CN110373715A - Prepare the chemical vapor depsotition equipment and method of two dimensional crystal material - Google Patents
Prepare the chemical vapor depsotition equipment and method of two dimensional crystal material Download PDFInfo
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- CN110373715A CN110373715A CN201910776832.5A CN201910776832A CN110373715A CN 110373715 A CN110373715 A CN 110373715A CN 201910776832 A CN201910776832 A CN 201910776832A CN 110373715 A CN110373715 A CN 110373715A
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- raw material
- dimensional crystal
- inlet pipe
- air inlet
- crystal material
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- 239000000463 material Substances 0.000 title claims abstract description 152
- 239000013078 crystal Substances 0.000 title claims abstract description 121
- 239000000126 substance Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 98
- 238000010438 heat treatment Methods 0.000 claims abstract description 93
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 130
- 239000012159 carrier gas Substances 0.000 claims description 47
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 46
- 229910052723 transition metal Inorganic materials 0.000 claims description 44
- 229910052717 sulfur Inorganic materials 0.000 claims description 42
- 239000011593 sulfur Substances 0.000 claims description 42
- 150000003624 transition metals Chemical class 0.000 claims description 42
- 239000000758 substrate Substances 0.000 claims description 41
- LJSQFQKUNVCTIA-UHFFFAOYSA-N diethyl sulfide Chemical compound CCSCC LJSQFQKUNVCTIA-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 238000009434 installation Methods 0.000 claims description 11
- 229910052961 molybdenite Inorganic materials 0.000 claims description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 11
- 230000007246 mechanism Effects 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- LALRXNPLTWZJIJ-UHFFFAOYSA-N triethylborane Chemical group CCB(CC)CC LALRXNPLTWZJIJ-UHFFFAOYSA-N 0.000 claims description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 7
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 6
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 claims description 6
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 5
- 239000011669 selenium Substances 0.000 claims description 5
- 239000005864 Sulphur Substances 0.000 claims description 4
- SSLSOHVYTNAFRT-UHFFFAOYSA-H [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[W+6] Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[W+6] SSLSOHVYTNAFRT-UHFFFAOYSA-H 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 claims description 4
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Chemical compound BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 claims description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 4
- RXHMDIUZIJSGAI-UHFFFAOYSA-J n,n-dimethylcarbamodithioate;molybdenum(4+) Chemical compound [Mo+4].CN(C)C([S-])=S.CN(C)C([S-])=S.CN(C)C([S-])=S.CN(C)C([S-])=S RXHMDIUZIJSGAI-UHFFFAOYSA-J 0.000 claims description 4
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 4
- OMAWWKIPXLIPDE-UHFFFAOYSA-N (ethyldiselanyl)ethane Chemical compound CC[Se][Se]CC OMAWWKIPXLIPDE-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- JZDKETLGZNAINJ-UHFFFAOYSA-H [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mo+6] Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mo+6] JZDKETLGZNAINJ-UHFFFAOYSA-H 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 229910052798 chalcogen Inorganic materials 0.000 claims description 3
- 150000001787 chalcogens Chemical group 0.000 claims description 3
- 238000010943 off-gassing Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 150000003942 tert-butylamines Chemical class 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 18
- 230000008901 benefit Effects 0.000 abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 84
- 229910052786 argon Inorganic materials 0.000 description 42
- 238000002156 mixing Methods 0.000 description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 230000003028 elevating effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910000058 selane Inorganic materials 0.000 description 5
- 239000002178 crystalline material Substances 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 3
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- AKUCEXGLFUSJCD-UHFFFAOYSA-N indium(3+);selenium(2-) Chemical compound [Se-2].[Se-2].[Se-2].[In+3].[In+3] AKUCEXGLFUSJCD-UHFFFAOYSA-N 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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
- C23C16/44—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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4485—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
Abstract
The present invention discloses a kind of chemical vapor depsotition equipment for preparing two dimensional crystal material and method, wherein chemical vapor depsotition equipment, comprising: vacuum chamber；Sample stage and gas distributor are provided in the vacuum chamber；First temperature-controlling chamber, for placing the first raw material, and for heating first raw material to generate the steam of the first raw material；First air inlet pipe is connected to first temperature-controlling chamber and the gas distributor；Second temperature-controlling chamber heats for placing the second raw material of solid-state or liquid, and for second raw material to generate the steam of the second raw material；Second air inlet pipe is connected to second temperature-controlling chamber and the gas distributor；Third air inlet pipe, one end are used to be connected to the gas source of second raw material, and the other end is connected to the gas distributor.Technical solution of the present invention has two dimensional crystal material preparation precision high, product uniformity and reproducible, chemical vapor depsotition equipment advantage applied widely.
Description
Technical field
The present invention relates to two dimensional crystal Material Field, in particular to a kind of chemical vapor deposition for preparing two dimensional crystal material
Device and method.
Background technique
Since discovery single-layer graphene in 2004, the preparation of various New Two Dimensional crystalline materials and application study layer go out not
Thoroughly.Because two dimensional crystal material shows physics abundant, chemical property, in nano electron device, nano photoelectric device, sensing
Device, catalysis and energy field show wide application prospect.Wherein Transition-metal dichalcogenide is two dimensional crystal material man
A huge branch in race.The two dimensional crystal material that the existing chemical vapor depsotition equipment for preparing two dimensional crystal material is prepared
The precision of material, repeatability and uniformity are poor, and thickness is usually larger, the existing chemical vapor deposition for preparing two dimensional crystal material
Product equipment the shortcomings that there is also poor universalities, it is difficult to preparation and different technique for different types of two dimensional crystal material
Prepare two dimensional crystal material.
Summary of the invention
The main object of the present invention is to propose a kind of chemical vapor depsotition equipment for preparing two dimensional crystal material, it is intended to be promoted
Uniformity, repeatability and the accuracy of control of two dimensional crystal material preparation.
To achieve the above object, the chemical vapor depsotition equipment proposed by the present invention for preparing two dimensional crystal material, comprising:
Vacuum chamber；Sample stage, the sample stage are arranged in the vacuum chamber, and heating dress is provided in the sample stage
It sets；
Gas distributor, the gas distributor are arranged in the vacuum chamber；
First temperature-controlling chamber, for placing the first raw material, and for heating first raw material to generate the first original
The steam of material；
First air inlet pipe is connected to first temperature-controlling chamber and the gas distributor；
Second temperature-controlling chamber heats for placing the second raw material of solid-state or liquid, and for second raw material to produce
The steam of raw second raw material；
Second air inlet pipe is connected to second temperature-controlling chamber and the gas distributor；
Third air inlet pipe, one end are used to be connected to the gas source of second raw material, and the other end is connected to the gas distribution
Device；
Three the 4th air inlet pipe, the 4th air inlet pipe is used to lead to carrier gas to the gas distributor, described in three
4th air inlet pipe is respectively communicated with first air inlet pipe, second air inlet pipe and the third air inlet pipe.
