to the liquid level of the graphene solution; the suction filtration substrate is a thin film containing pores; the transmission device comprises a plurality of transmission wheels, and is used for enabling the suction filtration substrate to pass through the space between the container opening and the suction filtration opening and move continuously, and in the moving process, graphene in the graphene solution is loaded on the surface of the suction filtration substrate under the action of the suction filtration device to form a graphene film; and the heating device is used for drying the graphene film coated on the suction filtration substrate.
In some embodiments, after the heating device, the method further comprises: the rolling device is used for rolling the graphene film to adjust the thickness; and/or the winding device is used for winding the graphene film; and/or, a separation device for separating the suction filtration substrate from the graphene film.
In some embodiments, after the filtration substrate is separated from the graphene film, the filtration substrate can pass through the filtration port and the container port again through the transmission device for recycling; and/or the transmission device comprises an adjusting transmission wheel for adjusting the tension of the suction filtration substrate.
In some embodiments, the system of the present invention further comprises an electroreduction apparatus comprising: the graphene film is electrically connected with the alternating current power supply, and the alternating current power supply is electrically connected with the first electrode and the second electrode; preferably, the voltage of the ac power source is between 0V and 220V.
In some embodiments, the system of the present invention further includes an electrochemical stripping apparatus for electrochemically stripping a solution for producing graphene, including: an electrolytic cell in which an electrolyte is contained; the electrodes comprise a working electrode and a counter electrode which are made of graphite materials; the alternating current power supply is electrically connected with the electrode and used for providing an alternating current electric field; preferably, the voltage of the ac power source is between 3V and 15V.
In some embodiments, a stirring wheel is further arranged in the graphene container, and the liquid level of the graphene solution forms a liquid flow in the same direction as the moving direction of the suction filtration substrate through the rotation of the stirring wheel; and/or the graphene container also comprises: the liquid inlet is used for adding or supplementing a graphene solution into the graphene container; and the liquid level control port is arranged at the upper end of the graphene container and is used for keeping the liquid level of the graphene solution stable.
In some embodiments, the pore size of the filtration pores is between 50 μm and 100 μm, 10 to 20 pores/cm2。
In some embodiments, the material of the suction filtration substrate is selected from polyvinylidene fluoride or polytetrafluoroethylene; and/or the aperture of the suction filtration substrate is 0.2-1 μm, or the mesh number is 800 meshes to 10000 meshes; and/or the width of the suction filtration substrate is between 0.1m and 1 m; and/or the thickness of the suction filtration substrate is between 0.05mm and 1 mm.
The invention also provides a method for continuously preparing the graphene film by adopting the system, which comprises the following steps: injecting a graphene solution into a graphene container; preferably, the mass concentration of the graphene solution is between 0.1% and 5%; a transmission step, namely enabling the suction filtration substrate to continuously move at a preset speed; preferably, the predetermined speed is between 0.005m/s and 0.1 m/s; a suction filtration step, wherein graphene is loaded on the surface of a suction filtration substrate through suction filtration to form a graphene film; a heating step of heating and drying the graphene film at a predetermined temperature; preferably, the predetermined temperature is between 100 ℃ and 150 ℃.
In some embodiments, the graphene in the graphene solution is prepared by an electrochemical stripping method; and/or, further comprising an electroreduction step: applying an alternating current electric field to the dried graphene film; preferably, the voltage of the alternating electric field is between 0 and 220V; and/or enabling the liquid level of the graphene solution to form a liquid flow consistent with the moving direction of the suction filtration substrate; and/or, the graphene film after drying has a thickness of between 20 μm and 500 μm.
Compared with the prior art, the beneficial technical effects of the invention are as follows:
1) according to the system, the graphene sheet layers are in a flat state under the action of the surface tension of liquid at a gas-liquid interface, a suction filtration port of a suction filtration device is opened downwards, suction filtration is performed in a suck-back mode, the suction filtration port can be in contact with or close to the liquid surface of a graphene solution, and graphene in the graphene solution at the gas-liquid interface is loaded on a suction filtration substrate in a sheet-flat state, so that the graphene film with uniform graphene sheet layer orientation is obtained.
