CN114349511A - Method for rapidly preparing high-conductivity graphene electromagnetic shielding film - Google Patents
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Abstract
The invention discloses a method for rapidly preparing a high-conductivity graphene electromagnetic shielding film, which comprises the steps of preparing a graphite oxide filter cake into a graphite oxide suspension, uniformly dispersing, and then stirring under vacuum to remove bubbles to obtain graphene oxide dispersion slurry; uniformly coating the obtained graphene oxide dispersion slurry on a substrate to form a graphene oxide blank film, drying to remove moisture, and then peeling off the substrate to obtain a graphene oxide film; irradiating the obtained graphene oxide film by adopting infrared rays in an air environment, then heating to 1500 ℃ under the protection of inert atmosphere, preserving heat for 0.5-2 h, and naturally cooling to obtain graphene foam; and finally, rolling the graphene foam to form a film. The method provided by the invention does not generate any toxic and harmful substances, is simple in preparation process, adopts an infrared lamp for green and efficient treatment, is low in heat treatment temperature and fast in temperature rise, and can realize efficient and high-quality preparation of the graphene film.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding films, and particularly relates to a method for quickly preparing a high-conductivity graphene electromagnetic shielding film.
Background
With the rapid development and wide application of wireless communication technology in recent years, excessive electromagnetic radiation appears around people, including public places, home environments, various buildings and the like, and has adverse effects on electronic equipment and human health. Because of poor flexibility and high density, the traditional metal-based electromagnetic shielding material cannot meet the application in the aspects of miniature and flexible electronic devices, and an ultrathin, flexible and lightweight thin-film material is urgently needed to replace the traditional metal material.
Graphene, as a two-dimensional nanocarbon material, has excellent thermal properties, electrical properties, mechanical properties and flexibility, and is widely applied to the field of thin film materials in recent years. The conduction mechanism of graphene is carrier transport. Carbon atom passage through sp of single-layer graphene2The formed delocalized pi bonds provide fast migration channels for carriers in a hybrid connection mode, and the theoretical carrier transmission rate is up to 15000cm2And/or (V s), more than twice as high as indium antimonide, which is known to have the highest carrier mobility. The high conductivity of graphene makes it have great potential for application in the field of electromagnetic shielding. Stacking graphene layers can constitute a graphene film.
At present, the preparation of graphene films by taking graphite oxide as a precursor is a main method for preparing graphene films on a large scale at present. The mainstream preparation process at present comprises the following steps: 1. journal of advanced functional materials in 2014The graphene oxide membrane is prepared by a solvent evaporation self-assembly method, and after high-temperature treatment at 2000 ℃, the electromagnetic shielding performance of the graphene membrane with the thickness of 0.0084mm reaches 20dB (adv.funct.mater.2014,24,4542.); 2. reduction of graphene oxide films by chemical reduction in 2015 in a journal of carbon materials, resulting in a conductivity of 243S cm-1The graphene film of (2) shows an electromagnetic shielding effectiveness of 20dB at 1 GHz. The preparation process has the following problems: 1. most of the reagents added by the chemical reduction method are harmful to the environment, and the waste liquid treatment cost is high; 2. during the heat treatment, a large amount of bubbles and gaps are caused by the decomposition of oxygen-containing functional groups in the graphite oxide, and the performance of the material is greatly reduced due to the defects; 3. the high-temperature graphitization process is needed, the temperature is as high as 2800-3000 ℃, the energy consumption is large, the preparation process is long, and the heat treatment efficiency is low.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a method for quickly preparing a graphene electromagnetic shielding film with high conductivity, flexibility and strength aiming at the defects of the prior art, and solves the defects of serious bubbling phenomenon, high-temperature graphitization energy consumption, long preparation process, low treatment efficiency and the like in the preparation process of the conventional graphene film.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for rapidly preparing a high-conductivity graphene electromagnetic shielding film comprises the following steps:
(1) preparing a graphite oxide filter cake into a graphite oxide suspension, uniformly dispersing, and then stirring under vacuum to remove bubbles to obtain graphene oxide dispersion slurry;
(2) uniformly coating the graphene oxide dispersion slurry obtained in the step (1) on a substrate to form a graphene oxide blank film, drying to remove moisture, and then peeling off the substrate to obtain a graphene oxide film;
(3) irradiating the graphene oxide film obtained in the step (2) by adopting infrared rays in an air environment, heating to 1500 ℃ under the protection of inert atmosphere, preserving heat for 0.5-2 h, and naturally cooling to obtain graphene foam;
(4) and (4) rolling the graphene foam in the step (3) to form a film, thus obtaining the graphene foam.
