CN114604863A - Graphene preparation method and graphene - Google Patents
Graphene preparation method and graphene Download PDFInfo
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- CN114604863A CN114604863A CN202210328362.8A CN202210328362A CN114604863A CN 114604863 A CN114604863 A CN 114604863A CN 202210328362 A CN202210328362 A CN 202210328362A CN 114604863 A CN114604863 A CN 114604863A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The invention discloses a graphene preparation method and graphene, and the method comprises the following steps: placing the flake graphite and the salt particles in a roller device according to a certain mass ratio; starting the roller device, rolling for a first mixing time, adding the auxiliary agent, and then rolling for a second mixing time to fully contact the flake graphite, the salt particles and the auxiliary agent; and (3) dissolving the mixed substances in water, filtering out solid substances by adopting a negative pressure method, cleaning the solid substances, filtering after ultrasonic stripping, freeze-drying, and heating in a vacuum furnace at the high temperature of 3200 ℃ to remove impurities to obtain the graphene. The roller rotation mode ensures that only the salt grains, the crystalline flake graphite and the auxiliary agent are subjected to friction collision in the mixing process, so that the graphene is adsorbed on the surface of the salt grains without damaging the physical form, the complete physical and chemical properties of the graphene are reserved, the preparation method is simple and reliable, and the purity of the graphene is high.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a graphene preparation method and graphene.
Background
The graphene is sp2The hybridized and connected carbon atoms are tightly packed into a new material with a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the 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.
Common powder production methods of graphene are a mechanical stripping method, a redox method and a SiC epitaxial growth method, and in commercial markets, a chemical method is mostly adopted for extracting graphene. Since graphene is hexagonal in physical form, when a chemical method is used for extraction, the used chemical raw materials are corrosive, and damage to one or more corners of graphene can cause loss of physical properties and chemical properties of graphene, such as conductivity or heat conductivity. By adopting a conventional chemical method, such as using chemical reagents like aqua regia, the extracted graphene has the condition that some corner structures are corroded, so that the conductivity is lost, and the quality of the final graphene is influenced.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention aims to provide a graphene preparation method and graphene, so as to solve the problems that in the prior art, the physical form of graphene is easily damaged when the graphene is prepared, and the quality of the graphene is further influenced.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present application provides a graphene preparation method, including the following steps:
s10, placing the flake graphite and the salt particles in a roller device according to a certain mass ratio;
s20, starting the roller device, rolling for a first mixing time, adding the auxiliary agent, and then rolling for a second mixing time to fully contact the flake graphite, the salt particles and the auxiliary agent;
and S30, dissolving the mixed substances in water, filtering out solid substances by adopting a negative pressure method, cleaning the solid substances, filtering after ultrasonic stripping, carrying out freeze-drying treatment, and placing in a vacuum furnace to raise the temperature and remove impurities to obtain the graphene.
As a possible embodiment, after step S20, the method further includes step S21:
and pouring the mixture in the roller device into a rolling device, rolling and crushing the mixture, putting the mixture back into the roller device for rolling and mixing, repeating the steps for a certain number of times, and then entering the step S30.
As a possible example, in step S21, the mixture is placed back into the roller device from the rolling device, and then the auxiliary agent is added to perform rolling mixing.
As a possible example, in steps S20 and/or S21, a carbon material selected from one or more of activated carbon, carbon aerogel or carbon fiber is further added to the drum device.
As a possible example, the mass ratio of the flake graphite to the salt particles is 1: 10000-1: 1.
as a possible example, the mass ratio of the flake graphite to the carbon material is 1: 1000-2: 1.
as a possible embodiment, before proceeding to step S30, step S23 is also passed:
when the surface color of the salt particles is visually observed and the surface color changes from white to bright gray-black, the mixing is stopped, and the process proceeds to step S30.
As a possible example, the adjuvant is selected from one or more of epoxy resin, polyethylene glycol, polytetrafluoroethylene, polyvinylidene fluoride or 70% pure alcohol.
As a possible embodiment, the inner wall of the roller device is provided with a convex part, and a layer of friction film is attached to the inner wall, wherein the surface roughness of the friction film ranges from Ra50 to 100.
