CN115058700A - Preparation method of molybdenum disulfide film and molybdenum disulfide film - Google Patents
Preparation method of molybdenum disulfide film and molybdenum disulfide film Download PDFInfo
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- CN115058700A CN115058700A CN202210728587.2A CN202210728587A CN115058700A CN 115058700 A CN115058700 A CN 115058700A CN 202210728587 A CN202210728587 A CN 202210728587A CN 115058700 A CN115058700 A CN 115058700A
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 66
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000011733 molybdenum Substances 0.000 claims abstract description 62
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 62
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000011521 glass Substances 0.000 claims abstract description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000010453 quartz Substances 0.000 claims abstract description 46
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 40
- 239000011593 sulfur Substances 0.000 claims abstract description 40
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000010431 corundum Substances 0.000 claims abstract description 14
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 43
- 239000010408 film Substances 0.000 claims description 38
- 230000008569 process Effects 0.000 claims description 17
- 238000000137 annealing Methods 0.000 claims description 15
- 239000010409 thin film Substances 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000009792 diffusion process Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 2
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 10
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000006060 molten glass Substances 0.000 abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 30
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 22
- 229910052786 argon Inorganic materials 0.000 description 17
- 239000013078 crystal Substances 0.000 description 14
- 239000005361 soda-lime glass Substances 0.000 description 13
- 239000011888 foil Substances 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 230000006911 nucleation Effects 0.000 description 9
- 238000010899 nucleation Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 230000003287 optical effect Effects 0.000 description 2
- 238000013386 optimize process Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 Transition metal sulfides Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Abstract
The application is suitable for the technical field of semiconductor materials, and provides a preparation method of a molybdenum disulfide film and the molybdenum disulfide film, which comprises the following steps: placing a sulfur source and a molybdenum source in a heating device, keeping the flow rate of inert gas of 10-50sccm under the normal pressure condition, and respectively heating the sulfur source and the molybdenum source for 2-20min to carry out chemical vapor deposition reaction to obtain a molybdenum disulfide film; wherein, the sulfur source is arranged in the corundum boat; the molybdenum source is placed on a quartz boat, an inert high-temperature-resistant gasket is placed in the quartz boat, and a glass substrate is placed above the gasket. According to the preparation method, the inert high-temperature-resistant material is used as the gasket to assist the glass substrate to grow the monocrystal molybdenum disulfide or the large-size molybdenum disulfide continuous film, redundant molybdenum source supply and other impurity introduction can be avoided, interference factors can be greatly reduced, the molten glass can be greatly spread due to good hydrophilicity of the inert high-temperature-resistant material, the chemical vapor deposition reaction is improved, and the preparation of the high-quality large monocrystal low-cost molybdenum disulfide semiconductor film can be realized.
Description
Technical Field
The application belongs to the technical field of semiconductor materials, and particularly relates to a preparation method of a molybdenum disulfide film and the molybdenum disulfide film.
Background
In recent years, with the increasing demand of microelectronic technology for integration and functionality, two-dimensional materials are receiving more and more attention from researchers at home and abroad. Molybdenum disulfide (MoS) 2 ) Transition metal sulfides, which are typical of semiconductor thin films, have a completely new research direction for the development of electronic information technology in the next Mole era due to their atomic-scale thickness, special layered structure, and excellent optical and electrical properties, and thus have attracted extensive attention in academic and industrial fields.
Currently, Chemical Vapor Deposition (CVD) is the most promising method for large-area production of high-quality semiconductor films of molybdenum disulfide. The common substrate for preparing the molybdenum disulfide semiconductor film by chemical vapor deposition at the present stage comprises sapphire and SiO 2 Si, quartz, glass, etc. Among these commonly used substrates, SiO 2 The surface of the/Si and quartz substrate has a large amount of charged impurities, so that the grown molybdenum disulfide is an n-type doped semiconductor, the sapphire substrate has high price and high nucleation density, a continuous film is easy to form, and the growth of large-size triangular molybdenum sulfide single crystals is not facilitated. The glass substrate has low cost, large single crystal size and MoS compared with the above materials 2 The growth speed is high, and the like, and the molybdenum disulfide semiconductor film is an important candidate substrate material for realizing the industrialized preparation of large-area high-quality molybdenum disulfide semiconductor films at the present stage.
