CN113174583A - Open quartz boat and preparation method of large-area continuous two-dimensional transition metal sulfur compound film - Google Patents
Open quartz boat and preparation method of large-area continuous two-dimensional transition metal sulfur compound film Download PDFInfo
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- CN113174583A CN113174583A CN202110282034.4A CN202110282034A CN113174583A CN 113174583 A CN113174583 A CN 113174583A CN 202110282034 A CN202110282034 A CN 202110282034A CN 113174583 A CN113174583 A CN 113174583A
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- 239000010453 quartz Substances 0.000 title claims abstract description 181
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 68
- -1 transition metal sulfur compound Chemical class 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 120
- 239000000843 powder Substances 0.000 claims abstract description 70
- 239000002243 precursor Substances 0.000 claims abstract description 69
- 239000011669 selenium Substances 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 40
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 37
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 37
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 37
- 239000011593 sulfur Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- 239000010408 film Substances 0.000 claims abstract description 28
- 239000010409 thin film Substances 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 36
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000005229 chemical vapour deposition Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000011780 sodium chloride Substances 0.000 claims description 18
- 239000011261 inert gas Substances 0.000 claims description 17
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical group O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910003090 WSe2 Inorganic materials 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 229910052961 molybdenite Inorganic materials 0.000 claims description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 2
- 230000007704 transition Effects 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 150000004770 chalcogenides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 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
-
- 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
- C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4485—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
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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)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
本发明涉及开口石英舟及大面积连续二维过渡金属硫化合物薄膜的制备方法，开口石英舟一端设有开口，大面积连续二维过渡金属硫化合物薄膜的制备的步骤包括：1)将前驱体粉末放置于开口石英舟A内设有开口的一端；2)将硫源或硒源放置于开口石英舟B内；3)将浸泡过催化剂溶液的基底倒扣在开口石英舟A中前驱体粉末的上方；4)将开口石英舟A、开口石英舟B分别置于管式炉的主炉加热区和预热加热区，开口石英舟A和开口石英舟B的开口一端相对；依次进行前驱体加热、硫源或硒源加热；6)生成二维过渡金属硫族化合物并沉积在基底表面。本发明在制备二维过渡金属硫化合物薄膜时，避免形成湍流，有助于获取大面积连续二维过渡金属硫化合物薄膜。
The invention relates to an open quartz boat and a method for preparing a large-area continuous two-dimensional transition metal sulfur compound film. One end of the open quartz boat is provided with an opening, and the preparation steps of the large-area continuous two-dimensional transition metal sulfur compound film include: 1) preparing a precursor The powder is placed in the open end of the quartz boat A; 2) The sulfur source or the selenium source is placed in the open quartz boat B; 3) The substrate soaked in the catalyst solution is inverted in the open quartz boat A. The precursor powder 4) place the open quartz boat A and the open quartz boat B in the main furnace heating zone and the preheating heating zone of the tube furnace respectively, and the open end of the open quartz boat A and the open quartz boat B are opposite; carry out the precursor successively heating, sulfur source or selenium source heating; 6) two-dimensional transition metal chalcogenide is generated and deposited on the surface of the substrate. The invention avoids the formation of turbulent flow when preparing the two-dimensional transition metal-sulfur compound thin film, and helps to obtain a large-area continuous two-dimensional transition metal-sulfur compound thin film.
Description
Technical Field
The invention belongs to the field of two-dimensional materials, and particularly relates to a large-opening quartz boat and a preparation method of a large-area continuous two-dimensional transition metal sulfur compound film based on the opening quartz boat.
Background
When conventional semiconductor materials are applied to develop flexible electronic sensors, for example, Si can be used to fabricate flexible devices by thinning it below a certain value. However, due to the fragile nature of silicon, it poses a serious threat to the reliability of the device. Other methods, including the use of organic materials to fabricate flexible devices, have also been extensively studied, but these techniques have not been universally applicable due to the inability to solve the problems of low carrier mobility, high operating voltage, large leakage current, etc. On the other hand, as the semiconductor technology develops, the feature size of the semiconductor device becomes smaller and smaller, and the device size also faces the 7nm bottleneck at present. As dimensions continue to shrink, more and more difficulties begin to arise, such as short channel effects, which are difficult to overcome, and can significantly degrade the performance of silicon-based devices. There is a strong need for a semiconductor material that can replace silicon.
