CN114574835A - Graphene/molybdenum disulfide heterojunction semiconductor film and preparation method thereof - Google Patents
Graphene/molybdenum disulfide heterojunction semiconductor film and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 184
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 115
- 239000004065 semiconductor Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 288
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- 239000010409 thin film Substances 0.000 claims description 23
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- 238000010438 heat treatment Methods 0.000 claims description 17
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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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
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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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
- C01B32/194—After-treatment
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a graphene/molybdenum disulfide heterojunction semiconductor film and a preparation method thereof, wherein the method comprises the following steps: respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate; growing a graphene film on the processed copper foil substrate; transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film; and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film. According to the invention, the large-area continuous high-quality two-dimensional molybdenum disulfide film is obtained by generating molybdenum disulfide on the silicon dioxide/silicon substrate deposited with the graphene film, so that the graphene and the molybdenum disulfide naturally form a van der Waals heterojunction under the action of van der Waals force, and the large-area continuous high-quality graphene/molybdenum disulfide heterojunction semiconductor film is obtained.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a graphene/molybdenum disulfide heterojunction semiconductor film and a preparation method thereof.
Background
Two-dimensional materials are an important part of the field of nanomaterials, and are a general term for a class of materials, which refer to thin film materials having a thickness of only one or a few atomic layers. It has been considered that a thin film having a thickness as small as an atomic size is considered to be thermodynamically unstable and thus cannot exist until graphene having a single-layer structure is prepared, and the existence of a two-dimensional material is not proved, and thus scientific research on the two-dimensional material has gradually started to attract a great deal of attention. The existing method for preparing the two-dimensional material mainly comprises a chemical vapor deposition method, a mechanical stripping method, a lithium ion intercalation method, a liquid phase stripping method, a chemical stripping method, a hydrothermal method and the like. The chemical vapor deposition method is a main method for preparing large-area two-dimensional materials at present.
Various two-dimensional materials can form heterojunctions under van der waals forces and the lattice mismatch is generally small. Therefore, the heterojunction formed by the two-dimensional materials with different layers is a fundamental stone for constructing a new generation of nano electronic devices. The current research on graphene and molybdenum disulfide heterojunctions has become one of the hot spots. Although graphene has excellent electrical and optical properties, the development of graphene is restricted by the fact that intrinsic graphene does not have band gap defects. Molybdenum disulfide has an adjustable band gap and good optical properties. The graphene/molybdenum disulfide heterojunction formed by the two can fully exert the respective advantages of the two.
At present, preparation of graphene and molybdenum disulfide thin films is reported, but reports of forming van der waals heterojunction between graphene and molybdenum disulfide are few, the process is not mature, and continuous research is needed to improve the preparation process so as to obtain a large-area and high-quality two-dimensional graphene/molybdenum disulfide heterojunction semiconductor thin film.
Disclosure of Invention
In view of the above, the present invention provides a graphene/molybdenum disulfide heterojunction semiconductor film and a method for manufacturing the same, so as to obtain a large-area and high-quality two-dimensional graphene/molybdenum disulfide heterojunction semiconductor film.
Based on the above purpose, the invention provides a preparation method of a graphene/molybdenum disulfide heterojunction semiconductor film, which comprises the following steps:
respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
growing a graphene film on the processed copper foil substrate;
transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
In some embodiments, growing a graphene thin film on a processed copper foil substrate includes:
placing the treated copper foil substrate in a quartz tube of a tube furnace;
vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen;
heating the tube furnace to a first preset temperature, and keeping the temperature constant for a preset time period;
continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at a first preset temperature to obtain graphene;
and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, growing the graphene thin film on the processed copper foil substrate further comprises:
placing the treated copper foil substrate in a first ceramic boat, and placing the first ceramic boat in a high-temperature area in a quartz tube of a tube furnace;
vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen;
heating the tube furnace to 1030 ℃, and keeping the temperature for 30 minutes;
continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at 1030 ℃ to obtain graphene;
and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, the step prior to transferring the grown graphene thin film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate further comprises:
and after the graphene film is obtained, continuously introducing hydrogen into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, growing a molybdenum disulfide film on a silicon dioxide/silicon substrate on which a graphene film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor film comprises:
placing the silicon dioxide/silicon substrate deposited with the graphene film, molybdenum trioxide and sulfur powder in a quartz tube;
vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas;
continuously introducing inert gas into the quartz tube, heating the tube furnace to a second preset temperature, and reacting molybdenum trioxide and sulfur powder at the second preset temperature to obtain molybdenum disulfide;
the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached to a silica/silicon substrate on which the graphene film is deposited.