Optionally, secondary heating mechanism and third are respectively equipped on the outside of first air inlet pipe and second air inlet pipe
Heating device, the secondary heating mechanism and the third heating device are respectively used to entirety and institute to first air inlet pipe
The entirety for stating the second air inlet pipe is heated.
Optionally, for placing the second raw material of liquid, the chemical vapor depsotition equipment includes for second temperature-controlling chamber
The inlet end of 5th air inlet pipe, the 5th air inlet pipe is connected to the 4th air inlet pipe, the outlet side of the 5th air inlet pipe
It is connected to second temperature-controlling chamber, the outlet side of the 5th air inlet pipe is for being inserted into second raw material；Either,
Second temperature-controlling chamber is used to place the second raw material of solid state powder, is equipped with bubbling in second temperature-controlling chamber
Device.
Optionally, the chemical vapor depsotition equipment further include:
Lifting device, one end of the lifting device connect the sample stage, and the other end connects the vacuum chamber, the liter
Falling unit is for adjusting the distance between the sample stage and the gas distributor；
Actuator, the lifting device and the vacuum chamber are rotatablely connected, and the actuator is connect with the lifting device,
To drive the lifting device to rotate；Alternatively,
The upper surface of the sample stage has circular installation region, and the upper surface of the sample stage is equipped with multiple stomatas,
Multiple stomatas are arranged along the edge interval of installation region, and the outgassing direction of the stomata is along the clockwise of the installation region
Or counterclockwise tilt, the stomata is for being connected to carrier gas source, to drive the substrate rotation on the sample stage.
Optionally, the first air inlet pipe described in depositing device, second air inlet pipe, the third air inlet pipe and the described 4th
Mass flowmenter and gas circuit valve are equipped in air inlet pipe.
Optionally, the chemical vapor depsotition equipment further includes plasma generator, the plasma generator packet
Two high frequency terminals are included, two high frequency terminal one of them are connect with the gas distributor, another one and the sample
Platform connection.
Optionally, the vacuum chamber is equipped with the 4th heating device.
Optionally, for heating transition metal source to generate steam, second temperature-controlling chamber is used for for first temperature-controlling chamber
Sulfur family material is heated to generate steam.
The present invention also proposes a kind of method for preparing two dimensional crystal material, comprising the following steps:
It places the substrate above on the indoor sample stage of the vacuum, by the vacuum chamber to back end vacuum；
First raw material are subjected to heating and generate steam, are passed through in the vacuum chamber；
Second raw material are carried out plus thermogenetic steam is passed through in the vacuum chamber, or by gaseous second raw material
It is passed through the vacuum chamber；
Growth air pressure needed for the indoor pressure of vacuum is adjusted to the growth two dimensional crystal material；
The substrate is heated to growth temperature needed for the two dimensional crystal material of growing up, rotates the substrate, it is described
First raw material and second raw material pass through chemical reaction on the substrate and generate the two dimensional crystal material.
Optionally, the two dimensional crystal material includes: transition metal sulfur family two dimensional crystal material MX2, III-VI race two dimension
Crystalline material VX and hexagonal boron nitride, wherein M is transition metal element, and X is chalcogen, and V is third major element.
Optionally, first raw material include: that Dimethyldithiocarbamate molybdenum, bis- (tert-butylamines) are bis- (dimethyl amine)
Tungsten, hexahydroxy molybdenum, hexahydroxy tungsten, tungsten hexachloride, trimethyl indium, indium trichloride, second raw material include: methyl disulfide,
Diethyl thioether, diethyl diselenide, hydrogen sulfide, hydrogen selenide, sulphur, selenium；Either,
First raw material include: boron triethyl, borazine, boron bromide, boron chloride, second raw material
It include: ammonium hydroxide, ammonium chloride.
Optionally, the two dimensional crystal material is MoS2, first raw material are Mo (CO)6, second raw material
(C2H5)2S。
Optionally, the heating temperature of first raw material is 100 DEG C~120 DEG C；
Steam is generated the first raw material are carried out heating, is passed through before the step in the vacuum chamber, further comprises the steps of:
The flow of the step of being passed through carrier gas into the vacuum chamber, the carrier gas is less than or equal to 100sccm.
Optionally, the two dimensional crystal material growth air pressure is 5Torr~10Torr；
The growth temperature of the two dimensional crystal material is 500 DEG C~600 DEG C, and the velocity of rotation of the substrate is less than or equal to
2000r/min；
The two dimensional crystal material with a thickness of 1~20 atomic layer.
Technical solution of the present invention heats transition metal source and sulfur family by using the first temperature-controlling chamber and the second temperature-controlling chamber respectively
Material, so that the steam of the steam of the first raw material and the second raw material maintains isolation from each other before entering vacuum chamber, until
Mixing reacts again after entering in vacuum chamber, ensures that reaction occurs in vacuum chamber, advantageously allows the base on sample stage
Bottom equably generates two dimensional crystal material.Steam is brought into vacuum chamber by technical solution of the present invention by carrier gas, therefore
It can be controlled by controlling the flow that gas distributor enters vacuum chamber to steam, be conducive to the steaming for controlling transition metal source
The ratio of the steam of gas and sulfur family material can effectively promote two-dimentional crystalline substance to promote the preparation precision of two dimensional crystal material
The repeatability and uniformity of body material preparation.Technical solution of the present invention can support using solid raw material, gas raw material and
Liquid raw material prepares two dimensional crystal material, the steam production supported the steam for carrying raw material with carrier gas, control raw material
The technological parameters such as raw amount, the steam air inflow of control vacuum chamber have and are suitable for a variety of two dimensional crystal materials preparation and a variety of
Process prepares the advantages of two dimensional crystal material, has the characteristics that applied widely.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is the knot for one embodiment of chemical vapor depsotition equipment that the present invention prepares transition metal sulfur family two dimensional crystal material
Structure schematic diagram；
Fig. 2 is the flow diagram for the method that the present invention prepares transition metal sulfur family two dimensional crystal material；
Fig. 3 is the Raman light of two dimensional crystal material prepared by the embodiment 1 for the method that the present invention prepares two dimensional crystal material
Spectrogram.
Drawing reference numeral explanation:
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
It is to be appreciated that if relating to directionality instruction (such as up, down, left, right, before and after ...) in the embodiment of the present invention,
Then directionality instruction be only used for explain under a certain particular pose (as shown in the picture) between each component relative positional relationship,
Motion conditions etc., if the particular pose changes, directionality instruction is also correspondingly changed correspondingly.
In addition, being somebody's turn to do " first ", " second " etc. if relating to the description of " first ", " second " etc. in the embodiment of the present invention
Description be used for description purposes only, be not understood to indicate or imply its relative importance or implicitly indicate indicated skill
The quantity of art feature." first " is defined as a result, the feature of " second " can explicitly or implicitly include at least one spy
Sign.It in addition, the technical solution between each embodiment can be combined with each other, but must be with those of ordinary skill in the art's energy
It is enough realize based on, will be understood that the knot of this technical solution when conflicting or cannot achieve when occurs in the combination of technical solution
Conjunction is not present, also not the present invention claims protection scope within.