However, the existing method for preparing the molybdenum disulfide semiconductor film by using the glass substrate has the problem that the growth of a large single-crystal high-quality molybdenum disulfide film is easily limited.
Disclosure of Invention
An object of an embodiment of the present application is to provide a method for preparing a molybdenum disulfide thin film, which aims to solve the problem that the growth of a large single crystal high quality molybdenum disulfide thin film is easily limited in the existing method for preparing a molybdenum disulfide semiconductor thin film on a glass substrate.
The embodiment of the application is realized in such a way that the preparation method of the molybdenum disulfide film comprises the following steps:
placing a sulfur source and a molybdenum source in a heating device, keeping the flow of inert gas of 10-50sccm under the normal pressure condition, and respectively heating the sulfur source and the molybdenum source for 2-20min to carry out chemical vapor deposition reaction to obtain a molybdenum disulfide film;
wherein the sulfur source is placed in the corundum boat; the molybdenum source is placed on a quartz boat, an inert high-temperature-resistant gasket subjected to annealing treatment is placed in the quartz boat, and a glass substrate is placed above the inert high-temperature-resistant gasket;
the temperature of the sulfur source heating treatment is 180-270 ℃; the heating treatment temperature of the molybdenum source is 800-1100 ℃.
Another object of an embodiment of the present invention is to provide a molybdenum disulfide film, which is prepared by the above method for preparing a molybdenum disulfide film.
According to the preparation method of the molybdenum disulfide film, the inert high-temperature-resistant material is used as the gasket to assist the glass substrate to grow the monocrystal molybdenum disulfide or the large-size molybdenum disulfide continuous film, redundant molybdenum source supply and other impurity introduction can be avoided, interference factors can be greatly reduced, molten glass can be greatly spread due to good hydrophilicity, chemical vapor deposition reaction is improved, and the preparation of the high-quality large-monocrystal low-cost molybdenum disulfide semiconductor film can be realized.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing molybdenum disulfide by chemical vapor deposition according to an embodiment of the present disclosure;
FIG. 2 is a graph showing the results of growing molybdenum disulfide on a glass substrate under different pad conditions according to the present application;
FIG. 3 is a graph showing the results of molybdenum disulfide growth on a glass substrate using an alumina spacer with optimized process parameters as provided by the examples herein;
FIG. 4 is a graph showing Raman test results of molybdenum disulfide prepared on a glass substrate using an alumina pad according to an embodiment of the present disclosure;
figure 5 is a graph showing the results of molybdenum disulfide growth at various argon flows as provided in the examples of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
Since the glass substrate is in a molten state at a high temperature, in order to prevent the glass from sticking to the chemical vapor deposition system after melting, a gasket is required to be added to assist the growth of the molybdenum disulfide on the glass substrate, and the gasket is most commonly used before, such as molybdenum foil, graphite, and the like. But the molybdenum foil gasket releases molybdenum atoms under high-temperature environment to act as an excessive molybdenum source to participate in reaction, and the hydrophobicity of the graphite enables the molten glass to be condensed into a ball shape under high temperature. In addition, the graphite pad may react with oxygen in an oxidizing atmosphere, particularly under oxygen-passing conditions. These factors all limit the growth of large single crystal high quality molybdenum disulfide films under the corresponding conditions. Therefore, the existing technology for preparing the glass substrate molybdenum disulfide needs to be improved.
The embodiment of the application provides a preparation method of a molybdenum disulfide film, which comprises the following steps:
and placing the sulfur source and the molybdenum source in a heating device, keeping the flow of inert gas of 10-50sccm under the normal pressure condition, and respectively heating the sulfur source and the molybdenum source for 2-20min to perform chemical vapor deposition reaction to obtain the molybdenum disulfide film.
