CN113122818A - Method for preparing wafer-level single-layer molybdenum disulfide film - Google Patents
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- CN113122818A CN113122818A CN201911392156.8A CN201911392156A CN113122818A CN 113122818 A CN113122818 A CN 113122818A CN 201911392156 A CN201911392156 A CN 201911392156A CN 113122818 A CN113122818 A CN 113122818A
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- 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
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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
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Abstract
The invention discloses a method for preparing a wafer-level single-layer molybdenum disulfide film. The method is based on the chemical vapor deposition technology, adopts a mode of providing molybdenum sources in a face-to-face mode, and can grow continuous and uniform single-layer molybdenum disulfide films on the sapphire wafer substrate. According to the method, a silica gel plate or an alumina plate is used as a molybdenum source carrier, and a molybdenum source precursor is dispersed on the silica gel plate or the alumina plate in the form of solution. In the dual-temperature-zone chemical vapor deposition system, sulfur powder is placed in the left-side temperature zone, and the sapphire substrate and the molybdenum source carrier are placed in the right-side temperature zone in a face-to-face manner. And (3) carrying out chemical reaction on the sulfur vapor and a molybdenum source at high temperature, and uniformly depositing on the sapphire substrate to obtain a large-area single-layer molybdenum disulfide film. The method is simple to operate, has good experimental result repeatability, and has important significance for continuous production of large-area single-layer molybdenum disulfide films and application of electronic devices.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a method for preparing a wafer-level single-layer molybdenum disulfide film.
Background
The monolayer molybdenum disulfide is a two-dimensional semiconductor material with atomic-level thickness, and has wide application prospect in the fields of electronic devices, photoelectric devices, sensors and the like. The single-layer molybdenum disulfide has a proper band gap and high carrier mobility, the field effect transistor with the single-layer molybdenum disulfide as a channel material has excellent performance, and meanwhile, the single-layer molybdenum disulfide has immunity to short channel effects. Therefore, the single-layer molybdenum disulfide is expected to be applied to a new generation of nano electronic devices.
In recent years, methods for synthesizing monolayer molybdenum disulfide mainly include mechanical stripping, liquid phase stripping, chemical vapor deposition, and the like. Molybdenum disulfide obtained by mechanical and liquid phase stripping methods is generally in the order of microns or less in size, and it is difficult to obtain a large area molybdenum disulfide film. Most of the conventional chemical vapor deposition methods use a solid molybdenum source (such as molybdenum oxide) as a precursor, and the solid molybdenum sources are gathered together during the reaction, which is not favorable for uniformly depositing a molybdenum disulfide film on a large-area substrate. Obtaining a large-area, uniform and high-quality single-layer molybdenum disulfide film is an important prerequisite for realizing the application of electronic devices. Therefore, the development of a controllable preparation method of the wafer-level single-layer molybdenum disulfide film is of great significance for meeting the practical application of molybdenum disulfide in the aspect of electronic devices.
Disclosure of Invention
The invention aims to provide a method for preparing a wafer-level single-layer molybdenum disulfide film. The method adopts the chemical vapor deposition technology, and ensures that a monolayer molybdenum disulfide film is uniformly deposited on the surface of the substrate in a mode of providing a molybdenum source in a face-to-face mode, and the film has large area and good uniformity and can be applied to electronic devices.
The invention provides a method for preparing a wafer-level single-layer molybdenum disulfide film, which comprises the following steps:
and placing the sulfur powder at the upstream of the gas path, placing the substrate and the molybdenum source carrier at the downstream of the gas path in a face-to-face manner, and carrying out chemical vapor deposition to obtain the wafer-level single-layer molybdenum disulfide film after the deposition is finished.
In the above method, the molybdenum source contains a molybdenum-containing compound;
the molybdenum-containing compound is specifically selected from at least one of ammonium molybdate, sodium molybdate and phosphomolybdic acid;
the molybdenum source is a mixed solution obtained by dissolving a molybdenum-containing compound and sodium chloride in water and ammonia water; in the mixed solution, the mass ratio of the molybdenum compound to the sodium chloride is 0.6g to 0.24g to 0.3g to 0.12 g;
the dosage ratio of the molybdenum compound to the water and the ammonia is 0.3g: 0.5 ml: 0.5ml-0.6g: 1 ml: 1 ml;
the mass ratio of the molybdenum-containing compound to the sulfur powder is 0.6g to 0.6g-1 g.