In the step (1), the average size of the graphite oxide filter cake is larger than 100 microns, a graphite oxide suspension with the concentration of 5-40 mg/mL is prepared, and ammonia water is added to adjust the pH value to 7-8.
Dispersing for 0.5-2 h in a high-speed shearing dispersion machine at a linear speed of 10-20 m/s in the step (1) to strip large-size graphite oxide into graphene oxide; and slowly stirring by using a vacuum stirrer under the vacuum assistance of-0.1 MPa at a linear speed of 1-5 m/s until bubbles are completely removed.
In the step (2), the substrate is polyethylene glycol terephthalate, and the thickness of the graphene oxide embryonic membrane on the substrate is 1-5 mm.
In the step (2), drying for 6-8 hours at 30-70 ℃ to remove water, and stripping the substrate to obtain the graphene oxide film with the film thickness of 10-200 microns.
In the step (3), an infrared lamp with the surface temperature of 300-400 ℃ is adopted to irradiate the graphene oxide film for 5-20 seconds. Heating by adopting an infrared thermal radiation heating method, wherein the functional groups and moisture in the graphene oxide film absorb radiation energy to raise the temperature; the reduction process of the graphene oxide film is initiated by absorbing energy and raising the temperature, and the graphite oxide is easy to decompose by heating due to a large amount of epoxy groups, hydroxyl groups, carboxyl groups and carbonyl groups, so that gases such as carbon dioxide, water molecules and the like are generated. In the process, the graphene oxide film is heated under the air condition, gas is generated at a very high speed and escapes from the layers of the graphene oxide film, so that a uniform mesoporous structure is formed, and the structure reduces the friction force between the layers by reducing the contact points between the layers, so that the pressure required by calendering is greatly reduced; in addition, in the subsequent deep reduction process, the generated gas can easily escape from the mesoporous structure, and the phenomenon of secondary bubbling can not be caused.
In the step (3), the temperature is increased to 1500 ℃ at the speed of 10-20 ℃/min.
In the step (4), a calender is adopted to calender the graphene foam into a film, and the pressure is 2-50 MPa. The surface flatness of the graphene film is improved through calendering; at the same time, due to the aboveThe existence of the compressive mesoporous structure in the step (3) can obtain a compact graphene film with the density as high as 1.6g/cm3。
Further, the high-conductivity graphene electromagnetic shielding film prepared by the preparation method is also in the protection scope of the invention.
Furthermore, the thickness range of the prepared high-conductivity graphene electromagnetic shielding film is 10-35 mu m, and the density is 1.3-1.6 g/cm3The conductivity reaches more than 1000S/cm, the tensile strength reaches more than 100MPa, and the electromagnetic shielding efficiency reaches more than 48dB in a wide frequency band.
