CN115058700B - 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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- CN115058700B CN115058700B CN202210728587.2A CN202210728587A CN115058700B CN 115058700 B CN115058700 B CN 115058700B CN 202210728587 A CN202210728587 A CN 202210728587A CN 115058700 B CN115058700 B CN 115058700B
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 68
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 60
- 239000011733 molybdenum Substances 0.000 claims abstract description 60
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000011521 glass Substances 0.000 claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000010453 quartz Substances 0.000 claims abstract description 48
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 37
- 239000011593 sulfur Substances 0.000 claims abstract description 37
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 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 33
- 238000000137 annealing Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000009792 diffusion 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
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 8
- 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
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 23
- 229910052786 argon Inorganic materials 0.000 description 17
- 239000005361 soda-lime glass Substances 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 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
- 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
- 230000006911 nucleation Effects 0.000 description 7
- 238000010899 nucleation Methods 0.000 description 7
- 125000006850 spacer group Chemical group 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 238000012360 testing method Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000006872 improvement Effects 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
- 238000005303 weighing Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 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
- 239000011229 interlayer Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfide Chemical class 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
-
- 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 applicable to the technical field of semiconductor materials, and provides a preparation method of a molybdenum disulfide film and the molybdenum disulfide film, comprising the following steps: placing a sulfur source and a molybdenum source into a heating device, and keeping the flow of inert gas of 10-50sccm under normal pressure, and respectively carrying out heating treatment on 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 the quartz boat and an inert, high temperature resistant gasket is placed in the quartz boat and a glass substrate is placed over the gasket. The glass substrate is used as the gasket to assist the glass substrate to grow the monocrystal molybdenum disulfide or the large-size molybdenum disulfide continuous film, so that the excessive molybdenum source supply and other impurity introduction can be stopped, the interference factors can be greatly reduced, the good hydrophilicity of the glass substrate can also greatly spread the molten glass, 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, along with micro-scaleThe requirements of the electronic technology on the integration and the functionality are continuously improved, and the two-dimensional material is increasingly focused by researchers at home and abroad. Molybdenum disulfide (MoS) 2 ) The transition metal sulfide represented by the semiconductor film has the characteristics of atomic-level thickness, special layered structure, excellent optical and electrical properties and the like, thus developing a brand new research direction for the development of the electronic information technology in the later molar age, and further bringing about wide attention in academia and industry.
At present, chemical Vapor Deposition (CVD) is the most promising method for realizing large-area preparation of high-quality molybdenum disulfide semiconductor films. The common substrate for preparing the molybdenum disulfide semiconductor film by adopting chemical vapor deposition at the present stage comprises sapphire and SiO 2 Si, quartz, glass, etc. Among these common substrates, siO 2 The surface of the Si and quartz substrate is provided with a large amount of charged impurities, so that the grown molybdenum disulfide is an n-type doped semiconductor, the sapphire substrate has higher price, the nucleation density is higher, a continuous film is easy to form, and the growth of a large-size triangle molybdenum sulfide monocrystal is unfavorable. The glass substrate has low cost, large single crystal size and MoS compared with the materials 2 The growth speed is high, and the like, and is an important candidate substrate material for realizing the industrialized preparation of the large-area high-quality molybdenum disulfide semiconductor film at the present stage.
However, the existing method for preparing the molybdenum disulfide semiconductor film by the glass substrate has the problem that the growth of the large single crystal high-quality molybdenum disulfide film is easy to limit.
Disclosure of Invention
The embodiment of the application aims to provide a preparation method of a molybdenum disulfide film, which aims to solve the problem that the existing method for preparing a molybdenum disulfide semiconductor film by a glass substrate is easy to limit the growth of a large single crystal high-quality molybdenum disulfide film.
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 into a heating device, and keeping the flow of inert gas of 10-50sccm under normal pressure, and respectively carrying out heating treatment on 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 a 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 ℃.
Another object of the embodiment of the present application is a molybdenum disulfide film, which is prepared by the preparation method of the 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, so that the introduction of excessive molybdenum source supply and other impurities can be avoided, interference factors can be greatly reduced, the good hydrophilicity of the film can also greatly spread molten glass, 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.