The present invention proposes a kind of chemical vapor depsotition equipment for preparing two dimensional crystal material.
In embodiments of the present invention, as shown in Figure 1, the chemical vapor depsotition equipment for preparing two dimensional crystal material, comprising:
Vacuum chamber 100, sample stage 200, gas distributor 110, the first temperature-controlling chamber 300, the first air inlet pipe 310, the second temperature-controlling chamber 400,
Second air inlet pipe 410, third air inlet pipe 500, the 4th air inlet pipe 600, the sample stage 200 are arranged in the vacuum chamber 100,
First heater is provided in the sample stage 200, the first heater is used to add for the substrate on sample stage 200
Heat；Gas distributor 110, the gas distributor 110 are arranged in the vacuum chamber 100；First temperature-controlling chamber 300, for putting
The first raw material are set, and for heating first raw material to generate the steam of the first raw material；First air inlet pipe 310 connects
Lead to first temperature-controlling chamber 300 and the gas distributor 110；Second temperature-controlling chamber 400 is former for placing solid-state or liquid second
Material, and heat for second raw material to generate the steam of the second raw material；Second air inlet pipe 410 is connected to described second
Temperature-controlling chamber 400 and the gas distributor 110；500 one end of third air inlet pipe is used to be connected to the gas source of second raw material,
The other end is connected to the gas distributor 110；Three the 4th air inlet pipe 600, the 4th air inlet pipe 600 are used for the gas
Distributor 110 leads to carrier gas, and three the 4th air inlet pipe 600 are respectively communicated with first air inlet pipe 310, described second
Air inlet pipe 410 and the third air inlet pipe 500, for diluting and carrying first air inlet pipe 310, second air inlet pipe
Gas in steam or the third air inlet pipe 500 in 410.It should be noted that in the present embodiment, first temperature-controlling chamber and
Second temperature-controlling chamber can also use 400 knot of identical temperature-controlling chamber 300 or temperature-controlling chamber according to the characteristic of the first, second raw material
Structure；It may include three or three or more the 4th air inlet pipe 600, the inlet end of the 4th all air inlet pipe 600 can connect
Wherein in the 4th air inlet pipe 600, it is subsequently used for one carrier gas source of connection, is also possible to the 4th all air inlets
The setting of the interval of pipe 600, is separately connected different carrier gas sources.
Specifically, the present embodiment is to prepare transition metal sulfur family two dimensional crystal material using transition metal source and sulfur family material
For, but be not limited only to prepare transition metal sulfur family two dimensional crystal material, in other embodiments, it is also possible to using boron source
Boron nitride two dimensional crystal material is prepared with nitrogen source；Either, selenizing phosphide material is prepared using indium source and selenium source.Utilize the chemistry
When vapor deposition apparatus prepares transition metal sulfur family two dimensional crystal material, transition metal source is put into the first temperature-controlling chamber 300, is added
Heat transition source metal is passed through to generate steam, by the steam of transition metal source by the first air inlet pipe 310 and gas distributor 110
Into vacuum chamber 100, solid-state sulfur family material is put into the second temperature-controlling chamber 400, heats sulfur family material to generate steam, by solid-state
The steam of sulfur family material is passed into vacuum chamber 100 by the second air inlet pipe 410 and gas distributor 110, transition metal source
The steam of steam and sulfur family material mixes in vacuum chamber 100, and chemical deposition is grown in the substrate of sample stage 200, forms two
Tie up crystalline material.When sulfur family material is gas, such as hydrogen sulfide, directly the gas source of sulfur family material can be connected to described
In third air inlet pipe 500, entered in vacuum chamber 100 by third air inlet pipe 500 and gas distributor 110, without using arriving
Second temperature-controlling chamber 400.When the air pressure of the steam of transition metal source or the steam of hot sulfur family material is small, the described 4th can be passed through
Air inlet pipe 600 leads to carrier gas to the first air inlet pipe 310 or the second air inlet pipe 410, so that carrier gas carries steam and enters
In vacuum chamber 100.It may be noted that when, the temperature-controlling chamber is not merely suitable for the device heated, and the temperature-controlling chamber can also be with
With refrigerating function, to control the speed that steam generates by temperature, to realize to the air inflow of 100 inner vapor of vacuum chamber
Control, to control the growth of two dimensional crystal material.
Technical solution of the present invention heats transition metal source by using the first temperature-controlling chamber 300 and the second temperature-controlling chamber 400 respectively
With sulfur family material so that the steam of the steam of transition metal source and sulfur family material enter vacuum chamber 100 before keep mutually every
From until just starting to mix after entering in vacuum chamber 100, guarantee chemical reaction occurs in the base heated by sample stage 200
On bottom, thus equably generated in substrate monoatomic layer to 20 atomic layers thicks transition metal sulfur family two dimensional crystal material.
Steam is brought into vacuum chamber 100 by technical solution of the present invention by carrier gas, therefore can pass through control gas distribution
The flow that device 110 enters vacuum chamber 100 to steam controls, and is conducive to the steam and sulfur family material that control transition metal source
The ratio of steam can effectively promote Transition Metal Sulfur to promote the preparation precision of transition metal sulfur family two dimensional crystal material
The repeatability and uniformity of race's two dimensional crystal material preparation.Technical solution of the present invention can be supported to use solid raw material, gas
Body raw material and liquid raw material prepare two dimensional crystal material, support to carry the steam of raw material, control former material with carrier gas
The technological parameters such as the steam yield of material, the steam air inflow for controlling vacuum chamber 100, have and are suitable for a variety of two dimensional crystal materials
The advantages of preparation and kinds of processes method prepare two dimensional crystal material, has the characteristics that applied widely.
The present embodiment is entered true using the steam of the flow control transition metal source of carrier gas and the steam of sulfur family material
The ratio and quality of empty room 100；Then with gas distributor 110 control transition metal source steam and sulfur family material steam into
Enter the spatial distribution and mixing of vacuum chamber 100, can further expand the preparation face of transition metal sulfur family two dimensional crystal material
The accuracy of product, the repeatability for improving preparation and thickness control.
Further, in the present embodiment, as shown in Figure 1, first air inlet pipe 310 and second air inlet pipe 410
Outside be respectively equipped with secondary heating mechanism 320 and third heating device 420, the secondary heating mechanism 320 and the third
Heating device 420 is respectively used to add the entirety of first air inlet pipe 310 and the entirety of second air inlet pipe 410
Heat.First raw material and the second raw material enter described in process first air inlet pipe 310 and the second air inlet pipe 410 respectively
In the way of vacuum chamber 100, it is easy to coagulate on tube wall due to the tube wall temperature of air inlet pipe is low, so that actually entering vacuum
Vapor volume in room 100 is reduced, and the present embodiment is distinguished using the secondary heating mechanism 320 and the third heating device 420
Entirety for entirety and second air inlet pipe 410 to first air inlet pipe 310 heats, and is conducive to avoid first
Steam in air inlet pipe 310 and the second air inlet pipe 410 is condensed in tube wall, promotes the utilization rate of raw material, is also helped control and is steamed
The precision of gas dosage, to promote the quality of two dimensional crystal material.