Since the discovery of graphene, two-dimensional materials have received increasing attention, and due to their excellent properties, are considered to have a great potential to replace silicon as a next-generation revolutionary semiconductor material.
The two-dimensional transition metal chalcogenide (TMDs) is a novel graphene-like nano material, has excellent performances such as good crystallinity, large specific surface area and high absorption coefficient, is linked by strong covalent bonds in the layer, has good stability, and is connected by Van der Waals force between layers, so that the effect between the transition metal chalcogenide layers is easily broken, the transition metal chalcogenide can be easily stripped from multiple layers to a single layer, the band gap of the transition metal chalcogenide is gradually increased along with the reduction of the number of the layers, the single layer is converted into a direct band gap, and the sensitivity of the transition metal chalcogenide is higher.
At present, among the methods for preparing a two-dimensional transition metal chalcogenide, the main methods are: lift-off methods and chemical vapor deposition methods.
The stripping method is a traditional method for preparing two-dimensional transition metal sulfide, and mainly comprises the following steps: ion intercalation stripping and mechanical stripping. For example, chinese patent CN108423642A discloses a method for preparing small-size transition metal chalcogenide two-dimensional nanosheets, which is to use bulk powder of transition metal chalcogenide as a raw material and polymer as an auxiliary agent, and prepare transition metal chalcogenide two-dimensional nanosheets of different sizes and different components by polymer-assisted ball milling, and includes 3 steps: weighing block powder prepared by high polymer and high polymer-assisted ball milling; ball milling and stripping, adding water, mixing and taking out; and (4) performing gradient centrifugation to obtain products with different sizes, and purifying to remove redundant macromolecules. The method has simple process, but cannot prepare large-area continuous two-dimensional transition metal chalcogenide, and the two-dimensional transition metal chalcogenide obtained by the stripping method is relatively dispersed, so that the method cannot meet the requirements of industrial and commercial production.
In addition to the conventional stripping method, a relatively emerging chemical vapor deposition method is concerned by more and more researchers, for example, a limited-area chemical vapor deposition preparation method of a two-dimensional transition metal alloy chalcogenide disclosed in chinese patent CN110155959A, the technical scheme is to fully grind and mix molybdenum oxide and tungsten oxide serving as precursor source materials, place a small amount of the obtained mixture on a silicon wafer, place the silicon wafer in a quartz tube with one end sealed, make a limited-area vapor chemical deposition device, and obtain a single-layer large-size transition metal alloy chalcogenide under the protection of argon and hydrogen in a tube furnace. The method for preparing the two-dimensional transition metal chalcogenide has poor stability, and the randomness of nucleation of the two-dimensional transition metal chalcogenide on the substrate is high, so how to make the nucleation of the two-dimensional transition metal chalcogenide on the substrate more stable, and the obtaining of the large-area, continuous and high-quality two-dimensional transition metal chalcogenide film becomes a key problem to be solved urgently for preparing flexible electrons.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method and a device of a large-area continuous two-dimensional transition metal sulfur compound film, and aims to solve the problems that the stability of the existing chemical vapor deposition method is poor, and the randomness of nucleation of a two-dimensional transition metal sulfur group compound on a substrate is high.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the invention relates to an open quartz boat, wherein one end of the open quartz boat is provided with an opening, when chemical vapor deposition is carried out, the two open quartz boats are used as carriers, and the open ends of the two open quartz boats are opposite to each other, so that turbulent flow is prevented from being formed at the opposite ends of the open quartz boats, and the airflow is more stable.
Preferably, the height of the open quartz boat is 1.5cm, the width is 2.5cm, the length is 10cm, and the thickness is 0.2 cm.