In the molybdenum source carrier, the carrier is a silica gel plate or an alumina plate.
The preparation of the molybdenum source carrier comprises the following steps: placing the molybdenum source on the carrier. In particular, the molybdenum source may be placed on the support by dropwise addition. The dropping rate is not particularly limited.
In the chemical vapor deposition step, the area where the sulfur powder is located is a low-temperature area; the temperature of the low-temperature zone is specifically 240-260 ℃;
the area where the substrate and the molybdenum source carrier are located is a high-temperature area; the temperature of the high-temperature zone is specifically 600-700 ℃; specifically 650-680 ℃.
The chemical vapor deposition comprises:
1) the low-temperature area keeps the room temperature unchanged, and the high-temperature area is heated to 120 ℃ from the room temperature after 5 minutes and then kept;
2) the low temperature zone is heated to 240-260 ℃ after 22 minutes; the temperature of the high-temperature zone is raised to 480 ℃ after 12min, and then raised to 650-680 ℃ after 10 min;
3) the constant temperature of the low temperature zone is kept at 240-260 ℃ for 15min or 16min, the constant temperature of the high temperature zone is kept at 650-680 ℃ for 12-20min or 15min or 16min, and the temperature is naturally reduced.
The carrier gas used for the chemical vapor deposition is argon;
the flow rate of the carrier is 90-120 sccm; specifically 90-100 sccm.
The substrate is a sapphire substrate.
The distance between the substrate and the molybdenum source carrier is 5-7 mm; in particular 5 mm.
In addition, the wafer-level single-layer molybdenum disulfide film prepared by the method also belongs to the protection scope of the invention.
Specifically, the wafer-level single-layer molybdenum disulfide film is a continuous film covering the substrate.
Compared with the prior art, the invention has the following beneficial effects:
1. the wafer-level continuous monolayer molybdenum disulfide film can be obtained by adopting a normal-pressure chemical vapor deposition method.
2. By adopting a mode of providing face-to-face raw materials, the molybdenum disulfide is uniformly deposited on the surface of the sapphire substrate, and the grown film is very uniform.
3. The method has good repeatability, is an ideal method for simply synthesizing the molybdenum disulfide single-layer film, and is expected to be applied to continuous mass production.
Drawings
FIG. 1 is a schematic view of an experimental apparatus for preparing a monolayer molybdenum disulfide film by chemical vapor deposition;
FIG. 2 is a scanning electron microscope image of molybdenum disulfide grown on a sapphire substrate;
FIG. 3 is a photograph of a real object of molybdenum disulfide grown on a 2 inch sapphire wafer substrate;
FIG. 4 is a Raman spectrum of a monolayer of molybdenum disulfide;
figure 5 is an atomic force microscope image of a monolayer of molybdenum disulfide.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Examples 1,
A preparation method of large-area monolayer molybdenum disulfide comprises the following steps:
the method adopts a normal pressure chemical vapor deposition method.
Preparing a silica gel plate, firstly dissolving 0.6g of ammonium molybdate in a mixed solution of 1ml of water and 1ml of ammonia, dissolving 0.24g of sodium chloride in water, mixing the two solutions, and dropwise adding the mixture onto the silica gel plate to obtain the molybdenum source carrier.
Weighing 0.6g of sulfur powder, placing the sulfur powder in a quartz boat in a temperature area on the left side of the tube furnace, and placing a molybdenum source carrier in a temperature area on the right side of a quartz tube of the tube furnace; the cleaned sapphire substrate was placed face down 5mm above the molybdenum source carrier.
Before heating, vacuumizing is carried out, air in the tube furnace is exhausted, and then argon with the flow rate of 100sccm is introduced to serve as carrier gas.
The specific temperature rising step is as follows:
in the first heating stage, the left temperature zone was kept at room temperature, and the right temperature zone was heated from room temperature to 120 ℃ over 5 minutes and then kept.
In the second heating stage, the temperature of the left temperature zone is raised to 260 ℃ after 22 minutes, the temperature of the right temperature zone is raised to 480 ℃ after 12 minutes, and then the temperature is raised to 680 ℃ after 10 minutes;
in the third heating stage, the left temperature zone is kept at the constant temperature of 260 ℃ for 15min, and the right temperature zone is kept at 680 ℃ for 12 min.
