CN114990523A - Two-dimensional material torsional angle WS 2 Preparation of (A) and torsion Angle WS of two-dimensional Material 2 - Google Patents
Two-dimensional material torsional angle WS 2 Preparation of (A) and torsion Angle WS of two-dimensional Material 2 Download PDFInfo
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- CN114990523A CN114990523A CN202210561461.0A CN202210561461A CN114990523A CN 114990523 A CN114990523 A CN 114990523A CN 202210561461 A CN202210561461 A CN 202210561461A CN 114990523 A CN114990523 A CN 114990523A
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 106
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 70
- 239000010453 quartz Substances 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 30
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 25
- 239000010937 tungsten Substances 0.000 claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012159 carrier gas Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical group O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 30
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 19
- 229910052717 sulfur Inorganic materials 0.000 claims description 15
- 239000011780 sodium chloride Substances 0.000 claims description 14
- 239000011593 sulfur Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052786 argon Inorganic materials 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000005693 optoelectronics Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 9
- 238000001237 Raman spectrum Methods 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 238000000103 photoluminescence spectrum Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000879 optical micrograph Methods 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 125000004434 sulfur atom Chemical group 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- XCUPBHGRVHYPQC-UHFFFAOYSA-N sulfanylidenetungsten Chemical compound [W]=S XCUPBHGRVHYPQC-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal chalcogenide compound Chemical class 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
- C23C16/52—Controlling or regulating the coating process
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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
The invention discloses a two-dimensional material torsion angle WS 2 Preparation of (A) and torsion Angle WS of two-dimensional Material 2 The method comprises the steps of taking silicon dioxide/silicon wafer as a substrate, taking a tungsten source and sulfur powder as raw materials, and performing two-dimensional material torsion angle WS on the silicon dioxide surface of the substrate by adopting a chemical vapor deposition method 2 Growing of (3); the two-dimensional material twist angle WS 2 The growth container is a quartz tube, and argon is introduced into the quartz tube to be used as carrier gas; the quartz tube is also internally provided with a quartz test tube with two open ends for placing a tungsten source and a substrate for chemical vapor deposition; the flow of argon is 50-180 sccm; the reaction temperature of the chemical vapor deposition is 750-850 ℃. The experimental process is simple, the cost is low, and the torsion angle WS of the prepared two-dimensional material 2 The surface is even and flat, the quality is high, and the method has important significance for researching novel torsion angle optoelectronics and photoelectric integrated devices.
Description
Technical Field
The invention belongs to the field of nano materials, and relates to a torsion angle WS of a two-dimensional material 2 Preparation and two-dimensional material torsion angle WS 2 。
Background
WS 2 Is a transition metal chalcogenide compound having a layered structure, and has a graphene-like layered structure. Single layer WS 2 The tungsten-sulfur composite material is composed of three layers of atoms, planes of tungsten atoms and planes of sulfur atoms are arranged in a hexagonal array mode, and the tungsten atoms are sandwiched between the two layers of sulfur atoms to form an S-W-S atomic layer structure with a sandwich structure. The tungsten atoms are respectively combined with three adjacent sulfur atoms on the upper layer and the lower layer by covalent bonds. Similarly, each sulfur atom is covalently bonded to three tungsten atoms, respectively, to form a triangular pyramid. Multilayer or bulk WS 2 Is formed by stacking single layers. WS 2 Has unique two-dimensional layered structure, resulting in excellent mechanical property, electrical property and optical property. Wherein chemical vapor deposition is applied to WS 2 Applications in semiconductor performance are of great interest and are currently recognized as the most promising WS 2 The preparation method of (1). In recent years, researchers have worked on WS 2 Is gradually increasing, but the twist angle WS is prepared in one step by the CVD method 2 The research of materials is relatively limited. Therefore, the inventors have made intensive studies to invent a method for preparing the twist angle WS of a two-dimensional material by a one-step CVD method 2 And obtaining a two-dimensional material torsion angle WS 2 。
Disclosure of Invention
The invention provides a two-dimensional material torsion angle WS by a one-step CVD method 2 Preparation and two-dimensional material torsion angle WS 2 . The experimental process is simple, the raw materials are easy to obtain, and the prepared torsion angle WS 2 Has clean surface, high quality and wide Moire angle distribution range.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
two-dimensional material torsion angle WS 2 The preparation process of (1) by oxidation ofThe silicon/silicon chip is used as a substrate, and the silicon dioxide surface of the substrate is subjected to two-dimensional material torsion angle WS by adopting a chemical vapor deposition method 2 Growing of (3); the growth container is a quartz tube, and the carrier gas in the quartz tube is inert gas; according to the flow direction of carrier gas, a sulfur source is placed in the quartz tube, a quartz test tube with openings at two ends is arranged at the downstream of the sulfur source, and a tungsten source and a substrate are placed in the quartz test tube; the flow rate of the carrier gas is 50-180 sccm; the reaction temperature of the chemical vapor deposition is 750-850 ℃.