The invention also relates to a preparation method of the large-area continuous two-dimensional transition metal sulfur compound film based on the open quartz boat, which comprises the following steps:
1) preparing a chemical vapor deposition precursor: weighing precursor powder, and placing the precursor powder in an open quartz boat A, wherein the precursor powder is placed at one end of the open quartz boat A, which is provided with an opening;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source, and placing the sulfur source or the selenium source in an open quartz boat B;
3) preparing a catalyst: dissolving a catalyst in deionized water to form a catalyst solution, soaking a substrate in the catalyst solution, drying the substrate by inert gas after soaking, and inversely covering the substrate above precursor powder in the open quartz boat A;
4) the opening quartz boat A is loaded by a quartz plate base and then is placed in a main furnace heating area of the tube furnace, the opening quartz boat B is integrally placed in a preheating heating area of the tube furnace, the main furnace heating area is communicated with the preheating heating area, one opening end of the opening quartz boat A is opposite to one opening end of the opening quartz boat B, turbulence is prevented from being formed at the opposite ends of the opening quartz boat A and the opening quartz boat B, and therefore airflow is more stable;
5) setting the heating temperature and the maintaining time of a main furnace heating area and a preheating heating area, heating the precursor to form precursor steam by the main furnace heating area, and starting heating a sulfur source or a selenium source by the preheating heating area to form sulfur source steam or selenium source steam after the main furnace heating area is heated to the set temperature;
6) and reacting the precursor vapor with sulfur source vapor or reacting the precursor vapor with selenium source vapor to generate a two-dimensional transition metal chalcogenide and depositing the two-dimensional transition metal chalcogenide on the surface of the substrate to form the two-dimensional transition metal chalcogenide film.
Preferably, the precursor is tungsten trioxide or molybdenum trioxide; the sulfur source is S powder, and the selenium source is Se powder; the two-dimensional transition metal chalcogenide film is WS2Or MoS2Or WSe2Or MoSe2A film.
Preferably, the mass of the tungsten trioxide and the molybdenum trioxide is controlled to be 70-80 mg.
Preferably, the quality of the sulfur source or the selenium source is controlled to be 180-200 mg.
Preferably, the catalyst is NaCl, when a NaCl solution is prepared, 20-25 mg of NaCl crystals are placed in a beaker and dissolved in 100-125 ml of deionized water, and a glass rod is used for stirring the deionized water to accelerate the dissolution of the NaCl crystals; the purity of the NaCl crystal is higher than 99.9%.
Preferably, before heating the precursor in step 5), the tube furnace is evacuated, and then inert gas is introduced, wherein the inert gas is always introduced into the tube furnace during the processes of heating the precursor, heating the sulfur source or the selenium source, and generating the two-dimensional transition metal chalcogenide.
Preferably, the inert gas is argon, and the argon is introduced into the tube furnace at a flow rate of 100-200 sccm.
Preferably, the heating temperature of the main furnace heating zone set in the step 5) is 950-1000 ℃, and the maintaining time of the main furnace heating zone is 30-40 min; the heating temperature of the preheating heating zone is set to be 120-150 ℃, and the maintaining time of the preheating heating zone is 40-50 min.
The width of the quartz plate base is 3-4 cm, the length is 10cm, and the thickness is 0.2 cm.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
1. when the two-dimensional transition metal sulfur compound film is generated by chemical vapor deposition, precursor powder is placed in an open quartz boat A with an opening at one end, a sulfur source or a selenium source is placed in an open quartz boat B with an opening at one end, when the open quartz boat A and the open quartz boat B are placed in a tube furnace, the open ends of the open quartz boat A and the open end of the open quartz boat B are opposite, and the chemical vapor deposition is carried out under the arrangement, so that turbulence can be prevented from being formed at the front part of the open quartz boat to a great extent, nucleation points of the two-dimensional transition metal sulfur compound on a substrate are more stable, and the problem that the randomness of the two-dimensional transition metal sulfur compound is large when the conventional open quartz boat is used for growing the two-dimensional transition metal sulfur compound is solved.
2. The invention only needs one precursor, and does not need H in the growth process2The method promotes the large-area continuous growth of the film material, can obtain the large-area continuous film material only under the inert gas environment, and has the characteristics of low cost, simple device, easy operation, good controllability and the like.
Drawings
FIG. 1 is a conventional closed quartz boat;
FIG. 2 is a schematic view of the structure of an open quartz boat for use in the present invention;
FIG. 3 is a diagram showing an apparatus for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to the present invention;
FIG. 4 is a schematic structural view of a quartz plate susceptor;
FIG. 5 is a flow chart of the preparation of a large area continuous two-dimensional transition metal sulfur compound thin film;
FIG. 6 is a schematic view of the precursor being tiled on an open quartz boat A;
FIG. 7 is a schematic view of a sulfur source (or selenium source) laid flat in an open quartz boat B;
FIG. 8 is a schematic view of the substrates being flipped over on the open quartz boat A;
FIG. 9 shows WS prepared in example 2 of the present invention2Optical microscopy of thin films;
Detailed Description
For further understanding of the present invention, the present invention will be described in detail with reference to examples, which are provided for illustration of the present invention but are not intended to limit the scope of the present invention.