2) According to the system disclosed by the invention, the graphene container is upwards opened and is arranged below the suction filtration device, and graphite flakes with low stripping degree tend to deposit at the bottom of the solution under the action of gravity, so that the graphite flakes with low stripping degree are prevented from being loaded on the suction filtration substrate in the suction filtration process, and a graphene film with higher quality can be obtained.
3) The system disclosed by the invention adopts the transmission device, and the transmission wheel in the transmission device is utilized to drive the suction filtration substrate to continuously move, so that the batch continuous preparation of the graphene film by the suction filtration method and the preparation of the large-area graphene film are realized.
4) According to the system and the method, when the graphene prepared by adopting the electrochemical stripping method is used as the raw material, the graphene film with good conductivity can be obtained, particularly, after an external electric field is applied, the conductivity of the graphene film can be further improved, the conductive graphene film can be produced continuously in batches, and the production process of the conductive graphene film is greatly simplified.
Drawings
Fig. 1 is a schematic view of a system for continuously preparing a graphene thin film in example 1 of the present invention;
fig. 2 is a schematic structural diagram of a graphene solution container in example 1 of the present invention;
FIG. 3 is a schematic view showing the construction of an electrochemical peeling apparatus in example 1 of the present invention;
FIG. 4 is a scanning electron microscope photograph of the graphene film obtained in example 4 of the present invention;
fig. 5 is a scanning electron microscope test photograph of the graphene film obtained in example 6 of the present invention.
Description of the main reference numerals:
100 of graphene solution; 110 graphene; 200 graphene films;
1 a graphene container; 11 a container mouth; 12 stirring wheels; 13 liquid inlet; 14 a liquid level control port;
2, a suction filtration device; 21, a filtration port is pumped; 211 suction filtration pores;
3, filtering the substrate;
4, a transmission device; 41 fixing a driving wheel; 42 adjusting the transmission wheel;
5 heating means;
6, rolling a device;
7, a winding device;
8, a separation device;
9 an electric reduction device; 91 a first electrode; 92 a second electrode; 93 an alternating current power supply;
10 an electrochemical peeling device;
20 an electrolytic cell; 201 an electrolyte; 202 graphene;
30 electrodes; 301 a working electrode; 302 pairs of electrodes;
40 ac power.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Example 1
The present embodiment provides a system for continuously preparing a graphene thin film, as shown in fig. 1 and 2, including: the device comprises a graphene container 1, a suction filtration device 2, a suction filtration substrate 3, a transmission device 4 and a heating device 5; the graphene container 1 is used for containing a graphene solution 100 and comprises a container opening 11 which is opened upwards; the suction filtration device 2 is arranged above the graphene container 1, and comprises a suction filtration port 21 with a downward opening, the suction filtration port 21 and the container port 11 are arranged in an up-down opposite mode, the suction filtration port 21 is provided with a plurality of suction filtration holes 211, and the suction filtration port 21 can be in contact with or close to the liquid level of the graphene solution 100; the suction filtration substrate 3 is a thin film containing pores; the transmission device 4 comprises a plurality of transmission wheels 41 and 42 and is used for enabling the suction filtration substrate 3 to pass through the space between the container opening 11 and the suction filtration opening 21 and move continuously, and in the moving process, the graphene 110 in the graphene solution 100 is loaded on the surface of the suction filtration substrate 3 under the action of the suction filtration device to form a graphene film 200; and the heating device 5 is used for drying the graphene film 200 coated on the suction filtration substrate 3.
Because the graphene sheet layers are in a flat state under the action of the surface tension of the liquid at the gas-liquid interface, the suction filtration port 21 of the suction filtration device 2 is downward opened, suction filtration is performed in a suck-back mode, so that the suction filtration port 21 can be in contact with or close to the liquid level of the graphene solution 100, the graphene 110 on the gas-liquid interface in the graphene solution 100 can be loaded on the suction filtration substrate 3 in a sheet-flat state, and the graphene film with uniform graphene sheet layer orientation is obtained. In addition, the graphene container 1 is arranged below the suction filtration device 2, and graphite flakes with lower stripping degree tend to deposit at the bottom of the solution under the action of gravity, so that the graphite flakes with lower stripping degree are prevented from being loaded on the suction filtration substrate 3 in the suction filtration process, and a graphene film with higher quality can be obtained.
