CN110980708A - Method for preparing graphene nanosheet through stripping method - Google Patents
Method for preparing graphene nanosheet through stripping method Download PDFInfo
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- CN110980708A CN110980708A CN201911261391.1A CN201911261391A CN110980708A CN 110980708 A CN110980708 A CN 110980708A CN 201911261391 A CN201911261391 A CN 201911261391A CN 110980708 A CN110980708 A CN 110980708A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01B2204/22—Electronic properties
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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
- C01B2204/32—Size or surface area
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Abstract
The invention belongs to the technical field of graphene, and particularly relates to a method for preparing graphene nanosheets by a stripping method. The invention can realize the regulation and control of the graphene sheet structure and the number of layers by regulating the proportion of the ionic liquid and the water in the ionic liquid aqueous solution and the magnitude of the external voltage, can control the functionalized density and has high yield; the technology has the advantages of low consumption, low cost, high yield, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of graphene, and particularly relates to a method for preparing graphene nanosheets by a stripping method.
Background
The existing preparation methods of graphene mainly comprise a chemical reduction oxidation graphite method, a vapor deposition method, an ultrasonic dispersion stripping method, an electrochemical method, a SiC epitaxial growth method, an arc discharge method, a template method and the like, and graphene with different shapes, sizes and structures can be prepared by using the methods. However, the development of more practical applications of graphene still needs to realize large-scale, environment-friendly and simple processes, and high-quality graphene materials with regular structures, controllable thickness and controllable size can be repeatedly prepared.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene nano material, which is simple in process, environment-friendly, low in cost and efficient.
The electrochemical-assisted stripping graphene nanosheet layer material is simple in preparation process and easy to build required instruments and equipment. The graphene nano-sheet material is prepared in the ionic liquid aqueous solution by being assisted with external voltage stripping, so that a green, simple and efficient preparation method is provided for the preparation of the graphene nano-sheet material.
In order to solve the problems, the technical scheme of the invention is as follows:
a method for preparing graphene nanosheets by a stripping method comprises the steps of taking a graphite rod as a raw material, taking an ionic liquid aqueous solution as an electrolyte and a modifier, and stripping a graphene bar under the action of an external voltage to obtain a functionalized graphene nanosheet layer.
Specifically, the method comprises the following steps:
1) preparation of an ionic liquid aqueous solution: adding a certain amount of ionic liquid into deionized water, and stirring the solution by using a magneton stirrer or mechanical stirring until a uniform solution is formed;
the ionic liquid used is various, and the ionic liquid with certain water solubility can be used as a solute.
2) The two high-purity graphite rods are respectively used as a cathode and an anode, the purity of the graphite rods is about 99.9 percent, the graphite rods are vertically inserted into the ionic liquid aqueous solution in the step 1), and the two graphite rods are kept insulated and the distance is constant; connecting two graphite rods to the positive and negative poles of power source separately with wires and setting the working voltage within 20V;
the structure, performance and yield of the graphene can be effectively controlled by regulating and controlling the concentration of the ionic liquid aqueous solution and the magnitude of the applied voltage.
3) After the step 2) is finished, collecting the black solution in the stripped container, and collecting the precipitate after centrifugation; centrifuging and cleaning the obtained precipitate by an organic reagent and water, and removing a small amount of residual ionic liquid; the cleaning solvent is one of ethanol, ethyl acetate and deionized water.
Graphene nanosheet layers and quantum dot slurry with different layers can be obtained by regulating and controlling the centrifugation rate and time.
4) After the step 3) is finished, obtaining a cleaned centrifugal product, removing residual moisture or organic reagent by using an air-blast drying oven, a vacuum drying oven or a freeze drying oven, thereby obtaining graphene nano-sheet layers with different layers.
The graphene nanosheet layer can be prepared in an environment-friendly and efficient manner by adopting the graphite rod as the raw material, taking the electrolyte and the modifier as the ionic liquid aqueous solution and assisting a direct current power supply or a direct current pulse power supply. Graphene is a graphite structure with a single atomic layer, in-plane carbon atoms hybridized by sp2 orbitals are combined in a covalent bond mode and are in a regular hexagon shape, and layers interact with each other by van der waals force, so that graphene is the thinnest crystal material in the world at present and is the material with the best conductivity at present.
The graphene has an ultrathin lamellar structure and excellent mechanical property and self-lubricating property, so that the graphene has a very low friction coefficient and can enter a friction interface more easily, and the graphene can be used as a nano lubricating material or a lubricating additive to improve the strong friction behavior of a workpiece in actual working conditions. Carbon atoms on the surface of the graphene mutually form a large pi bond, so that the electrochemical performance of the graphene is excellent, and the electron transfer rate at room temperature can reach 2 x 105cm 2/(V.s), so that the graphene has wide application in the electrochemical field.