The preparation method has the mechanism that infrared radiant heat initiates the rapid decomposition of epoxy groups, hydroxyl groups, carboxyl groups and carbonyl groups on the surface of graphene oxide, and gas is generated at a very high speed and escapes from the interlayer of the graphene oxide film, so that a uniform porous easy-pressing structure is formed, and the pressure required by subsequent calendering is greatly reduced; in addition, in the subsequent deep reduction process, the graphene oxide film is further reduced, most of oxygen-containing functional groups are removed, and the graphene film recovers large-area sp2And the intrinsic conductivity is improved. The method provided by the invention does not generate any toxic and harmful substances, is simple in preparation process, adopts an infrared lamp for green and efficient treatment, is low in heat treatment temperature and fast in temperature rise, and can realize efficient and high-quality preparation of the graphene film.
Has the advantages that:
(1) the method adopts an infrared lamp processing mode which is green and environment-friendly, the thermal reduction in the first step adopts an infrared thermal radiation mode, the process is rapid and efficient, a unique compressive mesoporous structure is obtained, and in the subsequent deep reduction process, the generated gas can easily escape from the mesoporous structure without causing a secondary bubbling phenomenon, so that the heating rate of subsequent heat treatment is greatly improved, the energy consumption and the processing time are reduced, and the preparation process is more economic, efficient and environment-friendly.
(2) The graphene film prepared by the invention has excellent conductivity and high strength. The mesoporous structure obtained by infrared treatment enables the defects of graphene to be better repaired through subsequent heat treatment, the large size of graphene is reserved, and the intrinsic conductivity and strength of the graphene film are greatly improved.
(3) The graphene film has high added value, and the obtained intermediate porous structure can be compounded with other metals with catalytic characteristics, so that the application field of the graphene film is widened, and a foundation is laid for a subsequent functionalized graphene film.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Fig. 1 is a sectional electron microscope image of the porous structure of the graphene film (before calendering) obtained in example 1.
Fig. 2 shows the electromagnetic shielding effectiveness of the graphene electromagnetic shielding film obtained in example 1 in the X-band.
Fig. 3 is a stress-strain curve of the graphene electromagnetic shielding film obtained in example 1.
FIG. 4 is a sectional electron micrograph of the porous structure obtained in comparative example 1.
Fig. 5 is a plot of isothermal nitrogen gas wash desorption for example 1 and comparative example 1.
Fig. 6 is a graph of pore size distribution for example 1 and comparative example 1.
Detailed Description
The invention will be better understood from the following examples.
Example 1
1) The graphite oxide filter cake with the average size of 1000 μm is prepared into a graphite oxide aqueous solution with the concentration of 20 mg/mL. Adding ammonia water into the prepared solution to adjust the pH value to 8, dividing the solution in a high-speed shearing dispersion machine for 2 hours at a linear speed of 20m/s, and then slowly stirring the solution for 30 minutes at a linear speed of 1m/s by using a vacuum stirrer under the vacuum assistance of-0.1 MPa to completely remove bubbles to obtain graphene oxide dispersion slurry;
2) uniformly coating the graphene oxide slurry on a PET substrate by adopting a scraper coating method to form a 2mm stock film of a graphene oxide film, drying at 40 ℃ for 8h to remove moisture, and stripping the substrate to obtain the graphene oxide film with the film thickness of 20 microns;
3) irradiating the graphene oxide film in the step 2) for 20 seconds by using an infrared lamp with the surface temperature of 400 ℃ in an air environment, then heating to 1500 ℃ at the speed of 10 ℃/min under the protection of argon atmosphere, preserving heat for 2 hours, and naturally cooling to obtain graphene foam;
4) and (3) calendering the graphene foam in the step 3) into a film by using a calender, wherein the pressure is 40MPa, and then carrying out post-treatment such as edge cutting and the like to obtain the high-conductivity graphene electromagnetic shielding film.
Fig. 1 is a cross-sectional electron microscope image of a porous structure of a graphite film, and it can be seen that many mesoporous structures (with a pore diameter of 2-50 μm) exist in a cross section of a graphene oxide film after thermal stripping, the mesoporous structures can provide channels for gas escape in a subsequent deep reduction process, so that the temperature rise rate in the subsequent deep reduction process is increased, and the mesoporous structures are easy to be rolled and can be rolled into a compact film structure under the pressure of 40 MPa. In addition, the compact thin film structure is not only beneficial to improving the conductivity and mechanical property, but also exhibits excellent flexibility and foldability.
