CN115321527A - Method for preparing single-layer and double-layer alternating graphene - Google Patents
Method for preparing single-layer and double-layer alternating graphene Download PDFInfo
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Abstract
The invention relates to a method for preparing single-layer and double-layer alternating graphene, which comprises the following steps: s1: placing the copper foil in a vapor deposition furnace, placing any one or more of a graphite box, graphite paper, graphite flakes and graphite scraps, introducing argon into the vapor deposition furnace, and heating the vapor deposition furnace to the temperature of 1000-1080 ℃; s2: introducing hydrogen into the vapor deposition furnace to anneal the copper foil; s3: introducing methane into the vapor deposition furnace, reducing the introduction amount of hydrogen and starting a growth process; s4: controlling the vapor deposition furnace to perform one or more temperature changes, wherein each temperature change is that the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ and then is immediately increased to 1000-1080 ℃; s5: maintaining the temperature of the vapor deposition furnace at 1000-1080 ℃, and continuing the growth process; s6: and after the growth is finished, stopping introducing the methane, and naturally cooling to room temperature. The method provided by the invention can be used for preparing the single-layer and double-layer alternating graphene superlattice, the steps are simple, and the preparation conditions are easy to realize and control.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a method for preparing single-layer and double-layer alternative graphene.
Background
Graphene is a two-dimensional lattice structure formed by arranging carbon atoms in a hexagonal manner, has a thickness of about 0.335nm, is thin, and is very firm and hard. As a simple substance, graphene is inThe speed of electron transfer at room temperature is faster than that of many conductors and semiconductors; and the theoretical specific surface area of the graphene is up to 2630m 2 /g, is a very potential energy storage active material. Graphene materials have unique physical properties and wide application prospects, so that the graphene materials are widely concerned and researched in recent years.
The double-layer graphene consists of two carbon atom layers, and due to the coupling effect between the atom layers, a band gap appears in an energy band structure, so that the graphene has a wide application prospect in the field of photoelectronics. Bi-layer graphene with different stacking directions has considerable application potential due to its unique electronic, optical and mechanical properties. For example, AB-stacked double-layer graphene (60 ° stack orientation angle) has been used in the fabrication of devices such as tunnel field effect transistors, high-switching-ratio digital transistors, tunable laser diodes, and infrared laser detectors due to its tunable band structure and high mobility.
Currently, there are few reports on the preparation of single-double layer alternating graphene, and the effective and controllable preparation of single-double layer alternating graphene is expected to be realized in the field.
Disclosure of Invention
Based on this, the invention aims to provide a method for preparing single-layer and double-layer alternating graphene, which can be used for effectively and controllably preparing the single-layer and double-layer alternating graphene.
The technical scheme adopted by the invention is as follows:
a method for preparing single-double layer alternating graphene comprises the following steps:
s1: placing the copper foil in a vapor deposition furnace, placing any one or more of a graphite box, graphite paper, graphite flakes and graphite scraps in the vapor deposition furnace, introducing argon into the vapor deposition furnace, and heating the vapor deposition furnace to the temperature of 1000-1080 ℃;
s2: keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, and introducing hydrogen into the vapor deposition furnace to anneal the copper foil;
s3: keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, introducing methane into the vapor deposition furnace, reducing the introduction amount of hydrogen, and starting a growth process;
s4: controlling the vapor deposition furnace to perform one or more temperature changes, wherein each temperature change is that the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ and then is immediately increased to 1000-1080 ℃;
s5: maintaining the temperature of the vapor deposition furnace at 1000-1080 ℃, and continuing the growth process;
s6: and after the growth is finished, stopping introducing the methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of hydrogen and argon.
The growth principle of the method is that the carbon-rich raw materials such as graphite boxes and the like generate an additional carbon source beneficial to double-layer growth through the treatment of temperature reduction and then rapid temperature rise. According to the method, the temperature change of 1030 +/-50 ℃→ 700 +/-50 ℃→ 1030 +/-50 ℃ is set in the graphene growth process, the single-double layer alternate growth of the graphene can be effectively controlled, and the structure of the single-double layer alternate graphene can be controlled by setting the frequency of the temperature change, so that the ideal single-double layer alternate graphene superlattice is obtained.
The patterning of single-layer and double-layer alternating graphene is an important technology which is expected to realize high-performance micro-nano devices. Compared with the prior art, the invention has the innovation points that the periodic growth of the single-layer and double-layer alternating graphene superlattice can be realized only by regulating and controlling the change of the temperature, and the size of the single layer and the double layer can be controlled by changing the growth time. Compared with the conventional wet transfer or top-down assembly photoetching technology, the method provided by the invention is more convenient, the steps are simpler, the preparation conditions are easy to realize and control, no organic chemical reagent is left, and the high-quality graphene patterned film with a clean surface can be obtained.