Example one
Referring to fig. 2, one end of the open quartz boat according to the embodiment is provided with an opening, and when the chemical vapor deposition is performed, the two open quartz boats are used as carriers, and the open ends of the two open quartz boats are opposite to each other, so that turbulence can be prevented from being formed at the opposite ends of the open quartz boats, and the gas flow is more stable. The height of the open quartz boat is 1.5cm, the width is 2.5cm, the length is 10cm, and the thickness is 0.2 cm.
Example two
Referring to fig. 3, the embodiment further relates to a device for preparing a large-area continuous two-dimensional transition metal sulfur compound film, which includes a tube furnace, an open quartz boat a1002 for containing a precursor and a substrate adsorbed with a catalyst, and an open quartz boat B1003 for containing a sulfur source or a selenium source, wherein the open quartz boat a and the open quartz boat B are both the open quartz boats according to embodiment 1. The tube furnace comprises a main furnace heating zone 1007 and a preheating heating zone 1008, and the main furnace heating zone 1007 and the preheating heating zone 1008 are communicated with each other.
The open quartz boat a1002 and the open quartz boat B1003 used in the present invention have openings at their ends, as compared to the conventional closed open quartz boat shown in fig. 1. The bottom of the open quartz boat A1002 is provided with a quartz plate base 1009 shown in FIG. 4, the open quartz boat A1002 is placed in the main furnace heating zone 1007, the open quartz boat B1003 is placed in the center of the preheating heating zone, and the ends of the open quartz boat A1002 and the open quartz boat B1003 provided with openings are opposite.
The height of the open quartz boat A1002 and the height of the open quartz boat B1003 are both 1.5cm, the width is 2.5cm, the length is 10cm, and the thickness is 0.2 cm; the quartz piece base 1009 has a width of 3 to 4cm, a length of 10cm, and a thickness of 0.2 cm.
EXAMPLE III
This example relates to a method for preparing large-area continuous two-dimensional transition metal sulfur compound film, before preparation, two open quartz boats as shown in fig. 2 are prepared, respectively marked as open quartz boat a1002 and open quartz boat B1003, and the structures of the open quartz boat a1002 and the open quartz boat B1003 are as described in the first example. Cleaning the open quartz boat A1002 and the open quartz boat B1003 by using clean water, putting the cleaned open quartz boat A1002 and the open quartz boat B1003 into an ultrasonic machine for ultrasonic treatment for 10min, further cleaning the open quartz boat A1002 and the open quartz boat B1003, and after cleaning is finished, putting the open quartz boat A1002 and the open quartz boat B1003 into a drying box for drying and standby.
Referring to fig. 5, the preparation of the large-area continuous two-dimensional transition metal sulfur compound thin film comprises the following steps:
1) preparing a chemical vapor deposition precursor: referring to FIG. 6, 70mg of WO was weighed3Powder is used as precursor powder 1004 and is placed in an open quartz boat A1002 with an opening at one end, the precursor powder 1004 is placed at the open end of the open quartz boat A, the tiled length of the precursor powder 1004 is within the interval of 0.8 cm-1 cm, and the width of the precursor powder 1004 is about 0.5 cm;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source 1005, wherein the sulfur source is adopted in the embodiment, specifically, S powder is adopted, 200mg of the S powder is weighed as shown in the attached figure 7, and the S powder is uniformly spread in the whole quartz boat B1003 with an opening;
3) preparing a catalyst: dissolving a catalyst (NaCl crystals with purity higher than 99.9%) in 100ml of deionized water, stirring the deionized water by using a glass rod, accelerating the dissolution of the NaCl crystals to form a catalyst solution, soaking the substrate 1006 in the catalyst solution, wherein the substrate 1006 in the embodiment is made of sapphire for 5 minutes, drying moisture on the surface of the substrate 1006 by using inert gas (argon) after the substrate 1006 is soaked, and inversely covering the substrate 1006 in the open quartz boat A1002 and above the precursor powder 1004;
4) the method comprises the following steps of carrying an open quartz boat A1002 by a quartz plate base 1009, then placing the quartz boat A1003 at the central position of a main furnace heating area 1007 of the tube furnace, placing the open quartz boat B1003 in the central position of a preheating heating area 1008 of the tube furnace, wherein the main furnace heating area 1007 is communicated with the preheating heating area 1008, and the open quartz boat A1002 is opposite to the open end of the open quartz boat B1003;
