CN111041449B - Preparation method of tungsten disulfide with specific morphology - Google Patents
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- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000012159 carrier gas Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 239000010453 quartz Substances 0.000 claims description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 58
- 239000000758 substrate Substances 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 25
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000010431 corundum Substances 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 229910052763 palladium Inorganic materials 0.000 abstract description 4
- 229910052786 argon Inorganic materials 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur 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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- 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
- C23C16/02—Pretreatment of the material to be coated
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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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- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
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Abstract
The invention discloses a preparation method of tungsten disulfide with a specific morphology, which takes argon and hydrogen as carrier gases and metal palladium as a catalyst to synthesize tungsten disulfide with a triangular frame structure by a CVD method at high temperature. Compared with the triangular and hexagonal solid continuous film synthesized by the existing CVD method, the proportion of the edge atoms in the tungsten disulfide film obtained by the method in the total atomic number is increased, and the catalytic activity of the tungsten disulfide when used as a catalyst material is improved.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of tungsten disulfide with a hollow triangular frame structure.
Background
The two-dimensional tungsten disulfide can be synthesized by a Chemical Vapor Deposition (CVD) method, wherein precursors are subjected to chemical reaction at high temperature, and then a tungsten sulfide monomolecular layer or polymolecular layer thick film material is deposited and grown on the surface of a substrate. The tungsten disulfide synthesized by the method is a film formed by the interconnection of single crystal domains or a plurality of crystal domains which are dispersed on the surface of a substrate and are separated from each other and have a triangular or hexagonal shape, and the crystal domains or the film is a continuous and non-hollow plane.
Sulfur reacts with most metals except gold at high temperature to form metal sulfides, so that a metal catalyst is hardly used in the sulfide preparation process. The growth of tungsten disulfide usually uses a mixed gas of argon and hydrogen as a carrier gas, and the mechanism of the influence of hydrogen on the synthesis of tungsten disulfide needs to be further researched.
Tungsten disulfide (WS)2) The forbidden bandwidth changes with the thickness of the material, the forbidden bandwidth of the monomolecular layer is about 2.0eV, the forbidden bandwidth of the bulk material is about 1.3eV, and the forbidden bandwidth of the tungsten disulfide is in the visible light energy range, so that the material can be used as a photoconductive detector and a photocatalytic material. When the catalyst is used as a catalyst material, the sites playing the role of catalytic activity are mainly the edge part of the tungsten disulfide material. In order to improve the catalytic performance, it is necessary to reduce the size of the material or to introduce defects.
Disclosure of Invention
The invention provides a method for synthesizing tungsten disulfide with a triangular frame structure by using argon and hydrogen as carrier gases and metal palladium as a catalyst through a CVD (chemical vapor deposition) method at high temperature. Compared with the triangular and hexagonal solid continuous film synthesized by the existing CVD method, the proportion of the edge atoms in the tungsten disulfide film obtained by the method in the total atomic number is increased, and the catalytic activity of the tungsten disulfide when used as a catalyst material is improved. In addition, the product is taken as a template, and other materials are continuously deposited and grown, so that the method can be used for synthesizing electronic devices with special structures.
The preparation method of the tungsten disulfide with the specific morphology comprises the following specific steps:
step (1) taking WS21-5 g of solid powder is put into a quartz boat, and then WS is filled in the quartz boat2The quartz boat of solid powder was placed in a quartz tube (1 inch diameter) in a tube-type electric furnace. The quartz boat is placed in the middle of the quartz tube.
Step (2), cleaning a substrate (with the size of 2.5-3.5 cm multiplied by 1.5-2.0 cm) by deionized water, drying by blowing nitrogen, and drying by blowing 0.05-0.2mol/l of palladium chloride (PdCl)2) Spraying hydrochloric acid solution onto the surface of the substrate, and heating to 80-100 deg.C with a heating plate to obtain PdCl2Spray droplet drying. Then, placing the substrate in a quartz tube, wherein the position is 20-25 cm away from the quartz boat in the downstream direction of the carrier gas flow;
and (3) starting a mechanical pump to pump vacuum, and simultaneously inputting carrier gas argon-hydrogen mixed gas (5% H) into the quartz tube2) The carrier gas flow is 20-50 sccm. The vacuum degree in the tube is 100-600 Pa.
And (4) heating the quartz tube to 900-1000 ℃, wherein the heating rate is 20-30 ℃/min. And (3) keeping the temperature after the temperature is increased to 900-1000 ℃, wherein the heat preservation time is 30-300 min.
