CN110040723B - Method for preparing graphene by using ion sputtering and laser composite technology - Google Patents
Method for preparing graphene by using ion sputtering and laser composite technology Download PDFInfo
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- CN110040723B CN110040723B CN201910343894.7A CN201910343894A CN110040723B CN 110040723 B CN110040723 B CN 110040723B CN 201910343894 A CN201910343894 A CN 201910343894A CN 110040723 B CN110040723 B CN 110040723B
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Abstract
A method for preparing graphene by using ion sputtering and laser composite technology comprises the following steps: (1) carrying out heat treatment on the nano carbon powder under a vacuum condition, and cooling the nano carbon powder to normal temperature along with a furnace to obtain heat-treated nano carbon powder; (2) placing the heat-treated nano carbon powder in an ion sputtering instrument as a carbon target; carrying out ion sputtering on the substrate to prepare a carbon film; (3) and (3) placing the substrate covered with the carbon film under a vacuum condition, and performing laser irradiation by using a laser emitting device, wherein the laser irradiation is divided into three stages of low-temperature irradiation, medium-temperature irradiation and high-temperature irradiation, and graphene is prepared on the surface of the substrate. The method has the advantages of high precision of the preparation process, good controllability, 100 percent of raw material utilization rate, no need of processing by-products, cleanness, environmental protection and no pollution.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a method for preparing graphene by utilizing an ion sputtering and laser composite technology.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb-lattice two-dimensional carbon nanomaterial; the graphene is one of the materials with the highest known strength, has good toughness and can be bent, has excellent optical, electrical and mechanical properties, and has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like.
Common powder production methods of graphene include a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method, and a film production method includes a chemical vapor deposition method and the like; the graphene material can be prepared by the methods, however, the problems of poor controllability, serious defects of the prepared material and the like still exist in the existing graphene preparation process.
Disclosure of Invention
The invention aims to provide a method for preparing graphene by using ion sputtering and laser compounding technologies.
The method of the invention comprises the following steps:
1. carrying out heat treatment on the nano carbon powder under a vacuum condition, wherein the heat treatment temperature is 1600-1700 ℃, the time is 1.5-2 h, and cooling to the normal temperature along with a furnace to obtain heat-treated nano carbon powder;
2. placing the heat-treated nano carbon powder in an ion sputtering instrument as a carbon target; placing the substrate in a vacuum chamber of an ion sputtering instrument; carrying out ion sputtering on the substrate by an ion sputtering instrument to prepare a carbon film on the surface of the substrate;
3. placing a substrate with a carbon film covered on the surface under a vacuum condition, and carrying out laser irradiation by a laser emitting device, wherein the laser irradiation is divided into three stages of low-temperature irradiation, medium-temperature irradiation and high-temperature irradiation, wherein the temperature of the substrate is controlled to be 500-600 ℃ during the low-temperature irradiation for at least 45min, the temperature of the substrate is controlled to be 1800-1900 ℃ during the medium-temperature irradiation for at least 45min, and the temperature of the substrate is controlled to be 2400-2550 ℃ during the high-temperature irradiation for at least 90 min; and preparing graphene on the surface of the substrate after laser irradiation is finished.
In the step 1, the particle size of the nano carbon powder is 8-20 nm.
In the step 1, the heat treatment equipment is a vacuum furnace, and the vacuum condition is 10-1～10-7mbar。
In the step 2, the vacuum condition is 0.1 to 1.0Pa when the ion sputtering is performed.
In the step 2, the substrate is made of molybdenum carbide and has a thickness of 3-5 mm.
In the step 2, the thickness of the carbon film is 10 to 300 nm.
The graphene prepared by the method is used for analyzing a product by adopting Raman spectroscopy and X-ray diffraction analysis technologies, and has a single-layer or multi-layer structure.
Compared with the prior art, the invention has the beneficial effects that: (1) the preparation process has high precision and good controllability, and can be used for preparing single-layer graphene and multi-layer graphene; (2) the process adaptability is strong to the product form adaptability, and the graphene powder and the graphene film can be prepared; (3) the utilization rate of the raw materials reaches 100%, by-products do not need to be treated, and the method is clean, environment-friendly and pollution-free.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing graphene by using an ion sputtering and laser composite technology according to the present invention.
Fig. 2 is a raman spectrum of graphene according to an embodiment of the present invention; in the figure, G is a characteristic peak of graphene, and the 2D peak is used to characterize the stacking mode of carbon atoms in the graphene sample.