Optionally, the silicon dioxide/silicon wafer substrates have two pieces, the silicon dioxide surfaces of the two silicon dioxide/silicon wafer substrates are respectively stacked back to back upwards or downwards, and the tungsten source is placed at a position 0.5cm in front of the substrates.
Optionally, the tungsten source is tungsten trioxide powder or tungsten chloride powder; the sulfur source is S powder; the dosage of the tungsten source is 10-40 mg, and the sulfur source is sufficient.
Optionally, NaCl is added into the tungsten source, and the addition amount of the NaCl is 1-4 mg.
Optionally, the temperature rise rate of the carrier gas is 10-50 ℃/min.
Optionally, the distance between the tungsten source and the sulfur source is 3-8 cm.
Optionally, the growth time of the chemical vapor deposition is 5-30 min.
Preferably, a two-dimensional material twist angle WS 2 The preparation method specifically comprises the following steps:
(1) cutting the silicon dioxide/silicon substrate into sheets of 0.9cm x 3cm, and stacking the silicon dioxide surfaces back to back in a quartz test tube with the inner diameter of 10mm and openings at two ends in the quartz test tube;
(2)20mg of tungsten source was placed in a quartz tube 0.5cm in front of the substrate and 1mg of sodium chloride was added;
(3) placing the quartz test tube into a quartz tube with an inner diameter of 25mm, placing the tungsten source end close to the air inlet of the quartz tube, heating the sulfur source and the tungsten source at a distance of 4cm in a tube-type atmosphere furnace to perform two-dimensional material torsion angle WS 2 Chemical vapor deposition of (2).
Two-dimensional material torsional angle WS 2 The two-dimensional material twist angle WS 2 Using any of the two dimensions of the inventionMaterial torsion angle WS 2 The preparation method is used for preparing the compound.
The invention has the advantages that:
the invention successfully prepares the two-dimensional material torsion angle WS with uniform surface, no pollution and high quality 2 The preparation process is simple and easy to operate.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure without limiting the disclosure. In the drawings:
FIG. 1 is a schematic diagram of experimental preparation of examples and comparative examples of the present invention;
FIG. 2 is an optical micrograph of example 1 of the present invention;
FIG. 3 is a Raman spectrum of example 1 of the present invention;
FIG. 4 shows photoluminescence spectra of example 1 according to the invention;
FIG. 5 is an optical micrograph of example 2 of the present invention;
FIG. 6 is a Raman spectrum of example 2 of the present invention;
FIG. 7 is a photoluminescence spectrum of example 2 of the present invention;
FIG. 8 is an optical micrograph of example 3 of the present invention;
FIG. 9 is a Raman spectrum of example 3 of the present invention;
FIG. 10 is a photoluminescence spectrum of example 3 in the present invention;
FIG. 11 is an optical micrograph of comparative example 1 according to the present invention;
FIG. 12 is a Raman spectrum of comparative example 1 in the present invention;
the invention is described in detail below with reference to the drawings and the detailed description.
Detailed Description
In order to make the objects and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples, and the advantages of the present invention are shown by comparative analysis. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Torsion angle WS prepared by the invention 2 And directly growing on the silicon dioxide/silicon substrate by adopting a chemical vapor deposition method. The two-dimensional material twist angle WS2 material is obtained by controlling the proportion of reaction sources, reaction temperature, reaction time, argon flow rate and other factors, and the method has the advantages of simple process and low cost.