Further, the vapor deposition furnace was heated to 1000-1080 ℃ within 75 minutes.
Further, in step S2, the flow rate of hydrogen gas was 40sccm, and the annealing time was 40 minutes.
Further, in step S3, the flow rate of methane was 4sccm, the flow rate of hydrogen was reduced to 10sccm, and the growth duration was 30 minutes.
Further, in each temperature change of step S4, the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ within 30 minutes, and is increased from 650-750 ℃ to 1000-1080 ℃ within 30 minutes.
Further, in step S4, the interval of the two adjacent temperature changes is 10 minutes, and the temperature of the vapor deposition furnace is maintained at 1000 to 1080 ℃ during the interval.
Further, in step S5, the growth duration was 30 minutes.
Further, in steps S1 to S6, the flow rate of argon gas was kept at 500sccm.
Further, in step S6, the flow rate of hydrogen gas was 10sccm.
Further, in step S1, the copper foil is carried by a quartz plate.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
Fig. 1A is a schematic diagram of a single-double layer alternating graphene prepared according to the method of the present invention;
FIG. 1B is an optical diagram of a single-double layer alternating graphene prepared according to the method of the present invention;
fig. 2A is a schematic of another single-double layer alternating graphene prepared according to the method of the present invention;
fig. 2B is an optical diagram of another single-double layer alternating graphene prepared according to the method of the present invention;
FIG. 3 is a schematic view of an apparatus for preparing single-double layer alternating graphene according to the present invention;
FIG. 4 is a graph showing temperature control curves in examples 1 to 3;
FIG. 5 is an optical diagram of single and double layer alternating graphene prepared by the example;
FIG. 6 is an optical diagram of single-layer graphene prepared by a comparative example;
fig. 7 is a raman spectrum of single-double layer alternating graphene prepared in example;
fig. 8 is a raman spectrum of single-layer graphene prepared in the comparative example.
Detailed Description
Referring to fig. 3 and 4, the method for preparing single-double layer alternating graphene according to the present invention includes the following steps:
s1: placing the copper foil in a vapor deposition furnace, placing any one or more of a graphite box, graphite paper, graphite flake and graphite scrap in the vapor deposition furnace, introducing argon into the vapor deposition furnace, and heating the vapor deposition furnace to 1000-1080 ℃.
Specifically, the copper foils were placed on a quartz plate and then put together in the vapor deposition furnace. More preferably, the vapor deposition furnace is heated to 1000-1080 ℃ within 75 minutes. The vapor deposition furnace is matched equipment of a CVD system, and is specifically a tubular furnace.
S2: and keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, and introducing hydrogen into the vapor deposition furnace to anneal the copper foil. Specifically, the hydrogen gas was introduced in an amount of 40sccm (standard milliliter per minute) and the annealing time was 40 minutes.
S3: and keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, introducing methane into the vapor deposition furnace, reducing the introduction amount of hydrogen, and starting the growth process of the single-layer and double-layer alternative graphene superlattice on the copper foil. Specifically, the introduction amount of methane is 4sccm, and the introduction amount of hydrogen is reduced to 10sccm; the duration of the growth process was 30 minutes.
S4: controlling the vapor deposition furnace to perform one or more temperature changes, wherein each temperature change is increased to 1000-1080 ℃ immediately after being reduced from 1000-1080 ℃ to 650-750 ℃, as shown by a curve in figure 4.
Specifically, in each temperature change, the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ within 30 minutes, and is increased from 650-750 ℃ to 1000-1080 ℃ within 30 minutes; the interval of the two adjacent temperature changes is 10 minutes, and the temperature of the vapor deposition furnace is kept between 1000 and 1080 ℃ in the interval.
S5: keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, and continuing the growth process.
S6: and after the growth is finished, stopping introducing the methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of hydrogen and argon. Specifically, the amount of hydrogen gas introduced was 10sccm.
Specifically, in steps S1-S6, the flow rate of argon gas was maintained at 500sccm.
According to the method, the temperature change of 1030 +/-50 ℃→ 700 +/-50 ℃→ 1030 +/-50 ℃ is set in the growth process of the graphene, the single-double layer alternate growth of the graphene can be effectively controlled, and the structure of the single-double layer alternate graphene can be controlled by setting the frequency of the temperature change, so that an ideal single-double layer alternate graphene superlattice is obtained.