Detailed Description
In the embodiment of the invention, when ion sputtering is carried out, the vacuum cavity is firstly vacuumized to 10 DEG-4～10-3And Pa, heating the substrate to 200-400 ℃, introducing argon and hydrogen as reaction gases to generate plasma, and continuously introducing argon until the substrate is cooled to the normal temperature after ion sputtering is finished.
In the embodiment of the invention, during ion sputtering, the flow rate of argon is 30-40 sccm, the flow rate of hydrogen is 10-15 sccm, the sputtering power is 200-250W, the pressure in the vacuum chamber is 0.1-1.0 Pa, and the sputtering time is 1-100 min.
The nano carbon powder adopted in the embodiment of the invention is a commercial product.
The molybdenum carbide substrate adopted in the embodiment of the invention is a commercial product.
The ion sputtering instrument adopted in the embodiment of the invention is a GVC-1000 type ion sputtering instrument of Micro Hezao.
In the embodiment of the invention, the dosage of the nano carbon powder is 5 g.
The present invention is further illustrated by the following specific examples.
Example 1
The flow is shown in figure 1, nanometer carbon powder with the particle size of 8nm is subjected to heat treatment under the vacuum condition of 10- 1mbar, heat treatment temperature of 1600 ℃, time of 90min, furnace cooling to normal temperature to obtain heat treatment nanometer carbon powder;
placing the heat-treated nano carbon powder in an ion sputtering instrument as a carbon target; placing the substrate in a vacuum chamber of an ion sputtering instrument; carrying out ion sputtering on the substrate by an ion sputtering instrument to prepare a carbon film on the surface of the substrate; the substrate is made of molybdenum carbide and has the thickness of 3 mm; the thickness of the carbon film is 16 nm;
placing the substrate with the carbon film covered on the surface under a vacuum condition, and performing laser irradiation by a laser emitting device, wherein the laser irradiation is divided into three stages of low-temperature irradiation, medium-temperature irradiation and high-temperature irradiation, wherein the temperature of the substrate is controlled to be 500 ℃ for 45min during the low-temperature irradiation, the temperature of the substrate is controlled to be 1800 ℃ for 45min during the medium-temperature irradiation, and the temperature of the substrate is controlled to be 2400 ℃ for 90min during the high-temperature irradiation; and preparing graphene on the surface of the substrate after laser irradiation is finished.
The product is analyzed by using Raman spectrum and X-ray diffraction analysis technology, the structure is double-layer, and the Raman spectrum is shown in figure 2.
Example 2
The method is the same as example 1, except that:
(1) the particle size of the nano carbon powder is 20 nm; vacuum condition of heat treatment is 10-7mbar, temperature of 1700 ℃, time of 2 h;
(2) the thickness of the substrate is 4 mm; the thickness of the carbon film is 60 nm;
(3) controlling the temperature of the substrate to be 600 ℃ for 50min during low-temperature irradiation, controlling the temperature of the substrate to be 1900 ℃ for 50min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2550 ℃ for 100min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is three layers.
Example 3
The method is the same as example 1, except that:
(1) the grain size of the nano carbon powder is 15 nm; vacuum condition of heat treatment is 10-2mbar, temperature 1650 deg.C, and time 100 min;
(2) the thickness of the substrate is 4 mm; the thickness of the carbon film is 48 nm;
(3) controlling the temperature of the substrate to be 550 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to be 1850 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2500 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is 3 layers.
Example 4
The method is the same as example 1, except that:
(1) the particle size of the nano carbon powder is 10 nm; vacuum condition for heat treatment is 10-3mbar, temperature 1650 deg.C, and time 120 min;
(2) the thickness of the substrate is 4 mm; the thickness of the carbon film is 70 nm;
(3) controlling the temperature of the substrate to be 580 ℃ during low-temperature irradiation for 50min, controlling the temperature of the substrate to be 1850 ℃ during medium-temperature irradiation for 50min, and controlling the temperature of the substrate to be 2500 ℃ during high-temperature irradiation for 100 min;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is 5 layers.
Example 5
The method is the same as example 1, except that:
(1) the grain size of the nano carbon powder is 15 nm; vacuum condition of heat treatment is 10-4mbar, temperature 1650 deg.C, and time 110 min;
(2) the thickness of the substrate is 4 mm; the thickness of the carbon film is 90 nm;
(3) controlling the temperature of the substrate to 590 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to 1900 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to 2550 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is 6 layers.