And (5) stopping heating the quartz tube, rapidly cooling the quartz tube to room temperature at a cooling rate of 10-100 ℃/min, then taking out the substrate, and obtaining the tungsten sulfide with the frame structure on the substrate.
The quartz tube in the step (1) is a quartz tube or a corundum tube, and the quartz boat is a quartz boat or a corundum boat.
And (3) the substrate in the step (2) is a silicon wafer or sapphire with an oxide layer growing on the surface.
Has the advantages that: according to the invention, metal palladium and hydrogen are applied to a chemical vapor deposition method to prepare tungsten disulfide, the product is in a triangular frame structure, the proportion of edge atoms in the tungsten disulfide film in the total atomic number is increased, and the catalytic activity of tungsten disulfide when used as a catalyst material is improved. The formation of the tungsten disulfide film with the triangular frame structure is related to metal palladium and hydrogen. Unlike gold as a catalyst, the synthesis of tungsten disulfide with a framework structure cannot be achieved by using gold as a catalyst.
Drawings
FIG. 1 is a scanning electron microscope photograph of a tungsten disulfide thin film single crystal domain with a triangular frame structure;
FIG. 2 is an optical microscope photograph of a tungsten disulfide thin film single crystal domain with a triangular frame structure;
fig. 3 is an optical microscope photograph of multiple domains of a tungsten disulfide thin film with a triangular frame structure.
Detailed Description
Example 1:
step (1) taking WS21g of solid powder, put into a quartz boat, and then put into a chamber containing WS2The quartz boat of solid powder was placed in a quartz tube (1 inch diameter) in a tube-type electric furnace. The quartz boat is placed in the middle of the quartz tube.
Step (2), the size of the substrate is 2.5cm multiplied by 1.5cm, the substrate is cleaned by deionized water and is dried by nitrogen, and 0.05mol/l of palladium chloride (PdCl) is dried2) Spraying hydrochloric acid solution on the surface of the silicon wafer substrate, and heating to 80 ℃ by a heating plate to ensure that PdCl is added2Spray droplet drying. The substrate, which is sapphire with an oxide layer grown on the surface, was then placed in a quartz tube downstream of the carrier gas.
And (3) starting a mechanical pump to pump vacuum, and simultaneously inputting carrier gas argon-hydrogen mixed gas (5% H) into the quartz tube2) The flow rate of the carrier gas was 20 sccm. The vacuum degree in the tube is 100 Pa.
And (4) heating the quartz tube to 900 ℃, wherein the heating rate is 20 ℃/min. And (3) keeping the temperature after the temperature is increased to 900 ℃, wherein the heat preservation time is 30 min.
Step (5), stopping heating the quartz tube, rapidly cooling the quartz tube to room temperature at a cooling rate of 10 ℃/min, then taking out the substrate, and obtaining tungsten sulfide with a frame structure on the substrate, as shown in fig. 1, 2 and 3;
example 2:
step (1) taking WS25g of solid powder, put into a corundum boat, and then filled with WS2The corundum boat of solid powder was placed in a quartz tube (1 inch diameter) in a tube electric furnace. The corundum boat is placed in the middle of the quartz tube.
Step (2), cleaning a substrate (with the size of 2.5cm multiplied by 2.0cm by deionized water, drying by nitrogen, and drying by blowing 0.2mol/l of palladium chloride (PdCl)2) Spraying hydrochloric acid solution on the surface of the silicon wafer substrate, and heating to 100 ℃ by a heating plate to ensure that PdCl is added2Spray droplet drying. The substrate was then placed in a quartz tube downstream of the carrier gas.
And (3) starting a mechanical pump to pump vacuum, and simultaneously inputting carrier gas argon-hydrogen mixed gas (5% H) into the quartz tube2) The flow rate of the carrier gas was 50 sccm. The vacuum degree in the tube is 600 Pa.
And (4) heating the quartz tube to 1000 ℃, wherein the heating rate is 30 ℃/min. And (3) keeping the temperature after the temperature is raised to 1000 ℃, wherein the heat preservation time is 300 min.
And (5) stopping heating the quartz tube, rapidly cooling the quartz tube to room temperature at a cooling rate of 100 ℃/min, then taking out the substrate, and obtaining the tungsten sulfide with the frame structure on the substrate.