Further, in the present embodiment, as shown in Figure 1, first air inlet pipe 310, second air inlet pipe 410,
The third air inlet pipe 500 and the 4th air inlet pipe 600 are equipped with mass flowmenter 800 and gas circuit section valve 900.The quality
Flowmeter 800 is capable of the flow of accurate control vector gas, thus the steam for the transition metal source that control vector gas carries and
The steam of sulfur family material enters the amount of vacuum chamber 100, to promote the preparation precision and repeatability of two dimensional crystal material.
Further, in the present embodiment, as shown in Figure 1, second temperature-controlling chamber 400 is for placing the second former material of liquid
Material, the chemical vapor depsotition equipment include the 5th air inlet pipe 700, the inlet end of the 5th air inlet pipe 700 and the 4th air inlet
Pipe 600 is connected to, and the outlet side of the 5th air inlet pipe 700 is connected to second temperature-controlling chamber, and the 5th air inlet pipe 700 goes out
Gas end is for being inserted into second raw material.5th air inlet pipe 700 can be bubbled for second temperature-controlling chamber 400, favorably
In the evaporation for the second raw material for accelerating liquid.The present embodiment is only limitted to above-mentioned technical proposal, in other implementations, can also be with
It is that second temperature-controlling chamber is used to place the second raw material of solid state powder, is equipped in second temperature-controlling chamber and emits bubbler, described
Emitting bubbler includes cage body and the 6th air inlet pipe, and one end of the 6th air inlet pipe is connected to the 4th air inlet pipe, and the other end extend into described
In cage body, there is placing chamber inside the cage body, surface has the stomata of connection placing chamber, powdered the second raw material of solid
It is put into the placing chamber, carrier gas is passed into placing chamber by the 6th air inlet pipe, and is flowed out from the stomata, so
The vacuum chamber is flowed to by the second air supply pipe afterwards, is conducive to promote the speed that the second raw material generate steam.
Further, in the present embodiment, the chemical vapor depsotition equipment further includes plasma generator, described etc.
Plasma generator includes two high frequency terminals, and the two high frequency terminal one of them are connect with the gas distributor 110, separately
One is connect with the sample stage 200.Specifically, gas distributor 110 or sample stage 200 are designed as and vacuum chamber 100
Other parts insulation, in growth course, make to feed to vacuum chamber by gas distributor 110 by opening plasma generator
100 gas is decomposed, activation, is even ionized, thus significantly reduce two dimensional crystal material temperature needed for substrate surface growth,
Improve growth rate, uniformity and the repeatability of two dimensional crystal material.
Further, in the present embodiment, the chemical vapor depsotition equipment further includes lifting device, the lifting device
One end connect the sample stage 200, the other end connects the vacuum chamber 100.Specifically, in the present embodiment, the lifting dress
It sets using elevating lever, the elevating lever can be electric drive bar and be also possible to pneumatic driving lever, can also be by manually adjusting
Section.Since mixing of the gas in vacuum chamber 100 is by the flow of each process gas, the air pressure of vacuum chamber 100, gas distribution
The influence of the factors such as sectional area, spray orifice size, distribution and the gas flow direction of device 110, so that in vacuum chamber 100
Gas concentration there are certain difference, the elevating lever is for adjusting position of the sample stage 200 in vacuum chamber 100, for will
It is suitably local that sample platform is adjusted to gas concentration, is conducive to transition metal sulfur family two dimensional crystal Material growth.Due to the first original
The flow for the carrier gas that the heating temperature of material and the second raw material can control accurately, carry steam accurately controls, because
The process conditions of this two dimensional crystal material can be with fine adjustment, and the repeatability grown is also significantly improved.
Lifting device described in the present embodiment is not limited only to above-mentioned technical proposal, in other implementations, is also possible to the liter
Falling unit is lifting platform, and the sample stage is arranged on the lifting platform.
Further, in the present embodiment, the lifting device and the vacuum chamber 100 are rotatablely connected, the chemistry gas
Phase depositing device further includes actuator, and the actuator is connect with the lifting device, to drive the lifting device to rotate.Institute
Stating actuator includes first motor, and the first motor has driving wheel, and the lifting device is equipped with driven wheel, the driving wheel
It is engaged with driven wheel, so that the first motor drives the lifting device rotation.The lifting device rotation drives sample stage
200 rotations so that steam in vacuum chamber 100 deposited on sample stage 200 it is more uniform so that being prepared
Transition metal sulfur family two dimensional crystal material is more uniform.
Specifically, in the present embodiment, the elevating lever includes mobile jib and secondary bar, and the mobile jib is equipped with mounting hole, the peace
Hole is filled along the axially extending of the mobile jib, the secondary bar part is slidably arranged in the mounting hole, and the outer surface of the secondary bar is set
There is the rack gear axially extending along the mobile jib, the second motor is connected on the mobile jib, second motor has gear, described
Gear is engaged with the rack gear.The mobile jib and the outer surface are equipped with the driven wheel, the first motor and described true
Empty room 100 connects.The first motor drives the elevating lever rotation, lifter rod lifting described in second motor driven.
Chemical deposition device described in the present embodiment is not limited only to above-mentioned technical proposal, in other embodiments, can also be with
It is that the upper surface of the sample stage has circular installation region, the upper surface of the sample stage is equipped with multiple stomatas, Duo Gesuo
It states stomata to be arranged along the edge interval of installation region, the clockwise or inverse time of the outgassing direction of the stomata along the installation region
The inclination of needle direction, the stomata is for being connected to carrier gas source, to drive the substrate rotation on the sample stage.The carrier gas
Body sprays the air-flow to form a rotation from the stomata, and when substrate is placed on the installation region of platform, substrate covers institute
Installation region is stated, air-flow can hold up the substrate rotation, advantageously allow the first raw material and second of each position in substrate
The distribution of raw material is more uniform, is conducive to two dimensional crystal material growth.
Further, in the present embodiment, the sample stage 200 includes first heater.The first heater
Transition metal sulfur family two dimensional crystal material on specimen heating holder 200, so that transition metal sulfur family two dimensional crystal material has
There is good growth temperature, is conducive to the quality for promoting transition metal sulfur family two dimensional crystal material.
Further, in the present embodiment, the vacuum chamber 100 is equipped with the 4th heating device.4th heating device
It can be used for the gas and vacuum chamber 100 itself in hot donut 100, prevent steam from condensing in the inner wall of vacuum chamber 100
Adherency is conducive to the utilization rate for promoting raw material, while can also give the one good life of material of transition metal sulfur family two dimensional crystal
Long temperature is conducive to the quality for promoting transition metal sulfur family two dimensional crystal material.
