CN110510604B - Graphene/boron nitride layered heterostructure and preparation method thereof - Google Patents
Graphene/boron nitride layered heterostructure and preparation method thereof Download PDFInfo
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- CN110510604B CN110510604B CN201910857578.1A CN201910857578A CN110510604B CN 110510604 B CN110510604 B CN 110510604B CN 201910857578 A CN201910857578 A CN 201910857578A CN 110510604 B CN110510604 B CN 110510604B
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Abstract
The invention belongs to the field of inorganic nano materials, and particularly relates to a graphene/boron nitride layered heterostructure and a preparation method thereof. According to the composite heterostructure provided by the scheme, the surface of graphene is covered by boron nitride, and the transverse length is 30-80 mu m. The method comprises the following steps: sequentially adding a dispersing agent and graphene into deionized water, processing to form a stable dispersion liquid, adding boron oxide, stirring at a constant temperature to be thick slurry, coating the slurry on the surface of a corundum boat, and drying in vacuum to obtain a precursor; and placing the material in a vacuum tube furnace, continuously heating the material to a certain temperature in an argon atmosphere, introducing ammonia gas to react to obtain a primary product, and treating the primary product to obtain the layered heterostructure material. The method has the advantages of simple process, no need of any metal catalyst, high material purity and good crystallinity, integrates the excellent performances of the graphene and the boron nitride, and provides a technical scheme for the industrial production of the two-dimensional material.
Description
Technical Field
The invention relates to the technical field of two-dimensional nano material preparation, in particular to a graphene/boron nitride layered heterostructure and a preparation method thereof.
Background
In recent years, with the successful preparation of two-dimensional nanomaterials such as graphene and the like and the continuous discovery of excellent performances in various aspects thereof, layered nanomaterials are gradually becoming hot spots of research. Among these materials, graphene and two-dimensional boron nitride nanostructures hold a significant position.
Graphene is a typical two-dimensional material, atoms of the graphene are combined with each other to form a honeycomb-shaped lattice of a monoatomic layer, the graphene has extremely high electron mobility, so that the graphene has wide potential application value in electronic devices, strong in-layer interaction, good mechanical property, high conductivity, high thermal conductivity and other advantages. The unique properties of graphene have also led to interest in layered materials of graphene-like structure. The two-dimensional hexagonal boron nitride nanosheet is similar to graphene in structure, adjacent atoms share the same number of electrons, and the lamellar layers are combined by Van der Waals force, so that the two-dimensional hexagonal boron nitride nanosheet has the structural characteristics and physical properties similar to those of graphene, such as high strength, high heat conductivity, high temperature resistance and the like, and also has the excellent properties of oxidation resistance, wide band gap, low thermal expansion coefficient, high chemical stability, neutron radiation shielding, super hydrophobicity, piezoelectric property, good biocompatibility and the like. Therefore, the hexagonal boron nitride nanosheet gradually occupies the final position in the fields of high-strength functional composite materials, biomedicine and the like, and has a wide application prospect. The graphene and the boron nitride nanometer material are perfectly combined, and the enhancement and the complementation of the characteristics of the graphene and the boron nitride nanometer material are utilized, so that the gate of more application fields, such as heat conduction, digital switches and the like, can be opened, and the application has greater practical advantages. Therefore, the controllable preparation and the mass production of the graphene/boron nitride composite material become an important research direction of the nanometer material science.
In the existing technical scheme, graphene and boron nitride are generally prepared step by step and then transferred to the surface of a corresponding substrate to realize the compounding of the graphene and the boron nitride, and a solvent or a transfer agent used in the transfer process is very easy to cause the pollution of an interface of the graphene and the boron nitride, so that the electrical and optical properties of the composite material are influenced. In some technical schemes, melamine which is easy to generate highly toxic cyanide through high thermal decomposition is added into the precursor, the preparation process is complex and difficult to control, and certain harm is caused to the environment and operators. In summary, a simple, effective and environment-friendly preparation method is sought to obtain a graphene/boron nitride heterostructure on the premise of maximally retaining the respective excellent properties of graphene and boron nitride, which is a critical technical problem to be solved urgently at present.
Disclosure of Invention
In view of this, the present invention aims to overcome the defects existing in the prior art, and provides a graphene/boron nitride layered heterostructure and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a graphene/boron nitride layered heterostructure, which is formed by covering graphene with two-dimensional layered boron nitride to form a graphene/boron nitride multilayer composite heterostructure with atomic-scale thickness.
Preferably, the lateral length of the graphene/boron nitride multilayer composite heterostructure is 50-70 μm.