Wherein the sulfur source is placed in the corundum boat; the molybdenum source is placed on a quartz boat, an inert high-temperature-resistant gasket subjected to annealing treatment is placed in the quartz boat, and a glass substrate is placed above the inert high-temperature-resistant gasket.
Wherein the temperature of the sulfur source heating treatment is 180-270 ℃, and preferably 200 ℃; the heating treatment temperature of the molybdenum source is 800-1100 ℃, and is preferably 1080 ℃.
Wherein the mass ratio of the molybdenum source to the sulfur source is (0.2-4): (500-3000), preferably 0.6: 1400.
Wherein, the inert gas flow rate is preferably 20 sccm. The time for heating the sulfur source and the molybdenum source, i.e., the chemical vapor deposition reaction time, is preferably 10 min.
In the embodiment of the application, the glass substrate and the inert high temperature-resistant gasket are subjected to conventional ultrasonic cleaning before use, for example, ultrasonic cleaning is sequentially carried out for 10min at 50 ℃ by using acetone, isopropanol and deionized water, and drying is carried out by using nitrogen.
In the embodiment of the application, the inert high-temperature-resistant gasket is one of an inert oxide gasket, an inert nitride gasket and an inert carbide gasket. The specific embodiment of the present application takes an alumina spacer as an example, but it can be replaced by other inert oxide, nitride or carbide dielectrics (such as hafnium oxide, titanium oxide, aluminum nitride, SiC, etc.), and should not limit the scope of the present application.
In an embodiment of the present application, the annealing process of the inert high temperature resistant gasket may be:
and (3) in an inert gas environment, placing the inert high-temperature-resistant gasket in an environment of not less than 1100 ℃ for annealing treatment, wherein the annealing time is not less than 10min, and the inert gas flow is not less than 50 sccm.
In a preferred embodiment of the present application, the molybdenum source is placed in a quartz boat, an inert refractory gasket after annealing treatment is placed in the quartz boat at a distance of 1-6mm from the edge of the molybdenum source, and a glass substrate is placed above the inert refractory gasket.
In a preferred embodiment of the present invention, the step of placing the sulfur source and the molybdenum source in a heating device, maintaining an inert gas flow rate of 10 to 50sccm under normal pressure, and performing a heating treatment on the sulfur source and the molybdenum source for 2 to 20min to perform a chemical vapor deposition reaction to obtain the molybdenum disulfide thin film includes:
respectively placing a sulfur source and a molybdenum source at the edges of a first temperature area and a second temperature area of a dual-temperature area tubular furnace, moving the sulfur source into the first temperature area when the temperature of the first temperature area reaches 180-plus-minus 270 ℃ and the temperature of the second temperature area reaches 800-plus-minus 1100 ℃, moving the molybdenum source into the second temperature area, carrying out chemical vapor deposition reaction after 10min, keeping the atmospheric pressure in a quartz tube at normal pressure in the chemical vapor deposition process, continuously introducing 10-50sccm inert gas as carrier gas for assisting the diffusion of the molybdenum source and the sulfur source, controlling the chemical vapor deposition reaction time to be 2-20min, and keeping the pressure in the cavity to be stabilized within +/-3 mbar when the molybdenum disulfide grows to obtain the molybdenum disulfide film.
Optionally, the method for preparing molybdenum disulfide from the glass substrate specifically comprises the following steps:
respectively aligning glass substrates (the size can be 2 multiplied by 2 cm) 2 Or 4X 4cm 2 ) Alumina pad (size can be 2 x 2 cm) 2 Or 4X 4cm 2 ) And the silicon oxide gasket is subjected to ultrasonic cleaning by sequentially using acetone, isopropanol and deionized water, the cleaning time is 10 minutes, and the set temperature of an ultrasonic cleaning machine is 50 ℃.
