CN109970047B - Method for preparing graphene quantum dots from carbon nanohorns - Google Patents
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Abstract
The invention discloses a method for preparing graphene quantum dots from carbon nanohorns, and belongs to the technical field of preparation of carbon nanomaterials. The method adopts a direct current arc method to prepare the nitrogen-doped carbon nanohorn: using graphite rods as the anode and the cathode of an electric arc, vertically placing the cathode and the anode, filling buffer gas and starting the electric arc after the electric arc furnace is vacuumized, and collecting sediment on the inner wall of a reaction cavity after the reaction is finished to obtain nitrogen-doped carbon nanohorns; and placing the nitrogen-doped carbon nanohorn into a tube furnace, calcining at a set atmosphere and temperature, and collecting a product, namely the graphene quantum dot. Judging that the calcined product is a graphene quantum dot by TEM and the size of the graphene quantum dot is 5-15 nm; the method adopts a direct current arc method to prepare the nitrogen-doped carbon nanohorn, converts the nitrogen-doped carbon nanohorn into the graphene quantum dot, has the advantages of safety, reliability, low cost and simple operation process, and develops a new idea for the preparation of the graphene quantum dot.
Description
Technical Field
The invention discloses a method for preparing graphene quantum dots from carbon nanohorns, and belongs to the field of preparation of carbon nanomaterials.
Background
In recent years, graphene receives increasing attention due to unique properties such as a large specific surface area, high carrier mobility, excellent mechanical flexibility, good thermal/chemical stability, and environmentally friendly features. Compared with two-dimensional Graphene Nano Sheets (GNSs) and one-dimensional Graphene Nanoribbons (GNRs), zero-dimensional Graphene Quantum Dots (GQDs) show stronger quantum confinement effect and boundary effect due to the size of the particles below 10 nm. At present, the graphene quantum dots contain (1) no high-toxicity metal elements, and are environment-friendly quantum dot materials; (2) stable structure, strong acid, strong alkali and photo corrosion resistance; (3) the band gap width range is adjustable; (4) surface functionalization is easy to achieve (5) properties of thinness to one single atom, chemical stability, etc. Therefore, the method has more attractive application prospect in many fields such as solar photoelectric devices, biomedicine, light-emitting diodes, sensors and the like.
Although GQDs have recently become a focus of scientists in various fields and their preparation is still in the beginning, the synthesis of carbon nanocrystals (including carbon nanotubes, graphene, nanocarbons, nanocarbon dots, collectively referred to as carbon dots) can be traced back to a longer time ago. At present, there are two methods for preparing GQDs with controllable properties, namely, top-down method and white-down method and top-up method. The top-down method refers to cutting large-sized graphene sheets into small-sized GQDs by a physical or chemical method, and comprises a hydrothermal method, an electrochemical method, a chemical carbon fiber stripping method and the like; the bottom-up method is to prepare GQDs from small molecules as precursors through a series of chemical reactions, mainly including solution chemical method, ultrasonic wave and microwave method.
However, there is still a long way to prepare high-yield and high-quality GQDs. The above-mentioned preparation methods all have certain defects, for example, the top-down method has relatively simple steps and high yield, but cannot realize precise control of the morphology and size of the GQDs. Most of the bottom-up methods have stronger controllability, but the steps are complicated and the operation is troublesome. Therefore, the method is simple in process, large-scale preparation of the graphene quantum dots is achieved, and the method is very important for promoting further research of graphene quantum. According to the invention, the nitrogen-doped graphene can be efficiently prepared by adopting a direct current arc method in a nitrogen-containing atmosphere, which is a key for converting carbon nanohorns into graphene quantum dots through high-temperature calcination, so that the technical problem of efficiently preparing the graphene quantum dots with a simple process can be solved.