Specifically, vacuum chamber 100 described in the present embodiment further includes pumped vacuum systems, and the pumped vacuum systems is for being true
Empty room 100 vacuumizes, and so as to back end vacuum needed for reaching transition metal sulfur family two dimensional crystal Material growth, can be used for will be true
Tail gas discharge in empty room 100.The pumped vacuum systems includes throttle valve, and operating air pressure can be all into vacuum chamber by adjusting
The opening degree of the flow of 100 gas and throttle valve is adjusted.The deposition of two dimensional crystal materials chemistry described in the present embodiment
Equipment can be set in draught cupboard or glove box, have the advantages that safety is good, be able to use with certain toxicity
One raw material, the second raw material prepare two dimensional crystal material.
The present invention also proposes that a kind of method for preparing two dimensional crystal material, the preparation method can choose using above-mentionedization
Vapor deposition apparatus is learned, as shown in Figure 2, comprising the following steps:
S1 is placed the substrate above in vacuum chamber, by the vacuum chamber to back end vacuum；
First raw material are carried out heating and generate steam by S2, are passed through in the vacuum chamber；
S3 carries out the second raw material plus thermogenetic steam is passed through in the vacuum chamber, or by gaseous second former material
Material is passed through the vacuum chamber；
Growth air pressure needed for the indoor pressure of vacuum is adjusted to the growth two dimensional crystal material by S4；
The substrate is heated to growth temperature needed for the two dimensional crystal material of growing up by S5, rotates the substrate, institute
It states the first raw material and second raw material passes through chemical reaction on the substrate and generate the two dimensional crystal material.
It should be noted that the sequence of above-mentioned steps is not fixed, according to the two dimensional crystal material of required preparation
The difference of material, or same two dimensional crystal material is prepared, but different technique is used, the sequence of the step is adjustable
, or even it is repeatedly inserted into a certain step between two steps.
Further, step S2 generates steam specifically, the first raw material are carried out heating, and mixed carrier gas is passed through institute
It states in vacuum chamber；In step S2, the flow of the carrier gas is 50sccm~100sccm；
Further, step S3 is specifically, the second raw material are carried out thermogenetic steam mixed carrier gas is added to be passed through
In the vacuum chamber, or gaseous second raw material are passed through the vacuum chamber；The flow of carrier gas described in step S3
Less than or equal to 50sccm.
Further, the two dimensional crystal material includes: transition metal sulfur family two dimensional crystal material MX2, III-VI race two
Crystalline material VX and hexagonal boron nitride are tieed up, wherein M is transition metal element, and X is chalcogen, and V is third major element.
Further, first raw material include: Dimethyldithiocarbamate molybdenum, bis- (tert-butylamine) bis- (dimethyl
Amine) tungsten, hexahydroxy molybdenum, hexahydroxy tungsten, tungsten hexachloride, trimethyl indium, indium trichloride, second raw material include: diformazan two
Sulphur, diethyl thioether, diethyl diselenide, hydrogen sulfide, hydrogen selenide, sulphur, selenium；Either,
First raw material include: boron triethyl, borazine, boron bromide, boron chloride, second raw material
It include: ammonium hydroxide, ammonium chloride.
Further, the two dimensional crystal material is MoS2, first raw material are Mo (CO)6, second raw material
(C2H5)2S。
Further, the heating temperature of the first raw material described in step S2 is 100 DEG C~120 DEG C.
Further, between step S1 and step S2 in further include that step S6 is passed through carrier gas into the vacuum chamber
The flow of step, the carrier gas is less than or equal to 100sccm.
Further, two dimensional crystal material growth air pressure described in step S4 is 5Torr~10Torr；
Further, the growth temperature of two dimensional crystal material described in step S5 is 500 DEG C~600 DEG C, the substrate
Velocity of rotation is less than or equal to 2000r/min；The thickness of the two dimensional crystal material is accurate from monoatomic layer to 20 atomic layers
Control.
Heating temperature of the technical solution of the present invention by the different transition metal sources of adjusting, the carrier gas of different transition metal sources
The flow of body and the flow of hydrogen, Enhancing Nucleation Density, grain size and the company of being formed of the two dimensional crystal material of adjustable generation
The time of continuous single layer two-dimensional film.The preparation method short time deposition can obtain discontinuous two-dimentional monocrystalline, long period
Growth can obtain continuous monoatomic layer two dimension polycrystal film, can obtain multilayer two-dimension crystal film for more time.Have
Homogeneous, the reproducible and accurate thickness control advantage of product.
Below in conjunction with specific embodiment, the preparation that the present invention will be described in detail the method for two dimensional crystal material specific reality
Apply mode:
Embodiment 1
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 10sccm, carrier gas is passed through into the vacuum chamber with 100sccm, institute
Stating carrier gas is argon gas；
By transition metal source Mo (CO)6It is put into the first temperature-controlling chamber, heating is carried out with 110 DEG C and generates steam, mix 60sccm
Argon gas be passed through in the vacuum chamber；
By sulfur family material (C2H5)2S is put into the second temperature-controlling chamber and carries out being heated to 50 DEG C, generates steam, mixes the argon of 50sccm
Gas is passed through in the vacuum chamber；
The indoor pressure of vacuum is adjusted to 50Torr；
The sample stage is heated to 600 DEG C, starts MoS2The growth of two dimensional crystal material.
Embodiment 2
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and be placed on sample stage using Si piece as substrate.Back end is evacuated to by safety regulation for operations again
Vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 20sccm, carrier gas is passed through into the vacuum chamber with 100sccm, institute
Stating carrier gas is argon gas；
By transition metal source Mo (CO)6It is put into the first temperature-controlling chamber, heating is carried out with 130 DEG C and generates steam, mix 50sccm
Argon gas be passed through in the vacuum chamber；
By sulfur family material (C2H5)2S is put into the second temperature-controlling chamber, carries out heating with 60 DEG C and generates steam, and passes through the 5th air inlet
Pipe to the second temperature-controlling chamber is passed through the argon gas of 5sccm to be bubbled, the argon for the 20sccm that argon gas carries steam and the 4th air inlet pipe is passed through
After gas further mixes, it is passed through in the vacuum chamber；
The indoor pressure of vacuum is adjusted to 100Torr；
The sample stage is heated to 620 DEG C, starts MoS2The growth of two dimensional crystal material.
Embodiment 3
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and be placed on sample stage using Si piece as substrate.Back end is evacuated to by safety regulation for operations again
Vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 5sccm, carrier gas, the load are passed through into institute's vacuum chamber with 30sccm
Body gas is argon gas；
By transition metal source Mo (CO)6It is put into the first temperature-controlling chamber, heating is carried out with 120 DEG C and generates steam, mix 10sccm
Argon gas be passed through in the vacuum chamber；
By sulfur family material (C2H5)2S is put into the second temperature-controlling chamber, carries out heating with 80 DEG C and generates steam, mixes the argon of 10sccm
Gas is passed through in the vacuum chamber；
The indoor pressure of vacuum is adjusted to 5Torr；
The sample stage is heated to 590 DEG C, starts MoS2The growth of two dimensional crystal material.