In some embodiments, growing a molybdenum disulfide film on a silicon dioxide/silicon substrate on which the graphene film is deposited to obtain the graphene/molybdenum disulfide heterojunction semiconductor film further comprises:
placing molybdenum trioxide in a second ceramic boat, placing the silicon dioxide/silicon substrate deposited with the graphene film in the second ceramic boat, placing the second ceramic boat in a high-temperature area in a quartz tube, placing sulfur powder in a third ceramic boat, and placing the third ceramic boat in a low-temperature area in the quartz tube;
vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas;
continuously introducing inert gas into a quartz tube, heating the tube furnace to 650 ℃, and reacting molybdenum trioxide and sulfur powder at 650 ℃ to obtain molybdenum disulfide;
the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached on a silicon dioxide/silicon substrate on which the graphene film is deposited.
In some embodiments, the method further comprises:
and after the graphene/molybdenum disulfide heterojunction semiconductor film is obtained, continuously introducing inert gas into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, the inert gas is argon.
In some embodiments, the cleaning process for the copper foil substrate and the silicon dioxide/silicon substrate respectively comprises:
respectively wiping the copper foil substrate and the silicon dioxide/silicon substrate, and respectively carrying out ultrasonic treatment in a liquid detergent solution to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned preliminarily;
sequentially and respectively carrying out ultrasonic treatment on the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned primarily in deionized water, alcohol and acetone to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned secondarily;
and respectively blowing the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned for the second time by using high-purity nitrogen, and cleaning in a plasma cleaning machine to remove organic impurities on the copper foil substrate and the silicon dioxide/silicon substrate.
In another aspect of the present invention, there is also provided a graphene/molybdenum disulfide heterojunction semiconductor film, which is prepared by the following method:
respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
growing a graphene film on the processed copper foil substrate;
transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
The invention has at least the following beneficial technical effects:
according to the preparation method of the graphene/molybdenum disulfide heterojunction semiconductor film, graphene is generated on the copper foil, the large-area continuous high-quality two-dimensional graphene film is obtained, and then the two-dimensional graphene film is transferred to the silicon dioxide/silicon substrate; the introduction of high-quality graphene provides a heterojunction nucleation point for the growth of molybdenum disulfide, reduces the surface energy and reduces the free energy barrier, so that the molybdenum disulfide is easier to deposit on the surface of the graphene; the method comprises the steps of generating molybdenum disulfide on a silicon dioxide/silicon substrate deposited with a graphene film to obtain a large-area continuous high-quality two-dimensional molybdenum disulfide film; under the action of van der waals force, graphene and molybdenum disulfide naturally form van der waals heterojunction, and therefore the large-area continuous high-quality two-dimensional graphene/molybdenum disulfide heterojunction semiconductor film is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained by using the drawings without creative efforts.
Fig. 1 is a schematic view of a method for preparing a graphene/molybdenum disulfide heterojunction semiconductor thin film according to an embodiment of the invention;
fig. 2 is a schematic structural diagram of graphene prepared in the preparation method of the graphene/molybdenum disulfide heterojunction semiconductor film according to the embodiment of the invention;
fig. 3 is a schematic structural diagram of preparing molybdenum disulfide in a preparation method of a graphene/molybdenum disulfide heterojunction semiconductor film according to an embodiment of the invention;
fig. 4 is a schematic structural diagram of a substrate placed in a ceramic boat in the method for preparing a graphene/molybdenum disulfide heterojunction semiconductor film according to the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are used for distinguishing two non-identical entities with the same name or different parameters, and it is understood that "first" and "second" are only used for convenience of expression and should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "comprises" and "comprising," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements does not include all of the other steps or elements inherent in the list.