And (5) naturally cooling.
FIG. 2 is a scanning electron microscope image of molybdenum disulfide grown on a sapphire substrate, showing the sample morphology as a large area continuous molybdenum disulfide film;
FIG. 3 is a photograph of a real object of molybdenum disulfide grown on a 2 inch sapphire wafer substrate;
FIG. 4 is a Raman spectrum of a single-layer molybdenum disulfide, which shows that the shift difference between two characteristic peaks of the molybdenum disulfide obtained in this example is 20.4cm-1The prepared molybdenum disulfide is a single-layer film;
figure 5 is an atomic force microscope image of a monolayer of molybdenum disulfide having a film thickness of 0.8nm, further demonstrating that the molybdenum disulfide obtained in this example is a monolayer film.
Examples 2,
A preparation method of large-area monolayer molybdenum disulfide comprises the following steps:
the method adopts a normal pressure chemical vapor deposition method.
The silica gel plate was prepared by dissolving 0.6g of ammonium molybdate in a mixed solution of 1ml of water and 1ml of ammonia, and 0.24g of sodium chloride in water, mixing the two solutions, and dropping the mixture onto the silica gel plate.
Weighing 0.6g of sulfur powder, placing the sulfur powder in a quartz boat in a left temperature area of the tube furnace, and placing a silica gel plate in a right temperature area of a quartz tube of the tube furnace; and putting the cleaned sapphire substrate face down at a position 5mm above the silica gel plate.
Before heating, vacuumizing is carried out, air in the tube furnace is exhausted, and then argon with the flow rate of 100sccm is introduced to serve as carrier gas.
The specific temperature rising step is as follows:
in the first heating stage, the left temperature zone is kept constant at room temperature, and the right temperature zone is heated to 120 ℃ from room temperature after 5min and then kept.
In the second heating stage, the temperature of the left temperature zone is raised to 260 ℃ after 22 minutes, the temperature of the right temperature zone is raised to 480 ℃ after 12 minutes, and then the temperature is raised to 650 ℃ after 10 minutes;
in the third heating stage, the left temperature zone is kept at the constant temperature of 260 ℃ for 15min, and the right temperature zone is kept at 650 ℃ for 20 min.
And (5) naturally cooling.
Example 3
A preparation method of large-area monolayer molybdenum disulfide comprises the following steps:
the method adopts a normal pressure chemical vapor deposition method.
The silica gel plate was prepared by dissolving 0.6g of ammonium molybdate in a mixed solution of 1ml of water and 1ml of ammonia, and 0.24g of sodium chloride in water, mixing the two solutions, and dropping the mixture onto the silica gel plate.
Weighing 0.6g of sulfur powder, placing the sulfur powder in a quartz boat in a left temperature area of the tube furnace, and placing a silica gel plate in a right temperature area of a quartz tube of the tube furnace; and putting the cleaned sapphire substrate face down at a position 5mm above the silica gel plate.
Before heating, vacuumizing is carried out, air in the tube furnace is exhausted, and then argon with the flow rate of 120sccm is introduced to serve as carrier gas.
The specific temperature rising step is as follows:
in the first heating stage, the left temperature zone is kept constant at room temperature, and the right temperature zone is heated to 120 ℃ from room temperature after 5min and then kept.
In the second heating stage, the temperature of the left temperature zone is raised to 260 ℃ after 22 minutes, the temperature of the right temperature zone is raised to 480 ℃ after 12 minutes, and then the temperature is raised to 680 ℃ after 10 minutes; in the third heating stage, the left temperature zone is kept at the constant temperature of 260 ℃ for 15min, and the right temperature zone is kept at 680 ℃ for 15 min.
And (5) naturally cooling.
Example 4
A preparation method of large-area monolayer molybdenum disulfide comprises the following steps:
the method adopts a normal pressure chemical vapor deposition method.
The silica gel plate was prepared by dissolving 0.6g of ammonium molybdate in a mixed solution of 1ml of water and 1ml of ammonia, and 0.24g of sodium chloride in water, mixing the two solutions, and dropping the mixture onto the silica gel plate.