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 application;
FIG. 2 is a graph showing the results of growing molybdenum disulfide on a glass substrate under different spacer conditions provided in the examples of the present application;
FIG. 3 is a schematic representation of molybdenum disulfide grown on a glass substrate using optimized process parameters, provided in the examples herein;
FIG. 4 is a schematic diagram of the result of a Raman test for preparing molybdenum disulfide on a glass substrate by using an alumina spacer according to an embodiment of the present application;
fig. 5 is a schematic diagram of molybdenum disulfide growth results under different argon flows 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 will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
Since the glass substrate is in a molten state at high temperature, in order to prevent glass from adhering to the chemical vapor deposition system after melting, a gasket is required to be added to assist the growth of molybdenum disulfide on the glass substrate, and molybdenum foil, graphite and the like are most commonly used before. However, the use of molybdenum foil gaskets releases molybdenum atoms under high temperature conditions to act as a source of excess molybdenum to participate in the reaction, while the hydrophobicity of graphite causes the molten glass to agglomerate into spheres at high temperatures. In addition, in an oxidizing atmosphere, particularly under oxygen-fed conditions, the graphite gasket may react with oxygen. These factors limit the growth of large single crystal high quality molybdenum disulfide films under the corresponding conditions. Therefore, the existing glass substrate molybdenum disulfide preparation technology needs to be improved.
The embodiment of the application provides a preparation method of a molybdenum disulfide film, which comprises the following steps:
and (3) placing a sulfur source and a molybdenum source in a heating device, keeping the flow of inert gas of 10-50sccm under normal pressure, and respectively carrying out heating treatment on the sulfur source and the molybdenum source for 2-20min to carry out chemical vapor deposition reaction to obtain the molybdenum disulfide film.
Wherein the sulfur source is placed in a 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 heating treatment temperature of the sulfur source is 180-270 ℃, preferably 200 ℃; the heating treatment temperature of the molybdenum source is 800-1100 ℃, 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 is preferably 20sccm. The time for heat-treating the sulfur source and the molybdenum source, i.e., the chemical vapor deposition reaction time, is preferably 10 minutes.
In the embodiment of the application, the glass substrate and the inert high temperature resistant gasket are subjected to conventional ultrasonic cleaning before being used, such as ultrasonic cleaning for 10min at 50 ℃ by acetone, isopropanol and deionized water in sequence, and drying by 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 embodiments herein take the example of aluminum oxide shims, but they may be replaced with other inert oxide, nitride, or carbide media (e.g., hafnium oxide, titanium oxide, aluminum nitride, siC, etc.), and should not be so limited in scope.
In the 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 the environment of not lower than 1100 ℃ for annealing treatment, wherein the annealing time is not less than 10min, and the flow of the inert gas is not less than 50sccm.
In a preferred embodiment of the application, the molybdenum source is placed in a quartz boat, an inert high temperature resistant 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 high temperature resistant gasket.
In a preferred embodiment of the present application, the steps of placing a sulfur source and a molybdenum source in a heating device, maintaining an inert gas flow of 10-50sccm under normal pressure, and performing a chemical vapor deposition reaction on the sulfur source and the molybdenum source for 2-20min, respectively, to obtain a molybdenum disulfide film, include:
and respectively placing a sulfur source and a molybdenum source at the edges of a first temperature region and a second temperature region of a double-temperature-region tube furnace, when the temperature of the first temperature region reaches 180-270 ℃ and the temperature of the second temperature region reaches 800-1100 ℃, moving the sulfur source into the first temperature region, moving the molybdenum source into the second temperature region, performing chemical vapor deposition reaction after 10min, keeping the atmospheric pressure in a quartz tube in the chemical vapor deposition process, continuously introducing inert gas of 10-50sccm 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 a cavity stable within +/-3 mbar when molybdenum disulfide grows to obtain a molybdenum disulfide film.