Disclosure of Invention
The invention aims to provide a method for preparing graphene quantum dots from carbon nanohorns, which can be used for efficiently and simply preparing the graphene quantum dots, and specifically comprises the following steps:
(1) preparing nitrogen-doped carbon nanohorns by a direct-current arc method: and (3) using graphite rods as the anode and the cathode of the electric arc, vertically placing the cathode and the anode, filling buffer gas and starting the electric arc after the electric arc furnace is vacuumized, and collecting sediment on the inner wall of the reaction cavity after the reaction is finished, namely the nitrogen-doped carbon nanohorn.
(2) And (2) putting the nitrogen-doped carbon nanohorn prepared in the step (1) into a tube furnace, calcining at a set atmosphere and temperature, and collecting a product, namely the graphene quantum dot.
Preferably, the conditions for preparing the nitrogen-doped carbon nanohorns in the step (1) of the present invention are as follows: the diameter of the electrode graphite rod is 10-30 mm, the distance between two electrodes is 1-3 mm, the arc discharge current is 100-250A, the arc discharge time is 5-30 min, and the pressure of buffer gas is 40-80 KPa.
Preferably, the buffer gas in step (1) of the present invention is nitrogen.
Preferably, the calcining atmosphere in step (2) of the present invention is one of air and oxygen or a mixture of two gases.
Preferably, in the step (2) of the invention, the calcination temperature is 600-800 ℃, and the calcination time is 30-240 min.
The invention has the beneficial effects that:
(1) the method adopts a direct current arc method to prepare the carbon nanohorn, and the prepared carbon nanohorn is calcined to prepare the graphene quantum dot, so that the method has the advantages of simple equipment, simple process, low production cost, high production efficiency, greenness and no pollution.
(2) According to the nitrogen-doped carbon nanohorn prepared by the invention, a transmission electron microscope is used for obtaining a carbon nanohorn monomer with the diameter of 2-5 nm, the carbon nanohorn monomer is aggregated into a spherical aggregate with the diameter of 50-100 nm, and a calcined product is judged to be graphene quantum dots with the size of 5-15 nm through TEM.
(3) Compared with other methods for preparing the graphene quantum dots, the method provided by the invention can be completed in one step, the conditions are controllable, the steps are simple, and the like, and the prepared graphene quantum dots have the advantages of high purity, uniform structure size, uniform particle size distribution and excellent fluorescence characteristics.
Drawings
Fig. 1 is a transmission electron microscope photograph of nitrogen-doped carbon nanohorns in example 1;
fig. 2 is an X-ray photoelectron spectrum of nitrogen-doped carbon nanohorns in example 1;
fig. 3 is a transmission electron microscope of the graphene quantum dots in example 1;
fig. 4 is a transmission electron microscope of the graphene quantum dots in example 2;
fig. 5 is a transmission electron microscope of the graphene quantum dots in example 3;
fig. 6 is a transmission electron microscope of the graphene quantum dots in example 4;
fig. 7 is a transmission electron microscope of the graphene quantum dots in example 5.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, but the scope of the invention is not limited thereto.
Example 1
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And (3) putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 240min at 600 ℃ in an air atmosphere, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
The transmission electron microscope image of the carbon nanohorn prepared in this example is shown in fig. 1, from which it can be seen that a 'dahlia' -shaped carbon nanohorn is prepared; an X-ray photoelectron spectrum is shown in FIG. 2, and nitrogen elements doped in the prepared carbon nanohorn can be seen from the graph; the single particles have a diameter of 2-5 nm and are aggregated into spherical aggregates having a diameter of 30-100 nm.
A transmission electron microscope image of the graphene quantum dots is shown in fig. 3, and the size of the obtained graphene quantum dots is 5-15 nm, and the graphene quantum dots are free of impurities and have a good monodisperse structure; meanwhile, the graphene quantum dots prepared by the method have a strong fluorescence effect.
Example 2
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 30 min at 800 ℃ in air atmosphere, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
A transmission electron microscope image of the graphene quantum dot prepared by the embodiment is shown in fig. 4, and it can be seen from the image that the size of the obtained graphene quantum dot is 5-15 nm, no impurity is generated, and the graphene quantum dot has a good monodisperse structure, and meanwhile, the graphene quantum dot prepared by the method has a strong fluorescence effect.
