CN115959655A - Graphene film preparation method and graphene film - Google Patents
Graphene film preparation method and graphene film Download PDFInfo
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- CN115959655A CN115959655A CN202211598492.XA CN202211598492A CN115959655A CN 115959655 A CN115959655 A CN 115959655A CN 202211598492 A CN202211598492 A CN 202211598492A CN 115959655 A CN115959655 A CN 115959655A
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Abstract
The embodiment of the invention provides a preparation method of a graphene film, which comprises the steps of forming a single-layer graphene film on a carrier, and solving the problem that the single-layer or multi-layer graphene film cannot be formed on the carrier by the existing organic solution of graphene; the film formed on the carrier can enable the graphene to form a uniform graphene film on the carrier during preparation due to the control of the content of the graphene, and due to the small particle size and thickness of the graphene, after the carrier is taken out of the solution, the organic solvent is volatilized, and the carbon-carbon bond of the graphene in the solution is recovered; in the recovery process, superposition exists, so that the cross section of the graphene film has a certain superposition state, the thickness of a single-layer film ranges from 0.4nm to 1.2nm, and the device volume of the graphene film is correspondingly reduced during application due to the small thickness of the single layer, thereby being beneficial to increasing the compaction density of a pole piece and improving the volume energy density of a battery.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a graphene film preparation method and a graphene film.
Background
Graphene is a new material with a monolayer two-dimensional honeycomb lattice structure formed by tightly stacking sp2 hybridized and connected carbon atoms, has excellent optical, electrical and mechanical properties, has important application prospects in aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The arrangement mode of the carbon atoms in the graphene is bonded by sp2 hybridized orbitals like a graphite monoatomic layer, and the graphene has the following characteristics: the carbon atom has 4 valence electrons, wherein 3 electrons generate sp2 bonds, that is, each carbon atom contributes an unbound electron on the pz orbital, the pz orbitals of neighboring atoms form pi bonds in a direction perpendicular to the plane, and the newly formed pi bonds are in a half-filled state. The research proves that the coordination number of carbon atoms in the graphene is 3, the bond length between every two adjacent carbon atoms is 1.42 multiplied by 10-10 meters, and the included angle between bonds is 120 degrees. In addition to the honeycomb-like layered structure in which the sigma bonds are linked to other carbon atoms in hexagonal rings, the pz orbital of each carbon atom perpendicular to the plane of the layer can form a large pi bond (similar to a benzene ring) of multiple atoms throughout the layer, thus having excellent electrical conductive and optical properties.
When graphene is used as an electrode material, the size, distribution and form of graphite particles have a great influence on various performance indexes of the negative electrode material, so the particle size and thickness of the graphite particles can influence the specific application of the graphite particles. For example, the particle size distribution of graphite directly affects the pulping process and volumetric energy density of the battery.
However, the existing graphene cannot be well dispersed in an organic solution (such as alcohol) due to reasons such as particle size and thickness, and thus cannot form a graphene organic solution, so that a single-layer or multi-layer graphene film cannot be formed on a carrier.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a graphene film preparation method and a graphene film that overcome the above problems or at least partially solve the above problems.
The embodiment of the application discloses a preparation method of a graphene film, which comprises the following steps:
uniformly dispersing the prepared graphene in a volatile organic solution to form a graphene organic solution of monomer graphene, wherein the sheet diameter of the monomer graphene is 30-150 nm;
determining and controlling the content of the graphene in the graphene organic solution by adjusting the concentration of the graphene organic solution; wherein the content ratio is 1;
determining a carrier for preparing the graphene film according to the content, and immersing the carrier into the graphene organic solution;
and after the infiltration is finished, taking out the carrier, and drying the carrier to form the graphene film on the surface of the carrier.
Further, the step of uniformly dispersing the prepared graphene in a volatile organic solution to form a graphene organic solution of monomer graphene includes: adding the prepared graphene into an organic solution, and destroying non-monomeric graphene in the organic solution by ultrasonic waves emitted by ultrasonic equipment to uniformly disperse the monomeric graphene in the organic solution to form a graphene organic solution of the monomeric graphene.
Further, the volatile organic solution is alcohol; the graphene organic solution is a graphene alcohol solution.
Further, the method for uniformly dispersing the prepared graphene in the volatile organic solution to form the graphene organic solution of the monomer graphene further comprises the following steps:
performing electromagnetic modification treatment on graphite by using microwaves, and performing gas milling correction, shaping and screening to obtain graphite particles;
precisely carrying out intercalation transformation on the graphite particles by using an initiator, and obtaining onion-roll-shaped graphite particles by using a cutting and shearing process;
and (3) carrying out self-deslagging on the graphite particles in the onion roll shape by using centrifugal equipment to obtain the monomer graphene.