Optionally, the method for preparing molybdenum disulfide by using the glass substrate specifically comprises the following steps:
(1) for glass substrates (size may be 2X 2cm 2 Or 4X 4cm 2 ) Alumina pads (size may be 2X 2 cm) 2 Or 4X 4cm 2 ) And the silicon oxide gasket are sequentially subjected to ultrasonic cleaning by using acetone, isopropanol and deionized water, the cleaning time is 10 minutes, and the temperature of the ultrasonic cleaning machine is set to be 50 ℃.
(2) And (3) carrying out annealing treatment on the alumina gasket in the step (1), wherein the annealing time is 30 minutes, the annealing temperature is 1100 ℃, the annealing atmosphere is Ar gas atmosphere, and the gas flow is 300sccm.
(3) Weighing 0.2-4mg of molybdenum trioxide (serving as a molybdenum source for growing molybdenum disulfide), placing the molybdenum trioxide on the silicon oxide gasket treated in the step (1), placing the silicon oxide substrate on a quartz boat, placing the aluminum oxide gasket treated in the step (2) in the quartz boat, and placing the glass substrate on the aluminum oxide gasket in the step (1). Weighing 0.5-3g of sulfur powder (serving as a sulfur source for growing molybdenum disulfide) and placing the sulfur powder into a corundum boat. The application selects an alumina gasket as a buffer interlayer of a glass substrate and a chemical vapor deposition system.
(4) According to the method, a double-temperature-zone tube furnace is selected, a growth system is shown in a figure 1, a first temperature zone and a second temperature zone are marked respectively, a corundum boat and a quartz boat in the step (2) are placed in the edges of the first temperature zone and the second temperature zone in sequence, when the temperature of the first temperature zone reaches a preset temperature value of 180-270 ℃, the temperature of the second temperature zone reaches a preset temperature value of 800-1100 ℃, the first tube furnace is moved to the first temperature zone, the second tube furnace is moved to the second temperature zone, after 10min, chemical vapor deposition reaction is carried out, the quartz tube of the chemical vapor deposition system is cooled for 2-20min until the chemical vapor deposition reaction reaches a preset time, and then high-quality molybdenum disulfide preparation can be achieved on a glass substrate. In addition, the pressure in the quartz tube is kept at normal pressure in the chemical vapor deposition process, and 10-50sccm of argon is continuously introduced as carrier gas for assisting the diffusion of the molybdenum source and the sulfur source.
Fig. 1 is a schematic diagram of a production device involved in a preparation method of a molybdenum disulfide film, wherein the production device comprises a first temperature zone and a second temperature zone, and the production device respectively heats sulfur powder, molybdenum oxide powder and a growth substrate. Wherein sulfur powder is contained in a corundum boat and placed in a first temperature zone. Molybdenum oxide powder is contained in Si/SiO 2 And on the gasket, an alumina gasket is placed under the growth glass substrate, and is placed in a quartz boat and placed in a second temperature zone. Here, 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, which 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 in the preparation of the various examples is shown in FIG. 1.
Example 1
In this embodiment, the preparation method of the molybdenum disulfide film includes the following steps:
1. the alumina pad and the glass substrate were each ultrasonically cleaned with acetone, isopropanol, deionized water at 50 ℃ for 10min, and blow-dried with a nitrogen gun.
2. The alumina shims were annealed at 1100 ℃ under an argon atmosphere. The annealing time was 30min and the argon flow was 300sccm.
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 molybdenum trioxide powder is placed in a quartz boat. A piece of quartz boat is placed at a position 3mm away from the edge of molybdenum trioxide, and a piece of quartz boat is placed at a position 2cm away from the edge of molybdenum trioxide 2 And a soda lime glass substrate of the same specification is placed over the spacerThe aluminum oxide gasket is used for preventing the soda lime glass from adhering to a quartz boat at the lower layer in a high-temperature melting state.
4. The quartz boat and the corundum boat are respectively placed in the positions of a second temperature zone and a first temperature zone in the quartz tube, and the intervals between the two are 20cm. The cvd system was then evacuated to 0.1mBar and then argon was introduced at 900sccm to atmospheric pressure, which was repeated three times to remove the gaseous impurities from the tube.