The preparation method of the torsion angle WS2 of the two-dimensional material takes silicon dioxide/silicon chip as a substrate, and the torsion angle WS of the two-dimensional material is carried out on the silicon dioxide surface of the substrate by adopting a chemical vapor deposition method 2 Growing of (3); the growth container is a quartz tube, and the carrier gas in the quartz tube is inert gas; according to the flow direction of carrier gas, a sulfur source is placed in the quartz tube, a quartz test tube with openings at two ends is arranged at the downstream of the sulfur source, and a tungsten source and a substrate are placed in the quartz test tube; the flow rate of the carrier gas is 50-180 sccm; the reaction temperature of the chemical vapor deposition is 750-850 ℃. Experiments show that the twist angle WS of the two-dimensional material can be obtained only by performing chemical vapor deposition reaction in a quartz test tube with openings at two ends by using the raw materials and the process conditions provided by the invention 2 The quartz test tube with two open ends is not used as a cavity, and under the condition of not changing other conditions, the material prepared on the substrate is a single-layer or multi-layer WS 2 No torsion between layers, no two-dimensional material torsion angle WS on the substrate 2 。
In the following experiments, all the raw materials are commercially available and all the methods are conventional in the art unless otherwise specified.
The first embodiment is as follows:
this example presents a method for preparing a twist angle WS2 of a two-dimensional material on a silicon dioxide/silicon substrate, comprising the steps of:
the method comprises the following steps: the silica/silicon substrate was cut into a 0.9X 3cm sheet and blown clean with an air gun, and the silica surface was stacked back to back in a quartz test tube having openings at both ends and an inner diameter of 10 mm.
Step two: 20mg of tungsten trioxide powder was added to the front end of the substrate at 0.5cm, and 1mg of NaCl was added to the tungsten trioxide powder.
Step three: a quartz test tube was placed in a quartz tube having an outer diameter of 25mm, one end to which tungsten trioxide powder and NaCl were added was close to the gas inlet, and an S source was spaced from the tungsten source by 4cm, and heated in a heating center position of a tube-type atmosphere furnace to perform chemical vapor deposition of a two-dimensional material twist angle WS2, as shown in FIG. 1 a.
Step four: and introducing argon of 200sccm for washing for 30min to thoroughly remove residual oxygen in the tube. Then, argon gas of 80sccm is continuously introduced, the tubular atmosphere furnace is heated to 820 ℃ at the heating rate of 30 ℃/min, and the temperature is kept for 5 min. Then the heater is closed, the temperature is naturally cooled to the room temperature, and the twist angle WS of the two-dimensional material obtained at the moment 2 The optical photograph is shown in FIG. 2. As can be seen from the optical photograph of FIG. 2, the material produced was the twist angle WS 2 The molar angle was 36.5 °. Raman spectra are shown in FIG. 3, with WS at both 1 and 2 positions 2 Indicating that the prepared material is WS 2 . Torsional angle WS 2 The photoluminescence spectrum of (a) is shown in FIG. 4, wherein the emission peak at position 1 is located at 638nm, the emission peak at position 2 is located at 642nm, and the emission peak intensity at position 1 is greater than that at position 2. It is shown that the twisted angle structure of the bilayer causes a change in the band structure of the system and causes a reduction in the photoluminescent intensity.
Example two:
this example presents a method for preparing a twist angle WS2 of a two-dimensional material on a silicon dioxide/silicon substrate, comprising the steps of:
the method comprises the following steps: the silica/silicon substrate was cut into a 0.9X 3cm sheet and blown clean with an air gun, and the silica surface was stacked back to back in a quartz test tube having openings at both ends and an inner diameter of 10 mm.
Step two: 30mg of tungsten trioxide powder was added to the tungsten trioxide powder, and the tungsten trioxide powder was placed at a position 0.5cm from the front end of the substrate, and 1.5mg of NaCl was added thereto.
Step three: the quartz test tube was placed in a quartz tube having an outer diameter of 25mm, one end to which tungsten trioxide powder and NaCl were added was close to the gas inlet, and the S source was spaced 4cm from the tungsten source, and heated in a heating center position of a tube-type atmosphere furnace to perform chemical vapor deposition of a two-dimensional material twist angle WS2, as shown in FIG. 1 a.