Example 6
The method is the same as example 1, except that:
(1) the grain size of the nano carbon powder is 15 nm; vacuum condition of heat treatment is 10-5mbar, temperature 1680 ℃, time 1.5 h;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 60 nm;
(3) controlling the temperature of the substrate to be 600 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to be 1890 ℃ for 50min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2520 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is 4 layers.
Example 7
The method is the same as example 1, except that:
(1) the particle size of the nano carbon powder is 20 nm; vacuum condition of heat treatment is 10-6mbar, temperature 1670 deg.C, time 100 min;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 230 nm;
(3) controlling the temperature of the substrate to be 600 ℃ for 50min during low-temperature irradiation, controlling the temperature of the substrate to be 1880 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2550 ℃ for 100min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is 11 layers.
Example 8
The method is the same as example 1, except that:
(1) the particle size of the nano carbon powder is 20 nm; vacuum condition of heat treatment is 10-6mbar, temperature 1600 deg.C, time 110 min;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 20 nm;
(3) controlling the temperature of the substrate to be 600 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to be 1850 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2550 ℃ for 100min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is a single layer.
Example 9
The method is the same as example 1, except that:
(1) the particle size of the nano carbon powder is 10 nm; vacuum condition of heat treatment is 10-7mbar, temperature 1600 ℃, time 1.5 h;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 12 nm;
(3) controlling the temperature of the substrate to 530 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to 1880 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to 2500 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is a single layer.
Example 10
The method is the same as example 1, except that:
(1) the grain size of the nano carbon powder is 15 nm; vacuum condition of heat treatment is 10-5mbar, temperature of 1610 ℃, time of 1.5 h;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 15 nm;
(3) controlling the temperature of the substrate to be 560 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to be 1830 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2480 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is a single layer.
Example 11
The method is the same as example 1, except that:
(1) the grain size of the nano carbon powder is 18 nm; vacuum condition for heat treatment is 10-7mbar, temperature 1660 ℃, time 1.5 h;
(2) the thickness of the substrate is 5 mm; the thickness of the carbon film is 20 nm;
(3) controlling the temperature of the substrate to be 510 ℃ for 45min during low-temperature irradiation, controlling the temperature of the substrate to be 1840 ℃ for 45min during medium-temperature irradiation, and controlling the temperature of the substrate to be 2550 ℃ for 90min during high-temperature irradiation;
the product is analyzed by adopting Raman spectrum and X-ray diffraction analysis technology, and the structure is double-layer.
The foregoing is illustrative of only some embodiments of the invention, which are presented for purposes of illustration only and not limitation; it will be understood by those skilled in the art that changes may be made thereto without departing from the scope of the invention defined by the claims and the appended claims.
Claims (2)
1. A method for preparing graphene by using ion sputtering and laser composite technology is characterized by comprising the following steps:
(1) carrying out heat treatment on the nano carbon powder under a vacuum condition, wherein the heat treatment temperature is 1600-1700 ℃, the time is 1.5-2 h, and cooling to the normal temperature along with a furnace to obtain heat-treated nano carbon powder; the particle size of the nano carbon powder is 8-20 nm; the heat treatment equipment is a vacuum furnace with the vacuum condition of 10-1~10-7mbar；
(2) Placing the heat-treated nano carbon powder in an ion sputtering instrument as a carbon target; placing the substrate in a vacuum chamber of an ion sputtering instrument; carrying out ion sputtering on the substrate by an ion sputtering instrument to prepare a carbon film on the surface of the substrate; when ion sputtering is carried out, the vacuum condition is 0.1-1.0 Pa; the substrate is made of molybdenum carbide and has the thickness of 3-5 mm; the thickness of the carbon film is 10-300 nm;
(3) placing a substrate with a carbon film covered on the surface under a vacuum condition, and carrying out laser irradiation by a laser emitting device, wherein the laser irradiation is divided into three stages of low-temperature irradiation, medium-temperature irradiation and high-temperature irradiation, wherein the temperature of the substrate is controlled to be 500-600 ℃ during the low-temperature irradiation for at least 45min, the temperature of the substrate is controlled to be 1800-1900 ℃ during the medium-temperature irradiation for at least 45min, and the temperature of the substrate is controlled to be 2400-2550 ℃ during the high-temperature irradiation for at least 90 min; and preparing graphene on the surface of the substrate after laser irradiation is finished.
2. The method for preparing graphene by using the ion sputtering and laser composite technology as claimed in claim 1, wherein the structure of the graphene is single-layer or multi-layer.
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