5) setting the heating temperature and the maintaining time of the heating zone 1007 and the preheating zone 1008 of the main furnace, wherein in the embodiment, the heating temperature of the heating zone 1007 of the main furnace is 975 ℃ and the time is 30 min; setting the heating temperature of the preheating zone 1008 to 150 ℃ for 40 min; before heating the precursor, the tube furnace is evacuated, then inert gas (argon) is introduced, and the heating zone 1007 of the main furnace first heats the precursor powder (WO)3Powder) 1004, heating to 975 ℃ after 1 hour, maintaining for 30min, then naturally cooling the main furnace heating zone 1007, and forming precursor steam in the main furnace heating zone 1007; when the temperature of the heating zone 1007 of the main furnace rises to the set temperature (975 ℃), the preheating heating zone 1008 starts to heat the S powder 1005, the temperature rises to 150 ℃ after 10min, the temperature is maintained for 40min, and then the preheating heating zone 1008 is naturally cooled to form sulfur source steam; argon gas was introduced into the tube furnace at a flow rate of 150sccm throughout the process.
6) The precursor vapor and the sulfur source vapor react to form a two-dimensional transition metal chalcogenide and deposit on the surface of the substrate 1006 to form a two-dimensional transition metal chalcogenide thin film (WS) as shown in FIG. 92A film).
Example four
This example relates to a method for preparing large-area continuous two-dimensional transition metal sulfur compound film, before preparation, two open quartz boats as shown in fig. 2 are prepared, respectively marked as open quartz boat a1002 and open quartz boat B1003, and the structures of the open quartz boat a1002 and the open quartz boat B1003 are as described in the first example. Cleaning the open quartz boat A1002 and the open quartz boat B1003 by using clean water, putting the cleaned open quartz boat A1002 and the open quartz boat B1003 into an ultrasonic machine for ultrasonic treatment for 10min, further cleaning the open quartz boat A1002 and the open quartz boat B1003, and after cleaning is finished, putting the open quartz boat A1002 and the open quartz boat B1003 into a drying box for drying and standby.
Referring to fig. 5, the preparation of the large-area continuous two-dimensional transition metal sulfur compound thin film comprises the following steps:
1) preparing a chemical vapor deposition precursor: as shown with reference to figure 6 of the drawings,weighing 70mg of WO3The powder was placed as precursor powder 1004 in an open quartz boat A1002 having an opening at one end, and the precursor powder 1004 was placed (WO powder 1004)3Powder) to the end of the open quartz boat a where the opening is provided, precursor powder 1004 (WO)3Powder) is spread in a range of 0.8cm to 1cm in length and about 0.5cm in width;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source 1005, wherein the selenium source is adopted in the embodiment, specifically, Se powder is adopted, and 200mg of Se powder is weighed and uniformly spread in the whole quartz boat B1003 with an opening, as shown in the attached figure 7;
3) preparing a catalyst: dissolving a catalyst (NaCl crystals with purity higher than 99.9%) in 100ml of deionized water, stirring the deionized water by using a glass rod to accelerate the dissolution of the NaCl crystals to form a catalyst solution, soaking the substrate 1006 in the catalyst solution, wherein the substrate 1006 in the embodiment is made of sapphire for 5 minutes, drying moisture on the surface of the substrate 1006 by using inert gas (argon) after the substrate 1006 is soaked, and inversely buckling the substrate 1006 in an open quartz boat A1002 and locating in precursor powder 1004 (WO)3Powder) above;
4) the method comprises the following steps of carrying an open quartz boat A1002 by a quartz plate base 1009, then placing the quartz boat A1003 at the central position of a main furnace heating area 1007 of the tube furnace, placing the open quartz boat B1003 in the central position of a preheating heating area 1008 of the tube furnace, wherein the main furnace heating area 1007 is communicated with the preheating heating area 1008, and the open quartz boat A1002 is opposite to the open end of the open quartz boat B1003;
5) setting the heating temperature and the maintaining time of the heating zone 1007 and the preheating zone 1008 of the main furnace, wherein in the embodiment, the heating temperature of the heating zone 1007 of the main furnace is 975 ℃ and the time is 30 min; setting the heating temperature of the preheating zone 1008 to 150 ℃ for 40 min; before heating the precursor, the tube furnace is evacuated, then inert gas (argon) is introduced, and the heating zone 1007 of the main furnace first heats the precursor powder (WO)3Powder) 1004, heating to 975 ℃ after 1 hour, maintaining for 30min, then naturally cooling the main furnace heating zone 1007, and forming precursor steam in the main furnace heating zone 1007; and whenAfter the heating zone 1007 of the main furnace is heated to the set temperature (975 ℃), the preheating heating zone 1008 starts to heat the Se powder 1005, the temperature is raised to 150 ℃ after 10min, the temperature is maintained for 40min, and then the preheating heating zone 1008 is naturally cooled to form selenium source steam; argon gas was introduced into the tube furnace at a flow rate of 150sccm throughout the process.
