CN113957412A - Molybdenum disulfide film with consistent grain orientation height and preparation method thereof - Google Patents
Molybdenum disulfide film with consistent grain orientation height and preparation method thereof Download PDFInfo
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- CN113957412A CN113957412A CN202111106386.0A CN202111106386A CN113957412A CN 113957412 A CN113957412 A CN 113957412A CN 202111106386 A CN202111106386 A CN 202111106386A CN 113957412 A CN113957412 A CN 113957412A
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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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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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
- C23C16/52—Controlling or regulating the coating process
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Abstract
The invention provides a method for preparing a molybdenum disulfide film with consistent grain orientation on a sapphire substrate. The method comprises the following steps: c-plane sapphire is used as a substrate, and high-temperature annealing treatment is carried out on the substrate before growth; placing the sapphire substrate into a first quartz boat, and adding MoO3Mixing and grinding the mixture and NaCl, weighing the mixture and placing the mixture in a second quartz boat, and placing S powder in a third quartz boat; and (3) putting the three quartz boats into a chemical vapor deposition system cavity, introducing carrier gas, controlling the temperature in the cavity to perform a chemical vapor deposition process, and obtaining the molybdenum disulfide film with consistent grain orientation height on the sapphire substrate. The method solves the problem of random crystal orientation of the molybdenum disulfide prepared by a chemical vapor deposition method, realizes the preparation of the molybdenum disulfide film with highly consistent crystal orientation,has the advantages of simple process, low cost and the like, and is suitable for industrial batch production.
Description
Technical Field
The invention belongs to the technical field of two-dimensional materials, relates to a molybdenum disulfide film with consistent grain orientation height and a preparation method thereof, and particularly relates to a preparation method for growing molybdenum disulfide with a specific crystal orientation on a sapphire substrate.
Background
Transition Metal Dichalcogenides (TMDCs) are hot research in recent years internationally, and have a honeycomb structure similar to graphene and a general chemical coordination formula MX2(where M represents a transition metal atom and X is a chalcogen atom), for example molybdenum or tungsten in combination with sulfur, selenium or tellurium, typically for example molybdenum disulfide (MoS)2). Because adjacent positions in the single-layer TMDCs crystal lattice are occupied by different atoms, the inversion symmetry of the crystal lattice is broken, and a new quantum state, namely an energy valley quantum state, is introduced, and is a third intrinsic degree of freedom after charge and spin; meanwhile, TMDCs have strong spin-orbit coupling, which causes splitting of electron energy bands. These characteristics in turn allow the TMDCs to exhibit a novel set of physical properties. Such as high current on/off ratio at room temperature, spin valley polarization, spin orbit splitting, valley hall effect, superconductivity, and extraordinary giant magnetoresistance. Thus, MoS2The graphene has potential application value in the field of two-dimensional electronic devices compared with graphene.
To realize the application of these two-dimensional devices, it is necessary to prepare large-scale, high-quality MoS2Thin film, the current chemical vapor deposition method is a method for growing large-area MoS2An efficient method for thin films. However, during deposition, MoS2The grains tend to nucleate in random orientations on the substrate. When the crystal grains with different crystal orientations grow and are combined together, a polycrystalline film with a plurality of crystal boundaries is formed, thereby introducing strain and defects and greatly reducing MoS2The quality of the film. For example, grain boundaries can significantly reduce their carrier mobility and negatively impact their electrical and optical properties. Thus growing MoS with uniform grain orientation2The film is of great importance and is a technical problem which needs to be solved in the industry.
Disclosure of Invention
In view of the above-mentioned shortcomings and drawbacks of the methods for preparing molybdenum disulfide thin films, it is an object of the present invention to provide a method for growing a molybdenum disulfide thin film on a sapphire substrate, which can effectively control the crystal orientation of molybdenum disulfide grains to prepare a high-quality molybdenum disulfide thin film with highly uniform grain orientation.
The technical scheme adopted by the invention is as follows:
in a first aspect, a method for preparing molybdenum disulfide with a specific crystal orientation grown on a sapphire substrate is provided, and the method comprises the following steps:
selecting a sapphire substrate as a substrate, and putting the sapphire substrate into a first quartz boat;
step (II) molybdenum source selection MoO3Grinding the mixture of NaCl and the NaCl, putting the ground mixture into a second quartz boat, selecting S powder as a sulfur source, and putting the S powder into a third quartz boat;
placing a third quartz boat containing a sulfur source at the upstream of the airflow of the tube furnace of the chemical vapor deposition system, marking as a first temperature zone, placing a second quartz boat containing a molybdenum source and a first quartz boat containing a sapphire substrate at the downstream of the airflow of the tube furnace, marking as a second temperature zone, and introducing protective gas into the tube furnace;
and (4) heating the tube furnace to the set temperature, enabling the temperature of the first temperature zone to be 150-.