In this embodiment, a separation device 8 is further disposed behind the heating device 5, and is configured to separate the suction filtration substrate 3 from the graphene film 200 to obtain a graphene film without the suction filtration substrate, and a rolling device 6 is disposed behind the separation device 8 and is configured to further roll the graphene film to adjust the thickness of the prepared graphene film; and (4) receiving the rolled graphene film by a winding device 7 to obtain a wound graphene film product.
In this embodiment, after the separation device 8 separates the filtration substrate 3 from the graphene film 200, the filtration substrate 3 passes through the space between the filtration port 21 and the container port 11 again through the driving wheel in the transmission device 4, so that continuous production of the graphene film and recycling of the filtration substrate are simultaneously realized.
In this embodiment, the transmission device 4 includes a fixed transmission wheel 41 and an adjusting transmission wheel 42, and the suction filtration substrate 3 is driven by the transmission wheels to continuously move, wherein the adjusting transmission wheel 42 can adjust the position to further adjust the tension of the suction filtration substrate 3 in the transmission device 4, so that the suction filtration substrate 3 has a flat surface, and a flat graphene film 200 is produced.
In the present embodiment, after the drying device 5, an electrical reduction device 9 is further provided for performing a reduction process on the dried graphene film 200, where the electrical reduction device 9 includes a first electrode 91, a second electrode 92, and an ac power supply 93, in the present embodiment, both the first electrode 91 and the second electrode 92 are cylindrical electrodes, and when the graphene film 200 passes between the first electrode 91 and the second electrode 92, the ac power supply 93 applies an ac electric field to the graphene film 200 through the first electrode 91 and the second electrode 92 to perform the reduction process; preferably, the voltage regulation range of the alternating current electric field is 0-220V, the reduction treatment time is 1-50 min, graphene films with different reduction degrees can be obtained by regulating the voltage, the reduction degree of the graphene film obtained at low voltage is lower, and the reduction degree of the graphene film obtained at high voltage is higher.
The electrical reduction device 9 is mainly applied to a graphene film capable of conducting electricity, and for a graphene oxide film, the graphene oxide film needs to be reduced into conductive graphene through HI and then subjected to electrical reduction. Therefore, in a preferred embodiment of the present invention, the graphene prepared by the electrochemical exfoliation method has good electrical conductivity, and after further processing by an electroreduction device, the electrical conductivity can be improved, so as to obtain a graphene film product with excellent electrical conductivity.
In this embodiment, the roller of the rolling device 6 is disposed between the first electrode 91 and the second electrode 92, so that the graphene film is rolled and reduced, thereby saving the arrangement space of the system.
In this embodiment, a stirring wheel 12 is further disposed in the graphene container 1, as shown in fig. 2, a liquid flow in a direction consistent with the moving direction of the pumping filtration substrate 3 is formed on the liquid surface of the graphene solution 100 by rotation of the stirring wheel 12, and the graphene 110 is arranged in parallel along the slit direction under the shearing action of the microscopic liquid flow, so that the graphene sheet layers are arranged more regularly when contacting the pumping filtration substrate, and the graphene film has good uniformity and high orientation in film formation.
In this embodiment, the graphene container 1 further includes: a liquid inlet 13, configured to add or supplement the graphene solution 100 into the graphene container 1; and the liquid level control port 14 is arranged at the upper end of the graphene container 1 and is used for keeping the liquid level of the graphene solution 100 stable.
In some embodiments, the system of the present invention further includes an electrochemical stripping apparatus 10 for electrochemically stripping to produce graphene 202, and obtain a graphene solution, as shown in fig. 3, including: an electrolytic cell 20 in which an electrolytic solution 201 is contained; the electrode 30 comprises a working electrode 301 and a counter electrode 302 which are made of graphite materials; and an alternating current power supply 40 electrically connected to the electrode 30 for providing an alternating current electric field. The graphene solution prepared by the electrochemical stripping apparatus 10 is purified (e.g., dialyzed, centrifugally washed, etc.) to be configured into a graphene solution, and the graphene solution enters the graphene container 1 through the liquid inlet 13.