Fig. 2 shows the electromagnetic shielding effectiveness of the graphene electromagnetic shielding film in the X band, and it can be seen that the graphene electromagnetic shielding film exhibits excellent electromagnetic shielding effectiveness (50 dB) in the X full-band thin film, which is much greater than the requirement (20dB) of the commercial shielding thin film.
Fig. 3 is a stress-strain curve of the graphene electromagnetic shielding film, and it can be seen that the mechanical strength of the graphene film is up to 160MPa, and the graphene electromagnetic shielding film has good mechanical properties.
Example 2
1) The graphite oxide filter cake with the average size of 500 mu m is prepared into a graphite oxide water solution with the concentration of 30 mg/mL. Adding ammonia water into the prepared solution to adjust the pH value to 8, dividing the solution in a high-speed shearing dispersion machine for 2 hours at a linear speed of 20m/s, and then slowly stirring the solution for 30 minutes at a linear speed of 1m/s by using a vacuum stirrer under the vacuum assistance of-0.1 MPa to completely remove bubbles to obtain graphene oxide dispersion slurry;
2) uniformly coating the graphene oxide slurry on a PET substrate by adopting a scraper coating method to form a blank film of a graphene oxide film with the thickness of 3mm, drying at 40 ℃ for 8h to remove moisture, and stripping the substrate to obtain the graphene oxide film with the film thickness of 45 mu m;
3) irradiating the graphene oxide film in the step 2) for 20 seconds by using an infrared lamp with the surface temperature of 400 ℃ in an air environment, then heating to 1500 ℃ at the speed of 10 ℃/min under the protection of argon atmosphere, preserving heat for 2 hours, and naturally cooling to obtain graphene foam;
4) and (3) calendering the graphene foam in the step 3) into a film by using a calender, wherein the pressure is 40MPa, and then carrying out post-treatment such as edge cutting and the like to obtain the high-conductivity graphene electromagnetic shielding film.
Example 3
1) The graphite oxide filter cake with the average size of 500 mu m is prepared into a graphite oxide water solution with the concentration of 40 mg/mL. Adding ammonia water into the prepared solution to adjust the pH value to 8, dividing the solution in a high-speed shearing dispersion machine for 2 hours at a linear speed of 10m/s, and then slowly stirring the solution for 30 minutes at a linear speed of 1m/s by using a vacuum stirrer under the vacuum assistance of-0.1 MPa to completely remove bubbles to obtain graphene oxide dispersion slurry;
2) uniformly coating the graphene oxide slurry on a PET substrate by adopting a scraper coating method to form a 1mm stock film of a graphene oxide film, drying at 40 ℃ for 8h to remove moisture, and stripping the substrate to obtain the graphene oxide film with the film thickness of 20 microns;
3) irradiating the graphene oxide film in the step 2) for 20 seconds by using an infrared lamp with the surface temperature of 400 ℃ in an air environment, then heating to 1500 ℃ at the speed of 20 ℃/min under the protection of argon atmosphere, preserving heat for 2 hours, and naturally cooling to obtain graphene foam;
4) and (3) calendering the graphene foam in the step 3) into a film by using a calender, wherein the pressure is 40MPa, and then carrying out post-treatment such as edge cutting and the like to obtain the high-conductivity graphene electromagnetic shielding film.
