CN108584888A - A kind of telluride vanadium two-dimensional material and its synthetic method and application - Google Patents
A kind of telluride vanadium two-dimensional material and its synthetic method and application Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 72
- 229910052720 vanadium Inorganic materials 0.000 title abstract description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title abstract description 5
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000010189 synthetic method Methods 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 53
- 239000002994 raw material Substances 0.000 claims abstract description 46
- 238000002360 preparation method Methods 0.000 claims abstract description 38
- 239000012159 carrier gas Substances 0.000 claims abstract description 37
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 claims abstract description 36
- 238000000151 deposition Methods 0.000 claims abstract description 33
- 230000004907 flux Effects 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 13
- 230000005611 electricity Effects 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 29
- 230000008021 deposition Effects 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000003708 ampul Substances 0.000 claims description 14
- 229910052573 porcelain Inorganic materials 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 14
- 238000011144 upstream manufacturing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 9
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- 230000009182 swimming Effects 0.000 claims 1
- 229910052681 coesite Inorganic materials 0.000 description 23
- 229910052906 cristobalite Inorganic materials 0.000 description 23
- 239000000377 silicon dioxide Substances 0.000 description 23
- 229910052682 stishovite Inorganic materials 0.000 description 23
- 229910052905 tridymite Inorganic materials 0.000 description 23
- 238000010586 diagram Methods 0.000 description 21
- 238000000034 method Methods 0.000 description 20
- 230000003287 optical effect Effects 0.000 description 20
- 230000005291 magnetic effect Effects 0.000 description 15
- 238000004062 sedimentation Methods 0.000 description 15
- 238000011160 research Methods 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 241000209094 Oryza Species 0.000 description 8
- 235000007164 Oryza sativa Nutrition 0.000 description 8
- 235000009566 rice Nutrition 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 230000005669 field effect Effects 0.000 description 7
- 239000010931 gold Substances 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 6
- 241000736199 Paeonia Species 0.000 description 5
- 235000006484 Paeonia officinalis Nutrition 0.000 description 5
- 241001104043 Syringa Species 0.000 description 5
- 235000004338 Syringa vulgaris Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 3
- 239000008246 gaseous mixture Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 2
- 150000004770 chalcogenides Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 150000004772 tellurides Chemical class 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKIIEJOIXGHUKX-UHFFFAOYSA-L Cadmium iodide Inorganic materials [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 229910003090 WSe2 Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- -1 chalcogenide compound Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000039 congener Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001511 metal iodide Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 150000004771 selenides Chemical class 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Chemical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to two-dimensional material preparation fields, and in particular to a kind of preparation method of telluride vanadium two-dimensional material, by Te and VCl3The heated volatilization of mixed raw material, and in the carrier gas flux of 40 80sccm, under 580 620 DEG C of depositing temperature, grow to form VTe in substrate surface2Two-dimensional material；The carrier gas is protection gas.In addition.The invention also includes using VTe made from the preparation method2Two-dimensional material and the application being applied in electricity device.In the present invention; in the material variety and the raw material being pre-mixed, the depositing temperature (present invention is also referred to as growth temperature) and under protecting the carrier gas of gas and the collaboration of carrier gas flux, it is nano level nanometer sheet that can be made with good pattern, thickness.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of preparation of magnetic metal telluride vanadium two-dimensional material and its
Application in electricity device, magnetics.
