CN110540197B - Method for cleaning graphene surface by using carbon nano material - Google Patents
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- CN110540197B CN110540197B CN201810534499.2A CN201810534499A CN110540197B CN 110540197 B CN110540197 B CN 110540197B CN 201810534499 A CN201810534499 A CN 201810534499A CN 110540197 B CN110540197 B CN 110540197B
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Abstract
The invention provides a method for cleaning the surface of graphene by using a carbon nano material, which comprises the following steps: providing a carbon nano material; contacting the carbon nanomaterial with the graphene surface; applying pressure to the graphene surface contacting the carbon nanomaterial; and separating the carbon nanomaterial from the graphene after the application of the pressure; wherein the carbon nano material is a carbon nanowall or a carbon nanowall composite. The method provided by the invention is simple and easy to implement, has a good cleaning effect on graphene on various substrates, and has important significance in further realizing and expanding high-end application of graphene.
Description
Technical Field
The invention relates to the field of graphene materials, in particular to a method for cleaning the surface of graphene by using a carbon nano material.
Background
Graphene is a carbon atom in sp2The excellent mechanical, electrical, optical and thermal properties of the two-dimensional material with a honeycomb structure formed by a hybrid mode are widely concerned by people, and various applications are promoted. Of the many methods for preparing graphene, Chemical Vapor Deposition (CVD) catalyzed by a copper metal substrate can be convenientThe method is a preferable method for preparing graphene because the large-area, uniform and single-layer large single-crystal graphene film is prepared.
However, the quality of the graphene prepared by the CVD method is not perfect, but has a serious problem of surface contamination, which is caused by intrinsic contamination in the growth process, i.e., amorphous carbon deposition; on the other hand, from the contamination of the high polymers caused during the transfer. These contaminants can greatly reduce the performance of graphene, for example, increase scattering of electrons and phonons, thereby reducing the mobility and thermal conductivity of graphene; contaminants also increase light absorption, thereby affecting its performance as a transparent electrode.
Therefore, the effective removal of the surface contaminants of the graphene prepared by the CVD method is an urgent problem to be solved in the field.
It is noted that the information disclosed in the foregoing background section is only for enhancement of background understanding of the invention and therefore it may contain information that does not constitute prior art that is already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention provides a method for cleaning the surface of graphene by using a carbon nano material, which is characterized in that the pollutants on the surface of the graphene are removed by utilizing the huge specific surface area and the strong interaction between an active terminal and the pollutants on the surface of the graphene, so that the clean surface of the graphene is obtained. The method has a good cleaning effect on graphene on various substrates, can be used for preparing clean graphene, and has important significance for further realizing and expanding high-end application of preparing graphene by a CVD method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a graphene surface treatment method, which comprises the following steps:
providing a carbon nano material;
contacting the carbon nanomaterial with the graphene surface;
applying pressure to the graphene surface contacting the carbon nanomaterial; and
separating the carbon nanomaterial from the pressurized graphene;
wherein the carbon nano material is a carbon nanowall or a carbon nanowall composite.
According to one embodiment of the invention, the carbon nanowall is a graphene sheet layer array supported on a carrier and grown perpendicular to the plane or the section of the carrier, and the carrier is a powdery carrier or a block carrier.
According to an embodiment of the present invention, the carbon nanomaterial is a carbon nanowall and the support is a powdered support, wherein the carbon nanomaterial is brought into contact with the graphene surface in a manner that: the carbon nanomaterial embeds the graphene surface.
According to one embodiment of the present invention, the carbon nanomaterial is a carbon nanowall, and the support is a bulk support, wherein the carbon nanomaterial is brought into contact with the graphene surface in a manner that: the carbon nanomaterial is stacked on the graphene surface.
According to an embodiment of the present invention, the carbon nanomaterial is a carbon nanowall composite, and the surface of the graphene is brought into contact with the carbon nanomaterial by: the carbon nanomaterial is stacked on a surface of the graphene.
According to one embodiment of the present invention, the carbon nanowall composite is a composite of a carbon nanowall, a binder and a bonding substrate, wherein the support of the carbon nanowall is a powdery support.