5. Subsequently, a sulfur source, a molybdenum source and a soda lime glass substrate were heated, respectively, in an atmosphere of normal pressure while maintaining an argon flow of 20sccm. 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 after the temperature is stable, controlling the growth time of molybdenum disulfide to be 10min, and keeping the pressure in the cavity stable within +/-3 mbar during growth.
6. After the growth is finished, the first temperature zone is pushed to be 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 to expose the quartz boat, opening a vacuum pump and an angle valve, and introducing argon with the flow of 300sccm to remove redundant sulfur vapor 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 2
In this embodiment, the preparation method of the molybdenum disulfide film includes the following steps:
1. the alumina pad and the glass substrate were each ultrasonically cleaned with acetone, isopropanol, deionized water at 50 ℃ for 10min, and blow-dried with a nitrogen gun.
2. The alumina shims were annealed at 1100 ℃ under an argon atmosphere. The annealing time was 30min and the argon flow was 300sccm.
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 molybdenum trioxide powder is placed in a quartz boat. A piece of quartz boat is placed at a position 3mm away from the edge of molybdenum trioxide, and a piece of quartz boat is placed at a position 2cm away from the edge of molybdenum trioxide 2 And a soda lime glass substrate with the same specification is placed above the gasket, and the adhesion of the soda lime glass with a quartz boat at the lower layer is prevented by the aid of the alumina gasket in a high-temperature melting state.
4. The quartz boat and the corundum boat are respectively placed in the positions of a second temperature zone and a first temperature zone in the quartz tube, and the intervals between the two are 20cm. The cvd system was then evacuated to 0.1mBar and then argon was introduced at 900sccm to atmospheric pressure, which was repeated three times to remove the gaseous impurities from the tube.
5. Subsequently, a sulfur source, a molybdenum source and a soda lime glass substrate were heated, respectively, in an atmosphere of normal pressure while maintaining an argon flow of 20sccm. 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 after the temperature is stable, controlling the growth time of molybdenum disulfide to be 10min, and keeping the pressure in the cavity stable within +/-3 mbar during growth.
6. After the growth is finished, the first temperature zone is pushed to be 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 to expose the quartz boat, opening a vacuum pump and an angle valve, and introducing argon with the flow of 300sccm to remove redundant sulfur vapor 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 preparation method of the molybdenum disulfide film includes the following steps:
1. the alumina pad and the glass substrate were each ultrasonically cleaned with acetone, isopropanol, deionized water at 50 ℃ for 10min, and blow-dried with a nitrogen gun.
2. The alumina shims were annealed at 1100 ℃ under an argon atmosphere. The annealing time was 30min and the argon flow was 300sccm.
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 molybdenum trioxide powder is placed in a quartz boat. A piece of quartz boat is placed at a position 3mm away from the edge of molybdenum trioxide, and a piece of quartz boat is placed at a position 2cm away from the edge of molybdenum trioxide 2 And a soda lime glass substrate with the same specification is placed above the gasket, and the adhesion of the soda lime glass with a quartz boat at the lower layer is prevented by the aid of the alumina gasket in a high-temperature melting state.
4. The quartz boat and the corundum boat are respectively placed in the positions of a second temperature zone and a first temperature zone in the quartz tube, and the intervals between the two are 20cm. The cvd system was then evacuated to 0.1mBar and then argon was introduced at 900sccm to atmospheric pressure, which was repeated three times to remove the gaseous impurities from the tube.
5. Subsequently, a sulfur source, a molybdenum source and a soda lime glass substrate were heated, respectively, in an atmosphere of normal pressure while maintaining an argon flow of 20sccm. 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 after the temperature is stable, controlling the growth time of molybdenum disulfide to be 10min, and keeping the pressure in the cavity stable within +/-3 mbar during growth.
Further, the application investigated the effect of different spacer conditions on the growth of molybdenum disulfide on glass substrates, and only the spacer type was changed on the basis of example 1 above, with the remaining process conditions unchanged.