The plurality of suction filtration holes 211 are arranged in the suction filtration port 21, the acting force of suction filtration can be dispersed through the plurality of suction filtration holes 211 and uniformly acts on the suction filtration substrate 3, so that the graphene 110 can form a uniform and flat graphene film 200 on the suction filtration substrate, and in a preferred embodiment, the aperture of the suction filtration holes 211 is 50-100 um, and the density is 10-20/cm2。
In some embodiments, the material of the suction filtration substrate of the present invention can be selected from polytetrafluoroethylene or polyvinylidene fluoride and mixed fibers; in a preferred embodiment, the material of the suction filtration substrate 3 is a polyvinylidene fluoride membrane; the aperture of the suction filtration substrate 3 is 0.2-1 um, and the mesh number is 800-10000 meshes; the width of the suction filtration substrate 3 is between 0.1 and 1 m; the thickness of the suction filtration substrate 3 is 0.05-1 mm.
Example 2
In this embodiment, the system described in embodiment 1 is used to provide a method for continuously preparing a graphene film, which includes the steps of:
1) injecting a graphene solution 100 into a graphene container 1;
2) a transmission step, starting the transmission device 4 to enable the suction filtration substrate 3 to continuously move at a preset speed;
3) a suction filtration step, wherein the suction filtration device 2 is started to enable the graphene 110 to be loaded on the surface of the suction filtration substrate 3 to form a graphene film 200;
4) a heating step, in which the heating device 5 is started to heat and dry the graphene film 200 at a predetermined temperature, and the graphene film is obtained through the separation device 8;
5) and a rolling step, starting the rolling device 6, rolling the graphene film, and adjusting the thickness to obtain a graphene film product.
In a preferred embodiment, the graphene solution 100 has a mass concentration of 0.1% to 5%, and is capable of forming a suitable viscosity;
in the process of suction filtration, the graphene sheet layer starts to be rapidly accumulated on the suction filtration substrate, the speed of rotation of the driving wheel is adjusted to control the moving speed of the suction filtration substrate, the thickness of the final product graphene film is further controlled, the speed of the driving wheel is reduced, the obtained graphene film is thicker, the speed of the driving wheel is increased, the obtained graphene film is thinner, and in a preferred embodiment, the preset moving speed of the suction filtration substrate 3 is between 0.005m/s and 0.05 m/s;
in a preferred embodiment, the method further comprises the step of starting the stirring wheel 12 to enable the liquid level of the graphene solution to form a liquid flow consistent with the moving direction of the suction filtration substrate, and preferably, the rotating speed of the stirring wheel 12 is set to be 20-1000 rpm.
In a preferred embodiment, the predetermined temperature of the heating device is between 100 ℃ and 150 ℃;
in a preferred embodiment, the rolling step adjusts the graphene film to have a thickness of 0.05 to 0.1 mm.
In a specific embodiment, the mass concentration of the graphene solution is 1%, the suction filtration substrate 3 is made of polyvinylidene fluoride material, the thickness is 20um, the width is 0.1m, the aperture is 0.44um, the adjustment tension is 20N/m, the preset moving speed of the suction filtration substrate 3 is 0.01m/s, the drying temperature is set to 105 ℃, and the thickness of the obtained graphene film product is 0.1 mm.
Example 3
The steps of the embodiment are similar to those of the embodiment 2, and the difference is that the method further comprises the following steps:
an electrode reduction treatment step, wherein an electric reduction device 9 is started to realize reduction treatment while rolling the graphene film; in the electrode reduction treatment step, the voltage regulation range of the alternating current applied by the electric reduction device 9 is between 0 and 220V; more preferably, the voltage regulation range is between 10V and 50V.