According to one embodiment of the invention, the binder is selected from one or more of polyvinylidene fluoride, polyacrylic acid, polyacrylonitrile, sodium carboxymethylcellulose and sodium alginate; the polar solvent is selected from one or more of N-methyl pyrrolidone, dimethyl sulfoxide and N, N-dimethylformamide; the bonding substrate is selected from one or more of foamed metal, metal foil, metal block, paper and cloth; the mass ratio of the carbon nanowall to the binder is 3-12: 1, the mass ratio of the polar solvent to the binder is 5-100: 1.
according to one embodiment of the invention, the method further comprises heating in an inert atmosphere while applying the pressure, wherein the heating temperature is 100-200 ℃, and the heating time is 5-10 min.
According to an embodiment of the present invention, the pressure includes a positive pressure, and the positive pressure is 100Pa to 10000 Pa.
According to one embodiment of the invention, the powdered carrier is selected from one or more of powdered silica, fumed silica, powdered alumina silicate, calcium silicate, powdered silica and powdered titanium dioxide.
According to one embodiment of the invention, the bulk carrier is selected from one or more of the group consisting of metal foil, metal plate, foamed metal, quartz, glass and sapphire.
The invention also provides clean graphene prepared by the method.
The invention also provides application of the clean graphene in packaging of transparent conductive films, transparent electrodes, high-frequency electronic devices, light-emitting devices, photovoltaic devices, photoelectric detection devices, electrooptical modulation devices, heat dissipation devices or hydrophobic devices.
According to the technical scheme, the invention has the beneficial effects that:
according to the method for cleaning the graphene surface by the carbon nano material, the surface pollutants are removed by utilizing the huge specific surface area of the carbon nano material and the strong interaction between the active tail end and the pollutants on the graphene surface, so that the clean graphene surface is obtained, and the surface clean area ratio can reach more than 60% and can reach more than 95% at most. The method for treating the surface of the graphene is simple and easy to operate, has an excellent cleaning effect, and is suitable for preparing clean graphene.
Drawings
FIG. 1a is an SEM image of carbon nanowalls loaded on a powdered silica substrate of example 1;
FIG. 1b is a TEM image of carbon nanowall supported on a powdered silica substrate of example 1;
figure 2a is a TEM image of graphene after treatment of example 1;
fig. 2b is a TEM image of untreated graphene of example 1;
fig. 3 is a TEM image of graphene after example 2 treatment;
figure 4a is an AFM image of graphene after example 3 processing;
figure 4b is an AFM image of untreated graphene of example 4.
Detailed Description
The technical solution of the present invention is further explained below according to specific embodiments. The scope of protection of the invention is not limited to the following examples, which are set forth for illustrative purposes only and are not intended to limit the invention in any way.
The invention provides a method for cleaning the surface of graphene by using a carbon nano material, which comprises the following steps:
providing a carbon nano material;
contacting the carbon nanomaterial with the graphene surface;
applying pressure to the graphene surface contacting the carbon nanomaterial; and
separating the carbon nanomaterial from the pressurized graphene;
wherein the carbon nano material is a carbon nanowall or a carbon nanowall composite.
In some embodiments, the carbon nanowall is an array of graphene sheets supported on a support and grown perpendicular to the plane or cut plane of the support, wherein "perpendicular" includes perpendicular or near perpendicular. The carrier is a powder carrier or a block carrier, namely the carbon nanowall comprises a powder-based carbon nanowall and a block-based carbon nanowall, wherein the powder-based carbon nanowall refers to a graphene lamellar array loaded or grown on the powder carrier; the bulk-based carbon nanowalls refer to graphene lamellar arrays supported or grown on a bulk carrier. Powdered carriers include, but are not limited to, one or more of powdered silica, fumed silica, powdered aluminum silicate, calcium silicate, powdered silica, and powdered titanium dioxide. The bulk carrier includes, but is not limited to, one or more of metal foil, metal plate, foamed metal, quartz, glass, and sapphire.