In view of the above objects, in a first aspect of the embodiments of the present invention, an embodiment of a method for manufacturing a graphene/molybdenum disulfide heterojunction semiconductor thin film is provided. Fig. 1 is a schematic diagram illustrating an embodiment of a method for preparing a graphene/molybdenum disulfide heterojunction semiconductor thin film provided by the invention. As shown in fig. 1, the embodiment of the present invention includes the following steps:
step S10, respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
step S20, growing a graphene film on the processed copper foil substrate;
step S30, transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and S40, growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
According to the preparation method of the graphene/molybdenum disulfide heterojunction semiconductor film, disclosed by the embodiment of the invention, the graphene is generated on the copper foil, so that the large-area continuous high-quality two-dimensional graphene film is obtained, and then the large-area continuous high-quality two-dimensional graphene film is transferred to the silicon dioxide/silicon substrate; the introduction of high-quality graphene provides a heterojunction nucleation point for the growth of molybdenum disulfide, reduces the surface energy and reduces the free energy barrier, so that the molybdenum disulfide is easier to deposit on the surface of the graphene; the method comprises the steps of generating molybdenum disulfide on a silicon dioxide/silicon substrate deposited with a graphene film to obtain a large-area continuous high-quality two-dimensional molybdenum disulfide film; under the action of van der waals force, graphene and molybdenum disulfide naturally form van der waals heterojunction, and therefore the large-area continuous high-quality two-dimensional graphene/molybdenum disulfide heterojunction semiconductor film is obtained.
In some embodiments, growing the graphene thin film on the processed copper foil substrate comprises: placing the treated copper foil substrate in a quartz tube of a tube furnace; vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen; heating the tube furnace to a first preset temperature, and keeping the temperature constant for a preset time period; continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at a first preset temperature to obtain graphene; and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, growing the graphene thin film on the processed copper foil substrate further comprises: placing the processed copper foil substrate in a first ceramic boat, and placing the first ceramic boat in a high-temperature area in a quartz tube of a tube furnace; vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen; heating the tube furnace to 1030 ℃, and keeping the temperature for 30 minutes; continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at 1030 ℃ to obtain graphene; and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, the step prior to transferring the grown graphene thin film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate further comprises: and after the graphene film is obtained, continuously introducing hydrogen into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, growing a molybdenum disulfide film on a silicon dioxide/silicon substrate on which a graphene film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor film comprises: placing the silicon dioxide/silicon substrate deposited with the graphene film, molybdenum trioxide and sulfur powder in a quartz tube; vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas; continuously introducing inert gas into the quartz tube, heating the tube furnace to a second preset temperature, and reacting molybdenum trioxide and sulfur powder at the second preset temperature to obtain molybdenum disulfide; the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached on a silicon dioxide/silicon substrate on which the graphene film is deposited.
In some embodiments, growing a molybdenum disulfide thin film on a silicon dioxide/silicon substrate on which a graphene thin film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor thin film further comprises: placing molybdenum trioxide in a second ceramic boat, placing the silicon dioxide/silicon substrate deposited with the graphene film in the second ceramic boat, placing the second ceramic boat in a high-temperature area in a quartz tube, placing sulfur powder in a third ceramic boat, and placing the third ceramic boat in a low-temperature area in the quartz tube; vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas; continuously introducing inert gas into a quartz tube, heating the tube furnace to 650 ℃, and reacting molybdenum trioxide and sulfur powder at 650 ℃ to obtain molybdenum disulfide; the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached to a silica/silicon substrate on which the graphene film is deposited.
In some embodiments, the method further comprises: and after the graphene/molybdenum disulfide heterojunction semiconductor film is obtained, continuously introducing inert gas into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, the inert gas is argon.
In some embodiments, the cleaning process for the copper foil substrate and the silicon dioxide/silicon substrate respectively comprises: respectively wiping the copper foil substrate and the silicon dioxide/silicon substrate, and respectively carrying out ultrasonic treatment in a liquid detergent solution to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned preliminarily; sequentially and respectively carrying out ultrasonic treatment on the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned primarily in deionized water, alcohol and acetone to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned secondarily; and respectively blowing the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned for the second time by using high-purity nitrogen, and cleaning in a plasma cleaning machine to remove organic impurities on the copper foil substrate and the silicon dioxide/silicon substrate.