And annealing the aluminum oxide gasket in the step I for 30 minutes at 1100 ℃ under Ar gas flow of 300 sccm.
Weighing 0.2-4mg of molybdenum trioxide (serving as a molybdenum source for growing molybdenum disulfide) and placing the molybdenum trioxide on the silicon oxide gasket treated in the step I, then placing the silicon oxide substrate on a quartz boat, placing the aluminum oxide gasket treated in the step II in the quartz boat, and placing the glass substrate on the aluminum oxide gasket in the step I. 0.5-3g of sulfur powder (as a sulfur source for growing molybdenum disulfide) is weighed and placed in a corundum boat. The application selects the alumina gasket as the buffering intermediate layer of the glass substrate and the chemical vapor deposition system.
Selecting a double-temperature-zone tube furnace, wherein a growth system is shown in figure 1, respectively marking a first temperature zone and a second temperature zone, sequentially placing the corundum boat and the quartz boat in the step II at the edges of the first temperature zone and the second temperature zone, moving the first tube furnace to the first temperature zone when the temperature of the first temperature zone reaches a preset temperature value of 180-. In addition, the pressure in the quartz tube is kept at normal pressure during the chemical vapor deposition process, and argon gas of 10-50sccm is continuously introduced to be used as a carrier gas for assisting the diffusion of the molybdenum source and the sulfur source.
Fig. 1 is a schematic view of a production apparatus involved in the method for preparing a molybdenum disulfide thin film of the present application, and the diagram includes a first temperature zone and a second temperature zone, which respectively perform heating functions on sulfur powder, molybdenum oxide powder and a growth substrate. Wherein the sulfur powder is placed in the corundum boat and is placed in the first temperature zone. The molybdenum oxide powder is contained in Si/SiO 2 On the gasket, an alumina gasket is placed under the growth glass substrate, and the alumina gasket is placed in the quartz boat and placed in the second temperature area. Here, the corundum boat, Si \ SiO 2 The gasket and the quartz boat are carriers corresponding to the reaction source and the growth substrate, the sulfur powder and the molybdenum oxide powder are sources for generating molybdenum disulfide through reaction, and the glass is a substrate for growing molybdenum disulfide through reaction. The alumina gasket is a carrier of the glass substrate, can buffer the glass substrate and the quartz boat carrier, and prevents the glass substrate from melting and sticking on the quartz boat carrier at high temperature.
The embodiment of the application also provides a molybdenum disulfide film, and the molybdenum disulfide film is prepared by the preparation method of the molybdenum disulfide film.
Examples of certain embodiments of the present application are given below, which are not intended to limit the scope of the present application. The apparatus used for the preparation process of each example is shown in FIG. 1.
Example 1
In this embodiment, the method for preparing the molybdenum disulfide thin film includes the following steps:
1. and ultrasonically cleaning the aluminum oxide gasket and the glass substrate by acetone, isopropanol and deionized water at 50 ℃ for 10min respectively in sequence, and drying by a nitrogen gun.
2. The alumina gasket was annealed at 1100 c under argon atmosphere. The annealing time was 30min and the argon flow was 300 sccm.
3. 1.4g of sulfur powder and 0.6mg of molybdenum trioxide powder were weighed. The weighed sulfur powder is placed in a corundum boat, and the molybdenum trioxide powder is placed in a quartz boat. Placing a piece of 2 multiplied by 2cm quartz boat at a position 3mm away from the edge of the molybdenum trioxide 2 The soda-lime glass substrate with the same specification is placed above the alumina gasket, and the soda-lime glass is prevented from being adhered to the quartz boat at the lower layer in a high-temperature melting state by the alumina gasket.
4. And respectively placing the quartz boat and the corundum boat into the second temperature zone and the first temperature zone in the quartz tube, wherein the interval between the two temperature zones is 20 cm. The CVD system was then evacuated to 0.1mBar and then filled with 900sccm argon to atmospheric pressure, which was repeated three times to remove the gaseous impurities in the tube.