Technical background
Graphene1Discovery caused research boom of the scientific circles to two-dimensional layer material, currently, two-dimensional material family
Member grow stronger day by day, including hexagonal boron nitride (BN), metal iodide (such as：CdI2And BiI3) 2-3And two-dimentional transition gold
Belong to two chalcogenides (2D-TMDs) (such as：MoS2, MoSe2, WS2And WSe2)4-6.Since 2D-TMDs has excellent object
Physicochemical property so that they have in fields such as electricity, photoelectricity, paddy electronics, spintronics and catalysis widely answers
With.As 2D-TMDsA member, metal chalcogenide compound (MTMDCs) have because of its special one zero band gap of electronic structure
Many unique properties, including magnetism, electron density wave, superconductivity etc.7-10。
However, current research largely all concentrates on 2D metal chalcogenides and selenides, about 2D metal tellurides
Basic research it is also fewer11,12。VTe2As a kind of typical tellurides material, also rested on mostly about its research
Theoretical calculation is based on block materials.For example, several layers of VTe of mechanical stripping2It is proved to be a kind of effective Electrocatalytic Activity for Hydrogen Evolution Reaction
Agent.Due to VTe2Metal ion is closed on to (V4+-V4+) between possess the coupling of very strong 3d orbital electron, based on Density functional
Theoretical calculation predicts single layer VTe2It is about 553K with room-temperature ferromagnetic and Curie temperature.Further, it is obtained by theoretical calculation
Go out single layer VTe2Magnetic moment consist of two parts, the magnetic moment of each vanadium atom is 0.986 μ B, and each Te atomic magnetic moments are
0.096μB。
Although magnetic metal VTe2With such unique property, but theory is based on more for their research at present
It calculates or bulk-shaped monocrystal, urgent need experimentally successfully prepares ultra-thin VTe2Two-dimensional material monocrystalline is to be carried out more to them
In-depth study provides platform.However, having no VTe in the prior art2The successful preparation case of two-dimensional material；And different elements,
Even if for the replacement of congeners, different outer shell electron distribution information, preparing the method for two-dimensional material, there is also very big differences
It is different, the two-dimensional material of Te systems cannot unambiguously be made simply by existing method.For example, VS2The synthesis master of nanometer sheet
If accurately controlling raw material VCl3Temperature (275 DEG C), otherwise temperature excessively high cannot be easy long thick, carrier gas is argon hydrogen gaseous mixture；
VSe2The synthesis VCl of nanometer sheet3Temperature be 500 DEG C, the substrate used be mica sheet, could be grown in mica sheet substrate it is thin,
Carrier gas is argon hydrogen gaseous mixture.One kind is badly in need of in this field can successfully prepare VTe2The method of two-dimensional material.
1 Novoselov, K.S.et al.Two-dimensional gas of massless Dirac fermions
In graphene.Nature 438,197-200 (2005)
2 Ai, R.et al.Growth of Single-Crystalline Cadmium Iodide Nanoplates,
CdI2/MoS2(WS2, WSe2) van der Waals Heterostructures, and Patterned Arrays.ACS
Nano 11,3413-3419 (2017)
3 Li, J.et al.Synthesis of 2D Layered BiI3Nanoplates, BiI3/WSe2van der
Waals Heterostructures and Their Electronic, Optoelectronic Properties.Small
13 (2017).
4 Liu, Z.et al.Strain and structure heterogeneity in MoS2atomic layers
5,5246 (2014) of grown by chemical vapour deposition.Nature communications
5 Shaw, J.C.et al.Chemical vapor deposition growth of monolayer MoSe2
Nanosheets.Nano Research7,511-517 (2014)
6 Zhao, W.et al.Evolution of electronic structure in atomically thin
sheets of WS2and WSe2.ACS nano 7,791-797(2012).
7 Cheng, R.et al.Few-layer molybdenum disulfide transistors and
circuits for high-speed flexible electronics.Nature communications 5(2014).
8 Wang, Q.H., Kalantar-Zadeh, K., Kis, A., Coleman, J.N.＆ Strano, M.S.
Electronics and optoelectronics of two-dimensional transition metal
Dichalcogenides. Nature nanotechnology 7,699-712 (2012)
9 Zeng, H., Dai, J., Yao, W., Xiao, D.＆ Cui, X.Valley polarization in MoS2
Monolayers by optical pumping.Nature nanotechnology 7,490-493 (2012)
10 Xu, X., Yao, W., Xiao, D.＆ Heinz, T.F.Spin and pseudospins in layered
Transition metal dichalcogenides.Nature Physics 10,343-350 (2014)
11 Zhang, E.et al.Tunable positive to negative magnetoresistance in
atomically thin WTe2.Nano 17 letters, 878-885 (2017)
12Zhou, J.et al.Large-Area and High-Quality 2D Transition Metal
Telluride.Advanced materials 29(2017).