Example 4
The embodiment provides a method for continuously preparing a graphene film, wherein the method for preparing graphene by an electrochemical stripping method (by using an electrochemical stripping device 10) comprises the following steps:
1) preparation of reactants: pressing graphite powder into graphite flakes through tabletting equipment, wherein the thickness of the pressed flakes is 3 mm; electrolyte A is 0.5mol/L tetrabutylammonium hydrogen sulfate (TBAHSO)4) Adding 3mL of 30% ammonia water in each 100mL of electrolyte A according to the volume ratio of 3% in the electrolyte A to obtain an electrolyte B;
2) pre-oxidation step: in the step (1), the graphite flake is taken as an electrode, is placed in an electrolyte A, and is stably kept for 2 hours under the direct current voltage of 3V;
3) the reaction steps are as follows: and (3) placing the electrode in the electrolyte B, electrifying for 1h under 10V alternating current, obtaining a precipitate at the bottom of the solution C, and washing and centrifugally recycling the obtained precipitate to obtain the graphene.
Preparing the obtained graphene into a graphene solution with a mass concentration of 1.5%, otherwise performing the same conditions as in the specific example of example 2 to obtain a graphene film product, and Scanning Electron Microscope (SEM) testing the graphene film product as shown in fig. 4It can be seen that the thickness of the graphene film product is 0.02mm, the surface of the graphene film is relatively flat, the orientation arrangement is relatively uniform, and the conductivity of the graphene film product is 2.5 x 10 measured by adopting a four-probe method5S/m。
Example 5
The method for preparing the graphene film product in this example is similar to that in example 4, except that the electrical reduction device 9 is turned on, the obtained graphene film is subjected to reduction treatment while being rolled, other conditions are consistent with those in example 4, the alternating voltage is set to be 220V, the frequency is 50Hz, the treatment time is 10 minutes, and the conductivity is measured by the same method to be 106S/m。
Therefore, the graphene film prepared by taking the graphene obtained by the electrochemical stripping method as the raw material has excellent electrical conductivity, on one hand, the graphene obtained by the method keeps excellent electrical conductivity, and on the other hand, the graphene layers of the graphene film obtained by the system suction filtration are uniform in orientation and are mutually and closely overlapped, so that the graphene film is beneficial to conduction of electrons and has good electrical conductivity. By comparing the conductivity tests of the graphene films in examples 4 and 5, it can be seen that the conductivity of the graphene film can be further improved after an external electric field is applied, and a high-quality conductive graphene film can be obtained. In addition, the graphene prepared by the electrochemical stripping method has the advantages of low cost and environmental friendliness, and the alternating current drives ions or charged molecules to migrate into the graphite layer interval and push away the graphene layer.
Example 6
In this embodiment, a method similar to that in example 4 is adopted, except that the stirring wheel 12 is turned on during the continuous production process, and other conditions are the same as those in example 4, wherein the linear velocity of the stirring wheel 12 is the same as the predetermined velocity of the movement of the filtration substrate 3, and a Scanning Electron Microscope (SEM) test photograph (SEM) of the obtained graphene film product is shown in fig. 5, it can be seen that the thickness of the graphene film product is 0.04mm, the surface of the graphene film is very flat, the orientation arrangement is uniform, and thus, the graphene solution 100 generates a liquid flow in the same direction as the movement direction of the filtration substrate 3 by the rotation of the stirring wheel 12, and the graphene film product with a flat surface and high orientation can be obtained.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A system for continuously preparing a graphene film, comprising:
the graphene container (1) is used for containing a graphene solution (100) and comprises a container opening (11);
the suction filtration device (2) is arranged above the graphene container (1), and comprises a suction filtration port (21) which is arranged opposite to the container port (11) up and down, the suction filtration port (21) is provided with a plurality of suction filtration holes (211), and the suction filtration port (21) can contact or approach the liquid level of the graphene solution (100);
the suction filtration substrate (3) is a thin film containing pores;
the transmission device (4) comprises a plurality of transmission wheels (41,42) and is used for enabling the suction filtration substrate (3) to pass through the space between the container opening (11) and the suction filtration opening (21) and move continuously, and in the moving process, the graphene (110) in the graphene solution (100) is loaded on the surface of the suction filtration substrate (3) under the action of the suction filtration device to form a graphene film (200);
and the heating device (5) is used for drying the graphene film (200) coated on the suction filtration substrate (3).