The invention provides a preparation method of the graphene/boron nitride layered heterostructure, which comprises the following steps:
(1) Preparing a precursor: sequentially adding a dispersing agent and graphene into deionized water, carrying out ultrasonic magnetic stirring treatment to form a stable dispersion liquid, adding boron oxide, stirring at a constant temperature to form a thick slurry, coating the slurry on the surface of a corundum boat, and carrying out vacuum drying to obtain a precursor;
(2) Preparing and purifying a graphene/boron nitride layered heterostructure: and (2) placing the precursor obtained in the step (1) in a vacuum tube furnace, continuously heating to a certain temperature in an argon atmosphere, introducing ammonia gas for reaction, naturally cooling to room temperature to obtain a primary product, and treating to obtain the graphene/boron nitride layered heterostructure.
Preferably, the dispersant in the step (1) is sodium dodecyl sulfate, and the concentration of the dispersant is 1-2 mg/ml.
Preferably, the mass ratio of the graphene to the dispersant in the step (1) is 1:2 to 4.
Preferably, the time of the magnetic stirring in the step (1) is 12 to 24 hours.
Preferably, the ultrasonic treatment time in the step (1) is 3-10 h.
Preferably, the mass ratio of graphene to boron oxide in the step (1) is 1:18.5 to 50.
Preferably, the specified temperature of the magnetic stirring in the step (1) is 80 ℃.
Preferably, in the step (1), the drying temperature is 60 ℃ and the drying time is 12h.
Preferably, the temperature of the tubular furnace in the step (2) is increased to 800-1300 ℃ at the heating rate of 5 ℃/min, and the reaction time is 2-6 h.
Preferably, the introducing rate of the argon in the step (2) is 200-300 ml/min, and the introducing rate of the ammonia gas is 20-80 ml/min.
Preferably, the treatment of the preliminary product of step (2) is: washing the product with deionized water at 80 ℃ for 3-5 times until the pH value is 7, and drying the obtained solid powder in a vacuum drying oven at 60 ℃ for 12 hours.
Compared with the prior art, the invention has the beneficial effects that: (1) According to the technical scheme provided by the invention, a single-layer or multi-layer two-dimensional layered boron nitride nanosheet can be directly and stably covered on the surface of the graphene thin layer to obtain the graphene/boron nitride layered heterostructure with the atomic-scale thickness, so that damages in the conventional graphene transfer process and surface and interface pollution caused by a transfer agent or a solvent are avoided. (2) According to the preparation method, the mixture of graphene and boron oxide is used as a precursor, sodium dodecyl sulfate is used as a dispersing agent, argon is used as a carrier gas, ammonia is used as a reaction gas, the preparation method is simple, a high-pressure environment is not needed, the requirement on equipment is low, and industrialization is easy to realize; the used chemical reaction reagent is cheap and easy to obtain, and both the precursor medicine and the later product are environment-friendly. (3) The graphene/boron nitride layered heterostructure with atomic-level thickness prepared by the method has high stability, excellent physicochemical characteristics and good repeatability, and has a wide application prospect in the field of two-dimensional functional materials.
Drawings
Fig. 1 is a raman spectrum of the graphene/boron nitride layered heterostructure prepared in example 1.
Fig. 2 is a transmission electron microscope picture of the graphene/boron nitride layered heterostructure prepared in example 1.
Fig. 3 is a transmission electron microscope high resolution image of the graphene/boron nitride layered heterostructure prepared in example 1.
Fig. 4 is a transmission electron microscope high resolution image of the graphene/boron nitride layered heterostructure prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to these examples.
Example 1
Weighing 20mg of sodium dodecyl sulfate, and dissolving the sodium dodecyl sulfate in 10ml of deionized water to form a solution for later use; weighing 10mg of graphene, adding the graphene into the solution, magnetically stirring for 12h, and then performing ultrasonic treatment for 3h to form a stable graphene dispersion liquid; then 230mg of boron oxide is added into the dispersion liquid at the temperature of 80 ℃, and is uniformly coated on the surface of the corundum boat after being magnetically stirred at constant temperature until thick slurry is formed, and is dried for 12 hours at the temperature of 60 ℃ for later use; and (3) placing the dried corundum boat in a tubular furnace, introducing 250ml/min argon gas for protection, heating to 1200 ℃ at the heating rate of 5 ℃/min, introducing 50ml/min ammonia gas for heat preservation for 3h, taking out the reacted substance, washing the reacted substance with hot water at 80 ℃ until the pH value is close to 7, and filtering and drying the reacted substance to obtain the graphene/boron nitride layered heterostructure.
Fig. 1 is a raman spectrogram of the prepared graphene/boron nitride layered heterostructure, a typical raman peak position of boron nitride appears at a position around 1345, and the typical raman peak position is superposed with a graphene D peak so that the peak value at the position is obviously enhanced compared with the typical graphene peak value. In addition, the G peak position of the graphene and the shortened and widened 2D characteristic peak of the graphene are also provided. The product is graphene boron nitride composite as shown in fig. 1. Fig. 2 is a transmission electron microscope image of the prepared graphene/boron nitride layered heterostructure reflecting the layered morphology of the prepared product.