Fig. 2 is a schematic structural diagram illustrating graphene prepared in a method for preparing a graphene/molybdenum disulfide heterojunction semiconductor thin film according to an embodiment of the invention; fig. 3 shows a schematic structural diagram of preparing molybdenum disulfide in a preparation method of a graphene/molybdenum disulfide heterojunction semiconductor thin film provided in an embodiment of the invention; fig. 4 shows a schematic structural diagram of a substrate placed in a ceramic boat in a preparation method of a graphene/molybdenum disulfide heterojunction semiconductor film provided by the embodiment of the invention. As shown in fig. 2, 3 and 4, an exemplary embodiment of a method for preparing a graphene/molybdenum disulfide heterojunction semiconductor thin film is as follows:
treatment of a substrate
In this embodiment, a copper foil is used as a substrate to grow graphene, and silicon dioxide/silicon is used as a substrate to grow molybdenum disulfide, and the processing procedure of the substrate is as follows: (1) firstly, wiping a substrate with cotton for 5min (minutes), and then carrying out ultrasonic treatment in a liquid detergent solution for 30 min; (2) then sequentially carrying out ultrasonic treatment in deionized water for 30min, carrying out ultrasonic treatment in alcohol for 30min, and finally carrying out ultrasonic treatment in acetone for 30 min; (3) taking out the substrate, drying the substrate by using high-purity nitrogen, and then cleaning the substrate for 10min by using a plasma cleaning machine to remove organic impurities on the substrate.
Preparation of graphene
As shown in fig. 2, the graphene is prepared by the following steps: (1) the processed copper foil substrate is placed in a ceramic boat with the front side facing downwards in a mode shown in figure 4, and then the ceramic boat is placed in the central position of a high-temperature constant-temperature area in a tube furnace; (2) connecting a vacuum pump for vacuum pumping, and then introducing hydrogen with the flow rate of 100sccm (volume flow unit, meaning: standard-state cubic meter per minute) to fill the whole quartz tube cavity with hydrogen, so as to ensure that the air in the cavity is exhausted. Simultaneously, the temperature is increased to 1030 ℃ within 30min, the temperature is kept for 30min, the surface oxide of the substrate is removed, and the grain size of the copper substrate can be increased; (3) then continuously introducing methane with the flow rate of 5sccm and hydrogen with the flow rate of 20sccm, and reacting at the constant temperature of 1030 ℃ for 10min to generate feldspar graphene; (4) after the growth is finished, continuously introducing hydrogen with the flow rate of 100sccm until the tubular furnace is cooled to the room temperature; (5) and finally, transferring the graphene film on the copper foil substrate to the processed silicon dioxide/silicon substrate.
Preparation of molybdenum disulfide
As shown in fig. 3, the molybdenum disulfide film is prepared as follows: (1) weighing 0.4g of molybdenum trioxide, then placing the molybdenum trioxide into a ceramic boat, placing a silicon dioxide/silicon substrate with the front side facing downwards into the ceramic boat filled with the molybdenum trioxide according to a mode shown in a figure 4, and then placing the ceramic boat in the central position of a high-temperature constant-temperature area in a tubular furnace; (2) weighing 2g of sulfur powder in a ceramic boat, and then placing the ceramic boat in a low-temperature area in a tube furnace; (3) connecting a vacuum pump for vacuumizing, and then introducing argon with the flow rate of 100sccm for 60min to fill the whole quartz tube cavity with argon, so as to ensure that the air in the cavity is exhausted; (4) continuously introducing argon with the flow rate of 100sccm as protective atmosphere, heating the tubular furnace to 650 ℃ within 30min, and reacting at constant temperature for 30min to grow molybdenum disulfide; (5) and after the growth is finished, continuously introducing argon with the flow rate of 100sccm until the tubular furnace is cooled to room temperature.
In the above embodiment, (1) by controlling specific reaction conditions such as flow rate of introduced methane and hydrogen, growth time, growth temperature, and the like, under the mature reaction conditions, and by selecting a copper foil as a substrate, under the catalytic action of copper, carbon atoms obtained by cracking methane are deposited on the surface of the copper foil, so as to obtain a large-area continuous high-quality two-dimensional graphene film; (2) the prepared high-quality graphene provides a heterojunction nucleation point for the growth of molybdenum disulfide, reduces the surface energy and the free energy barrier, so that the molybdenum disulfide is easier to deposit on the surface of the graphene; (3) specific reaction conditions for generating molybdenum disulfide by reacting molybdenum trioxide with sulfur powder are adopted, and under the mature reaction conditions, the promotion effect of the graphene film is added, so that a large-area continuous high-quality two-dimensional molybdenum disulfide film is obtained; (4) firstly growing a high-quality two-dimensional graphene film on a copper foil substrate, then transferring the high-quality two-dimensional graphene film to a silicon dioxide/silicon substrate to grow a high-quality two-dimensional molybdenum disulfide film, and simultaneously forming a van der Waals heterojunction by the aid of van der Waals force to obtain a large-area continuous high-quality two-dimensional graphene/molybdenum disulfide heterojunction semiconductor film.