Example 4
1) The graphite oxide filter cake with the average size of 500 mu m is prepared into a graphite oxide water solution with the concentration of 40 mg/mL. Adding ammonia water into the prepared solution to adjust the pH value to 8, dividing the solution in a high-speed shearing dispersion machine for 2 hours at a linear speed of 20m/s, and then slowly stirring the solution for 30 minutes at a linear speed of 1m/s by using a vacuum stirrer under the vacuum assistance of-0.1 MPa to completely remove bubbles to obtain graphene oxide dispersion slurry;
2) uniformly coating the graphene oxide slurry on a PET substrate by adopting a scraper coating method to form a blank film of a graphene oxide film with the thickness of 3mm, drying at 40 ℃ for 8h to remove moisture, and stripping the substrate to obtain the graphene oxide film with the film thickness of 60 mu m;
3) irradiating the graphene oxide film in the step 2) for 20 seconds by using an infrared lamp with the surface temperature of 400 ℃ in an air environment, then heating to 1500 ℃ at the speed of 20 ℃/min under the protection of argon atmosphere, preserving heat for 2 hours, and naturally cooling to obtain graphene foam;
4) and (3) calendering the graphene foam in the step 3) into a film by using a calender, wherein the pressure is 40MPa, and then carrying out post-treatment such as edge cutting and the like to obtain the high-conductivity graphene electromagnetic shielding film.
Comparative example 1
1) The graphite oxide filter cake with the average size of 1000 μm is prepared into a graphite oxide aqueous solution with the concentration of 20 mg/mL. Slowly stirring for 30min at a linear speed of 1m/s by using a vacuum stirrer under the vacuum assistance of-0.1 MPa to obtain graphene oxide dispersion slurry;
2) uniformly coating the graphene oxide slurry on a PET substrate by adopting a scraper coating method to form a 2mm stock film of a graphene oxide film, drying at 40 ℃ for 8h to remove moisture, and stripping the substrate to obtain the graphene oxide film with the film thickness of 20 microns;
3) then, under the protection of argon atmosphere, heating to 1500 ℃ at the speed of 10 ℃/min, preserving heat for 2h, and naturally cooling to obtain graphene foam;
4) and (3) calendering the graphene foam in the step 3) into a film by using a calender, wherein the pressure is 40MPa, and then carrying out post-treatment such as edge cutting and the like to obtain the high-conductivity graphene electromagnetic shielding film.
Fig. 4 is a cross-sectional electron microscope image of the porous structure obtained in comparative example 1, and it can be seen that after the graphene oxide film is directly subjected to heat treatment without being thermally peeled, the obtained porous structure is mostly a macroporous structure, and sheets constituting the macroporous structure are not peeled, so that no mesopores (with a pore diameter of 2-50 μm) exist, and the structure enables a product to show an incompressible characteristic in a calendering process, so that the structure is not compact enough, the obtained mechanical property is poor, the tensile strength is only 40MPa, the number of pores in the structure is too large, and the electrical conductivity is far smaller than that in example 1.
Fig. 5 and 6 further confirm the above results, i.e., that the graphene oxide film exhibits a high specific surface area (116 m) after infrared thermal exfoliation2/g) and the obtained mesopores are mainly concentrated around 2nm, while the graphene oxide film without thermal exfoliation has only 6.24m after the temperature-rising heat treatment2The specific surface area is extremely low per gram, and almost no mesopores exist.
For the graphene electromagnetic shielding films provided in examples 1 to 4 and comparative example 1, the electrical conductivity, the thermal conductivity and the tensile strength were characterized. The conductivity test method is a four-probe method (DB 32/T4027-: the specimens were 5X 1cm in size, 5mm/min in tensile rate, 10mm in initial spacing, and the test results are shown in Table 1.
TABLE 1 Performance of graphene electromagnetic shielding films
As can be seen from table 1, the graphene film provided by the present invention has better electromagnetic shielding effectiveness and mechanical properties than the comparative example. The main reasons are as follows: 1. the embodiment adopts high-speed dispersion to strip and disperse the graphite oxide to obtain single-layer graphene oxide, and the graphene oxide is more compact in stacking and less in defects in the film forming process; 2. the mesoporous structure which is easy to be rolled is obtained by adopting an infrared thermal stripping mode, and the compactness of the final product graphene film is greatly improved, so that the conductivity and the mechanical property of the graphene film are improved, and excellent flexibility and foldability are shown.