Step four: and introducing argon of 200sccm for washing for 30min to thoroughly remove residual oxygen in the tube. Then, argon gas of 60sccm is continuously introduced, the tubular atmosphere furnace is heated to 820 ℃ at the heating rate of 30 ℃/min, and the temperature is kept for 5 min. Then the heater is closed, the temperature is naturally cooled to the room temperature, and the twist angle WS of the two-dimensional material obtained at the moment 2 Optical photograph As shown in FIG. 5, it can be seen from the optical photograph of FIG. 5 that the material to be prepared is the twist angle WS 2 The morse angle was 44.3 °. The Raman spectrum is shown in FIG. 6, and both of the 1 and 2 positions have WS 2 Indicating that the prepared material is WS 2 . Torsional angle WS 2 The photoluminescence spectrum of (a) is shown in fig. 7, in which the emission peak at position 1 is at 634nm, the emission peak at position 2 is at 633nm, and the emission peak intensity at position 1 is greater than that at position 2. It is shown that the twisted angle structure of the bilayer causes a change in the band structure of the system and causes a reduction in the photoluminescent intensity.
Example three:
this example presents a method for preparing a twisted angle WS2 of two-dimensional material on a silicon dioxide/silicon substrate, comprising the following steps:
the method comprises the following steps: the silicon dioxide/silicon substrate is cut into a sheet shape of 1.0 multiplied by 3.2m and blown clean by an air gun, and the silicon dioxide surface is stacked back to back in a quartz test tube with two open ends and an inner diameter of 10 mm.
Step two: 20mg of tungsten trioxide powder was added to the front end of the substrate at 0.5cm, and 1mg of NaCl was added to the tungsten trioxide powder.
Step three: the quartz test tube was placed in a quartz tube having an inner diameter of 20mm, one end to which tungsten trioxide powder and NaCl were added was close to the gas inlet, and the S source was spaced 4cm from the tungsten source, and heated in a heating center position of a tube-type atmosphere furnace to perform chemical vapor deposition of a two-dimensional material twist angle WS2, as shown in FIG. 1 a.
Step four: and introducing argon of 200sccm for washing for 30min to thoroughly remove residual oxygen in the tube. Then, argon gas of 80sccm is continuously introduced, the tubular atmosphere furnace is heated to 800 ℃ at the heating rate of 28 ℃/min, and the temperature is kept for 10 min. Then the heater is turned off, and the two-dimensional material obtained at the moment is naturally cooled to the room temperatureTorsional angle WS 2 Optical photograph As shown in FIG. 8, it can be seen from the optical photograph of FIG. 8 that the material to be prepared is a two-dimensional material with a twist angle WS 2 The molar angle was 88.5 °. Raman spectra are shown in FIG. 9, with WS at both 1 and 2 positions 2 Indicating that the prepared material is WS 2 . Torsion angle WS 2 The photoluminescence spectrum of (a) is shown in FIG. 10, in which the emission peak at position 1 is at 632nm, the emission peak at position 2 is at 638nm, and the emission peak intensity at position 1 is greater than that at position 2. It is shown that the twisted angle structure of the bilayer causes a change in the system band structure and causes a decrease in the photoluminescence intensity.
Comparative example one:
this comparative example shows a method for preparing a material without using a quartz cuvette with open ends, comprising the steps of:
the method comprises the following steps: the silica/silicon substrate was cut into a 0.9X 3cm sheet and blown clean with an air gun, and the silica face was stacked back to back on a quartz crucible.
Step two: 30mg of tungsten trioxide powder was added to the front end of the substrate at 0.5cm, and 1.5mg of NaCl was added to the tungsten trioxide powder.
Step three: the quartz crucible was placed in a quartz tube having an inner diameter of 20mm, one end to which the tungsten trioxide powder and NaCl were added was close to the gas inlet, and the S source was placed at a distance of 4cm from the tungsten source, directly at the heating center of the tube-type atmosphere furnace, as shown in FIG. 1 b.
Step four: WS obtained at this time, as in the example two 2 The optical photograph is shown in FIG. 11, and the Raman spectrum is shown in FIG. 12.