In another aspect of the embodiments of the present invention, there is also provided a graphene/molybdenum disulfide heterojunction semiconductor film, which is prepared by the following method:
respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
growing a graphene film on the processed copper foil substrate;
transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
In some embodiments, growing the graphene thin film on the processed copper foil substrate comprises: placing the treated copper foil substrate in a quartz tube of a tube furnace; vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen; heating the tube furnace to a first preset temperature, and keeping the temperature constant for a preset time period; continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at a first preset temperature to obtain graphene; and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, growing the graphene thin film on the processed copper foil substrate further comprises: placing the processed copper foil substrate in a first ceramic boat, and placing the first ceramic boat in a high-temperature area in a quartz tube of a tube furnace; vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen; heating the tube furnace to 1030 ℃, and keeping the temperature for 30 minutes; continuously introducing methane and hydrogen into the quartz tube, and reacting the methane and the hydrogen at 1030 ℃ to obtain graphene; and obtaining the graphene film based on the processed graphene on the copper foil substrate.
In some embodiments, the step prior to transferring the grown graphene thin film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate further comprises: and after the graphene film is obtained, continuously introducing hydrogen into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, growing a molybdenum disulfide film on a silicon dioxide/silicon substrate on which a graphene film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor film comprises: placing the silicon dioxide/silicon substrate deposited with the graphene film, molybdenum trioxide and sulfur powder in a quartz tube; vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas; continuously introducing inert gas into the quartz tube, heating the tube furnace to a second preset temperature, and reacting molybdenum trioxide and sulfur powder at the second preset temperature to obtain molybdenum disulfide; the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached to a silica/silicon substrate on which the graphene film is deposited.
In some embodiments, growing a molybdenum disulfide film on a silicon dioxide/silicon substrate on which the graphene film is deposited to obtain the graphene/molybdenum disulfide heterojunction semiconductor film further comprises: placing molybdenum trioxide in a second ceramic boat, placing the silicon dioxide/silicon substrate deposited with the graphene film in the second ceramic boat, placing the second ceramic boat in a high-temperature area in a quartz tube, placing sulfur powder in a third ceramic boat, and placing the third ceramic boat in a low-temperature area in the quartz tube; vacuumizing the quartz tube, and introducing inert gas into the quartz tube so as to fill the chamber of the quartz tube with the inert gas; continuously introducing inert gas into a quartz tube, heating the tube furnace to 650 ℃, and reacting molybdenum trioxide and sulfur powder at 650 ℃ to obtain molybdenum disulfide; the graphene/molybdenum disulfide heterojunction semiconductor film is obtained based on molybdenum disulfide attached to a silica/silicon substrate on which the graphene film is deposited.
In some embodiments, the steps further comprise: and after the graphene/molybdenum disulfide heterojunction semiconductor film is obtained, continuously introducing inert gas into the quartz tube until the quartz tube is cooled to room temperature.
In some embodiments, the inert gas is argon.
In some embodiments, the cleaning process for the copper foil substrate and the silicon dioxide/silicon substrate respectively comprises: respectively wiping the copper foil substrate and the silicon dioxide/silicon substrate, and respectively carrying out ultrasonic treatment in a liquid detergent solution to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned preliminarily; sequentially and respectively carrying out ultrasonic treatment on the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned primarily in deionized water, alcohol and acetone to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned secondarily; and respectively blowing the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned for the second time by using high-purity nitrogen, and cleaning in a plasma cleaning machine to remove organic impurities on the copper foil substrate and the silicon dioxide/silicon substrate.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the present disclosure as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
It should be understood that, as used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly supports the exception. It should also be understood that "and/or" as used herein is meant to include any and all possible combinations of one or more of the associated listed items. The numbers of the embodiments disclosed in the embodiments of the present invention are merely for description, and do not represent the merits of the embodiments.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A preparation method of a graphene/molybdenum disulfide heterojunction semiconductor film is characterized by comprising the following steps:
respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
growing a graphene film on the processed copper foil substrate;
transferring the grown graphene film from the processed copper foil substrate to a processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
2. The method of claim 1, wherein growing the graphene film on the processed copper foil substrate comprises:
placing the treated copper foil substrate in a quartz tube of a tube furnace;
vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen;
heating the tube furnace to a first preset temperature, and keeping the temperature constant for a preset time period;
continuously introducing methane and the hydrogen into the quartz tube, and reacting the methane and the hydrogen at the first preset temperature to obtain graphene;
and obtaining the graphene film based on the graphene on the processed copper foil substrate.