Further, the electromagnetic modification treatment of graphite by using microwaves, and the gas milling correction, shaping and screening are performed, and before the obtained graphite particles, the method further comprises the following steps:
transferring a natural graphite raw material into a hopper through a vacuum feeding machine, and putting the hopper into an air jet mill for air jet milling;
and collecting the graphite with the required particle size grade by using a cyclone dust collector.
Further, after the graphite particles in the shape of an onion roll are subjected to self-discharge by a centrifugal device to obtain the graphene monomer, the method further includes:
and drying the monomer graphene, and performing magnetic 5 separation on the dried monomer graphene to obtain pure monomer graphene.
Further, the method also comprises the following steps: carrying out surface treatment on the carrier;
and the surface treatment comprises hot pressing and/or polishing the surface of the carrier.
Further, the method also comprises the following steps:
and repeating the steps of taking out the carrier after the infiltration is finished, drying the carrier to form the graphene film on the surface of the carrier 0, and forming a multilayer graphene film on the carrier.
The embodiment of the application also discloses a graphene film, wherein the graphene film is coated on the surface of a carrier and is prepared by any one of the methods.
5 the embodiment of the application also discloses a negative electrode material, which comprises the following components
The graphene film prepared by the method and a carrier for coating the graphene film, wherein,
the carrier of the graphene film comprises a copper foil and an aluminum foil.
The embodiment of the invention has the following advantages:
in the embodiment of the invention, the prepared graphene is uniformly dispersed in a volatile organic solution 0 to form a graphene organic solution of monomer graphene, wherein the thickness of the monomer graphene is 0.4-1.2 nm, and the sheet diameter of the monomer graphene is 30-150 nm; determining and controlling the content of the graphene in the graphene organic solution by adjusting the concentration of the graphene organic solution; wherein the content ratio is 1; according to the content, determining a carrier for preparing the graphene film, and mixing the carrier and the graphene film
Immersing the carrier into the graphene organic solution; and after the infiltration is finished, taking out the carrier, and drying the carrier 5 to form the graphene film on the surface of the carrier. By forming a single-layer graphene film on a carrier, the problem that the single-layer or multi-layer graphene film cannot be formed on the carrier by the conventional organic solution of graphene is solved; since the thickness of the monomer graphene is 0.4-1.2 nm, the content of the graphene is controlled through the film formed on the carrier, so that the graphene can form a uniform graphene film on the carrier during preparation, and since the particle size and the thickness of the graphene are small, after the carrier is taken out of the solution, the organic solvent is volatilized, and the carbon-carbon bond of the graphene in the solution is recovered; in the recovery process, superposition exists, so that the cross section of the graphene film has a certain superposition state, the thickness of a single-layer film ranges from 0.4nm to 1.2nm, and the device volume of the graphene film is correspondingly reduced during application due to the small thickness of the single layer, thereby being beneficial to increasing the compaction density of a pole piece and improving the volume energy density of a battery.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the description of the present invention will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
Fig. 1 is a flowchart illustrating steps of a method for preparing a graphene film according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description thereof. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a flow chart illustrating steps of a graphene film preparation method according to an embodiment of the present invention is shown, and specifically, the method may include the following steps:
step S101, uniformly dispersing the prepared graphene in a volatile organic solution to form a graphene organic solution of monomer graphene, wherein the sheet diameter of the monomer graphene is 30-150 nm;
step S102, determining and controlling the content of the graphene in the graphene organic solution by adjusting the concentration of the graphene organic solution; wherein the content ratio is 1;
step S103, determining a carrier for preparing the graphene film according to the content, and immersing the carrier into the graphene organic solution;
and S104, after the infiltration is finished, taking out the carrier, and drying the carrier to form the graphene film on the surface of the carrier.
In the embodiment, the single-layer graphene film is formed on the carrier by the method, so that the problem that the single-layer or multi-layer graphene film cannot be formed on the carrier by the conventional organic solution of graphene is solved; the thickness of the monomer graphene is 0.334nm, and the content of the graphene is controlled through the film formed on the carrier, so that the graphene can form a uniform graphene film on the carrier during preparation, and the principle is that the carbon-carbon bond of the graphene in the solution is recovered in the volatilization process of the organic solution in the solution when the carrier is taken out from the solution due to small particle size and thickness of the graphene; in the recovery process, superposition exists, so that the cross section of the graphene film has a certain superposition state, the thickness of a single-layer film ranges from 0.4nm to 1.2nm, and the device volume of the graphene film is correspondingly reduced during application due to the small thickness of the single layer, thereby being beneficial to increasing the compaction density of a pole piece and improving the volume energy density of a battery.