Weighing 0.6g of sulfur powder, placing the sulfur powder in a quartz boat in a left temperature area of the tube furnace, and placing a silica gel plate in a right temperature area of a quartz tube of the tube furnace; and putting the cleaned sapphire substrate face down at a position 5mm above the silica gel plate.
Before heating, vacuumizing is carried out, air in the tube furnace is exhausted, and then argon with the flow rate of 100sccm is introduced to serve as carrier gas.
The specific temperature rising step is as follows:
in the first heating stage, the left temperature zone was kept at room temperature, and the right temperature zone was heated from room temperature to 120 ℃ over 5 minutes and then kept.
In the second heating stage, the temperature of the left side temperature zone is raised to 240 ℃ after 22 minutes, the temperature of the right side temperature zone is raised to 480 ℃ after 12 minutes, and then the temperature is raised to 650 ℃ after 10 minutes;
in the third heating stage, the left temperature zone is kept at the constant temperature of 240 ℃ for 16min, and the right temperature zone is kept at 650 ℃ for 16 min.
And (5) naturally cooling.
Claims (10)
1. A method of preparing a wafer-level monolayer molybdenum disulfide film, comprising:
and placing the sulfur powder at the upstream of the gas path, placing the substrate and the molybdenum source carrier at the downstream of the gas path in a face-to-face manner, and carrying out chemical vapor deposition to obtain the wafer-level single-layer molybdenum disulfide film after the deposition is finished.
2. The method of claim 1, wherein: the molybdenum source contains a molybdenum-containing compound;
the molybdenum-containing compound is specifically selected from at least one of ammonium molybdate, sodium molybdate and phosphomolybdic acid;
the molybdenum source is a mixed solution obtained by dissolving a molybdenum-containing compound and sodium chloride in water and ammonia water; in the mixed solution, the mass ratio of the molybdenum compound to the sodium chloride is 0.6g to 0.24g to 0.3g to 0.12 g;
the dosage ratio of the molybdenum compound to the water and the ammonia is 0.3g: 0.5 ml: 0.5ml-0.6g: 1 ml: 1 ml;
the mass ratio of the molybdenum-containing compound to the sulfur powder is 0.6g to 0.6g-1 g.
3. The method according to claim 1 or 2, characterized in that: in the molybdenum source carrier, the carrier is a silica gel plate or an alumina plate.
4. A method according to any one of claims 1 to 3, wherein: in the chemical vapor deposition step, the area where the sulfur powder is located is a low-temperature area; the temperature of the low-temperature zone is specifically 240-260 ℃;
the area where the substrate and the molybdenum source carrier are located is a high-temperature area; the temperature of the high-temperature zone is specifically 600-700 ℃; specifically 650-680 ℃.
5. The method according to any one of claims 1 to 4, wherein: the chemical vapor deposition comprises:
1) the low-temperature area keeps the room temperature unchanged, and the high-temperature area is heated from the room temperature to 120 ℃ after 5 minutes and then kept for 8 minutes;
2) the low temperature zone is heated to 240-260 ℃ after 22 minutes; the temperature of the high-temperature zone is raised to 480 ℃ after 12min, and then raised to 650-680 ℃ after 10 min;
3) the constant temperature of the low temperature zone is kept at 240-260 ℃ for 15min or 16min, the constant temperature of the high temperature zone is kept at 650-680 ℃ for 12-20min or 15min or 16min, and the temperature is naturally reduced.
6. The method according to any one of claims 1 to 5, wherein: the carrier gas used for the chemical vapor deposition is argon;
the flow rate of the carrier is 90-120 sccm; specifically 90-100 sccm.
7. The method according to any one of claims 1 to 6, wherein: the substrate is a sapphire substrate.
8. The method according to any one of claims 1 to 7, wherein: the distance between the substrate and the molybdenum source carrier is 5-7 mm.
9. A wafer-level monolayer molybdenum disulfide film prepared by the method of any of claims 1-8.
10. The wafer-level single layer molybdenum disulfide film of claim 9, wherein: the wafer-level single-layer molybdenum disulfide film is a continuous film covering the substrate.
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| CN115354392A (en) * | 2022-08-16 | 2022-11-18 | 武汉大学 | Preparation method of large-size single crystal molybdenum disulfide |
| CN115491656A (en) * | 2022-08-09 | 2022-12-20 | 大连理工大学盘锦产业技术研究院 | Single-layer tungsten diselenide and preparation method thereof |
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