CN111041450A - Preparation method for growing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition - Google Patents
Preparation method for growing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition Download PDFInfo
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- CN111041450A CN111041450A CN202010007011.8A CN202010007011A CN111041450A CN 111041450 A CN111041450 A CN 111041450A CN 202010007011 A CN202010007011 A CN 202010007011A CN 111041450 A CN111041450 A CN 111041450A
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- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000002356 single layer Substances 0.000 title claims abstract description 27
- 239000003513 alkali Substances 0.000 title claims abstract description 26
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 24
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000012159 carrier gas Substances 0.000 claims description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011144 upstream manufacturing Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000005424 photoluminescence Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- 238000001237 Raman spectrum Methods 0.000 description 6
- 238000000879 optical micrograph Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Classifications
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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
-
- 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
Abstract
The invention discloses a preparation method for growing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition, belonging to the field of nano materials. The method adopts alkali as an accelerant to assist in growing the monolayer tungsten disulfide in the growth process of the chemical vapor deposition method. Wherein the mass ratio of the tungsten oxide source to the alkali is 8:1-2: 1. The invention uses alkali to assist the growth of tungsten disulfide, can effectively reduce the growth temperature, realizes the rapid growth and preparation of a large-area single-layer tungsten disulfide sample under normal pressure, and the prepared tungsten disulfide has high photoluminescence intensity. The experimental method has the advantages of simple process, good repeatability, environmental friendliness, low raw material cost and suitability for large-scale production.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a tungsten disulfide single-layer thin film material and a preparation method thereof.
Background
In 2004, the successful preparation of graphene opens a new era of two-dimensional materials. For two-dimensional materials, which are only a few atoms thick, the electrons are confined to a two-dimensional scale, and their electronic properties are enhanced. Therefore, the two-dimensional material is used as the channel material, so that the electrical property of the device is enhanced, and the device has the characteristics of higher switching ratio, responsivity, carrier mobility and the like compared with the traditional material. Tungsten disulfide is an important two-dimensional material, the band gap of the tungsten disulfide increases (1.3-2.0eV) with the decrease of the number of layers, the multiple layers are indirect band gap semiconductors, the single-layer tungsten disulfide is converted into a direct band gap semiconductor material, and the photoelectric conversion efficiency is obviously improved. Therefore, the single-layer tungsten disulfide has a great application prospect in the fields of electronic and photoelectric devices such as nonlinear optical devices, light emitting diodes, ultra-sensitive photodetectors, field effect transistors and the like.
The existing methods for preparing the monolayer tungsten disulfide mainly comprise a mechanical stripping method, a hydrothermal synthesis method, a Chemical Vapor Deposition (CVD) method and the like. But compared with the defects of uncontrollable sample size and layer number of a stripping method and a hydrothermal method, the chemical vapor deposition method can realize large-area single-layer preparation, has good repeatability and is expected to realize industrial production. Although studies have reported CVD preparation of tungsten disulfide, it is very challenging to synthesize high quality monolayers of tungsten disulfide with larger sample sizes at lower temperatures, which greatly limits their practical applications.
Disclosure of Invention
The invention provides a preparation method for growing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition, aiming at the problems that the shape and the number of layers of a sample prepared by a stripping method and a hydrothermal method are uncontrollable, the time cost is high, and the general growth temperature of growing tungsten disulfide on a silicon/silicon dioxide substrate by a chemical vapor deposition method is higher at present. The process is simple and low in material cost.
In order to solve the problems, the invention adopts the technical scheme that:
a preparation method for growing large-area monolayer tungsten disulfide by alkali-assisted chemical vapor deposition is characterized in that alkali is used as an accelerant and is added into a tungsten source, so that the growth temperature is reduced to 700-800 ℃, and the preparation of large-area monolayer tungsten disulfide at a lower temperature is realized.
The method specifically comprises the following steps:
(1) cleaning the surface of the growth substrate;
(2) preparing a tungsten source precursor, namely mixing tungsten oxide powder and alkali according to a certain mass ratio, and mechanically grinding by using a mortar;
(3) transferring a tungsten source prepared by mixing tungsten oxide powder and alkali into a crucible, placing a growth substrate above the tungsten source, wherein the substrate is parallel to a crucible opening and has a gap, and a polishing surface faces downwards and is used for growing tungsten disulfide on the substrate, and then placing the crucible in a central temperature area of a tube furnace; weighing excessive high-purity sulfur powder, placing the weighed high-purity sulfur powder in another crucible, placing the crucible in a low-temperature region with relatively low upstream of carrier gas flow, wherein the carrier gas enters from one end of the tube furnace, and is discharged from the other end of the tube furnace;
(4) in the chemical vapor deposition reaction process, inert gas is used as carrier gas, and the temperature of the center of the tube furnace is set according to time periods as follows: the temperature is divided into four stages, wherein the first stage is a stage of exhausting in the tubular furnace, the second stage is a stage of removing the combined water in the precursor source, the third stage is a growth stage of tungsten disulfide, and the fourth stage is a natural cooling stage.