6) The precursor vapor reacts with the selenium source vapor to generate a two-dimensional transition metal chalcogenide which is deposited on the surface of the substrate 1006 to form a two-dimensional transition metal chalcogenide film (WSe)2A film).
EXAMPLE five
This example relates to a method for preparing large-area continuous two-dimensional transition metal sulfur compound film, before preparation, two open quartz boats as shown in fig. 2 are prepared, respectively marked as open quartz boat a1002 and open quartz boat B1003, and the structures of the open quartz boat a1002 and the open quartz boat B1003 are as described in the first example. Cleaning the open quartz boat A1002 and the open quartz boat B1003 by using clean water, putting the cleaned open quartz boat A1002 and the open quartz boat B1003 into an ultrasonic machine for ultrasonic treatment for 10min, further cleaning the open quartz boat A1002 and the open quartz boat B1003, and after cleaning is finished, putting the open quartz boat A1002 and the open quartz boat B1003 into a drying box for drying and standby.
Referring to fig. 5, the preparation of the large-area continuous two-dimensional transition metal sulfur compound thin film comprises the following steps:
1) preparing a chemical vapor deposition precursor: referring to FIG. 6, 70mg of MoO was weighed3The powder was placed as precursor powder 1004 in an open quartz boat A1002 having an opening at one end, and the precursor powder 1004 (MoO)3Powder) to the open-ended quartz boat a, precursor powder 1004 (MoO) was placed on the open-ended quartz boat a3Powder) is spread in a range of 0.8cm to 1cm in length and about 0.5cm in width;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source 1005, wherein the sulfur source is adopted in the embodiment, specifically, S powder is adopted, 200mg of the S powder is weighed as shown in the attached figure 7, and the S powder is uniformly spread in the whole quartz boat B1003 with an opening;
3) preparing a catalyst: dissolving catalyst (NaCl crystal with purity higher than 99.9%) (sodium chloride)Stirring deionized water by using a glass rod in 100ml of deionized water to accelerate the dissolution of NaCl crystals to form a catalyst solution, soaking a substrate 1006 in the catalyst solution, wherein the substrate 1006 in the embodiment is made of sapphire, the soaking time is 5 minutes, blowing moisture on the surface of the substrate 1006 by using inert gas (argon) after the substrate 1006 is soaked, and reversely buckling the substrate 1006 in an open quartz boat A1002 and locating in precursor powder 1004 (MoO)3Powder) above;
4) the method comprises the following steps of carrying an open quartz boat A1002 by a quartz plate base 1009, then placing the quartz boat A1003 at the central position of a main furnace heating area 1007 of the tube furnace, placing the open quartz boat B1003 in the central position of a preheating heating area 1008 of the tube furnace, wherein the main furnace heating area 1007 is communicated with the preheating heating area 1008, and the open quartz boat A1002 is opposite to the open end of the open quartz boat B1003;
5) setting the heating temperature and the maintaining time of the heating zone 1007 and the preheating zone 1008 of the main furnace, wherein in the embodiment, the heating temperature of the heating zone 1007 of the main furnace is 975 ℃ and the time is 30 min; setting the heating temperature of the preheating zone 1008 to 150 ℃ for 40 min; before heating the precursor, the tube furnace is evacuated, then inert gas (argon) is introduced, and the heating zone 1007 of the main furnace first heats the precursor powder (MoO)3Powder) 1004, heating to 975 ℃ after 1 hour, maintaining for 30min, then naturally cooling the main furnace heating zone 1007, and forming precursor steam in the main furnace heating zone 1007; when the temperature of the heating zone 1007 of the main furnace rises to the set temperature (975 ℃), the preheating heating zone 1008 starts to heat the S powder 1005, the temperature rises to 150 ℃ after 10min, the temperature is maintained for 40min, and then the preheating heating zone 1008 is naturally cooled to form sulfur source steam; argon gas was introduced into the tube furnace at a flow rate of 150sccm throughout the process.