Embodiment 4
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
Hydrogen is passed through into the vacuum chamber with 5sccm；
By transition metal source Mo (CO)6It is put into the first temperature-controlling chamber, heating is carried out with 140 DEG C and generates steam, mix 10sccm
Argon gas be passed through in the vacuum chamber；
By sulfur family material (C2H5)2S is put into the second temperature-controlling chamber, carries out heating with 70 DEG C and generates steam, and passes through the 5th air inlet
Pipe to the second temperature-controlling chamber is passed through the argon gas of 5sccm to be bubbled, the argon for the 10sccm that argon gas carries steam and the 4th air inlet pipe is passed through
After gas further mixes, it is passed through in the vacuum chamber；
The indoor pressure of vacuum is adjusted to 0.5Torr；
The sample stage is heated to 610 DEG C, starts MoS2The growth of two dimensional crystal material.
After growth 1-24 hours, first transition metal source Mo (CO) is closed6Gas circuit and heating power supply；By the temperature of sample stage
It is increased to 750-950 DEG C, and is kept for 1-2 hours；It is then shut off sulfur family material (C2H5)2The gas circuit and heating power supply of S close sample
The heating power supply and rotating device of sample platform, to obtain higher-quality MoS2Two dimensional crystal material.
Embodiment 5
Safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Torr is then broken by safety regulation for operations
Except the vacuum of vacuum chamber, and by SiO2Piece is placed on sample stage as substrate.Back end is evacuated to by safety regulation for operations again
Vacuum 1 × 10-6Torr；
It is passed through hydrogen into institute's vacuum chamber with 8sccm, carrier gas, the carrier are passed through into institute's vacuum chamber with 80sccm
Gas is argon gas；
Selenium powder is put into the first temperature-controlling chamber, heating generates steam, and the argon gas for mixing 60sccm is passed through in the vacuum chamber；
Indium nitrate is put into the second temperature-controlling chamber and carries out heating generation steam, the argon gas for mixing 48sccm is passed through the vacuum chamber
It is interior；
The indoor pressure of vacuum is adjusted to 9Torr；
The sample stage is heated to the growth for starting indium selenide two dimensional crystal material.
Embodiment 6
Safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Torr is then broken by safety regulation for operations
Except the vacuum of vacuum chamber, and by SiO2Piece is placed on sample stage as substrate.Back end is evacuated to by safety regulation for operations again
Vacuum 1 × 10-6Torr；
It is passed through after the ammonia of 5-500sccm is mixed with the argon gas of 50-500sccm in the CVD chamber；
By the air pressure adjustment in CVD chamber to 0.1-50Torr；
The distance between sample stage and gas distributor are adjusted to 20-50mm, and pass through rotating device specimen rotating holder；
The sample stage is heated to 800-1200 DEG C；
By heating jacket by the source MO BH3NH3It is heated to 60-120 DEG C, heating is generated into BH3NH3Steam and 20-
It is passed through in the CVD chamber after the argon gas mixing of 100sccm；The gas circuit in the source MO is heated by heating tape simultaneously, heating temperature is not low
Set temperature in the source MO, but it is not higher by 10 DEG C；
It further adjusts and stablizes the pressure in CVD chamber to 0.1-50Torr；
After growth 1-24 hours, the source MO BH is closed3NH3Gas circuit, the heating power supply in the source MO and its gas circuit, sample stage plus
Thermoelectric generator and rotating device；Sample closes all gases for being passed through CVD chamber after being cooled to room temperature and CVD chamber is evacuated to back end
Vacuum；The vacuum of CVD chamber is abolished by safety regulation for operations, that is, can be taken off prepared h-BN two dimensional crystal material sample.
Embodiment 7
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
It is passed through hydrogen into institute's vacuum chamber with 8sccm, carrier gas, the carrier are passed through into institute's vacuum chamber with 80sccm
Gas is argon gas；
Dimethyldithiocarbamate molybdenum is put into the first temperature-controlling chamber, heating is carried out and generates steam, mix the argon gas of 60sccm
It is passed through in the vacuum chamber；
Hydrogen sulfide is connected to third air supply pipe, the argon gas for mixing 48sccm is passed through in the vacuum chamber；
The indoor pressure of vacuum is adjusted to 9Torr；
The sample stage is heated to 560 DEG C, obtains MoS2Two dimensional crystal material.
Embodiment 8
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 8sccm, carrier gas is passed through into the vacuum chamber with 80sccm, it is described
Carrier gas is argon gas；
Hexahydroxy tungsten will be crossed and be put into the first temperature-controlling chamber, heating is carried out and generate steam, mix 60sccm argon gas be passed through it is described
In vacuum chamber；
Methyl disulfide is put into the second temperature-controlling chamber and carries out heating generation steam, the argon gas for mixing 48sccm is passed through the vacuum
It is indoor；
The indoor pressure of vacuum is adjusted to 9Torr；
Growth temperature needed for the sample stage is heated to tungsten sulfide crystal starts the life of tungsten sulfide two dimensional crystal material
It is long.
Embodiment 9
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 8sccm, carrier gas is passed through into the vacuum chamber with 80sccm, it is described
Carrier gas is argon gas；
Tungsten hexachloride will be crossed and be put into the first temperature-controlling chamber, heating is carried out and generate steam, mix 60sccm argon gas be passed through it is described
In vacuum chamber；
Diethyl thioether be put into the second temperature-controlling chamber carry out heating and generate steam, mix 48sccm argon gas be passed through it is described true
In empty room；
The indoor pressure of vacuum is adjusted to 9Torr；
Growth temperature needed for the sample stage is heated to tungsten sulfide crystal obtains tungsten sulfide two dimensional crystal material.
Embodiment 10
The present embodiment uses trimethyl indium ((CH3)3In, solid) and H2Se prepares indium selenide two dimensional crystal material.Due to
H2Se has toxicity, this equipment is mounted in a closed glove box, and tail gas carries out innoxious place by tail gas treating unit
Reason.
By safety regulation for operations, CVD chamber is evacuated to back end vacuum 5 × 10-7Torr is then broken by safety regulation for operations
It grown 300 Nano-meter SiO_2s except the vacuum of CVD chamber, and by surface heat22 inches of Silicon Wafers be placed on sample stage as substrate.
Back end vacuum 5 × 10 is evacuated to by safety regulation for operations again-7Torr；
The nitrogen of 50-500sccm is passed through in the CVD chamber；
By the air pressure adjustment in CVD chamber to 0.1-100Torr；
The distance between sample stage and gas distributor are adjusted to 20-50mm, and pass through rotating device specimen rotating holder；
The sample stage is heated to 400-700 DEG C；
By heating jacket by the source MO (CH3)3In is heated to 40-80 DEG C, and heating is generated BH3NH3Steam and 20-
It is passed through in the CVD chamber after the nitrogen mixing of 100sccm；The gas circuit in the source MO is heated by heating tape simultaneously, heating temperature is not low
Set temperature in the source MO, but it is not higher by 10 DEG C；
It simultaneously will be by the H of 50-500sccm2Se gas is passed through in the CVD chamber；
It further adjusts and stablizes the pressure in CVD chamber to 0.1-100Torr；
After growing a few houres a few minutes-, the source MO (CH is closed3)3The heating electricity of In and its heating power supply of gas circuit, sample stage
Source and rotating device close H2Se gas；Sample is cooled to after room temperature and closes nitrogen and that CVD chamber is evacuated to back end is true
It is empty；The vacuum of CVD chamber is abolished by safety regulation for operations, that is, can be taken off prepared InSe two dimensional crystal material sample.