Comparison with the examples shows that, instead of using a quartz cuvette with two open ends as the chamber, the material prepared on the substrate is single-layer or multi-layer WS under otherwise unchanged conditions 2 No torsion between layers, and no two-dimensional material torsion angle WS on the substrate 2 。
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 amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (9)
1. Two-dimensional material torsional angle WS 2 The preparation method is characterized in that silicon dioxide/silicon chip is used as a substrate, and the silicon dioxide surface of the substrate is subjected to two-dimensional material torsion angle WS by adopting a chemical vapor deposition method 2 Growing of (3);
the growth container is a quartz tube, and the carrier gas in the quartz tube is inert gas;
according to the flow direction of carrier gas, a sulfur source is placed in the quartz tube, a quartz test tube with openings at two ends is arranged at the downstream of the sulfur source, and a tungsten source and a substrate are placed in the quartz test tube;
the flow rate of the carrier gas is 50-180 sccm; the reaction temperature of the chemical vapor deposition is 750-850 ℃.
2. Two-dimensional material twist angle WS as claimed in claim 1 2 The preparation method is characterized in that the silicon dioxide/silicon wafer substrates are provided with two silicon dioxide/silicon wafer substrates, the silicon dioxide surfaces of the two silicon dioxide/silicon wafer substrates are respectively stacked back to back upwards or downwards, and a tungsten source is placed at the position 0.5cm in front of the substrates.
3. Two-dimensional material twist angle WS as claimed in claim 1 or 2 2 The preparation method is characterized in that the tungsten source is tungsten trioxide powder or tungsten chloride powder; the sulfur source is S powder;
the dosage of the tungsten source is 10-40 mg, and the sulfur source is sufficient.
4. Two-dimensional material twist angle WS according to claim 3 2 The preparation method is characterized in that NaCl is added into the tungsten source, and the addition amount of the NaCl is 1-4 mg.
5. Two-dimensional material twist angle WS according to claim 1 or 2 2 The preparation method is characterized in that the temperature rise rate of the carrier gas is 10-50 ℃/min.
6.Two-dimensional material twist angle WS as claimed in claim 1 or 2 2 The preparation method is characterized in that the distance between the tungsten source and the sulfur source is 3-8 cm.
7. Two-dimensional material twist angle WS as claimed in claim 1 or 2 2 The preparation method is characterized in that the growth time of the chemical vapor deposition is 5-30 min.
8. Two-dimensional material torsional angle WS 2 The preparation method is characterized by comprising the following steps:
(1) cutting the silicon dioxide/silicon substrate into a sheet shape of 0.9cm by 3cm, and stacking the silicon dioxide surface back to back in a quartz test tube with the inner diameter of 10mm and openings at two ends inside;
(2)20mg of tungsten source was placed in a quartz tube 0.5cm in front of the substrate and 1mg of sodium chloride was added;
(3) placing the quartz test tube into a quartz tube with an inner diameter of 25mm, placing the tungsten source end close to the air inlet of the quartz tube, heating the sulfur source and the tungsten source at a distance of 4cm in a tube-type atmosphere furnace to perform two-dimensional material torsion angle WS 2 Chemical vapor deposition of (2).
9. Two-dimensional material torsion angle WS 2 Characterized in that the two-dimensional material twist angle WS 2 Using the two-dimensional material twist angle WS of any of claims 1-8 2 The preparation method is used for preparing the compound.
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| CN115385378A (en) * | 2022-09-27 | 2022-11-25 | 暨南大学 | Preparation method and application of two-dimensional double-layer tungsten sulfide homojunction |
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| CN115385378A (en) * | 2022-09-27 | 2022-11-25 | 暨南大学 | Preparation method and application of two-dimensional double-layer tungsten sulfide homojunction |
| CN115385378B (en) * | 2022-09-27 | 2023-10-13 | 暨南大学 | Preparation method and application of two-dimensional double-layer tungsten sulfide homojunction |
| WO2024066206A1 (en) * | 2022-09-27 | 2024-04-04 | 暨南大学 | Preparation method for and use of two-dimensional double-layer tungsten sulfide homojunction |
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| CN114990523B (en) | 2024-04-26 |
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