Example 3:
step (1) taking WS23g of solid powder, put into a quartz boat, and then put into a chamber containing WS2The quartz boat of solid powder was placed in a quartz tube (1 inch diameter) in a tube-type electric furnace. The quartz boat is placed in the middle of the quartz tube.
Step (2), the size of the substrate is 3.5cm multiplied by 2.0cm, the substrate is cleaned by deionized water and is dried by nitrogen, and 0.1mol/l of palladium chloride (PdCl) is dried2) Hydrochloric acid solutionSpraying the solution on the surface of a silicon wafer substrate, and heating the solution to 95 ℃ through a heating plate to ensure that PdCl is added2Spray droplet drying. The substrate, which is a silicon wafer with an oxide layer grown on the surface, was then placed in a quartz tube downstream of the carrier gas.
And (3) starting a mechanical pump to pump vacuum, and simultaneously inputting carrier gas argon-hydrogen mixed gas (5% H) into the quartz tube2) The flow rate of the carrier gas was 30 sccm. The vacuum degree in the tube is 450 Pa.
And (4) heating the quartz tube to 950 ℃ at a heating rate of 25 ℃/min. And keeping the temperature for 100min after the temperature is raised to 950 ℃.
And (5) stopping heating the quartz tube, rapidly cooling the quartz tube to room temperature at a cooling rate of 50 ℃/min, then taking out the substrate, and obtaining the tungsten sulfide with the frame structure on the substrate.
Claims (5)
1. The preparation method of tungsten disulfide with specific morphology is characterized by specifically comprising the following steps
The method comprises the following steps:
step (1) taking WS21-5 g of solid powder is put into a quartz boat, and then WS is filled in the quartz boat2Putting the quartz boat of the solid powder into a quartz tube in the tube type electric furnace; the quartz boat is placed in the middle of the quartz tube;
cleaning the substrate with deionized water, drying the substrate with nitrogen, spraying a palladium chloride hydrochloric acid solution with the concentration of 0.05-0.2mol/l to the surface of the substrate, and heating the substrate to 80-100 ℃ through a heating plate to ensure that PdCl is subjected to PdCl2Spray droplet drying; then, placing the substrate in a quartz tube, wherein the position is 20-25 cm away from the quartz boat in the downstream direction of the carrier gas flow;
and (3) starting a mechanical pump to pump vacuum, and simultaneously inputting carrier gas argon-hydrogen mixed gas into the quartz tube, wherein H is2The volume content of the catalyst is 5%, and the flow rate of carrier gas is 20-50 sccm; the vacuum degree in the tube is 100-600 Pa;
step (4), heating the quartz tube to 900-1000 ℃, wherein the heating rate is 20-30 ℃/min; keeping the temperature after the temperature is increased to 900-1000 ℃, wherein the heat preservation time is 30-300 min;
and (5) stopping heating the quartz tube, rapidly cooling the quartz tube to room temperature at a cooling rate of 10-100 ℃/min, then taking out the substrate, and obtaining tungsten sulfide with a frame structure on the substrate, wherein the proportion of edge atoms in the total number of atoms is increased.
2. The method for preparing tungsten disulfide with a specific morphology as claimed in claim 1, wherein: in the step (1), a corundum tube is used for replacing a quartz tube, and a corundum boat is used for replacing a quartz boat.
3. The method for preparing tungsten disulfide with a specific morphology as claimed in claim 1, wherein: and (3) the substrate in the step (2) is a silicon wafer or sapphire with an oxide layer growing on the surface.
4. The method for preparing tungsten disulfide with a specific morphology as claimed in claim 1, wherein: the quartz tube diameter was 1 inch.
5. The method for preparing tungsten disulfide with a specific morphology as claimed in claim 1, wherein: the size of the substrate is 2.5-3.5 cm x 1.5-2.0 cm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101184690B (en) * | 2005-04-07 | 2013-03-20 | 耶达研究与开发有限公司 | Process and apparatus for producing inorganic fullerene-like nanoparticles |
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| EP1060141A1 (en) * | 1998-03-03 | 2000-12-20 | PPG Industries Ohio, Inc. | Impregnated glass fiber strands and products including the same |
| JP2004156197A (en) * | 1998-03-03 | 2004-06-03 | Ppg Ind Ohio Inc | Impregnated glass fiber strand and products including the same |
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| CN110373718A (en) * | 2019-05-30 | 2019-10-25 | 杭州电子科技大学 | A kind of preparation method of two dimension tungsten disulfide film |
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