In particular to a preparation method for preparing a graphene nanosheet layer material by using a green solvent ionic liquid as an electrolyte and applying a certain working voltage to a graphite rod for liquid-phase stripping. The technology can be used for efficiently preparing the functionalized solid nano material, and solves the problems of low yield, pollution and difficult structure control, thereby providing material and technical guarantee for preparing the composite material reinforced by the solid nano material, such as graphene lubricating grease, graphene batteries, graphene liquid crystal materials, graphene composite materials and the like.
The invention can realize the regulation and control of the graphene sheet structure and the number of layers by regulating the proportion of the ionic liquid and the water in the ionic liquid aqueous solution and the magnitude of the external voltage, can control the functionalized density and has high yield; the technology not only realizes high-density in-situ modification in the preparation process of the graphene nanosheet layer by the aid of the ionic liquid aqueous solution, can regulate and control the physical and chemical properties of the graphene nanosheet layer, but also can obtain graphene quantum dots, single-layer/few-layer graphene and multi-layer graphene by controlling the centrifugal rate, and meets the structure and performance requirements of different fields; in addition, the ionic liquid aqueous solution can be recycled, and under the assistance of low external voltage (less than or equal to 20V), the preparation process is energy-saving and environment-friendly and has high yield, so that two problems in the process of preparing the nano material are successfully solved. Therefore, the technology has the advantages of low consumption, low cost, high yield, environmental protection and the like, accords with the great trend of green, environmental protection and high-efficiency preparation advocated in recent years, not only realizes the large-scale preparation of the graphene nanosheet layer, but also solves the two bottleneck problems of limiting the wide application and the structure regulation of the graphene, and can widen the new chapter of the application of the graphene with excellent performance in more fields by using the method for modifying the graphene nanosheet in situ through the physical and chemical adsorption effects of the ionic liquid, wherein the method is simple, effective and easy to operate.
Claims (4)
1. The method for preparing the graphene nanosheet by the stripping method is characterized by comprising the following steps: the method comprises the steps of taking a graphite rod as a raw material, taking an ionic liquid aqueous solution as an electrolyte and a modifier, and peeling off a graphene bar under the action of an external voltage to obtain a functionalized graphene nanosheet layer.
2. A method for preparing graphene nanoplatelets according to the exfoliation method of claim 1, wherein: the method comprises the following steps:
1) preparation of an ionic liquid aqueous solution: adding a certain amount of ionic liquid into deionized water, and stirring the solution by using a magneton stirrer or mechanical stirring until a uniform solution is formed;
2) two high-purity graphite rods are respectively used as a cathode and an anode and are vertically inserted into the ionic liquid aqueous solution in the step 1), and the two graphite rods are kept insulated and have a constant distance; connecting two graphite rods to the positive and negative poles of power source separately with wires and setting the working voltage within 20V;
3) after the step 2) is finished, collecting the black solution in the stripped container, and collecting the precipitate after centrifugation; centrifuging and cleaning the obtained precipitate by an organic reagent and water, and removing a small amount of residual ionic liquid;
4) after the step 3) is finished, obtaining a cleaned centrifugal product, removing residual moisture or organic reagent by using an air-blast drying oven, a vacuum drying oven or a freeze drying oven, thereby obtaining graphene nano-sheet layers with different layers.
3. The method for producing graphene nanoplatelets according to the exfoliation method of claim 2, wherein: the ionic liquid in the step 1) is water-soluble ionic liquid.
4. The method for producing graphene nanoplatelets according to the exfoliation method of claim 2, wherein: the graphene nanosheet layer slurry and the quantum dot slurry with different layers are obtained by regulating the concentration of the ionic liquid aqueous solution, regulating the centrifugal rate and time and regulating the voltage.
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| CN201911261391.1A CN110980708A (en) | 2019-12-11 | 2019-12-11 | Method for preparing graphene nanosheet through stripping method |
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| CN201911261391.1A CN110980708A (en) | 2019-12-11 | 2019-12-11 | Method for preparing graphene nanosheet through stripping method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408370A (en) * | 2020-12-11 | 2021-02-26 | 中国科学院兰州化学物理研究所 | Preparation method of graphene additive for industrial lubricating oil |
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- 2019-12-11 CN CN201911261391.1A patent/CN110980708A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408370A (en) * | 2020-12-11 | 2021-02-26 | 中国科学院兰州化学物理研究所 | Preparation method of graphene additive for industrial lubricating oil |
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