In a second aspect, an embodiment of the present application further provides graphene prepared by the graphene preparation method, wherein the graphene is seven layers or less of graphene with a purity of not less than 99.999%, and the thickness range is 1 to 4 nanometers.
Compared with the prior art, the invention at least comprises the following beneficial effects:
the utility model provides a graphene preparation method, mode through the roll mixing, realize abundant contact between salt grain and the scale graphite, in mixing process, except the auxiliary agent between salt grain and the scale graphite, there is not other external force effect part, only salt grain, the friction and collision between scale graphite and the auxiliary agent three are guaranteed to cylinder pivoted mode in mixing process, make graphite alkene adsorb on the salt grain surface under the condition of not destroying physical form, the complete physics of graphite alkene has been kept, chemical properties, the preparation method is simple and reliable, graphite alkene purity is high.
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
Fig. 1 is a schematic flow chart of a graphene preparation method according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a graphene preparation method according to another embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. 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.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, when it is described that a specific device is located between a first device and a second device, there may or may not be an intervening device between the specific device and the first device or the second device. When a particular device is described as being coupled to other devices, that particular device may be directly coupled to the other devices without intervening devices or may be directly coupled to the other devices with intervening devices.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In a first aspect, with reference to fig. 1, this embodiment provides a graphene preparation method, including the following steps:
s10, placing the flake graphite and the salt particles in a roller device according to a certain mass ratio;
s20, starting the roller device, rolling for a first mixing time, adding the auxiliary agent, and then rolling for a second mixing time to fully contact the flake graphite, the salt particles and the auxiliary agent;
and S30, dissolving the mixed substances in water, filtering out solid substances by adopting a negative pressure method, cleaning the solid substances, filtering after ultrasonic stripping, carrying out freeze-drying treatment, and placing in a vacuum furnace to raise the temperature and remove impurities to obtain the graphene.
It should be noted that, the salt grains in this embodiment are halogen salts, which are salts formed by halogen and metal elements, and under a certain temperature and humidity, the surfaces of the salt grains have viscosity, and the salt grains and the flake graphite having viscosity are placed into the roller device according to a certain mass ratio, and under rolling mixing of the roller device, the flake graphite and the salt grains are contacted sufficiently for a long time, and the flake graphite is adhered to the surfaces thereof layer by the salt grains, so as to achieve an effect of peeling off the flake graphite layer by layer. In the contact process, the drum device is equivalent to a drum of a washing machine, friction force is applied to the scale graphite and the salt grains in the drum device only through the drum wall, and no other external force action part exists, namely, no part such as stirring, grinding and the like directly applies pressure to the scale graphite and the salt grains, so that the graphene is adsorbed on the surface of the salt grains under the condition that the physical form is not damaged, and the complete physical and chemical properties of the graphene are reserved.
In order to improve the adhesion degree of salt grains and crystalline flake graphite, after rolling for a first mixing time, adding an auxiliary agent into the roller device, then rolling for a second mixing time, and utilizing the auxiliary agent to enable the crystalline flake graphite and the salt grains around the crystalline flake graphite to form an adhesive body so as to improve the peeling speed of the crystalline flake graphite.
After the crystalline flake graphite is fully stripped to the salt grains, the mixed substance is placed into water to be dissolved, the salt grains are dissolved in the water, graphene attached to the salt grains is separated from the salt grains in the water, the graphene floats on the upper layer of the water surface, solid substances are filtered out by using a negative pressure method, after 10-50 times of clear water cleaning, the ultrasonic stripping and filtering are carried out, the salt content in the substance is further reduced, and at the moment, the content of the salt grains and other impurities is lower than 5%.
At the moment, the filtered graphene is subjected to freeze-drying by a freeze dryer, and heat drying cannot be used here, so that the problem that the graphene is agglomerated into multilayer graphite is avoided, after freeze-drying, the graphene is placed in a heating container, the temperature is raised to 3200 ℃ in a vacuum furnace, and residual impurities, salt and the like are removed, because the graphene can resist the high temperature of more than 3200 ℃ in an oxygen-free environment; and finally, obtaining a graphene product and storing the graphene product.