Example 3
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 90 min at 700 ℃ in air atmosphere, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
A transmission electron microscope image of the graphene quantum dot prepared by the embodiment is shown in fig. 5, and it can be seen from the image that the size of the obtained graphene quantum dot is 5-15 nm, no impurity is generated, and the graphene quantum dot has a good monodisperse structure, and meanwhile, the graphene quantum dot prepared by the method has a strong fluorescence effect.
Example 4
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 120 min at 650 ℃ in an oxygen atmosphere, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
A transmission electron microscope image of the graphene quantum dot prepared in this embodiment is shown in fig. 6, and it can be seen from the image that the size of the obtained graphene quantum dot is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 5
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 120 min at 700 ℃ in a mixed atmosphere of oxygen and air, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
A transmission electron microscope image of the graphene quantum dot prepared in this embodiment is shown in fig. 7, and it can be seen from the image that the size of the obtained graphene quantum dot is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 6
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 60 min at 750 ℃ in a mixed atmosphere of oxygen and air, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
The size of the graphene quantum dot prepared by the embodiment is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 7
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 200 min at 650 ℃ in a mixed atmosphere of oxygen and air, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
The size of the graphene quantum dot prepared by the embodiment is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 8
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And putting the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 100 min at 800 ℃ in a mixed atmosphere of oxygen and air, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature.
The size of the graphene quantum dot prepared by the embodiment is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 9
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and the cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is filled in and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) And placing the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 30 min at 800 ℃ in a mixed atmosphere of oxygen and air, and collecting a product which is the graphene quantum dot when the temperature is cooled to room temperature.
The size of the graphene quantum dot prepared by the embodiment is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Example 10
A method for preparing graphene quantum dots from carbon nanohorns specifically comprises the following steps:
(1) graphite rods are used as the anode and cathode of the electric arc, the diameter of each graphite rod is 10mm, the distance between the anode and the cathode is 1mm, the anode and the cathode are vertically placed, after the electric arc furnace is pumped to the vacuum degree of 3Pa, the direct current electric arc discharge current is 200A, 70 KPa nitrogen is charged and the electric arc is started, and after 5min of discharge, the sediment on the inner wall of the reaction cavity is collected, namely the nitrogen-doped carbon nanohorn.
(2) Placing the prepared nitrogen-doped carbon nanohorn into a tube furnace, calcining for 60 min at 700 ℃ in air atmosphere, and collecting the obtained product, namely the graphene quantum dot, when the temperature is cooled to room temperature; the size of the graphene quantum dot prepared by the embodiment is 5-15 nm, and the graphene quantum dot is free of impurities and has a good monodisperse structure.
Claims (2)
1. A method for preparing graphene quantum dots from carbon nanohorns is characterized by specifically comprising the following steps of:
(1) preparing nitrogen-doped carbon nanohorns by a direct-current arc method: using graphite rods as the anode and the cathode of an electric arc, vertically placing the cathode and the anode, filling buffer gas and starting the electric arc after the electric arc furnace is vacuumized, and collecting sediment on the inner wall of a reaction cavity after the reaction is finished, namely the nitrogen-doped carbon nanohorn;
(2) putting the nitrogen-doped carbon nanohorn prepared in the step (1) into a tube furnace, calcining at a set atmosphere and temperature, and collecting a product, namely the graphene quantum dot; wherein the calcination temperature is 600-800 ℃, and the size of the graphene quantum dots is 5-15 nm;
the diameter of the electrode graphite rod is 10-30 mm, the distance between two electrodes is 1-3 mm, the arc discharge current is 100-250A, the arc discharge time is 5-30 min, and the pressure of buffer gas nitrogen is 40-80 kPa;
in the step (1), the buffer gas is nitrogen;
the calcining atmosphere is one of air and oxygen or the mixture of the two gases.
2. The method of preparing graphene quantum dots from carbon nanohorns as claimed in claim 1, wherein: the calcination time is 30-240 min.
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