3. The method of claim 2, wherein growing the graphene thin film on the processed copper foil substrate further comprises:
placing the treated copper foil substrate in a first ceramic boat, and placing the first ceramic boat in a high-temperature area in a quartz tube of a tube furnace;
vacuumizing the quartz tube, introducing hydrogen into the quartz tube, and filling the chamber of the quartz tube with the hydrogen;
heating the tube furnace to 1030 ℃, and keeping the temperature for 30 minutes;
continuously introducing methane and the hydrogen into the quartz tube, and reacting the methane and the hydrogen at the temperature of 1030 ℃ to obtain graphene;
and obtaining the graphene film based on the graphene on the processed copper foil substrate.
4. The method of claim 2, wherein the step prior to transferring the grown graphene film from the processed copper foil substrate to the processed silicon dioxide/silicon substrate further comprises:
and after the graphene film is obtained, continuously introducing the hydrogen into the quartz tube until the quartz tube is cooled to room temperature.
5. The method of claim 2, wherein growing a molybdenum disulfide film on the silicon dioxide/silicon substrate on which the graphene film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor film comprises:
placing the silicon dioxide/silicon substrate deposited with the graphene film, molybdenum trioxide and sulfur powder in the quartz tube;
vacuumizing the quartz tube, and introducing inert gas into the quartz tube so that the chamber of the quartz tube is filled with the inert gas;
continuously introducing the inert gas into the quartz tube, heating the tube furnace to a second preset temperature, and reacting the molybdenum trioxide with the sulfur powder at the second preset temperature to obtain molybdenum disulfide;
and obtaining the graphene/molybdenum disulfide heterojunction semiconductor film based on the molybdenum disulfide attached to the silicon dioxide/silicon substrate on which the graphene film is deposited.
6. The method of claim 5, wherein growing a molybdenum disulfide film on the silicon dioxide/silicon substrate on which the graphene film is deposited to obtain a graphene/molybdenum disulfide heterojunction semiconductor film further comprises:
placing molybdenum trioxide in a second ceramic boat, placing the silicon dioxide/silicon substrate deposited with the graphene film in the second ceramic boat, placing the second ceramic boat in a high-temperature area in the quartz tube, placing sulfur powder in a third ceramic boat, and placing the third ceramic boat in a low-temperature area in the quartz tube;
vacuumizing the quartz tube, and introducing inert gas into the quartz tube so that the chamber of the quartz tube is filled with the inert gas;
continuously introducing the inert gas into the quartz tube, heating the tube furnace to 650 ℃, and reacting the molybdenum trioxide and the sulfur powder at 650 ℃ to obtain molybdenum disulfide;
and obtaining the graphene/molybdenum disulfide heterojunction semiconductor film based on the molybdenum disulfide attached to the silicon dioxide/silicon substrate on which the graphene film is deposited.
7. The method of claim 6, further comprising:
and after the graphene/molybdenum disulfide heterojunction semiconductor film is obtained, continuously introducing the inert gas into the quartz tube until the quartz tube is cooled to room temperature.
8. The method of claim 5, wherein the inert gas is argon.
9. The method of claim 1, wherein the cleaning the copper foil substrate and the silicon dioxide/silicon substrate respectively comprises:
respectively wiping the copper foil substrate and the silicon dioxide/silicon substrate, and respectively carrying out ultrasonic treatment in a liquid detergent solution to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned preliminarily;
sequentially and respectively carrying out ultrasonic treatment on the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned primarily in deionized water, alcohol and acetone to obtain a copper foil substrate and a silicon dioxide/silicon substrate which are cleaned secondarily;
and respectively drying the copper foil substrate and the silicon dioxide/silicon substrate which are cleaned for the second time by using high-purity nitrogen, and cleaning in a plasma cleaning machine to remove organic impurities on the copper foil substrate and the silicon dioxide/silicon substrate.
10. A graphene/molybdenum disulfide heterojunction semiconductor film is prepared by the following method:
respectively cleaning the copper foil substrate and the silicon dioxide/silicon substrate;
growing a graphene film on the processed copper foil substrate;
transferring the grown graphene film from the processed copper foil substrate to a processed silicon dioxide/silicon substrate to obtain the silicon dioxide/silicon substrate deposited with the graphene film;
and growing a molybdenum disulfide film on the silicon dioxide/silicon substrate deposited with the graphene film to obtain the graphene/molybdenum disulfide heterojunction semiconductor film.
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