As a further preferred aspect of the present invention, in the step (one), the sapphire substrate selected is c-plane Al2O3The sapphire substrate is sequentially placed in acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, and then dried by dry nitrogen. Before growth, the first quartz boat containing sapphire substrate is sent into a heating zone of a tube furnace, and the sapphire substrate is annealed at 1000 ℃ in air, so that an edge is formed on the surface of the sapphire substrate<11-20>An atomically flat step of a particular crystal orientation. More preferably, the annealing treatment is carried out at 1000 ℃ for 1 hour.
As a further preferred aspect of the present invention, in the step (one), the annealed sapphire substrate polished surface is placed in a first quartz boat in a downward direction.
As a further preferred of the present invention, the first quartz boat, the second quartz boat and the third quartz boat are sequentially placed in acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes before use, and then dried by dry nitrogen.
As a further preferred aspect of the present invention, in the step (ii), the S powder: MoO3The mass ratio of (A) to (B) is 14: 1 to 26: 1, preferably 23: 1; in the molybdenum source, MoO3The mass ratio of NaCl to NaCl is 1.5: 1 to 2.5: 1, preferably 2: 1.
in a further preferred embodiment of the present invention, the first quartz boat and the second quartz boat are spaced apart by 5cm, and the second quartz boat and the third quartz boat are spaced apart by 6 cm.
In a further preferred embodiment of the present invention, in the step (iii), the protective gas is argon.
In the step (iv), before the temperature of the tube furnace is raised, the tube furnace is evacuated to approximately 0Pa, then gas replacement is performed using 500sccm of argon gas, and after the gas replacement operation is repeated three times, the argon gas is adjusted to 100sccm, and the pressure in the tube furnace is maintained at normal pressure.
As a further preferable aspect of the present invention, in the step (iv), the heating temperature and time of the second temperature zone are set by a program, and the first temperature zone is radiatively heated; and the second temperature zone is heated from room temperature to 550 ℃ at the heating rate of 10 ℃/min, then is heated to 650 ℃ at the heating rate of 7.5 ℃/min, grows at the constant temperature for 4-7 minutes, ends the experiment, and cools the sample to room temperature.
As a further preferable mode of the present invention, in the step (IV), when the temperature of the second temperature zone is increased to 300 ℃, the argon gas is reduced to 50sccm, and is kept unchanged in the subsequent temperature increasing and maintaining processes until the temperature of the second temperature zone is reduced to below 500 ℃ after the growth is finished, the argon gas is regulated to 100sccm, and is maintained at 100sccm until the experiment is finished.
In a second aspect, a molybdenum disulfide film is provided, which is prepared by the method. The crystal grain orientation of the molybdenum disulfide film is highly consistent.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the invention can prepare the molybdenum disulfide film with highly consistent crystal grain orientation.
(2) The molybdenum disulfide film obtained by the invention has the advantages of few crystal boundaries, less strain and defects, high quality and wide application prospect.
(3) The invention obviously reduces the evaporation MoO3Temperature required to make MoO3The evaporation temperature of the evaporator is reduced from about 1000 ℃ to 650 ℃, so that the large-scale industrial production becomes possible.
(4) The two-dimensional material prepared by the method has higher electron mobility and has wide application prospect in chiral luminescence transistors, high-performance integrated circuits and piezoelectric transistors.
Drawings
FIG. 1 is a schematic temperature profile of a molybdenum disulfide single crystal film prepared in example 1 of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of a highly uniform grain orientation molybdenum disulfide single crystal film prepared by chemical vapor deposition of example 1 of the present invention.
FIG. 3 is a Raman spectrum of a single crystal film of molybdenum disulfide prepared in example 1 of the present invention.
FIG. 4 is a photoluminescence spectrum of a single crystal film of molybdenum disulfide prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail with reference to the accompanying drawings and examples, but the present invention is not limited to the specific implementation.
In the following examples, S powder and MoO3Powders and NaCl powders were purchased from Alfa Aesar and were 99.5%, 99.95% and 99% pure, respectively. A single-side polished c-plane sapphire substrate was purchased from Jiangyin-Blueco Crystal Material Co.
Example 1
(1) And (3) placing the sapphire substrate in acetone, ethanol and deionized water in sequence, ultrasonically cleaning for 10 minutes, and then drying by dry nitrogen. The quartz boat was cleaned by the same cleaning method, and was sequentially placed in acetone, ethanol, deionized water for ultrasonic cleaning for 10 minutes, followed by blow-drying with dry nitrogen.