Invention content
It is an object of the present invention to solve at present for VTe2Research depend on theoretical calculation or blocky single more
Brilliant problem provides a kind of by testing simple preparation VTe for the first time2(present invention is known as VTe to two-dimensional material2Two-dimensional material or
VTe2Nanometer sheet) method.
The second object of the present invention is to provide using VTe made from the preparation method2Two-dimensional material (the present invention
Also referred to as VTe2Nanometer sheet).
The third object of the present invention is to provide VTe made from the preparation method2The application of two-dimensional material, is answered
The research of the intrinsic magnetism of preparation and two-dimensional material for electricity device.
A kind of VTe2The preparation method of two-dimensional material, by Te and VCl3The heated volatilization of mixed raw material, and in 40-
The carrier gas flux of 80sccm, under 580-620 DEG C of depositing temperature, grow to form VTe in substrate surface2Two-dimensional material；It is described
Carrier gas be protection gas.
VTe is successfully made in the present invention for the first time2Two-dimensional material is a kind of exploration for the first time of uncharted field；In order to overcome tellurium powder
Activity it is relatively low, realize successfully prepare TaTe for the first time2Two-dimensional material, the present inventor carry out many explorations, summarize unsuccessfully pass through extensively
It tests, finally found that, VTe is successfully made2Two-dimensional material needs the type of Collaborative Control raw material, the dosing method of raw material, carrier gas class
The depositing temperature of material after type, carrier gas flux and volatilization is in the range.
In the present invention, in the material variety and the raw material being pre-mixed, the depositing temperature (present invention
Referred to as growth temperature) and protect under the carrier gas of gas and the collaboration of carrier gas flux, it is to receive that can be made with good pattern, thickness
The nanometer sheet of meter level.
The inventors discovered that preparing ultra-thin VTe2When nanometer sheet, under the growth temperature and carrier gas flux, have
Help improve VTe obtained2The pattern of nanometer sheet, the thickness for controlling nanometer sheet, the crystal property etc. for improving material.The present invention
People's research also found, be controlled in addition to required range except by carrier gas flux, depositing temperature, the ratio of further regulation and control raw material,
The parameters such as volatilization temperature, the sedimentation time of raw material can further promote VTe2The preparation effect of two-dimensional material, for example, further
The thickness of two-dimensional material is reduced, the pattern of two-dimensional material obtained is improved.
In the present invention, in advance by Te and VCl3Mixing, then the mixed raw material is heated into volatilization, carries out CVD systems
It is standby.Different from other such as VS2, VSe2The synthesis of two-dimensional material, the present inventor is the study found that VTe2Raw material needs when nanometer sheet synthesizes
It is placed on after being sufficiently mixed in same porcelain boat, so contributes to that VTe is successfully made2Two-dimensional material, by Te and VCl3Separately do
Two porcelain boats are placed, and raw material reaction is insufficient, does not react even.
The present inventor also found by numerous studies, by VCl3, Te powder control in the mass ratio, contribute into one
The performance for successfully preparing and being promoted two-dimensional material obtained is walked,
Preferably, Te powder, VCl3Mass ratio be 1: 1~3: 1；Under the mass ratio, help to be made functional
Two-dimensional material.The study found that raw material (Te：VCl3) for mass ratio more than 3: 1, obtained nanometer sheet is imperfect, has part to be carved
Erosion；Raw material (Te：VCl3) mass ratio is less than 1: 1, it cannot get spawn in silicon chip substrate.
Further preferably, Te powder, VCl3Mass ratio be 2.5~3: 1；Most preferably 3: 1.
In the present invention, controlling the heating volatilization temperature of raw material helps successfully to prepare VTe2Two-dimensional material.In the present invention,
Volatilization temperature can pass through the set temperature of each warm area of control, the heating volatilization temperature of control material.
Preferably, the temperature of the heating volatilization of mixed raw material is 580-620 DEG C.Further preferably 600-620 DEG C.
In the preferred range, help that VTe is further successfully made2Two-dimensional material；In addition, additionally aiding what improvement obtained
The performance of two-dimensional material, for example, contribute to hexagon, the triangle of further rule, sample surfaces are smooth and thinner thickness
Two-dimensional material.