By controlling the number of the temperature changes, the single-double layer alternating graphene prepared by the method has various structures, such as shown in fig. 1A, 1B, 2A and 2B.
Example 1
As shown in fig. 3 and 4, in this embodiment, a temperature change is adopted during the growth process, and the following steps are specifically performed:
1) The copper foil and the graphite box are respectively placed on a quartz plate and are placed into a vapor deposition furnace of a CVD system, argon gas of 500sccm is introduced, and the temperature of the vapor deposition furnace is raised to 1030 ℃ within 75 min.
2) And introducing 40sccm hydrogen gas when the temperature of the vapor deposition furnace reaches 1030 ℃, and annealing the copper foil for 40min.
3) And (3) keeping the temperature of the vapor deposition furnace at 1030 ℃, introducing 4sccm of methane as a growth carbon source, reducing the introduction amount of hydrogen to 10sccm, and starting the growth process, wherein the duration of the growth process is 30min.
4) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
5) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is increased to 1030 ℃ within 30min, and then the growth is continued for 30min.
6) And after the growth is finished, closing methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of 10sccm hydrogen and 500sccm argon to obtain the single-layer and double-layer alternative graphene.
Example 2
As shown in fig. 3 and 4, in this embodiment, two temperature changes are adopted in the growth process, and the method specifically includes the following steps:
1) The copper foil and the graphite box are respectively placed on a quartz plate and are placed into a vapor deposition furnace of a CVD system, argon gas of 500sccm is introduced, and the temperature of the vapor deposition furnace is raised to 1030 ℃ within 75 min.
2) And introducing 40sccm hydrogen gas when the temperature of the vapor deposition furnace reaches 1030 ℃, and annealing the copper foil for 40min.
3) And (3) keeping the temperature of the vapor deposition furnace at 1030 ℃, introducing 4sccm of methane as a growth carbon source, reducing the introduction amount of hydrogen to 10sccm, and starting the growth process, wherein the duration of the growth process is 30min.
4) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
5) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is raised to 1030 ℃ within 30min, and then the growth is continued for 10min.
6) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
7) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is raised to 1030 ℃ within 30min, and then the growth is continued for 30min.
8) And after the growth is finished, closing methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of 10sccm hydrogen and 500sccm argon to obtain the single-layer and double-layer alternating graphene.
Example 3
As shown in fig. 3 and fig. 4, in this embodiment, three temperature changes are adopted in the growth process, which specifically includes the following steps:
1) The copper foil and the graphite box are respectively placed on a quartz plate and are placed into a vapor deposition furnace of a CVD system, then argon gas of 500sccm is introduced, and the temperature of the vapor deposition furnace is raised to 1030 ℃ within 75 min.
2) And introducing 40sccm hydrogen gas when the temperature of the vapor deposition furnace reaches 1030 ℃, and annealing the copper foil for 40min.
3) And (3) keeping the temperature of the vapor deposition furnace at 1030 ℃, introducing 4sccm of methane as a growth carbon source, reducing the introduction amount of hydrogen to 10sccm, and starting the growth process, wherein the duration of the growth process is 30min.
4) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
5) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is raised to 1030 ℃ within 30min, and then the growth is continued for 10min.
6) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
7) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is raised to 1030 ℃ within 30min, and then the growth is continued for 10min.
8) Keeping other growth parameters unchanged, and cooling the vapor deposition furnace to 700 ℃ within 30min.
9) After the temperature of the vapor deposition furnace reaches 700 ℃, the temperature of the vapor deposition furnace is raised to 1030 ℃ within 30min, and then the growth is continued for 30min.
10 And) after the growth is finished, closing methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of 10sccm hydrogen and 500sccm argon to obtain the single-layer and double-layer alternative graphene.
Comparative example 1
The comparative example was carried out as follows:
1) The copper foil and the graphite box are respectively placed on a quartz plate and are placed into a vapor deposition furnace of a CVD system, argon gas of 500sccm is introduced, and the temperature of the vapor deposition furnace is raised to 1030 ℃ within 75 min.
2) And introducing 40sccm hydrogen gas when the temperature of the vapor deposition furnace reaches 1030 ℃, and annealing the copper foil for 40min.
3) Introducing 4sccm of methane serving as a growth carbon source into the vapor deposition furnace, reducing the introduction amount of hydrogen to 10sccm, and starting a growth process with the duration of the growth process being 40min.
4) And after the growth is finished, closing the methane, closing the power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of 10sccm hydrogen and 500sccm argon to obtain the single-layer graphene.