5. Subsequently, the sulfur source, the molybdenum source, and the soda-lime glass substrate were heated, respectively, in an atmospheric pressure environment, maintaining an argon flow of 20 sccm. Wherein the heating temperature of the sulfur source is 200 ℃, and the heating temperature of the molybdenum source and the soda-lime glass substrate is 1080 ℃. And when the temperature is stable, controlling the growth time of the molybdenum disulfide to be 10min, and keeping the pressure in the cavity to be within +/-3 mbar during growth.
6. After the growth is finished, the first temperature zone is pushed away from the sulfur powder. And then, when the temperature of the second temperature zone furnace body is reduced to 680 ℃, pushing the second temperature zone furnace body until the quartz boat is exposed, opening a vacuum pump and an angle valve, and introducing argon gas with the flow of 300sccm to remove the redundant sulfur steam in the tube. And breaking vacuum for sampling when the temperature in the quartz tube is lower than 100 ℃ and the temperature of the quartz boat sample is lower than 50 ℃.
Example 2
In this embodiment, the method for preparing the molybdenum disulfide thin film includes the following steps:
1. and ultrasonically cleaning the aluminum oxide gasket and the glass substrate by acetone, isopropanol and deionized water at 50 ℃ for 10min respectively in sequence, and drying by a nitrogen gun.
2. The alumina gasket was annealed at 1100 c under argon atmosphere. The annealing time was 30min and the argon flow was 300 sccm.
3. 1.4g of sulfur powder and 2.0mg of molybdenum trioxide powder were weighed. The weighed sulfur powder is placed in a corundum boat, and the molybdenum trioxide powder is placed in a quartz boat. Placing a piece of 2X 2cm quartz boat at a position 3mm away from the edge of the molybdenum trioxide 2 The alumina gasket is arranged, a soda-lime glass substrate with the same specification is arranged above the gasket, and the soda-lime glass is prevented from being adhered to the quartz boat at the lower layer in a high-temperature melting state by the alumina gasket.
4. And respectively placing the quartz boat and the corundum boat into the second temperature zone and the first temperature zone in the quartz tube, wherein the interval between the two temperature zones is 20 cm. The CVD system was then evacuated to 0.1mBar and then filled with 900sccm argon to atmospheric pressure, which was repeated three times to remove gaseous impurities from the tube.
5. Subsequently, the sulfur source, the molybdenum source, and the soda-lime glass substrate were heated, respectively, in an atmospheric pressure environment, maintaining an argon flow of 20 sccm. Wherein the heating temperature of the sulfur source is 200 ℃, and the heating temperature of the molybdenum source and the soda-lime glass substrate is 1050 ℃. And when the temperature is stable, controlling the growth time of the molybdenum disulfide to be 10min, and keeping the pressure in the cavity to be within +/-3 mbar during growth.
6. After the growth is finished, the first temperature zone is pushed away from the sulfur powder. And then, when the temperature of the second temperature zone furnace body is reduced to 680 ℃, pushing the second temperature zone furnace body until the quartz boat is exposed, opening a vacuum pump and an angle valve, and introducing argon gas with the flow of 300sccm to remove the redundant sulfur steam in the tube. And breaking vacuum and sampling when the temperature in the quartz tube is lower than 100 ℃ and the temperature of the quartz boat sample is lower than 50 ℃.
Example 3
In this embodiment, the method for preparing the molybdenum disulfide thin film includes the following steps:
1. and ultrasonically cleaning the aluminum oxide gasket and the glass substrate by acetone, isopropanol and deionized water at 50 ℃ for 10min respectively in sequence, and drying by a nitrogen gun.
2. The alumina pad was annealed at 1100 c under an argon atmosphere. The annealing time was 30min, and the argon flow was 300 sccm.