6) The precursor vapor reacts with the sulfur source vapor to generate a two-dimensional transition metal chalcogenide which is deposited on the surface of the substrate 1006 to form a two-dimensional transition metal chalcogenide thin film (WoS)2A film).
EXAMPLE six
This example relates to a method for preparing large-area continuous two-dimensional transition metal sulfur compound film, before preparation, two open quartz boats as shown in fig. 2 are prepared, respectively marked as open quartz boat a1002 and open quartz boat B1003, and the structures of the open quartz boat a1002 and the open quartz boat B1003 are as described in the first example. Cleaning the open quartz boat A1002 and the open quartz boat B1003 by using clean water, putting the cleaned open quartz boat A1002 and the open quartz boat B1003 into an ultrasonic machine for ultrasonic treatment for 10min, further cleaning the open quartz boat A1002 and the open quartz boat B1003, and after cleaning is finished, putting the open quartz boat A1002 and the open quartz boat B1003 into a drying box for drying and standby.
Referring to fig. 5, the preparation of the large-area continuous two-dimensional transition metal sulfur compound thin film comprises the following steps:
1) preparing a chemical vapor deposition precursor: referring to FIG. 6, 70mg of MoO was weighed3The powder was placed as precursor powder 1004 in an open quartz boat A1002 having an opening at one end, and the precursor powder 1004 (MoO)3Powder) to the open-ended quartz boat a, precursor powder 1004 (MoO) was placed on the open-ended quartz boat a3Powder) is spread in a range of 0.8cm to 1cm in length and about 0.5cm in width;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source 1005, wherein the selenium source is adopted in the embodiment, specifically, Se powder is adopted, and 200mg of Se powder is weighed and uniformly spread in the whole quartz boat B1003 with an opening, as shown in the attached figure 7;
3) preparing a catalyst: dissolving a catalyst (NaCl crystals with purity higher than 99.9%) in 100ml of deionized water, stirring the deionized water with a glass rod to accelerate the dissolution of the NaCl crystals to form a catalyst solution, soaking the substrate 1006 with the catalyst solution, wherein the substrate 1006 is made of sapphire in the embodiment, the soaking time is 5 minutes, after the substrate 1006 is soaked, blowing moisture on the surface of the substrate 1006 with inert gas (argon), and inversely buckling the substrate 1006 in an open quartz boat A1002 and locating in precursor powder 1004 (MoO)3Powder) above;
4) the method comprises the following steps of carrying an open quartz boat A1002 by a quartz plate base 1009, then placing the quartz boat A1003 at the central position of a main furnace heating area 1007 of the tube furnace, placing the open quartz boat B1003 in the central position of a preheating heating area 1008 of the tube furnace, wherein the main furnace heating area 1007 is communicated with the preheating heating area 1008, and the open quartz boat A1002 is opposite to the open end of the open quartz boat B1003;
5) setting the heating temperature and the maintaining time of the heating zone 1007 and the preheating zone 1008 of the main furnace, wherein in the embodiment, the heating temperature of the heating zone 1007 of the main furnace is 975 ℃ and the time is 30 min; setting the heating temperature of the preheating zone 1008 to 150 ℃ for 40 min; before heating the precursor, the tube furnace is evacuated, then inert gas (argon) is introduced, and the heating zone 1007 of the main furnace first heats the precursor powder (MoO)3Powder) 1004, heating to 975 ℃ after 1 hour, maintaining for 30min, then naturally cooling the main furnace heating zone 1007, and forming precursor steam in the main furnace heating zone 1007; and when the heating zone 1007 of the main furnace is heated to the set temperature (975 ℃), the preheating heating zone 1008 starts to heat the Se powder 1005, the temperature is raised to 150 ℃ after 10min, the temperature is maintained for 40min, and then the preheating heating zone 1008 is naturally cooled to form selenium source steam; argon gas was introduced into the tube furnace at a flow rate of 150sccm throughout the process.