In the above embodiment, when graphene is deposited on the surface of the carrier, new van der waals force is formed on the surface of the carrier, and a carrier such as copper forms new van der waals force of a carbon-copper bond on the surface of copper, so that the deposition is more stable, thereby solving the problem that in the prior art, graphene needs to be attached to the carrier through an adhesive, and the adhesive is unstable, so that the graphene on the carrier is easy to fall off and is unstable; the graphene film formed on the carrier by the method does not need an adhesive and is connected by a carbon bond, so that the graphene film is stably attached to the surface of the carrier.
In any embodiment of the present application, the single-layer graphene is single-layer graphene, the standard thickness of the single-layer graphene is 0.334nm, and the maximum thickness of the single-layer graphene is not more than 0.4nm, and the thickness of the single-layer graphene is the thickness of a graphene film formed on a support, and a corresponding bond formed between the single-layer graphene and the support, for example, a carbon-copper bond is formed when the support is copper, so that the thickness of the film is slightly thicker than that of the single-layer graphene (single-layer graphene).
It should be noted that the content ratio of 1 to 1000000 is an optimal ratio, and if it is too high, stacking may be formed on the surface of the support, and if it is too low, the concentration is not sufficient, that is, the number of graphene monolayers cannot cover the whole surface area of the support surface, so that the formed film is incomplete.
In an embodiment of the present application, the "uniformly dispersing the prepared graphene in the volatile organic solution to form a graphene organic solution of monomeric graphene" in step S101 includes: adding the prepared graphene into an organic solution, and destroying non-monomeric graphene in the organic solution by ultrasonic waves emitted by ultrasonic equipment to uniformly disperse the monomeric graphene in the organic solution to form a graphene organic solution of the monomeric graphene.
In the above embodiment, due to the limitation of the current graphene preparation process and the reason of graphene, the prepared graphene monomer contains about 10% of impurities (no monomer is formed), and in a certain probability, carbon-carbon bonds between some monomers are bonded to form non-monomeric graphene, and the non-monomeric graphene is an impurity in the solution.
In one embodiment of the present application, the volatile organic solution is alcohol; the graphene organic solution is a graphene alcohol solution.
In the above embodiment, the alcohol (ethanol) is a volatile colorless transparent liquid at normal temperature and pressure, and has low toxicity. It can be dissolved with water at any ratio, and can be dissolved with chloroform, ether, methanol, acetone and other organic solvents. When the graphene is taken out of the solution, the surface of the carrier can be quickly dried due to the volatile property of alcohol, and other auxiliary equipment (such as heating and air drying equipment) is not needed in the alcohol drying process, and only natural drying is needed, so that the cost can be reduced; because the cost of the alcohol is low, and the volatilization of the alcohol can not cause environmental pollution, the cost is reduced, and the environment is protected.
In an embodiment of the present application, before "uniformly dispersing the prepared graphene in the volatile organic solution to form a graphene organic solution of monomeric graphene" in step S101, the method further includes:
performing electromagnetic modification treatment on graphite by using microwaves, and performing gas milling correction, shaping and screening to obtain graphite particles; based on the microwave heating basis, the microwave can interact with the graphite to generate a new action mechanism so as to assist the modification of the graphite material, particularly, the graphite material absorbs the microwave energy to break the carbon-carbon bond of the graphite material, and the selective heating of the microwave and the sensitivity of the chemical reaction rate to the temperature can be used for assisting the chemical reaction to accelerate the reaction rate and realize the modification of the graphite.
Precisely carrying out intercalation transformation on the graphite particles by using an initiator (catalyst), and obtaining onion-roll-shaped graphite particles by using a cutting and shearing process; the structure of the graphite is modified by a precise intercalation method, wherein the precise intercalation method is to modify the interlayer spacing of the graphite by using an initiator to replace the traditional method for changing the interlayer spacing of the graphite by using heat energy. The depth of the graphite interlayer spacing is precisely controlled by controlling the process parameters of the initiator, then the particle modification after the precise intercalation is carried out by the shearing process, the modification of the graphite particles is completed, and the nature of the initiator is recovered to be recycled in the system after the particle modification is completed. And (3) carrying out self-deslagging on the graphite particles in the onion roll shape by using centrifugal equipment to obtain the monomer graphene.