3. 1.4g of sulfur powder and 0.6mg of molybdenum trioxide powder were weighed. The weighed sulfur powder is placed in a corundum boat, and the molybdenum trioxide powder is placed in a quartz boat. Placing a piece of 2 multiplied by 2cm quartz boat at a position 3mm away from the edge of the molybdenum trioxide 2 The soda-lime glass substrate with the same specification is placed above the alumina gasket, and the soda-lime glass is prevented from being adhered to the quartz boat at the lower layer in a high-temperature melting state by the alumina gasket.
4. And respectively placing the quartz boat and the corundum boat into the second temperature zone and the first temperature zone in the quartz tube, wherein the interval between the two temperature zones is 20 cm. The CVD system was then evacuated to 0.1mBar and then filled with 900sccm argon to atmospheric pressure, which was repeated three times to remove gaseous impurities from the tube.
5. Subsequently, the sulfur source, the molybdenum source, and the soda-lime glass substrate were heated, respectively, in an atmospheric pressure environment, maintaining an argon flow of 20 sccm. Wherein the heating temperature of the sulfur source is 200 ℃, and the heating temperature of the molybdenum source and the soda-lime glass substrate is 1050 ℃. And when the temperature is stable, controlling the growth time of the molybdenum disulfide to be 10min, and keeping the pressure in the cavity to be within +/-3 mbar during growth.
Further, the influence of different gasket conditions on the growth of the molybdenum disulfide on the glass substrate is researched, on the basis of the embodiment 1, only the type of the gasket is changed, and the rest process conditions are not changed.
The results of growing molybdenum disulfide on glass substrates under different pad conditions are shown in FIG. 2, FIGS. 2(a) - (b) are the results of growing using molybdenum foil as the pad, and FIGS. 2(c) - (d) are the results of growing using alumina pad (i.e., example 2, process parameters: molybdenum source (MoO) 3 ) Quality: 2.0mg, sulfur powder mass: 1.4g, growth temperature: 1050 ℃, carrier gas flow (Ar gas): 20sccm, growth time: 10 min). Wherein the scales of fig. 2(a) and 2(c) are both 200 microns and fig. 2(b) and 2(d) are both 5 microns. As can be seen from the direct comparison between FIG. 2(b) and FIG. 2(d), the triangular molybdenum disulfide crystal is grown by using the alumina pad, and the molybdenum disulfide crystal surface has no double-layer nucleation points, so that the prepared molybdenum disulfide single crystal is more uniform.
It is noted that conventional technical methods generally employ molybdenum foils or graphite as the support for the glass substrate. As graphite is used as a carrier, glass is easy to melt and form a sphere under high temperature conditions due to the better hydrophobicity of the graphite surface, and the result is shown in the literature of Bandgap tuning of two-dimensional materials by sphere diameter engineering. As a result of using molybdenum foil as a glass substrate gasket, as shown in fig. 2(a) and 2(b), the molybdenum disulfide single crystal grown on the surface of the substrate is prone to double layer nucleation sites and has poor uniformity, generally because the molybdenum foil provides an additional molybdenum source. According to the technical scheme, the alumina gasket is used as the carrier of the glass substrate, the growth result is shown in figures 2(c) and 2(d), firstly, the alumina gasket can still play a role of a buffer layer of the glass substrate and the quartz boat carrier, secondly, the molybdenum foil is used as the gasket to avoid secondary supply of a molybdenum source, reasonable control of growth reaction factors is facilitated, thirdly, a spherical glass body surface with a large radian is not easy to form relative to the graphite gasket, molybdenum disulfide is easy to transfer to other substrates, and the photoelectric performance and further device application research are further researched. In addition, the alumina gasket has relatively weak chemical activity, so that the process condition range of the chemical vapor deposition molybdenum disulfide early-stage experimental study can be further expanded, for example, the processes of preparing molybdenum disulfide by introducing oxygen to grow on a glass substrate at a high temperature can be studied.