The carbon nanowall composite is a composite of a carbon nanowall, an adhesive and a bonding substrate, wherein the carrier of the carbon nanowall is the powdery carrier, namely the powder-based carbon nanowall. Wherein, the binder includes but is not limited to one or more of polyvinylidene fluoride, polyacrylic acid, polyacrylonitrile, sodium carboxymethylcellulose and sodium alginate. The bonding substrate includes, but is not limited to, one or more of metal foam, metal foil, metal block, paper, and cloth.
In some embodiments, when the carbon nanomaterial is a carbon nanowall and the support is a powdered support, that is, when the carbon nanomaterial is a powder-based carbon nanowall, the manner of cleaning the surface of the graphene includes: the graphene to be cleaned is embedded in the powder-based carbon nanowall and pressure is applied, and then the powder-based carbon nanowall is separated from the graphene after the pressure is applied, for example, the graphene is taken out of the powder-based carbon nanowall. In some embodiments, the method further comprises purging the surface of the removed graphene with an inert gas after the graphene is removed to remove powder-based carbon nanowalls and/or other impurities remaining on the surface, wherein the inert gas includes, but is not limited to, nitrogen or argon.
In some embodiments, when the carbon nanomaterial is a carbon nanowall and the carrier is a bulk carrier, that is, when the carbon nanomaterial is a bulk-based carbon nanowall, the manner of cleaning the surface of the graphene includes: stacking the graphene to be cleaned and the block-based carbon nanowall together, applying pressure after the surface of the graphene to be cleaned is contacted with the surface of the block-based carbon nanowall, and then separating the block-based carbon nanowall from the graphene after the pressure is applied. In some embodiments, when bulk-based carbon nanowalls or other impurities remain on the surface of the graphene, the surface of the removed graphene may be purged with an inert gas, including but not limited to nitrogen or argon.
In some embodiments, when the carbon nanomaterial is a carbon nanowall composite, the manner of cleaning the graphene surface includes: stacking the graphene to be cleaned and the carbon nanowall composite together, applying pressure after the surface of the graphene to be cleaned is contacted with the surface of the carbon nanowall composite, and then separating the carbon nanowall composite from the graphene after the pressure is applied.
In some embodiments, the pressure is applied while heating in an inert atmosphere, the heating temperature is 100 ℃ to 200 ℃, and the heating time is 5min to 10 min. The applied pressure includes, but is not limited to, a positive pressure ranging from 100Pa to 10000 Pa. The applied pressure may also include a certain range of lateral pressure effects, thereby facilitating closer contact between the carbon nanowall or the carbon nanowall composite and the graphene surface and better cleaning effect. The manner of applying the pressure includes a static applying pressure and a rolling applying pressure.
In some embodiments, the graphene is graphene grown on a metal substrate, for example: graphene on copper foil, and the like; or graphene transferred onto a functional substrate, for example: graphene transferred onto a silicon wafer substrate, and the like.
The invention also provides a preparation method of the carbon nanowall composite, which comprises the following steps:
providing a carbon nanowall, wherein a carrier of the carbon nanowall is a powdery carrier;
mixing the carbon nanowall with a binder and a polar solvent to form slurry;
and coating the slurry on a bonding substrate to obtain the carbon nanowall composite.
Specifically, for example, the carbon nanowall supported on a powdery carrier and a binder are uniformly stirred in a polar solvent to form a slurry, the slurry is uniformly coated on a bonding substrate, and then the slurry is heated and dried to prepare the carbon nanowall composite for the clean post-treatment of graphene.
In some embodiments, the binder includes, but is not limited to, one or more of polyvinylidene fluoride, polyacrylic acid, polyacrylonitrile, sodium carboxymethyl cellulose, and sodium alginate. The bonding substrate includes, but is not limited to, one or more of metal foam, metal foil, metal block, paper, and cloth. The polar solvent includes, but is not limited to, one or more of N, N-dimethylformamide, N-dimethyl sulfoxide, N-methylpyrrolidone, N-dimethylformamide, N-dimethylformamide, and N-methylpyrrolidone.