In conjunction with fig. 2, in some embodiments, after step S20, step S21 is further included:
after the preliminary mixing is performed in the roller device, the mixture in the roller device is poured into a rolling device, the mixture is rolled and crushed, and then placed back into the roller device for rolling and mixing, and after repeating for a certain number of times, the process goes to step S30.
The step aims to solve the problem that salt grains are large in volume compared with flake graphite, so that the contact probability and the combination area of the salt grains and the flake graphite are improved, the salt grains are broken as much as possible through rolling, the surface area of the broken particles can be extended by multiple times, the particle size of the particles can be further reduced, the flake graphite can be easily adhered to the broken salt grains, a structural model similar to a noodle press is adopted in the rolling process, the rolling pressure degree of the structural model is gradually increased, the flake graphite can be adjusted to be in a planar state according to the force application change in the force application process, the salt grains with the large particle size can bear larger acting force, the damaged degree of the flake graphite is low under the support of the salt grains, and the complete physical and chemical properties of the salt grains can be guaranteed.
With the alternation of the rolling and the rolling crushing of the roller, after repeating for 50-200 times, the crystalline flake graphite, the salt particles and the auxiliary agent are fully contacted, and then the finally mixed substances are put into water for dissolving, and the step S30 is carried out.
Preferably, in step S21, the mixture is placed back into the roller device from the rolling device, and then the auxiliary agent is added to perform rolling mixing. The auxiliary agent is added in one step, but is added gradually while the two actions of rolling and crushing the roller are alternately carried out, more specifically, the auxiliary agent is added when the mixture is put into the roller device after being rolled, and the mixture is put into the roller device after being rolled and mixed, and is rolled and crushed in the rolling device, and the steps are continuously repeated. The advantage of doing so lies in, avoids adding too much auxiliary agent for scale graphite and salt grain form a large scale bulk form, is unfavorable for rolling the mixture, consequently through adding the auxiliary agent a small amount of times, more is favorable to the auxiliary agent to disperse in scale graphite and salt grain, forms a plurality of little local adherends on a large scale, is favorable to the successive layer of scale graphite to peel off.
In one embodiment, in step S20 and/or S21, a carbon material selected from one or more of activated carbon, carbon aerogel or carbon fiber is further added to the drum device, the auxiliary agent is responsible for forming the scale graphite, the salt particles and the carbon material into a binder body during the bonding and peeling process of the scale graphite and the salt particles, the scale graphite, the salt particles and the carbon material form a small-scale electric adsorption field in the relatively independent space, the scale graphite and the carbon material are contacted to form a composite material, the composite material forms a certain degree of electric adsorption effect during the contact friction process of the salt particles, and the scale graphite is sufficiently peeled off to the salt particles under the action of the adsorption force.
Preferably, after adding the carbon material, the mixture is dissolved in water, and a flocculant may be added to allow the carbon material to settle to the bottom of the water while the graphene is still floating on the surface of the water.
Preferably, the mass ratio of the crystalline flake graphite to the salt particles is 1: 10000-1: 1; the mass ratio of the scale graphite to the carbon material is 1: 1000-2: 1.
in some possible embodiments, one gram of crystalline flake graphite is matched with one kilogram of salt grains, so that sufficient contact between the crystalline flake graphite and the salt grains is ensured, and the stripping conversion efficiency is improved.
In the present embodiment, before proceeding to step S30, step S23 is also passed:
when the surface color of the salt particles is visually observed and the surface color changes from white to bright gray-black, the mixing is stopped, and the process proceeds to step S30.
The initial color of the salt particles is white, graphene is slowly attached to the salt particles after the salt particles are fully mixed, the surfaces of the salt particles become bright gray black, a visual method is needed because the transfer degree cannot be measured through equipment in the process, when the color transfer is not fast enough, rolling, adding an auxiliary agent and a carbon material are carried out, after roller mixing, whether the transfer is finished or not is judged through the visual method, if the transfer is not finished, the step of rolling and crushing is carried out, then rolling and visual inspection are carried out repeatedly, and the process is repeated.
In this embodiment, the auxiliary agent is selected from one or more of epoxy resin, polyethylene glycol, polytetrafluoroethylene, polyvinylidene fluoride or 70% purity alcohol.