Further, the present application also conducted relevant studies on the effect of different process parameters on molybdenum disulfide growth on a glass substrate based on alumina spacers, wherein optimized process parameters (i.e., example 3: molybdenum source (MoO) are employed as shown in FIG. 3 3 ) Quality: 0.6mg, sulfur powder mass: 1.4g, growth temperature: 1050 ℃, carrier gas flow (Ar gas): 20sccm, growth time: 10min) based on the optical photo result of the millimeter-sized molybdenum disulfide monocrystal grown on the glass substrate by the alumina gasket, the graph shows that the triangular molybdenum disulfide monocrystal prepared by the method can be larger than 2mm, the improvement is nearly doubled compared with the traditional technical method, and the beneficial benefit of the technical scheme is further shown. Meanwhile, by combining with the embodiment 2, the nucleation density is reduced by reducing the quality of the molybdenum source, and the size of the single crystal is increased.
In addition, this applicationPlease refer to example 3, which uses an alumina pad to prepare molybdenum disulfide on a glass substrate for raman test, and the test result is shown in fig. 4. From FIG. 4, it can be seen that E for preparing molybdenum disulfide from alumina gasket 1 2g And A 1g The characteristic peaks are at 387.3 and 405.2cm respectively -1 And the difference of 17.9 wave numbers is consistent with the result of monolayer molybdenum disulfide in the literature, and further proves that high-quality monolayer molybdenum disulfide is grown in the method.
In addition, in the early stage experiment process, the influence of molybdenum disulfide growing on the glass substrate based on the molybdenum foil gasket under different argon flows is subjected to relevant research, and the process parameters are as follows: the mass of sulfur powder is 1.4g, the temperature is 200 ℃, and a molybdenum source (MoO) 3 ) The mass is 3mg, the temperature is 880 ℃, the growth time is 10min, the growth pressure is 1000mBar, only the argon flow is adjusted, other process parameters are kept unchanged, the research result is shown in FIG. 5, the growth result (molybdenum foil is used as a gasket) under different argon flows is shown in FIG. 5(a)20sccm, FIG. 5(b)30sccm, FIG. 5(c)40sccm and FIG. 5(d)50 sccm; it can be seen that changing the argon flow rate for the growth system of the present application primarily changes the supply ratio and rate of the S source and Mo source, thus resulting in an increase in the size of the crystal as the Ar flow rate increases, but thicker nucleation sites also tend to occur on the triangular crystal, affecting the uniformity of the crystal. In summary, the alumina gasket is used as the gasket of the soda-lime glass in the embodiment of the application, so that the defects that the nucleation density of molybdenum disulfide is high and multilayer growth nucleation points exist due to the fact that molybdenum atoms are supplied to participate in a reaction in a traditional method by adopting molybdenum foil as the gasket (as shown in fig. 2), and the phenomenon that the multilayer growth nucleation points exist due to uneven film growth is avoided, and the adverse factors that the stress exists in the molybdenum disulfide film due to the fact that hydrophobic molten glass of the graphite gasket is easy to form a spherical shape at high temperature and the like are relieved. Meanwhile, the alumina has the advantages of high melting point, good chemical stability and the like, so that the process conditions of chemical vapor deposition of molybdenum disulfide on the glass substrate can be expanded, such as high-temperature oxygen introduction process research and other process methods which are difficult to perform by adopting the traditional molybdenum foil and graphite gasket. In general, the preparation of molybdenum disulfide with an alumina gasket as an auxiliary glass substrate is a new process, and the molybdenum disulfide prepared by the method has small nucleation density,The advantages of good growth stability, large single crystal size and the like (as shown in figures 2 and 3) are of great significance for realizing the industrial preparation of the low-cost glass substrate molybdenum disulfide.
In addition, the scheme of the application can be applied to preparing molybdenum disulfide on a glass substrate, and can also be applied to preparing other valuable materials on the glass substrate, such as a two-dimensional semiconductor, a semi-metal or an insulator film, and the adoption of an alumina gasket to assist the glass substrate to grow the molybdenum disulfide can be considered as a special example of the patent method. The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent application shall be subject to the appended claims.