The results of growing molybdenum disulfide on glass substrates under different gasket conditions are shown in FIG. 2, wherein FIGS. 2 (a) - (b) are the results of growing with molybdenum foil as the gasket, and FIGS. 2 (c) - (d) are the results of growing with aluminum oxide gasket (i.e., example 2, process parameters: molybdenum source (MoO) 3 ) Mass: 2.0mg of sulfur powder: 1.4g, growth temperature: 1050 ℃, carrier gas flow (Ar gas): 20sccm, growth time: 10 min). Wherein the scale of fig. 2 (a) and fig. 2 (c) is 200 microns and the scale of fig. 2 (b) and fig. 2 (d) is 5 microns. It can be seen from a direct comparison of fig. 2 (b) and fig. 2 (d) that not only triangular molybdenum disulfide crystals are grown by using the alumina spacer, but also the surface of the molybdenum disulfide crystals has no double-layer nucleation points, and the prepared molybdenum disulfide single crystals are more uniform.
Notably, conventional technical methods typically employ molybdenum foil or graphite as a support for the glass substrate. Graphite is used as a carrier, and the glass is easy to melt to form a sphere under the high-temperature condition due to the good hydrophobicity of the graphite surface, and the result is shown in the document Bandgap tuning of two-dimensional materials by sphere diameter engineering. As a result of using the molybdenum foil as the glass substrate spacer, as shown in fig. 2 (a) and 2 (b), the grown molybdenum disulfide monocrystal surface is prone to forming double-layer nucleation sites and has poor uniformity due to the additional molybdenum source provided by the molybdenum foil. According to the technical scheme, the aluminum oxide gasket is adopted as the carrier of the glass substrate, the growth result is shown in fig. 2 (c) and 2 (d), firstly, the effect of a buffer layer of the glass substrate and the quartz boat carrier can be still achieved, secondly, the molybdenum foil is used as the gasket, the secondary supply of a molybdenum source is avoided, the reasonable control of growth reaction factors is facilitated, thirdly, the surface of the spherical glass body with larger 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 of the glass substrate are further researched. In addition, the alumina gasket has weaker relative chemical activity, so that the range of process conditions for early-stage experimental research of chemical vapor deposition of molybdenum disulfide can be further expanded, and processes of preparing the molybdenum disulfide by growing on a glass substrate at high temperature by introducing oxygen can be researched.
Further, the present application was also directed to a study of the effect of various process parameters on the growth of molybdenum disulfide on glass substrates based on alumina shims, wherein, as shown in FIG. 3, optimized process parameters (i.e., example 3: molybdenum source (MoO 3 ) Mass: 0.6mg, sulfur powder mass: 1.4g, growth temperature: 1050 ℃, carrier gas flow (Ar gas): 20sccm, growth time: 10 min) based on the optical photo result of the millimeter-sized molybdenum disulfide monocrystal grown on the glass substrate by the alumina gasket, the triangle-shaped molybdenum disulfide monocrystal prepared by the scheme can be more than 2mm, and the method has nearly doubled improvement compared with the traditional technical method, and further shows the beneficial benefit of the technical scheme. Meanwhile, it is possible to increase the single crystal size by decreasing the nucleation density by decreasing the quality of the molybdenum source in combination with example 2.
In addition, the present application performs raman test on molybdenum disulfide prepared on a glass substrate using an alumina spacer in example 3, and the test results are shown in fig. 4. From FIG. 4, it can be seen that alumina shims produce E of molybdenum disulfide 1 2g And A 1g Characteristic peaks are at 387.3 and 405.2cm, respectively -1 The difference of 17.9 wave numbers is consistent with the single-layer molybdenum disulfide in the literature, and further proves that the high-quality single-layer molybdenum disulfide grows in the method.