Example 2
In example 1, the reaction temperature was changed from 1200 ℃ to 1000 ℃, and other steps were the same as in example 1, and a graphene/boron nitride layered heterostructure similar to that in example 1 was obtained. Fig. 3 is a transmission electron microscope high resolution image of the prepared graphene/boron nitride layered heterostructure, which can clearly see the respective lattice distribution and the obvious layered structure of the two-phase product.
Example 3
In example 1, the mass of graphene and boron oxide were increased to 20mg and 460mg, respectively, and other steps are the same as in example 1, and a graphene/boron nitride layered heterostructure similar to that in example 1 can still be obtained. FIG. 4 is a high resolution image of a transmission electron microscope of the prepared graphene/boron nitride layered heterostructure, in which the layered overlapping morphology and the apparent lattice distribution can be seen.
Example 4
In example 1, the reaction time was changed from 3h to 5h, and other steps were the same as in example 1, to obtain a graphene/boron nitride layered heterostructure similar to that in example 1.
Example 5
In example 1, the flow rate of argon gas was changed to 300ml/min, the flow rate of ammonia gas was changed to 30ml/min, and other steps were the same as in example 1, to obtain a graphene/boron nitride layered heterostructure.
Example 6
In example 1, the ultrasonic time is changed from 3h to 6h, and other steps are the same as in example 1, so that the graphene/boron nitride layered heterostructure similar to that in example 1 can be obtained.
Comparative example 1
In example 1, the mass of boron oxide alone was increased by 1000mg, the other conditions were kept unchanged, the procedure was the same as in example 1, and the graphene/boron nitride layered heterostructure described above could not be obtained.
Comparative example 2
In example 1, the ammonia flow rate was changed to 120ml/min, and other steps were the same as in example 1, and a graphene/boron nitride layered heterostructure could not be obtained.
Comparative example 3
In example 1, the reaction temperature was changed from 1200 ℃ to 1400 ℃, and other steps were the same as in example 1, and a graphene/boron nitride layered heterostructure could not be obtained.
Comparative example 4
In example 1, the reaction time was changed from 3h to 1h, and other steps were the same as in example 1, and a graphene/boron nitride layered heterostructure could not be obtained.
The invention provides a graphene/boron nitride layered heterostructure with atomic scale thickness and a preparation method thereof, and is not limited to the specific experimental operation described in the specification and the embodiment. Therefore, all equivalent changes/variations or changes in the sequence of the precursors, processes and principles described in the claims of the present invention should be included in the scope of the present invention.
Claims (6)
1. A preparation method of a graphene/boron nitride layered heterostructure is characterized in that the surface of graphene in the structure is covered by boron nitride to form a graphene/boron nitride multilayer composite heterostructure with atomic-scale thickness, and the transverse length is 30-80 μm; the method comprises the following steps:
(1) Preparing a precursor: sequentially adding a dispersing agent and graphene into deionized water, performing ultrasonic magnetic stirring treatment to form a stable dispersion liquid, adding boron oxide, stirring at a constant temperature to be thick slurry at a certain temperature, coating the mixture on the surface of a corundum boat, and performing vacuum drying to obtain a precursor;
(2) Preparing and purifying a graphene/boron nitride layered heterostructure: placing the corundum boat with the precursor obtained in the step (1) in a vacuum tube furnace, continuously heating to a certain temperature in an argon atmosphere, introducing ammonia gas for reaction, naturally cooling to room temperature to obtain a primary product, and treating to obtain a graphene/boron nitride layered heterostructure;
the mass ratio of the graphene to the boron oxide in the step (1) is 1: 50-100 ℃, wherein the specified temperature of the magnetic stirring after adding the boron oxide is 80-100 ℃;
the tubular furnace in the step (2) is heated to 800-1300 ℃ at the heating rate of 5 ℃/min, and the reaction time is 1.5-6 h;
the introducing speed of the argon in the step (2) is 150-300 ml/min, and the introducing speed of the ammonia is 20-100 ml/min.
2. The method for preparing a graphene/boron nitride layered heterostructure according to claim 1, wherein the dispersant in the step (1) is sodium dodecyl sulfate, the concentration of the dispersant is 1-2 mg/ml, and the mass ratio of graphene to the dispersant is 1:0.5 to 2.
3. The method for preparing the graphene/boron nitride layered heterostructure according to claim 1, wherein the magnetic stirring time in the step (1) is 12-24 hours, and the ultrasonic treatment time is 1-10 hours.
4. The method for preparing a graphene/boron nitride layered heterostructure according to claim 1, wherein the temperature of vacuum drying in step (1) is 60 ℃ and the drying time is 12h.
5. The method for preparing a graphene/boron nitride layered heterostructure according to claim 1, wherein the preliminary product in step (2) is treated by: washing the product with deionized water at 80 deg.c for 3-5 times until pH is 7, and drying the solid powder in a vacuum drying oven at 60 deg.c for 12 hr.
6. Use of a material having a graphene/boron nitride layered heterostructure prepared by the method of any one of claims 1 to 5.
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