In one embodiment, the inner wall of the roller device is provided with a convex part which can be integrally formed with the inner wall, presents a wave shape, a wave point shape, a protruding rib shape and the like and can improve the disturbance to the scale graphite and the salt particles in the rolling process, in addition, the inner wall is also attached with a layer of friction film, the friction film is arranged on the upper part of the convex part, namely, the friction film is directly contacted with the crystalline flake graphite and the salt particles, the surface roughness range of the friction film is Ra 50-100, that is, the surface of the friction film has fine grooves, the pitch of the grooves is 50 to 100 μm, the diameter of the salt particles is 25 to 100mm, after rolling and rolling, the salt grains are crushed into fine salt, the fine salt can be clamped in the groove of the friction film, a salt layer is formed on the inner cylinder wall, so that the contact area of the crystalline flake graphite and salt particles under marginal conditions is increased.
In a second aspect, an embodiment of the present application further provides graphene prepared by the graphene preparation method according to the above embodiment, the graphene is seven layers of graphene with a purity of not less than 99.999% and less, and has a thickness range of 1 to 4 nanometers.
Compared with the prior art, the embodiment provides a graphene preparation method and graphene, through the mode of rolling mixing, realize abundant contact between salt grain and the scale graphite, in the mixing process, except that the auxiliary agent between salt grain and the scale graphite, there is not other external force effect parts, the mode of cylinder rotation guarantees only the friction collision between salt grain, scale graphite and the auxiliary agent in the mixing process, make graphene adsorb on the salt grain surface under the condition of not destroying physical form, the complete physics of graphite alkene, chemical properties have been kept, the preparation method is simple and reliable, the graphite purity is high.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A graphene preparation method is characterized by comprising the following steps:
s10, placing the flake graphite and the salt particles in a roller device according to a certain mass ratio;
s20, starting the roller device, rolling for a first mixing time, adding the auxiliary agent, and then rolling for a second mixing time to fully contact the flake graphite, the salt particles and the auxiliary agent;
and S30, dissolving the mixed substances in water, filtering out solid substances by adopting a negative pressure method, cleaning the solid substances, filtering after ultrasonic stripping, carrying out freeze-drying treatment, and placing in a vacuum furnace to raise the temperature and remove impurities to obtain the graphene.
2. The method for preparing graphene according to claim 1, further comprising step S21 after step S20:
and pouring the mixture in the roller device into a rolling device, rolling and crushing the mixture, putting the mixture back into the roller device for rolling and mixing, repeating the steps for a certain number of times, and then entering the step S30.
3. The method of claim 2, wherein in step S21, the mixture is placed from the rolling device back into the roller device, and then the auxiliary agent is added to perform rolling mixing.
4. The method of claim 3, wherein a carbon material is further added to the roller device in steps S20 and/or S21, wherein the carbon material is selected from one or more of activated carbon, carbon aerogel or carbon fiber.
5. The method for preparing graphene according to claim 4, wherein the mass ratio of the crystalline flake graphite to the salt particles is 1: 10000-1: 1.
6. the method for preparing graphene according to claim 5, wherein the mass ratio of the scale graphite to the carbon material is 1: 1000-2: 1.
7. the method for preparing graphene according to claim 4, further comprising a step S23 before proceeding to step S30:
when the surface color of the salt particles is visually observed and the surface color changes from white to bright gray-black, the mixing is stopped, and the process proceeds to step S30.
8. The method for preparing graphene according to claim 7, wherein the auxiliary agent is one or more selected from epoxy resin, polyethylene glycol, polytetrafluoroethylene, polyvinylidene fluoride and 70% pure alcohol.
9. The graphene preparation method according to any one of claims 1 to 8, wherein a protrusion is arranged on an inner wall of the roller device, and a friction film is further attached to the inner wall, wherein the surface roughness of the friction film is Ra 50-100.
10. The graphene prepared by the graphene preparation method according to any one of claims 1 to 9, wherein the graphene is seven layers or less of graphene with a purity of not less than 99.999% and has a thickness in a range of 1 to 4 nm.
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