In addition, the application also aims at the influence of molybdenum disulfide grown on the glass substrate based on the molybdenum foil gasket under different argon flow rates in the early experiment processThe relevant research is carried out, and the technological parameters are as follows: sulfur powder 1.4g in mass, temperature 200 ℃, 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 regulated, other process parameters are kept unchanged, the research results are shown in fig. 5, the growth results (molybdenum foil is used as a gasket) under different argon flows, fig. 5 (a) is 20sccm, fig. 5 (b) is 30sccm, fig. 5 (c) is 40sccm, and fig. 5 (d) is 50sccm; it can be seen that changing the argon flow rate mainly changes the supply ratio and speed of the S source and Mo source for the growth system of the present application, thus resulting in an increase in single crystal size with an increase in Ar flow rate, but thicker nucleation sites are also likely to occur on triangular single crystals, affecting the uniformity of the single crystals. In summary, according to the embodiment of the application, by using the aluminum oxide gasket as the gasket of the soda lime glass, the defects that the molybdenum disulfide nucleation density is high, the film growth is uneven and a plurality of layers of growth nuclear points exist due to the fact that the molybdenum foil is used as the gasket in the traditional method to participate in the reaction when molybdenum atoms are supplied (as shown in fig. 2) are avoided, and adverse factors such as stress of the molybdenum disulfide film due to the fact that the hydrophobic molten glass of the graphite gasket is easy to form a sphere at high temperature are also relieved. Meanwhile, because the alumina has the advantages of high melting point, good chemical stability and the like, the process conditions of the glass substrate chemical vapor deposition molybdenum disulfide can be expanded, for example, the high-temperature oxygen-introducing process research and the like are carried out by adopting the process methods which are difficult to carry out by adopting the traditional molybdenum foil and the graphite gasket. In whole, the preparation of the glass substrate molybdenum disulfide assisted by the alumina gasket is a new process method, and the preparation of the molybdenum disulfide by the method has the advantages of small nucleation density, good growth stability, large single crystal size and the like (as shown in figures 2 and 3), and has important significance for realizing the industrialized preparation of the low-cost glass substrate molybdenum disulfide.
In addition, the scheme can be applied to preparing molybdenum disulfide on a glass substrate, and can also be applied to preparing other valuable materials such as two-dimensional semiconductors, semi-metals or insulator films on the glass substrate, and the use of an alumina gasket to assist the glass substrate in growing the molybdenum disulfide can be considered as a special example of the method. The above examples only represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the present application. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (7)
1. The preparation method of the molybdenum disulfide film is characterized by comprising the following steps:
placing a sulfur source and a molybdenum source into a heating device, and keeping the flow of inert gas of 20-30sccm under normal pressure, and respectively carrying out heating treatment on 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 a corundum boat; 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;
the heating treatment temperature of the sulfur source is 180-270 ℃; the heating treatment temperature of the molybdenum source is 1050 ℃; the mass ratio of the molybdenum source to the sulfur source is 0.6:1400.
2. The method for preparing a 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.
3. The method for preparing a molybdenum disulfide film according to claim 1 or 2, 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.
4. 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 the environment of not lower than 1100 ℃ for annealing treatment, wherein the annealing time is not less than 10min, and the flow of the inert gas is not less than 50sccm.
5. The method for preparing a molybdenum disulfide 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 20-30sccm under normal pressure, and performing a chemical vapor deposition reaction on the sulfur source and the molybdenum source for 2-20min, respectively, comprises:
and respectively placing a sulfur source and a molybdenum source at the edges of a first temperature region and a second temperature region of the double-temperature-region tube furnace, when the temperature of the first temperature region reaches 180-270 ℃ and the temperature of the second temperature region reaches 1050 ℃, moving the sulfur source into the first temperature region, moving the molybdenum source into the second temperature region, performing chemical vapor deposition reaction after 10min, keeping the atmospheric pressure in a quartz tube in the chemical vapor deposition process, continuously introducing 20-30sccm 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 a cavity to be stabilized within +/-3 mbar when molybdenum disulfide grows to obtain a molybdenum disulfide film.
6. The method for producing a molybdenum disulfide film according to claim 1 or 5, wherein the sulfur source heat treatment temperature is 200 ℃; the heating treatment temperature of the molybdenum source is 1050 ℃; the inert gas flow rate is 20sccm.
7. The molybdenum disulfide film is characterized by being prepared by the preparation method of the molybdenum disulfide film in any one of claims 1-6.
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