In some embodiments, the mass ratio of the carbon nanowall to the binder is 3 to 12: 1, the mass ratio of the polar solvent to the binder is 5-100: 1.
the invention also provides clean graphene prepared by the method. The clean graphene in the invention means that the percentage of the area of the clean surface reaching the atomic level in the total area is more than 60%.
The invention also provides application of the clean graphene in packaging of transparent conductive films, transparent electrodes, high-frequency electronic devices, light-emitting devices, photovoltaic devices, photoelectric detection devices, electrooptical modulation devices, heat dissipation devices or hydrophobic devices.
The following is illustrated by specific examples:
example 1 carbon nanowalls supported on powdered silica were used for graphene surface treatment on copper foil.
The graphene selected in this example was graphene grown on copper foil. The selected carbon nano material is a carbon nano wall loaded on a powdery silicon dioxide substrate, the appearance under a scanning electron microscope is shown as figure 1a, and the appearance under a transmission electron microscope is shown as figure 1 b. The specific operation steps are as follows:
step 1: taking out a clean quartz vessel, putting a carbon nano wall loaded on a powder silicon dioxide substrate into the quartz vessel, embedding graphene grown on copper foil into the nano wall, and pressing a weight with the mass of 200g to maintain a certain positive pressure.
Step 2: and (3) placing the system in a tube furnace, heating to 170 ℃ in an argon protective atmosphere, maintaining for 10 minutes, then taking out the graphene growing on the copper foil after the system is cooled to room temperature, and blowing the surface of the graphene by using nitrogen flow.
And step 3: and transferring the treated graphene to a Transmission Electron Microscope (TEM) carrying net to perform corresponding TEM characterization on the graphene.
The transmission electron microscope characterization of the treated graphene is shown in fig. 2a, and the transmission electron microscope characterization of the untreated graphene is shown in fig. 2b, so that the cleanliness of the graphene treated by the steps is greatly improved. Therefore, the carbon nanowall loaded on the powder can effectively remove the intrinsic pollutants of the graphene grown on the copper foil.
Example 2 use of carbon nanowall composites for graphene surface treatment on copper foil
The specific operation steps are as follows:
step 1: preparing the carbon nanowall composite. Adding adhesive into the carbon nanowall loaded on the powdery silicon dioxide, and uniformly stirring the adhesive by using a glass rod to prepare the carbon nanowall slurry. And then uniformly coating the carbon nano wall slurry on the surface of the foam copper, and heating and airing to obtain the carbon nano wall composite. The carbon nanowall slurry comprises the following components: n-methyl pyrrolidone: polyvinylidene fluoride: carbon nanowall supported on powder silica 20: 1: 5 (mass ratio)
Step 2: and (3) placing the graphene on the copper foil upwards and the carbon nanowall composite downwards, and stacking the graphene and the carbon nanowall composite together face to face and placing the copper foil and the carbon nanowall composite on a platform. And applying positive pressure of 5000Pa to the carbon nanowall composite by a physical static pressure application method, and heating to 170 ℃ under the protection of argon atmosphere for 5 min. And then taking out the graphene growing on the copper foil after the system is cooled to room temperature, and blowing the surface of the graphene by using nitrogen flow.
And step 3: and (3) transferring the graphene processed in the step (2) to a TEM grid, and performing corresponding TEM characterization on the graphene.
The transmission electron microscope characterization of the graphene processed by the steps is shown in fig. 3, and it can be seen that the carbon nanowall composite can effectively remove the surface intrinsic pollutants of the graphene on the copper foil. In addition, the carbon nanowall composite has an advantage in that it is easier to be applied to mass production than a carbon nanowall supported on a powder substrate.
Example 3 use of carbon nanowall composites for graphene surface treatment on silicon wafers
In this embodiment, the post-processing object is graphene on a silicon substrate with an oxide layer thickness of 90nm assisted by polymethyl methacrylate (PMMA). In this example, a carbon nanowall composite was selected as a processing material, and the cleanliness of graphene before and after cleaning was characterized by an Atomic Force Microscope (AFM). The rest of the process is the same as in example 2.