The invention provides a method and a thought for rapidly preparing a highly conductive graphene electromagnetic shielding film, and a method and a way for implementing the technical scheme are numerous, the above description is only a preferred embodiment of the invention, and it should be noted that, for a person skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the invention, and these improvements and decorations should also be regarded as the protection scope of the invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (10)
1. A method for rapidly preparing a high-conductivity graphene electromagnetic shielding film is characterized by comprising the following steps:
(1) preparing a graphite oxide filter cake into a graphite oxide suspension, uniformly dispersing, and then stirring under vacuum to remove bubbles to obtain graphene oxide dispersion slurry;
(2) uniformly coating the graphene oxide dispersion slurry obtained in the step (1) on a substrate to form a graphene oxide blank film, drying to remove moisture, and then peeling off the substrate to obtain a graphene oxide film;
(3) irradiating the graphene oxide film obtained in the step (2) by adopting infrared rays in an air environment, heating to 1500 ℃ under the protection of inert atmosphere, preserving heat for 0.5-2 h, and naturally cooling to obtain graphene foam;
(4) and (4) rolling the graphene foam in the step (3) to form a film, thus obtaining the graphene foam.
2. The method for rapidly preparing a highly conductive graphene electromagnetic shielding film according to claim 1, wherein in the step (1), the average size of the graphite oxide filter cake is greater than 100 μm, the graphite oxide filter cake is prepared into a graphite oxide suspension with a concentration of 5-40 mg/mL, and ammonia water is added to adjust the pH value to 7-8.
3. The method for rapidly preparing a highly conductive graphene electromagnetic shielding film according to claim 1, wherein in the step (1), the large-size graphite oxide is exfoliated into graphene oxide by dispersing in a high-speed shear disperser at a linear speed of 10-20 m/s for 0.5-2 h; and slowly stirring by using a vacuum stirrer under the vacuum assistance of-0.1 MPa at a linear speed of 1-5 m/s until bubbles are completely removed.
4. The method for rapidly preparing a highly conductive graphene electromagnetic shielding film according to claim 1, wherein in the step (2), the substrate is polyethylene terephthalate, and the thickness of the graphene oxide green film on the substrate is 1-5 mm.
5. The method for rapidly preparing the high-conductivity graphene electromagnetic shielding film according to claim 1, wherein in the step (2), the graphene oxide film with the film thickness of 10-200 μm is obtained by drying at 30-70 ℃ for 6-8 h to remove water and peeling off the substrate.
6. The method for rapidly preparing the high-conductivity graphene electromagnetic shielding film according to claim 1, wherein in the step (3), an infrared lamp with a surface temperature of 300-400 ℃ is adopted to irradiate the graphene oxide film for 5-20 seconds.
7. The method for rapidly preparing a highly conductive graphene electromagnetic shielding film according to claim 1, wherein in the step (3), the temperature is increased to 1500 ℃ at a rate of 10-20 ℃/min.
8. The method for rapidly preparing a highly conductive graphene electromagnetic shielding film according to claim 1, wherein in the step (4), a calendar is used for calendaring the graphene foam into a film, and the pressure is 2-50 MPa.
9. The high-conductivity graphene electromagnetic shielding film prepared by the preparation method of any one of claims 1-8.
10. The highly conductive graphene electromagnetic shielding film according to claim 9, wherein the thickness of the highly conductive graphene electromagnetic shielding film is 10-35 μm, and the density of the highly conductive graphene electromagnetic shielding film is 1.3-1.6 g/cm3The conductivity reaches more than 1000S/cm, the tensile strength reaches more than 100MPa, and the electromagnetic shielding efficiency reaches more than 48dB in a wide frequency band.
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