6) The precursor vapor reacts with the selenium source vapor to generate a two-dimensional transition metal chalcogenide which is deposited on the surface of the substrate 1006 to form a two-dimensional transition metal chalcogenide film (WoSe)2A film).
The present invention has been described in detail with reference to the embodiments, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. An opening quartz boat which is characterized in that: its one end is equipped with the opening, when carrying out chemical vapor deposition, regards two quartz boats as the carrier, and the opening one end of two quartz boats is relative, avoids forming the torrent in the relative one end of quartz boat for the air current is more steady.
2. The open quartz boat of claim 1, wherein: the height of the open quartz boat is 1.5cm, the width is 2.5cm, the length is 10cm, and the thickness is 0.2 cm.
3. A method for preparing large-area continuous two-dimensional transition metal sulfur compound film based on the quartz boat with opening of claim 1 is characterized in that: which comprises the following steps:
1) preparing a chemical vapor deposition precursor: weighing precursor powder, and placing the precursor powder in an open quartz boat A, wherein the precursor powder is placed at one end of the open quartz boat A, which is provided with an opening;
2) preparing a sulfur source or a selenium source by chemical vapor deposition: weighing a sulfur source or a selenium source, and placing the sulfur source or the selenium source in an open quartz boat B;
3) preparing a catalyst: dissolving a catalyst in deionized water to form a catalyst solution, soaking a substrate in the catalyst solution, drying the substrate by inert gas after soaking, and inversely covering the substrate above precursor powder in the open quartz boat A;
4) the opening quartz boat A is loaded by a quartz plate base and then is placed in a main furnace heating area of the tube furnace, the opening quartz boat B is integrally placed in a preheating heating area of the tube furnace, the main furnace heating area is communicated with the preheating heating area, one opening end of the opening quartz boat A is opposite to one opening end of the opening quartz boat B, turbulence is prevented from being formed at the opposite ends of the opening quartz boat A and the opening quartz boat B, and therefore airflow is more stable;
5) setting the heating temperature and the maintaining time of a main furnace heating area and a preheating heating area, heating the precursor to form precursor steam by the main furnace heating area, and starting heating a sulfur source or a selenium source by the preheating heating area to form sulfur source steam or selenium source steam after the main furnace heating area is heated to the set temperature;
6) and reacting the precursor vapor with sulfur source vapor or reacting the precursor vapor with selenium source vapor to generate a two-dimensional transition metal chalcogenide and depositing the two-dimensional transition metal chalcogenide on the surface of the substrate to form the two-dimensional transition metal chalcogenide film.
4. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 3, characterized in that: the precursor is tungsten trioxide or molybdenum trioxide; the sulfur source is S powder and selenium sourceIs Se powder; the two-dimensional transition metal chalcogenide film is WS2Or MoS2Or WSe2Or MoSe2A film.
5. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 4, characterized in that: the mass of the tungsten trioxide and the molybdenum trioxide is controlled to be 70-80 mg.
6. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 4, characterized in that: the quality of the sulfur source or the selenium source is controlled to be 180-200 mg.
7. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 3, characterized in that: the catalyst is NaCl, when a NaCl solution is prepared, 20-25 mgNaCl crystals are placed in a beaker and dissolved in 100-125 ml of deionized water, and a glass rod is used for stirring the deionized water to accelerate the dissolution of the NaCl crystals; the purity of the NaCl crystal is higher than 99.9%.
8. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 3, characterized in that: before heating the precursor in the step 5), vacuumizing the tube furnace, introducing inert gas, and introducing the inert gas into the tube furnace all the time in the processes of heating the precursor, heating the sulfur source or the selenium source and generating the two-dimensional transition metal chalcogenide.
9. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 8, characterized in that: the inert gas is argon and is introduced into the tubular furnace at a flow rate of 100-200 sccm.
10. The method for producing a large-area continuous two-dimensional transition metal sulfur compound thin film according to claim 4, characterized in that: the heating temperature of the heating zone of the main furnace set in the step 5) is 950-1000 ℃, and the maintaining time of the heating zone of the main furnace is 30-40 min; the heating temperature of the preheating heating zone is set to be 120-150 ℃, and the maintaining time of the preheating heating zone is 40-50 min.
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