AFM images of graphene after carbon nanowall composite post-processing are shown in fig. 4a, and AFM pictures of untreated graphene are shown in fig. 4 b. It can be seen that the roughness of the graphene surface after the cleaning treatment becomes small, and the amount of residual glue is reduced. The carbon nanowall composite also has a better cleaning effect on graphene transferred to a silicon wafer substrate.
The present invention has been disclosed in several embodiments above to facilitate the understanding of the present invention by those of ordinary skill in the art. Those skilled in the art may now appreciate that they may readily use the present disclosure as a basis for designing or modifying other processes and structures for carrying out the same purposes of the embodiments and/or achieving the same advantages of the embodiments. Those skilled in the art should understand that they can make various changes, substitutions and alterations herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (12)
1. A method for cleaning the surface of graphene by using a carbon nano material is characterized by comprising the following steps:
providing a carbon nano material;
contacting the carbon nanomaterial with the graphene surface;
applying pressure to the graphene surface contacting the carbon nanomaterial; and
separating the carbon nanomaterial from the pressurized graphene;
wherein the carbon nano material is a carbon nanowall or a carbon nanowall composite;
and heating the surface of the graphene contacted with the carbon nano material in an inert atmosphere while applying pressure, wherein the heating temperature is 100-200 ℃, the pressure comprises positive pressure, and the positive pressure is 100-10000 Pa.
2. The method of claim 1, wherein the carbon nanowall is an array of graphene sheets supported on a support and grown perpendicular to the plane or cut surface of the support, the support being a powdered support or a bulk support.
3. The method of claim 2, wherein the carbon nanomaterial is a carbon nanowall and the support is a powdered support, and wherein the carbon nanomaterial is brought into contact with the graphene surface by: the carbon nanomaterial embeds the graphene surface.
4. The method of claim 2, wherein the carbon nanomaterial is a carbon nanowall and the support is a bulk support, and wherein the carbon nanomaterial is brought into contact with the graphene surface by: the carbon nanomaterial is stacked on the graphene surface.
5. The method of claim 2, wherein the carbon nanomaterial is a carbon nanowall composite, and the surface of the graphene is contacted with the carbon nanomaterial by: the carbon nanomaterial is stacked on a surface of the graphene.
6. The method of claim 5, wherein the carbon nanowall composite is a composite of a carbon nanowall, a binder and a bonding substrate, wherein the support of the carbon nanowall is a powdered support.
7. The method of claim 6, further comprising mixing the carbon nanowall, a binder and a polar solvent to form a slurry, and coating the slurry on the bonding substrate to obtain the carbon nanowall composite, wherein the binder is selected from one or more of polyvinylidene fluoride, polyacrylic acid, polyacrylonitrile, sodium carboxymethylcellulose and sodium alginate; the polar solvent is selected from one or more of N-methyl pyrrolidone, dimethyl sulfoxide and N, N-dimethylformamide; the bonding substrate is selected from one or more of foamed metal, metal foil, metal block, paper and cloth; the mass ratio of the carbon nanowall to the binder is 3-12: 1, the mass ratio of the polar solvent to the binder is 5-100: 1.
8. the method of claim 1, wherein the heating time is 5min to 10 min.
9. The method of claim 2, 3 or 6, wherein the powdered carrier is selected from one or more of powdered silica, fumed silica, powdered aluminum silicate, calcium silicate, powdered silica and powdered titanium dioxide.
10. The method according to claim 2 or 4, wherein the bulk carrier is selected from one or more of metal foil, metal plate, foamed metal, quartz, glass and sapphire.
11. Clean graphene prepared according to the method of any one of claims 1 to 10.
12. The use of the clean graphene according to claim 11 in transparent conductive films, transparent electrodes, high frequency electronic devices, light emitting devices, photovoltaic devices, photoelectric detection devices, electro-optic modulation devices, heat dissipation devices, or hydrophobic device packaging.
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| CN106672956A (en) * | 2017-01-21 | 2017-05-17 | 德阳烯碳科技有限公司 | Large-scale graphene transferring method |
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