Embodiment 11
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and by SiO2Piece is placed on sample stage as substrate.Back is evacuated to by safety regulation for operations again
Bottom vacuum 1 × 10-6Torr；
It is passed through hydrogen into the vacuum chamber with 8sccm, carrier gas is passed through into the vacuum chamber with 80sccm, it is described
Carrier gas is argon gas；
Any one in boron triethyl excessively, borazine, boron bromide is put into the first temperature-controlling chamber, carries out heating generation
Steam, the argon gas for mixing 60sccm are passed through in the vacuum chamber；
Ammonium chloride is put into the second temperature-controlling chamber and carries out heating generation steam, the argon gas for mixing 48sccm is passed through the vacuum chamber
It is interior；
The indoor pressure of vacuum is adjusted to 9Torr；
Growth temperature needed for the sample stage is heated to six square boron nitride crystals obtains boron nitride two dimensional crystal material
Material.
Embodiment 12
The present embodiment utilizes invented MOCVD device, using two kinds of sources MO: Mo (CO)6(C2H5)2S prepares MoS2
Two dimensional crystal material, carrier gas use argon gas, and using hydrogen as intermediate reaction gas.Secondary heating mechanism and third add
Hot charging is set to heating tape.
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, and surface heat be grown into 300 Nano-meter SiO_2s24 inches of Silicon Wafers be placed on sample stage as substrate
On.Back end vacuum 1 × 10 is evacuated to by safety regulation for operations again-6Torr；
It is passed through after the hydrogen of 5sccm~50sccm is mixed with the argon gas of 50~200sccm in the vacuum chamber；
By the indoor air pressure adjustment of vacuum to 0.5~100Torr；
The distance between sample stage and gas distributor are adjusted to 20~50mm, and rotating substrate；By the sample stage
It is heated to 500~650 DEG C；
By heating jacket by the source MO Mo (CO)660~150 DEG C are heated to, heating is generated into Mo (CO)6Steam and 20~
It is passed through in the vacuum chamber after the argon gas mixing of 100sccm；The source MO Mo (CO) is heated by heating tape simultaneously6Gas circuit, heating
Temperature is not less than the set temperature in the source MO, but is not higher by 10 DEG C；
The source MO (C is heated by heating jacket2H5)2S (source MO using emits bubbler design) to 40~80 DEG C, and pass through to
Described to emit the argon gas that 1~10sccm is passed through in bubbler, which carries (C2H5)2S steam further with the argon of 20~100sccm
It is passed through in the vacuum chamber after gas mixing.The source MO (C is heated by heating tape simultaneously2H5)2The gas circuit of S, heating temperature are not less than MO
The set temperature in source, but it is not higher by 10 DEG C；
It further adjusts and stablizes the indoor pressure of vacuum to 0.5~100Torr；
After growth 1~24 hour, first the source MO Mo (CO) is closed6Gas circuit and heating power supply；The temperature of sample stage is increased
To 750~950 DEG C, and kept for 1~2 hour；It is then shut off the source MO (C2H5)2The gas circuit and heating power supply of S close sample stage
Heating power supply and rotating device.Sample closes all gases for being passed through vacuum chamber after being cooled to room temperature；
By vacuum chamber to back end vacuum；By the vacuum of safety regulation for operations breaking vacuum room, that is, can be taken off made
Standby MoS2Two dimensional crystal material sample.
Embodiment 13
Using the single source MO BH3NH3(solid) prepares h-BN two dimensional crystal material, and carrier gas uses argon gas, and utilize
Ammonia is as intermediate reaction gas.Secondary heating mechanism and third heating device are heating tape.
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, the copper foil for using surface to do electrochemical polish are placed on sample stage as substrate.Again by safety behaviour
Back end vacuum 1 × 10 is evacuated to as regulation-6Torr；
It is passed through after the ammonia of 5~500sccm is mixed with the argon gas of 50~500sccm in the vacuum chamber；
By the indoor air pressure adjustment of vacuum to 0.1~50Torr；
The distance between sample stage and gas distributor are adjusted to 20~50mm, rotate sample；The sample stage is added
Heat is to 800 DEG C~1200 DEG C；
By heating jacket by the source MO BH3NH360 DEG C~120 DEG C are heated to, heating is generated into BH3NH3Steam and 20~
It is passed through in the vacuum chamber after the argon gas mixing of 100sccm；The gas circuit in the source MO is heated by heating tape simultaneously, heating temperature is not low
Set temperature in the source MO, but it is not higher by 10 DEG C；
It further adjusts and stablizes the indoor pressure of vacuum to 0.1~50Torr；
After growth 1~24 hour；Sample closes all gases for being passed through vacuum chamber after being cooled to room temperature and takes out vacuum chamber
Vacuum is to back end vacuum；By the vacuum of safety regulation for operations breaking vacuum room, that is, it can be taken off prepared h-BN two dimensional crystal material
Expect sample.
Embodiment 14
Using the single source MO boron triethyl [(C2H5)3B, liquid] h-BN two dimensional crystal material is prepared, carrier gas makes
With argon gas, and using ammonia as reaction gas.5th air inlet pipe leads to carrier gas.Secondary heating mechanism and third heating device
For heating tape.
By safety regulation for operations, by vacuum chamber to back end vacuum 1 × 10-6Then Torr presses safety regulation for operations
The vacuum of breaking vacuum room, the copper foil for using surface to do electrochemical polish are placed on sample stage as substrate.Again by safety behaviour
Back end vacuum 1 × 10 is evacuated to as regulation-6Torr；
The ammonia of 5~500sccm is passed through in the vacuum chamber；
By the indoor air pressure adjustment of vacuum to 10~50Torr；
The distance between sample stage and gas distributor are adjusted to 20~50mm, rotate sample；The sample stage is added
Heat is to 800~1200 DEG C；
By heating jacket by the source MO (C2H5)3B is heated to 30~60 DEG C, and heating is generated BH3NH3Steam and 20~
It is passed through in the vacuum chamber after the argon gas mixing of 100sccm；The source MO (C is heated by heating tape simultaneously2H5)3The gas circuit of B, heating
Temperature is not less than the set temperature in the source MO, but is not higher by 10 DEG C；
It further adjusts and stablizes the indoor pressure of vacuum to 10~50Torr；
The plasma generator of unlatching MOCVD device, the generation plasma between gas distributor and sample stage,
Start the growth of two dimensional crystal material.