Preferably, the cleaning in the step (1) is ultrasonic cleaning by sequentially using acetone, isopropanol and deionized water, wherein the ultrasonic time is 15min, and the power is set to be 60W.
Wherein, the alkali in the step (2) preferably comprises one or more of potassium hydroxide, sodium hydroxide and the like.
Preferably, in the step (2), the tungsten oxide powder and the alkali are mixed and ground according to the mass ratio of 8:1-2: 1.
Wherein, the temperature range of the sulfur powder position in the step (3) is preferably 120-300 ℃, and the sulfur powder is introduced in the third stage to provide a sulfur source for the reaction.
Preferably, in the step (4), the first stage is to introduce 300-; in the second stage, the flow rate is reduced to 100-200sccm and used as carrier gas to carry out reaction, the temperature of the tubular furnace is heated to 100-300 ℃ at the heating rate of 20-50 ℃/min, the temperature is kept for 20-60min, and the bound water is removed; in the third stage, keeping the air flow unchanged, heating the furnace temperature to 700-800 ℃ at the temperature rise rate of 20-50 ℃/min, and the growth time is 1-15 min; and finally, naturally cooling the tube furnace to room temperature after the growth is finished.
The growth substrate includes: silicon/silicon dioxide substrates, sapphire, mica, and the like.
The invention has the following beneficial effects:
the invention adopts the atmospheric pressure chemical vapor deposition method to grow the tungsten disulfide film, controls the stable volatilization of the tungsten source through the alkali-assisted growth, reduces the growth temperature of the tungsten disulfide to 700-800 ℃, effectively prepares the single-layer film, and improves the area and the photoluminescence intensity of the single-layer tungsten disulfide sample. The preparation method has the advantages of simple process, good repeatability, environmental friendliness, low raw material cost and suitability for large-scale production.
Drawings
FIG. 1 is a schematic diagram of an experimental apparatus for growing a large-area single layer of tungsten disulfide by alkali-assisted chemical vapor deposition according to the present invention;
FIG. 2 is an optical microscope image in example 1;
FIG. 3 is a Raman spectrum of example 1;
FIG. 4 is a photoluminescence spectrum of example 1;
FIG. 5 is an optical microscope image in example 2;
FIG. 6 is a Raman spectrum of example 2;
FIG. 7 is a photoluminescence spectrum of example 2;
FIG. 8 is an optical microscope image of example 3;
FIG. 9 is a Raman spectrum of example 3;
FIG. 10 is the photoluminescence spectrum of example 3;
1: carrier gas inlet
2: heating belt
3: muffle furnace
4: sulfur powder
5: crucible pot
6: growth substrate
7: tungsten source and alkali mixed powder
8: crucible pot
9: and a carrier gas outlet.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1:
referring to fig. 1, a large area monolayer of tungsten disulfide is grown by an alkali-assisted chemical vapor deposition process.
SiO2Cleaning a/Si substrate, in the experiment, 400-micron-thick SiO2/Si (wherein SiO2 is 300nm) is used as a growth substrate, a 4-inch silicon wafer is cut into square substrates with the size of 1cm x 1cm, and then cleaning is carried out, wherein the cleaning process comprises the following steps: respectively performing ultrasonic treatment for 15min by using acetone, isopropanol and deionized water, and setting the power to be 60W;
taking a proper amount of mixed powder of potassium hydroxide and tungsten trioxide, wherein the mass ratio of tungsten trioxide to potassium hydroxide is 2:1, putting the mixed powder into an alumina crucible as a tungsten source, placing a silicon/silicon dioxide substrate sheet right above the mixed powder, reversely covering the substrate sheet on the crucible, and then placing the substrate sheet in the center of a heating temperature zone of a tubular furnace;
weighing excess sulfur powder with the purity of 99.999 percent, placing the excess sulfur powder in an alumina crucible, and placing the alumina crucible in a quartz tube at the upstream of a tube furnace, wherein the distance from the center of a temperature zone is 20-25 cm; and the heating belt is wrapped on the periphery of the tube wall of the quartz tube at the position of the sulfur source (the upstream refers to the flowing direction of argon);
in the first stage of growth, argon gas of 300sccm is introduced for 15min at room temperature, and the furnace tube is replaced and cleaned to exhaust air in the furnace tube; in the second stage, the flow rate is adjusted to be reduced to 100sccm and used as carrier gas to carry out reaction, the temperature of the tubular furnace is heated to 170 ℃ at the heating rate of 20 ℃/min, the temperature is kept for 30min, and bound water in the precursor is removed; in the third stage, keeping the air flow unchanged, heating the furnace temperature to 750 ℃ at the heating rate of 50 ℃/min, opening a sulfur temperature zone heating belt when the temperature of a central temperature zone is heated to 500 ℃, setting the temperature of the sulfur heating belt to be 200 ℃, starting to supply a sulfur source for an experiment, and keeping the temperature for 5min when the temperature is heated to 750 ℃; and finally, after the growth is finished, closing the sulfur heating belt, moving the heating belt to the cold end of the quartz tube, and naturally cooling the quartz tube to room temperature by using the tube furnace.
After preparation, the samples were removed for testing.