(2) The c-plane sapphire substrate was annealed at high temperature (1000 c) for 1 hour in air to obtain an atomically flat step along the <11-20> specific crystal orientation.
(3) And weighing the precursor by using a weighing balance. 6mg of MoO are weighed3The powder and 3mg NaCl powder were mixed well, ground for 10 minutes and placed in the second temperature zone. The annealed sapphire was also placed in the second temperature zone, downstream of the carrier gas at a distance of 5cm from the Mo source. 138mg of S powder was weighed and placed in the first warm zone.
(4) Before the temperature of the tube furnace is raised, a quartz tube of the tube furnace is vacuumized to be close to 0Pa, then high-purity argon of 500sccm is used for gas replacement to remove air in the quartz tube, the argon is adjusted to be 100sccm, and the pressure in the tube furnace is kept constant.
Setting the heating temperature and time of the second temperature zone by a program, and heating the first temperature zone in a radiation manner; and the second temperature zone is heated to 550 ℃ at the heating rate of 10 ℃/min, then heated to 650 ℃ at the heating rate of 7.5 ℃/min, and after the constant temperature growth is carried out for 6 minutes, the experiment is finished, a molybdenum disulfide film with consistent grain orientation height is grown on the sapphire substrate, and the sample is cooled to room temperature.
When the temperature of the second temperature zone is increased to 300 ℃, the argon is reduced to 50sccm and is kept unchanged in the subsequent temperature increasing and constant temperature processes until the temperature of the second temperature zone is reduced to below 500 ℃ after the growth is finished, the argon is regulated to 100sccm and is maintained at 100sccm until the experiment is finished.
FIG. 1 is a schematic temperature curve for preparing a molybdenum disulfide single crystal film.
Fig. 2 is a molybdenum disulfide film grown on a sapphire substrate for 6 minutes, and it can be clearly seen that the molybdenum disulfide film has a regular triangular shape and the orientation of the grains is highly uniform, including a small amount of 0/60 degree turning.
FIG. 3 is a Raman spectrum of a molybdenum disulfide single crystal film having a highly uniform grain orientation after 6 minutes of isothermal growth. An emission intensity of 417.6cm was observed in the Raman spectrum-1The obvious peak belongs to the signal of the sapphire substrate. 384.4cm-1The peak at (A) belongs to the in-plane E2gVibration mode, 405.0cm-1Out-of-plane A corresponding to the molybdenum disulfide film1gVibration mouldFormula (II) is shown. The distance between the two peaks is about 20.6cm-1The molybdenum disulfide film proved to be a single layer. A. the1gHas a full width at half maximum (FWHM) of about 4.5cm-1The result shows that the quality of the molybdenum disulfide single crystal film is very high.
FIG. 4 is a photoluminescence spectrum of the prepared molybdenum disulfide single crystal film. The strong peak at 694.4 nm was attributed to the sapphire substrate and the a peak at 661.2 nm corresponded to a direct exciton transition, indicating that a monolayer of molybdenum disulfide was a direct bandgap semiconductor. The full width at half maximum of the peak in the photoluminescence spectrum a was about 22.0 nm, indicating that the grown molybdenum disulfide film was a single layer with excellent optical characteristics.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method for growing molybdenum disulfide with a specific crystal orientation on a sapphire substrate is characterized by comprising the following steps:
selecting a sapphire substrate as a substrate, and putting the sapphire substrate into a first quartz boat;
step (II) molybdenum source selection MoO3Grinding the mixture of NaCl and the NaCl, putting the ground mixture into a second quartz boat, selecting S powder as a sulfur source, and putting the S powder into a third quartz boat;
placing a third quartz boat containing a sulfur source at the upstream of the airflow of the tube furnace of the chemical vapor deposition system, marking as a first temperature zone, placing a second quartz boat containing a molybdenum source and a first quartz boat containing a sapphire substrate at the downstream of the airflow of the tube furnace, marking as a second temperature zone, and introducing protective gas into the tube furnace;
and (4) heating the tube furnace to the set temperature, enabling the temperature of the first temperature zone to be 150-.
2. The method of claim 1The preparation method for growing the molybdenum disulfide with specific crystal orientation on the sapphire substrate is characterized in that in the step (I), the selected sapphire substrate is c-plane Al2O3Before growth, the first quartz boat containing sapphire substrate is fed into the heating zone of tube furnace, and the sapphire substrate is annealed at 1000 deg.C in air to form edge on the surface of sapphire substrate<11-20>An atomically flat step of a particular crystal orientation.