The above description is only a preferred embodiment of the present application and should not be taken as limiting the present application, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a molybdenum disulfide film is characterized by comprising the following steps:
placing a sulfur source and a molybdenum source in a heating device, keeping the flow of inert gas of 10-50sccm under the normal pressure condition, and respectively heating the sulfur source and the molybdenum source for 2-20min to perform chemical vapor deposition reaction to obtain a molybdenum disulfide film;
wherein the sulfur source is placed in the corundum boat; the molybdenum source is placed on a quartz boat, an inert high-temperature-resistant gasket subjected to annealing treatment is placed in the quartz boat, and a glass substrate is placed above the inert high-temperature-resistant gasket;
the heating treatment temperature of the sulfur source is 180-270 ℃; the heating treatment temperature of the molybdenum source is 800-1100 ℃.
2. The method of claim 1, wherein the mass ratio of the molybdenum source to the sulfur source is (0.2-4): (500- > 3000).
3. The method for preparing a molybdenum disulfide thin film according to claim 1 or 2, wherein the mass ratio of the molybdenum source to the sulfur source is 0.6: 1400.
4. The method for preparing the molybdenum disulfide film according to claim 1, wherein the inert high-temperature-resistant gasket is one of an inert oxide gasket, an inert nitride gasket and an inert carbide gasket.
5. The method for preparing the molybdenum disulfide film according to claim 1 or 4, wherein the inert high-temperature-resistant gasket is one of an aluminum oxide gasket, a hafnium oxide gasket, a titanium oxide gasket, an aluminum nitride gasket and a silicon carbide gasket.
6. The method for preparing the molybdenum disulfide film according to claim 1, wherein the molybdenum source is placed in a quartz boat, an inert high temperature-resistant gasket subjected to annealing treatment is placed in the quartz boat at a position 1-6mm away from the edge of the molybdenum source, and a glass substrate is placed above the inert high temperature-resistant gasket.
7. The method for preparing the molybdenum disulfide film according to claim 1, wherein the annealing treatment process of the inert high-temperature-resistant gasket is as follows:
and (3) in an inert gas environment, placing the inert high-temperature-resistant gasket in an environment of not less than 1100 ℃ for annealing treatment, wherein the annealing time is not less than 10min, and the inert gas flow is not less than 50 sccm.
8. The method for preparing a molybdenum disulfide thin film according to claim 1, wherein the step of placing a sulfur source and a molybdenum source in a heating device, maintaining an inert gas flow of 10 to 50sccm under normal pressure, and performing a chemical vapor deposition reaction by heating the sulfur source and the molybdenum source for 2 to 20min to obtain the molybdenum disulfide thin film comprises:
respectively placing a sulfur source and a molybdenum source at the edges of a first temperature area and a second temperature area of a dual-temperature area tubular furnace, moving the sulfur source into the first temperature area when the temperature of the first temperature area reaches 180-plus-minus 270 ℃ and the temperature of the second temperature area reaches 800-plus-minus 1100 ℃, moving the molybdenum source into the second temperature area, carrying out chemical vapor deposition reaction after 10min, keeping the pressure in a quartz tube at normal pressure in the chemical vapor deposition process, continuously introducing 10-50sccm inert gas as carrier gas for assisting the diffusion of the molybdenum source and the sulfur source, controlling the chemical vapor deposition reaction time to be 2-20min, and keeping the pressure in the cavity to be stabilized within +/-3 mbar when the molybdenum disulfide grows to obtain the molybdenum disulfide film.
9. The method for preparing a molybdenum disulfide film according to claim 1 or 8, wherein the temperature of the sulfur source is 200 ℃; the molybdenum source heating treatment temperature is 1080 ℃; the inert gas flow rate was 20 sccm.
10. A molybdenum disulfide film produced by the method for producing a molybdenum disulfide film according to any one of claims 1 to 8.
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