2. The system according to claim 1, characterized in that it further comprises, after said heating means (5):
a rolling device (6) for rolling the graphene film (200) to adjust the thickness; and/or the presence of a gas in the gas,
a winding device (7) for winding the graphene film (200); and/or the presence of a gas in the gas,
a separation device (8) for separating the suction filtration substrate (4) from the graphene membrane (200).
3. The system of claim 2, wherein the suction filtration substrate (4) is separated from the graphene membrane (200) and can pass through the suction filtration port (21) and the container port (11) again through the transmission device (3) for recycling; and/or the presence of a gas in the gas,
the transmission device (4) comprises an adjusting transmission wheel (42) which is used for adjusting the tension of the suction filtration substrate (3).
4. A system according to claim 1, further comprising an electro-reduction device (9) comprising:
an alternating current power supply (93) and a first electrode (91) and a second electrode (92) which are electrically connected with the alternating current power supply, wherein an alternating current electric field is applied to the graphene film (200) through the first electrode (91) and the second electrode (92) for reduction treatment; preferably, the voltage of the alternating current power supply (93) is between 0V and 220V.
5. The system of claim 1, further comprising an electrochemical stripping apparatus (10) for electrochemically stripping a solution for producing graphene, comprising:
an electrolytic cell (20) in which an electrolytic solution (201) is contained;
the electrode (30) comprises a working electrode (301) and a counter electrode (302), and both are made of graphite materials;
an alternating current power supply (40) electrically connected with the electrode (30) and used for providing an alternating current electric field; preferably, the voltage of the alternating current power supply (40) is between 3V and 15V.
6. The system according to claim 1, wherein a stirring wheel (12) is further arranged in the graphene container (1), and the liquid level of the graphene solution (100) forms a liquid flow consistent with the moving direction of the suction filtration substrate (4) through the rotation of the stirring wheel (12); and/or the presence of a gas in the gas,
the graphene container (1) further comprises:
a liquid inlet (13) for adding or supplementing a graphene solution (100) into the graphene container (1);
and the liquid level control port (14) is arranged at the upper end of the graphene container (1) and is used for keeping the liquid level height of the graphene solution (100) stable.
7. The system of claim 1, wherein the pore size of the filtration pores (211) is between 50 μm and 100 μm, 10 to 20/cm2。
8. The system according to claim 1, characterized in that the material of the suction filtration substrate (3) is selected from polyvinylidene fluoride or polytetrafluoroethylene;
and/or the aperture of the suction filtration substrate (3) is 0.2-1 μm, or the mesh number is 800 meshes to 10000 meshes;
and/or the width of the suction filtration substrate (3) is between 0.1m and 1 m;
and/or the thickness of the suction filtration substrate (3) is between 0.05mm and 1 mm.
9. A method for continuously preparing a graphene thin film using the system of any one of claims 1 to 8, comprising the steps of:
injecting a graphene solution into a graphene container; preferably, the graphene solution has a mass concentration of 0.1% to 5%;
a transmission step, namely enabling the suction filtration substrate to continuously move at a preset speed; preferably, said predetermined speed is comprised between 0.005m/s and 0.1 m/s;
a suction filtration step, wherein graphene is loaded on the surface of the suction filtration substrate through suction filtration to form a graphene film;
a heating step of heating and drying the graphene film at a predetermined temperature; preferably, the predetermined temperature is between 100 ℃ and 150 ℃.
10. The method according to claim 9, wherein the graphene in the graphene solution is prepared by an electrochemical exfoliation method; and/or the presence of a gas in the gas,
further comprises an electroreduction step: applying an alternating current electric field to the dried graphene film; preferably, the voltage of the alternating electric field is between 0 and 220V; and/or the presence of a gas in the gas,
enabling the liquid level of the graphene solution to form a liquid flow consistent with the moving direction of the suction filtration substrate; and/or the presence of a gas in the gas,
the graphene film after drying has a thickness of 20 μm to 500 μm.
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| CN114774087A (en) * | 2022-04-11 | 2022-07-22 | 广州大学 | Method for preparing graphene heat-conducting film |
| CN115744884A (en) * | 2022-11-07 | 2023-03-07 | 厦门大学 | Continuous preparation method and system of graphene film with directional heat conduction function |
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