CN113122818A - Method for preparing wafer-level single-layer molybdenum disulfide film - Google Patents
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 50
- 239000002356 single layer Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 36
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 34
- 239000011733 molybdenum Substances 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 19
- 239000000741 silica gel Substances 0.000 claims abstract description 18
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 14
- 239000010980 sapphire Substances 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 6
- 239000011609 ammonium molybdate Substances 0.000 claims description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 239000005078 molybdenum compound Substances 0.000 claims description 4
- 150000002752 molybdenum compounds Chemical class 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract 4
- 238000010924 continuous production Methods 0.000 abstract 1
- 230000009977 dual effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 16
- 239000010453 quartz Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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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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- 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
- C23C16/44—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 method of coating
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
本发明公开了一种制备晶圆级积单层二硫化钼薄膜的方法。该方法基于化学气相沉积技术，采用“面对面”提供钼源的方式，可以在蓝宝石晶圆衬底上生长连续、均匀的单层二硫化钼薄膜。该方法使用硅胶板或氧化铝板作为钼源载体，钼源前驱体以溶液的形式分散在硅胶板或氧化铝板上。在双温区化学气相沉积系统中，硫粉放置于左侧温区，蓝宝石衬底和钼源载体“面对面”放置于右侧温区。在高温下，硫蒸气与钼源发生化学反应，在蓝宝石衬底均匀沉积，得到大面积的单层二硫化钼薄膜。该方法操作简单，实验结果重复性好，对大面积单层二硫化钼薄膜的连续化生产和电子器件应用具有重要意义。The invention discloses a method for preparing a wafer-level monolayer molybdenum disulfide thin film. The method is based on chemical vapor deposition technology, and the molybdenum source is provided "face-to-face" to grow a continuous and uniform monolayer molybdenum disulfide thin film on a sapphire wafer substrate. The method uses a silica gel plate or an alumina plate as the molybdenum source carrier, and the molybdenum source precursor is dispersed on the silica gel plate or the alumina plate in the form of a solution. In the dual temperature zone chemical vapor deposition system, the sulfur powder is placed in the left temperature zone, and the sapphire substrate and the molybdenum source carrier are placed "face to face" in the right temperature zone. At high temperature, the sulfur vapor reacts with the molybdenum source and is uniformly deposited on the sapphire substrate to obtain a large-area monolayer molybdenum disulfide thin film. The method is simple to operate and has good repeatability of experimental results, which is of great significance for the continuous production of large-area monolayer molybdenum disulfide thin films and the 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)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115058700A (en) * | 2022-06-24 | 2022-09-16 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
| CN115354392A (en) * | 2022-08-16 | 2022-11-18 | 武汉大学 | A kind of preparation method of large-scale 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 | Monolayer tungsten diselenide and its preparation method |
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| US20140353166A1 (en) * | 2013-05-09 | 2014-12-04 | North Carolina State University | Novel process for scalable synthesis of molybdenum disulfide monolayer and few-layer films |
| CN105272358A (en) * | 2015-06-01 | 2016-01-27 | 湘潭大学 | Preparation method for a large-area single-layer or few-layer molybdenum disulfide film |
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| CN106835073A (en) * | 2016-11-17 | 2017-06-13 | 北京交通大学 | A kind of preparation method of individual layer molybdenum bisuphide |
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| CN115058700A (en) * | 2022-06-24 | 2022-09-16 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
| CN115058700B (en) * | 2022-06-24 | 2023-07-07 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
| CN115491656A (en) * | 2022-08-09 | 2022-12-20 | 大连理工大学盘锦产业技术研究院 | Monolayer tungsten diselenide and its preparation method |
| CN115354392A (en) * | 2022-08-16 | 2022-11-18 | 武汉大学 | A kind of preparation method of large-scale single crystal molybdenum disulfide |
| CN115354392B (en) * | 2022-08-16 | 2023-09-01 | 武汉大学 | A kind of preparation method of large-scale single crystal molybdenum disulfide |
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