In the embodiment, the surfaces of the graphite particles are physically treated by the modified graphite process, an ordered arrangement state is formed in an electromagnetic modification link, and a friction effect is formed on the graphite surfaces, so that the surfaces of the graphite particles are smoother; then, intercalation treatment is carried out on the graphite by an intercalation method of a pure carbon single-layer graphene preparation process, so that the number of graphite layers is reduced; and then, the surface of the graphite is cut by a cutting method to form an onion roll structure, so that the form of the natural graphite is changed, and various indexes of the material, such as conductivity, are improved.
As in the step S102, the concentration of the graphene organic solution is adjusted to determine and control the content of the graphene in the graphene organic solution; wherein the content ratio is 1; the amount of graphene deposited on the surface of the support is controlled by adjusting the ratio of the dispersion (graphene) to the solvent.
As the step S103, determining a carrier for preparing the graphene film according to the content, and immersing the carrier into the graphene organic solution; when the dispersion is performed at a ratio of 1.
In an embodiment of the present application, the electromagnetic modification treatment of graphite by using microwaves, and the grinding, modifying, shaping, and screening to obtain graphite particles further include: the method comprises the following steps of (1) transferring a natural graphite raw material into a hopper through a vacuum feeding machine, and then putting the hopper into an airflow mill for airflow milling; and collecting the graphite with the required particle size grade by using a cyclone dust collector.
In the embodiment, the vacuum feeding machine is used for automatically feeding, sealing and collecting through the cyclone dust collector, so that dust can be prevented from leaking in the production process, and dust pollution is avoided.
In an embodiment of the present application, after the graphite particles in the shape of an onion roll are self-discharged by a centrifugal device to obtain single graphene, the method further includes: and drying the monomer graphene, and performing magnetic separation on the dried monomer graphene to obtain pure monomer graphene.
In the embodiment, the pure monomer graphene is obtained by the high-speed centrifuge and the dryer, and the negative electrode material prepared from the monomer graphene can be well applied to the lithium ion battery, so that good economic and social benefits are obtained.
In an embodiment of the present application, the method further includes: carrying out surface treatment on the carrier; and the surface treatment comprises hot pressing and/or polishing the surface of the carrier.
In the embodiment, as the sheet diameter of the graphene is 30-150 nm, when the surface of the carrier is uneven, the graphene of the monomer is easy to fall to a low-lying position; and the graphene in the low-lying position and the graphene in the flat position are not easily connected at the low-lying wall, so that the formed film is not complete enough, and the graphene film formed on the surface of the carrier has continuity and flatness through the surface treatment.
In an embodiment of the present application, the method further includes: and (S104) repeating the step of taking out the carrier after the infiltration is finished, drying the carrier to form the graphene film on the surface of the carrier, and forming a multilayer graphene film on the carrier.
In the above-described examples, a multilayer sheet of a silylene film, preferably a 48-layer film in the present application, can be formed on the support by immersing the support in a solution, taking out and drying the support, and repeating these steps a plurality of times. The graphene deposited on the surface of the carrier after infiltration can form a single-layer graphene film in a self-assembly mode, two layers of graphene films can be obtained through secondary infiltration, and the like, so that the number of layers of the graphene film formed in the process is controllable.
In an embodiment of the application, the graphene film is coated on the surface of the carrier, and is prepared by the method, wherein the thickness of the single-layer film is in a range of 0.4-1.2 nm.
In an embodiment of the application, the negative electrode material comprises the graphene film prepared by the method and a carrier for coating the graphene film, wherein the carrier of the graphene film comprises a copper foil and an aluminum foil. Because copper has good conductive performance, copper foil is preferably used in the application, the resistance value of the electrode can be effectively reduced, after the battery is manufactured, the internal resistance of the battery is lower, the heat productivity of the battery during power supply is reduced, and the electric heating power formula W = I 2 R, when the supply current is not changed, the heat productivity of the battery is in direct proportion to the internal resistance, so that the cathode material is used as the material of the battery, the heat productivity of the battery is reduced, and the popularization of the battery is facilitated.
It should be noted that, the volume filling parts of the graphene are the same, the larger the particle size is, the wider the distribution is, and the smaller the viscosity of the slurry is; the small particles can be filled in the gaps of the large particles, so that the compaction density of the pole piece is increased, and the volume energy density of the battery is improved. In addition, particle morphology also has a large impact on rate, low temperature performance, etc., and small particles can improve rate performance and extend cycle life.