After time within growth 3 minutes to 4 hours, the power supply of plasma generator is first closed, the source MO is then shut off
(C2H5)3B and its heating power supply of gas circuit, the heating power supply of sample stage and actuator or carrier gas source；When sample stage is cooled to
All gases for being passed through vacuum chamber are closed after room temperature and by vacuum chamber to back end vacuum；It is abolished very by safety regulation for operations
The vacuum of empty room can be taken off prepared h-BN two dimensional crystal material sample.
MoS prepared by embodiment 122Two dimensional crystal material carries out Raman spectrum test, as a result as shown in Figure 3.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
It is included in other related technical areas in scope of patent protection of the invention.
Claims (10)
1. a kind of chemical vapor depsotition equipment for preparing two dimensional crystal material characterized by comprising
Vacuum chamber；
Sample stage, the sample stage are arranged in the vacuum chamber, are provided with first heater in the sample stage；Gas point
Orchestration, the gas distributor are arranged in the vacuum chamber；
First temperature-controlling chamber, for placing the first raw material, and for heating first raw material to generate the first raw material
Steam；
First air inlet pipe is connected to first temperature-controlling chamber and the gas distributor；
Second temperature-controlling chamber for placing the second raw material of solid-state or liquid, and heats for second raw material to generate the
The steam of two raw material；
Second air inlet pipe is connected to second temperature-controlling chamber and the gas distributor；
Third air inlet pipe, one end are used to be connected to the gas source of second raw material, and the other end is connected to the gas distributor；
Three the 4th air inlet pipe, the 4th air inlet pipe be used for the gas distributor lead to carrier gas, three the described 4th
Air inlet pipe is respectively communicated with first air inlet pipe, second air inlet pipe and the third air inlet pipe.
2. chemical vapor depsotition equipment as described in claim 1, which is characterized in that first air inlet pipe and described second into
Secondary heating mechanism and third heating device, the secondary heating mechanism and third heating dress are respectively equipped on the outside of tracheae
It sets and is respectively used to heat the entirety of first air inlet pipe and the entirety of second air inlet pipe.
3. chemical vapor depsotition equipment as described in claim 1, which is characterized in that second temperature-controlling chamber is for placing liquid
Second raw material, the chemical vapor depsotition equipment include the 5th air inlet pipe, the inlet end of the 5th air inlet pipe and the 4th into
Tracheae connection, the outlet side of the 5th air inlet pipe are connected to second temperature-controlling chamber, and the outlet side of the 5th air inlet pipe is used
In insertion second raw material；Either,
Second temperature-controlling chamber is used to place the second raw material of solid state powder, is equipped in second temperature-controlling chamber and emits bubbler.
4. chemical vapor depsotition equipment as described in claim 1, which is characterized in that the chemical vapor depsotition equipment also wraps
It includes:
Lifting device, one end of the lifting device connect the sample stage, and the other end connects the vacuum chamber, the lifting dress
It sets for adjusting the distance between the sample stage and the gas distributor；
Actuator, the lifting device and the vacuum chamber are rotatablely connected, and the actuator is connect with the lifting device, to drive
Move the lifting device rotation；Alternatively,
The upper surface of the sample stage has circular installation region, and the upper surface of the sample stage is equipped with multiple stomatas, multiple
The stomata is arranged along the edge interval of installation region, and the outgassing direction of the stomata is along the clockwise or inverse of the installation region
Clockwise inclination, the stomata is for being connected to carrier gas source, to drive the substrate rotation on the sample stage.
5. a kind of method for preparing two dimensional crystal material, which comprises the following steps:
It places the substrate above in vacuum chamber, by the vacuum chamber to back end vacuum；
First raw material are subjected to heating and generate steam, are passed through in the vacuum chamber；
Second raw material are carried out plus thermogenetic steam is passed through in the vacuum chamber, or gaseous second raw material are passed through
The vacuum chamber；
Growth air pressure needed for the indoor pressure of vacuum is adjusted to the growth two dimensional crystal material；
The substrate is heated to growth temperature needed for the two dimensional crystal material of growing up, rotates the substrate, described first
Raw material and second raw material pass through chemical reaction on the substrate and generate the two dimensional crystal material.
6. the method for preparing two dimensional crystal material as claimed in claim 5, which is characterized in that the two dimensional crystal material packet
It includes: transition metal sulfur family two dimensional crystal material MX2, III-VI race two dimensional crystal material VX and hexagonal boron nitride, wherein M be
Metallic element is crossed, X is chalcogen, and V is third major element.
7. the method for preparing two dimensional crystal material as claimed in claim 6, which is characterized in that first raw material include:
Dimethyldithiocarbamate molybdenum, bis- (tert-butylamines) bis- (dimethyl amine) tungsten, hexahydroxy molybdenum, hexahydroxy tungsten, tungsten hexachloride, front three
Base indium, indium trichloride, second raw material include: methyl disulfide, diethyl thioether, diethyl diselenide, hydrogen sulfide, selenizing
Hydrogen, sulphur, selenium；Either,
First raw material include: boron triethyl, borazine, boron bromide, boron chloride, the second raw material packet
It includes: ammonium hydroxide, ammonium chloride.
8. the method for preparing two dimensional crystal material as claimed in claim 6, which is characterized in that the two dimensional crystal material is
MoS2, first raw material are Mo (CO)6, the second raw material (C2H5)2S。
9. the method for preparing two dimensional crystal material as claimed in claim 8, which is characterized in that the heating of first raw material
Temperature is 100 DEG C~120 DEG C；
Steam is generated the first raw material are carried out heating, is passed through before the step in the vacuum chamber, further comprises the steps of: to institute
The step of carrier gas is passed through in vacuum chamber is stated, the flow of the carrier gas is less than or equal to 100sccm.
10. the method for preparing two dimensional crystal material as claimed in claim 8, which is characterized in that
The two dimensional crystal material growth air pressure is 5Torr~10Torr；
The growth temperature of the two dimensional crystal material is 500 DEG C~600 DEG C, and the velocity of rotation of the substrate is less than or equal to
2000r/min；
The two dimensional crystal material with a thickness of 1~20 atomic layer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111893456A (en) * | 2020-07-09 | 2020-11-06 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional transition metal chalcogenide compound and preparation method and device thereof |
| CN115094400A (en) * | 2022-06-28 | 2022-09-23 | 瑞砻科技股份有限公司 | Two-dimensional semiconductor material chemical vapor deposition method and device |
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| US20160314968A1 (en) * | 2015-04-22 | 2016-10-27 | Samsung Electronics Co., Ltd. | Composition for layered transition metal chalcogenide compound layer and method of forming layered transition metal chalcogenide compound layer |
| CN110129881A (en) * | 2019-05-06 | 2019-08-16 | 杭州弘晟智能科技有限公司 | A kind of air bearing pedestal for wafer rotation |
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| JPH05102422A (en) * | 1991-10-07 | 1993-04-23 | Matsushita Electric Ind Co Ltd | Formation of tantalum oxide thin film |
| JP2000277436A (en) * | 1999-03-24 | 2000-10-06 | Japan Science & Technology Corp | Manufacture of nitride semiconductor |
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