Fig. 2 is an optical microscope image of the prepared sample, and it can be seen that the sample is relatively uniform and the sample size can reach 129 μm.
FIG. 3 is a Raman spectrum of a prepared sample, in which a difference in wavenumber of 65.6cm can be seen-1It was demonstrated that a single layer film of tungsten disulfide was obtained.
Figure 4 is a photoluminescence spectrum of a sample prepared with a relatively sharp single peak at 628.7nm and a relative photoluminescence intensity of about 55000 at a laser power of 300W, again indicating that the large area tungsten disulphide prepared by this method is a monolayer and of relatively high quality.
Example 2 (i.e., comparative example)
The same as example 1, except that the mass ratio of tungsten trioxide to potassium hydroxide was 1:1, the other steps were identical.
FIG. 5 is an optical microscope image of a prepared sample, where it can be seen that the sample is small in size and not very uniform; FIG. 6 is a Raman spectrum of a prepared sample, in which a wave number difference of 68.4cm can be seen-1It was confirmed that a multilayer film of tungsten disulfide was obtained; it can be seen in fig. 7 that the relative value of photoluminescence intensity is about 3700 and the crystal quality is poor at the same laser power as in example 1.
Example 3
The same as example 1, the difference with example 1 is that NaOH is used as the base, and the other steps are the same.
FIG. 5 is an optical microscope image of the prepared sample, and it can be seen that the sample is relatively uniform and the sample size is increased to 203 μm; FIG. 6 is a Raman spectrum of a prepared sample, in which a difference in wavenumber of 65.7cm can be seen-1The obtained tungsten disulfide single-layer film is proved to be obtained; fig. 7 shows that the relative value of photoluminescence intensity is 65000 and the crystal quality is further improved under the same laser power as in example 1.
In conclusion, the invention provides a novel method for preparing a large-area single-layer tungsten disulfide material, and the controllable growth of the large-area single-layer tungsten disulfide at a lower temperature is realized by adding alkali for auxiliary growth.
Claims (7)
1. A preparation method for growing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition is characterized by comprising the following steps:
(1) cleaning the surface of the growth substrate;
(2) preparing a tungsten source precursor, namely mixing tungsten oxide powder and alkali according to a certain mass ratio, and mechanically grinding by using a mortar;
(3) transferring a tungsten source prepared by mixing tungsten oxide powder and alkali into a crucible, placing a growth substrate above the tungsten source, wherein the substrate is parallel to a crucible opening and has a gap, and a polishing surface faces downwards and is used for growing tungsten disulfide on the substrate, and then placing the crucible in a central temperature area of a tube furnace; weighing excessive high-purity sulfur powder, placing the weighed high-purity sulfur powder in another crucible, placing the crucible in a low-temperature region with relatively low upstream of carrier gas flow, wherein the carrier gas enters from one end of the tube furnace, and is discharged from the other end of the tube furnace;
(4) in the chemical vapor deposition reaction process, inert gas is used as carrier gas, and the temperature of the center of the tube furnace is set according to time periods as follows: the temperature is divided into four stages, wherein the first stage is a stage of exhausting in the tubular furnace, the second stage is a stage of removing the combined water in the precursor source, the third stage is a growth stage of tungsten disulfide, and the fourth stage is a natural cooling stage.
2. The preparation method for large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition growth according to claim 1, wherein the cleaning in step (1) is ultrasonic cleaning with acetone, isopropanol and deionized water in sequence, the ultrasonic time is 15min, and the power is set to be 60W.
3. The method for preparing large-area single-layer tungsten disulfide by alkali-assisted chemical vapor deposition according to claim 1, wherein the alkali in step (2) is one or more selected from potassium hydroxide and sodium hydroxide.
4. The preparation method for growing the large-area single-layer tungsten disulfide by the alkali-assisted chemical vapor deposition as claimed in claim 1, wherein in the step (2), the tungsten oxide powder and the alkali are mixed and ground according to the mass ratio of 8:1-2: 1.
5. The method as claimed in claim 1, wherein the temperature of the sulfur powder in step (3) is in the range of 120-300 ℃, and the sulfur powder is introduced in the third stage to provide a sulfur source for the reaction.
6. The method as claimed in claim 1, wherein the first step of step (4) is performed by introducing 300-500sccm inert gas at room temperature for 15-30min to replace and clean the furnace tube, so as to exhaust the air in the tube furnace; in the second stage, the flow rate is reduced to 100-200sccm and used as carrier gas to carry out reaction, the temperature of the tubular furnace is heated to 100-300 ℃ at the heating rate of 20-50 ℃/min, the temperature is kept for 20-60min, and the bound water is removed; in the third stage, keeping the air flow unchanged, heating the furnace temperature to 700-800 ℃ at the temperature rise rate of 20-50 ℃/min, and the growth time is 1-15 min; and finally, naturally cooling the tube furnace to room temperature after the growth is finished.
7. A monolayer of tungsten disulphide obtainable by a process according to any one of claims 1 to 6.
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| CN111893565A (en) * | 2020-08-04 | 2020-11-06 | 中国人民解放军国防科技大学 | Method for growing single-layer molybdenum disulfide or molybdenum diselenide by using promoter |
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