In one embodiment of the present application, the graphite is subjected to electromagnetic modification by microwaves, and H (hydrogen) atoms and O (oxygen) atoms are bonded to form H by graphite modification 2 In the process of O (water), the heat energy generated by the initiator is conducted between the carbon layer and the carbon layer to promote the van der Waals force between the C (carbon) layers to be broken by the energy and pry the van der Waals force to achieve the delamination effect, and the main aim is to form a two-dimensional material effect through different intercalation and remove oxygen atom functional groups through chemical potential energyThe material physical property is improved, the charge and discharge performance of the graphite can be improved, the specific capacity is improved, and the battery prepared from the material has good charge and discharge performance and cycle performance. The modified graphite cathode material not only maintains the advantages of a discharge voltage platform and higher lithium intercalation capacity of graphite, but also improves the compatibility of the graphite and electrolyte and the high-current charge and discharge performance. This is because, in graphite with a high ordering degree, not only is graphite interlayer shedding caused by graphite expansion during charging prevented, but also the specific surface area is increased, the arrangement of C molecules is promoted to be more ordered, and good conductive and electric storage effects are formed.
In the above embodiment, through practical tests, in an environment at-25 ℃, the number of charging times of the battery made of the negative electrode material in the present application is increased from 2000 to 5000, and the battery attenuation is increased from 25% to 10%. Therefore, the energy storage efficiency of the battery is greatly improved, and the service life of the battery is prolonged by more than 2 times, so that a battery product made of the cathode material has high application value and commercial popularization.
The embodiments in the present specification are all described in a progressive manner, and each embodiment focuses on differences from other embodiments, and portions that are the same and similar between the embodiments may be referred to each other.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
Finally, it should also be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "include", "including" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or terminal device including a series of elements includes not only those elements but also other elements not explicitly listed or inherent to such process, method, article, or terminal device. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or terminal device that comprises the element.
The graphene film and the method for preparing the graphene film provided by the invention are described in detail, and the principle and the embodiment of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (9)
1. A method for preparing a graphene film, the method comprising:
uniformly dispersing the prepared graphene in a volatile organic solution to form a graphene organic solution of monomer graphene, wherein the sheet diameter of the monomer graphene is 30-150 nm;
determining and controlling the content of the graphene in the graphene organic solution by adjusting the concentration of the graphene organic solution; wherein the content ratio is 1;
determining a carrier for preparing the graphene film according to the content, and immersing the carrier into the graphene organic solution;
and after the infiltration is finished, taking out the carrier, and drying the carrier to form the graphene film on the surface of the carrier.
2. The method of claim 1, wherein the step of uniformly dispersing the prepared graphene in a volatile organic solution to form a graphene organic solution of monomeric graphene comprises: adding the prepared graphene into an organic solution, and destroying non-monomeric graphene in the organic solution by ultrasonic waves emitted by ultrasonic equipment to uniformly disperse the monomeric graphene in the organic solution to form a graphene organic solution of the monomeric graphene.
3. The method according to claim 1 or 2, wherein the volatile organic solution is alcohol; the graphene organic solution is a graphene alcohol solution.
4. The method as claimed in claim 1 or 2, wherein the step of uniformly dispersing the prepared graphene into the volatile organic solution to form a graphene organic solution of the graphene monomer further comprises:
performing electromagnetic modification treatment on graphite by using microwaves, and performing gas milling correction, shaping and screening to obtain graphite particles;
precisely carrying out intercalation transformation on the graphite particles by using an initiator, and obtaining onion-roll-shaped graphite particles by using a cutting and shearing process;
and (3) carrying out self-deslagging on the graphite particles in the onion roll shape by using centrifugal equipment to obtain the monomer graphene.
5. The method as claimed in claim 4, wherein the electromagnetic modification treatment of graphite by microwave and the gas milling correction shaping screening are carried out, and before the obtained graphite particles, the method further comprises:
the method comprises the following steps of (1) transferring a natural graphite raw material into a hopper through a vacuum feeding machine, and placing the natural graphite raw material into an airflow mill from the hopper for airflow milling;
and collecting the graphite with the required particle size grade by using a cyclone dust collector.
6. The method of claim 4, wherein after the self-tapping of the graphite particles in the form of onion rolls by a centrifugal device to obtain the single graphene, the method further comprises:
and drying the monomer graphene, and performing magnetic separation on the dried monomer graphene to obtain pure monomer graphene.
7. The method of claim 1, further comprising: carrying out surface treatment on the carrier;
and the surface treatment comprises hot pressing and/or polishing the surface of the carrier.
8. The method of claim 1, further comprising:
and repeating the steps of taking out the carrier after the infiltration is finished, drying the carrier, and forming the graphene film on the surface of the carrier, so as to form a multilayer graphene film on the carrier.
9. Graphene film coated on a support surface, which is prepared by the method of any one of claims 1 to 8.
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