3. The method of claim 1, wherein in step (one), the polished sapphire substrate is placed in a first quartz boat with the polished surface facing downward.
4. The method for preparing molybdenum disulfide with specific crystal orientation grown on a sapphire substrate according to claim 1, wherein in step (II), S powder: MoO3The mass ratio of (A) to (B) is 14: 1 to 26: 1, preferably 23: 1; in the molybdenum source, MoO3The mass ratio of NaCl to NaCl is 1.5: 1 to 2.5: 1, preferably 2: 1.
5. the method of claim 1, wherein the first quartz boat is separated from the second quartz boat by 5cm, and the second quartz boat is separated from the third quartz boat by 6 cm.
6. The method according to claim 1, wherein in the fourth step, before the temperature of the tube furnace is raised, the tube furnace is evacuated to a pressure close to 0Pa, then gas replacement is performed using 500sccm of argon gas, and after the gas replacement operation is repeated three times, the pressure of the argon gas is adjusted to 100sccm, and the pressure in the tube furnace is kept constant.
7. The method for preparing molybdenum disulfide with a specific crystal orientation grown on a sapphire substrate as claimed in claim 1, wherein in step (IV), the heating temperature and time of the second temperature zone are set by a program, and the first temperature zone is heated by radiation; and the second temperature zone is heated from room temperature to 550 ℃ at the heating rate of 10 ℃/min, then is heated to 650 ℃ at the heating rate of 7.5 ℃/min, grows at the constant temperature for 4-7 minutes, ends the experiment, and cools the sample to room temperature.
8. The method according to claim 7, wherein in the step (IV), when the temperature of the second temperature zone is increased to 300 ℃, the amount of argon gas is reduced to 50sccm, and the argon gas is kept unchanged during the subsequent temperature increasing and maintaining processes until the temperature of the second temperature zone is reduced to below 500 ℃ after the growth is finished, the amount of argon gas is regulated to 100sccm, and the argon gas is maintained at 100sccm until the experiment is finished.
9. A molybdenum disulfide film produced by the method of any one of claims 1-8.
10. The molybdenum disulfide film of claim 9, wherein the molybdenum disulfide film has a highly uniform grain orientation.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380334A (en) * | 2022-01-26 | 2022-04-22 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
| CN114737164A (en) * | 2022-04-19 | 2022-07-12 | 电子科技大学 | Method for preparing centimeter-level multiphase molybdenum disulfide film |
| CN114855266A (en) * | 2022-03-25 | 2022-08-05 | 南京邮电大学 | Identification method of two-dimensional tungsten disulfide film grain boundary |
| 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 | Preparation method of large-size single crystal molybdenum disulfide |
| CN115650297A (en) * | 2022-11-10 | 2023-01-31 | 江南大学 | Large-area controllable preparation method of two-dimensional molybdenum disulfide dendritic crystal |
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| US20190330735A1 (en) * | 2017-04-17 | 2019-10-31 | Massachusetts Institute Of Technology | Chemical Vapor Transport Growth of Two-Dimensional Transition-Metal Dichalcogenides |
| CN110777356A (en) * | 2019-11-12 | 2020-02-11 | 天津理工大学 | Rare earth doped molybdenum sulfide monomolecular layer film and preparation method thereof |
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| US20190330735A1 (en) * | 2017-04-17 | 2019-10-31 | Massachusetts Institute Of Technology | Chemical Vapor Transport Growth of Two-Dimensional Transition-Metal Dichalcogenides |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380334A (en) * | 2022-01-26 | 2022-04-22 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
| CN114380334B (en) * | 2022-01-26 | 2023-09-19 | 江西师范大学 | Preparation method and application of molybdenum disulfide with spiral pyramid structure |
| CN114855266A (en) * | 2022-03-25 | 2022-08-05 | 南京邮电大学 | Identification method of two-dimensional tungsten disulfide film grain boundary |
| CN114737164A (en) * | 2022-04-19 | 2022-07-12 | 电子科技大学 | Method for preparing centimeter-level multiphase molybdenum disulfide film |
| 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 | Preparation method of large-size single crystal molybdenum disulfide |
| CN115354392B (en) * | 2022-08-16 | 2023-09-01 | 武汉大学 | Preparation method of large-size monocrystalline molybdenum disulfide |
| CN115650297A (en) * | 2022-11-10 | 2023-01-31 | 江南大学 | Large-area controllable preparation method of two-dimensional molybdenum disulfide dendritic crystal |
| CN115650297B (en) * | 2022-11-10 | 2024-01-26 | 江南大学 | Large-area controllable preparation method of two-dimensional molybdenum disulfide dendrites |
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