Comparative example 2
The comparative example was carried out as follows:
1) The copper foil and the graphite box are respectively placed on a quartz plate and are placed into a vapor deposition furnace of a CVD system, then argon gas of 500sccm is introduced, and the temperature of the vapor deposition furnace is raised to 1030 ℃ within 75 min.
2) And introducing 40sccm hydrogen gas when the temperature of the vapor deposition furnace reaches 1030 ℃, and annealing the copper foil for 40min.
3) Introducing 4sccm of methane serving as a growth carbon source into the vapor deposition furnace, reducing the introduction amount of hydrogen to 10sccm, and starting a growth process with the duration of the growth process being 30min.
4) And after the growth is finished, closing methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of 10sccm hydrogen and 500sccm argon to obtain the single-layer graphene.
And (3) test results:
in examples 1 to 3, a temperature change stage of 1030 ℃→ 700 ℃→ 1030 ℃ is set in the growth process of graphene, and each temperature change is as an inverted triangular peak in a curve shown in fig. 4, so that a single-double layer alternating graphene superlattice shown in fig. 5 is prepared, and the raman spectrum of fig. 7 further illustrates that the prepared graphene is a single double layer.
In contrast, in comparative examples 1-2, the aforementioned temperature change is not set during the growth of graphene, so that the single-layer graphene shown in fig. 6 is obtained, and the raman spectrum of fig. 8 further illustrates that the obtained graphene is a single layer.
The above-mentioned embodiments only express several 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.
Claims (10)
1. A method for preparing single-layer and double-layer alternating graphene is characterized by comprising the following steps: the method comprises the following steps:
s1: placing the copper foil in a vapor deposition furnace, placing any one or more of a graphite box, graphite paper, a graphite flake and graphite scraps in the vapor deposition furnace, introducing argon into the vapor deposition furnace, and heating the vapor deposition furnace to 1000-1080 ℃;
s2: keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, introducing hydrogen into the vapor deposition furnace, and annealing the copper foil;
s3: keeping the temperature of the vapor deposition furnace at 1000-1080 ℃, introducing methane into the vapor deposition furnace, reducing the introduction amount of hydrogen, and starting a growth process;
s4: controlling the vapor deposition furnace to perform one or more temperature changes, wherein each temperature change is that the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ and then is immediately increased to 1000-1080 ℃;
s5: maintaining the temperature of the vapor deposition furnace at 1000-1080 ℃, and continuing the growth process;
s6: and after the growth is finished, stopping introducing the methane, closing a power supply of the vapor deposition furnace, and naturally cooling the vapor deposition furnace to room temperature in the atmosphere of hydrogen and argon.
2. The method of claim 1, wherein: in step S1, the vapor deposition furnace is heated to 1000-1080 ℃ within 75 minutes.
3. The method of claim 2, wherein: in step S2, the introduction amount of hydrogen is 40sccm, and the annealing time is 40 minutes.
4. The method of claim 3, wherein: in step S3, the introduction amount of methane is 4sccm, the introduction amount of hydrogen is reduced to 10sccm, and the growth duration is 30 minutes.
5. The method of claim 4, wherein: in each temperature change of the step S4, the temperature is reduced from 1000-1080 ℃ to 650-750 ℃ within 30 minutes, and is increased from 650-750 ℃ to 1000-1080 ℃ within 30 minutes.
6. The method of claim 4, wherein: in step S4, the interval of the temperature changes of two adjacent times is 10 minutes, and the temperature of the vapor deposition furnace is maintained at 1000 to 1080 ℃ in the interval.
7. The method of claim 4, wherein: in step S5, the growth duration was 30 minutes.
8. The method according to any one of claims 1 to 7, wherein: in steps S1-S6, the flow rate of argon gas is maintained at 500sccm.
9. The method according to any one of claims 1 to 7, wherein: in step S6, the flow rate of hydrogen gas is 10sccm.
10. The method according to any one of claims 1 to 7, wherein: in step S1, the copper foil is supported by a quartz plate.
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| US20120225296A1 (en) * | 2010-09-03 | 2012-09-06 | The Regents Of The University Of Michigan | Uniform multilayer graphene by chemical vapor deposition |
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| US20120225296A1 (en) * | 2010-09-03 | 2012-09-06 | The Regents Of The University Of Michigan | Uniform multilayer graphene by chemical vapor deposition |
| CN103708448A (en) * | 2014-01-03 | 2014-04-09 | 中国科学院化学研究所 | Atmospheric pressure controlled growth method for graphene |
| CN104211054A (en) * | 2014-09-09 | 2014-12-17 | 中国科学院化学研究所 | Method for controllably preparing graphene |
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