In the present invention, the carrier gas is protection gas, and the protection gas is, for example, inert gas, further preferably
Ar.The present inventor is the study found that the protection gas/atmosphere of hydrogen recognized using this field, VCl3React insufficient with Te powder,
Obtained reaction product size is obviously less than normal.
The study found that flow is higher than the preferred range limit of institute, the nanometer sheet density deposited in substrate is big and size very
It is small or do not deposit nanometer sheet substantially；Flow is less than the preferred flux lower limit, and obtained nanometer sheet surface irregularity has
Fold.
Preferably, the flow of carrier gas is preferably 60-80sccm.
In the present invention, the raw material of volatilization under the carrying of carrier gas, reacts, and be deposited under suitable depositing temperature
Substrate surface.Suitable depositing temperature helps successfully to prepare VTe2Two-dimensional material additionally aids improvement and prepares effect.
Research also found that growth temperature is excessively high (for example, higher than upper limit of range of the presently claimed invention), obtained portion
Divide VTe2At an angle and thickness reaches micron level with silicon chip substrate；Less than the preferable temperature lower limit, between raw material
Fundamental reaction is insufficient, and that obtain is not pure VTe2Nanometer sheet.
Preferably, depositing temperature is 590-620 DEG C；Still more preferably it is 590~610 DEG C；Most preferably 600~
610℃。
The present inventor the study found that mixed raw material volatilization temperature and reaction deposition temperature range relatively, precisely
The temperature of both regulation and control helps successfully to prepare VTe2Two-dimensional material；The study found that using having to mixed raw material and substrate point
The dual temperature area CVD consersion units of other temperature control contribute to accurate temperature control, contribute to VTe2The successful preparation of two-dimensional material.Research is also sent out
It is existing, mixed raw material and substrate are placed on same warm area, such as the porcelain boat equipped with the two is disposed adjacently (for example, the two
Distance be less than 6cm) in same warm area, be unfavorable for that VTe is successfully made instead2Two-dimensional material.
Preferably, mixed raw material is 21~24cm at a distance from substrate；Preferably 23cm.
Method of the present invention, wherein the precipitation equipment for implementing the preparation method includes the quartz ampoule of sealing, institute
Entrance of one end setting for the quartz ampoule stated for inputting carrier gas into quartz ampoule chamber, the other end are provided with for exporting stone
The outlet of English pipe gas to chamber；According to carrier gas stream direction, the chamber of the quartz ampoule is divided into upstream flat-temperature zone and downstream
Flat-temperature zone；Above-mentioned upstream flat-temperature zone and downstream flat-temperature zone is both provided with heating device, and Te powder and VCl are housed3Porcelain boat place
In upstream flat-temperature zone, downstream flat-temperature zone is arranged in the porcelain boat equipped with substrate.
The present inventor is successfully to prepare VTe the study found that be precisely controlled mixed raw material and the temperature of depositing temperature2Two
Tie up the key of material.In actual fabrication process, mixed raw material and depositing temperature are contributed to using precipitation equipment of the present invention
Control accurate, help that VTe is successfully made2Two-dimensional material.The present invention attempts single temperature zone equipment early stage and prepares, but does not have
Successfully obtain VTe2Nanometer sheet, obtained product are mostly the compound containing V and Cl.
Precipitation equipment of the present invention, the region close to carrier gas inlet side is upstream flat-temperature zone, from upstream flat-temperature zone
The raw material that gasification is added extremely is located in the transport of carrier gas close to the downstream flat-temperature zone of gas vent, and in the region suitable
It is grown in substrate surface under depositing temperature.
Preferably, the distance of two warm areas is 21~24cm；Preferably 23cm.
The study found that mixed raw material be arranged in upstream flat-temperature zone, if by substrate setting upstream and downstream flat-temperature zone it
Between, reaction is not thorough, and obtained product has part to contain V, tri- kinds of elements of Te, Cl；Substrate is arranged in downstream flat-temperature zone, and
Accurate temperature control is carried out by upstream and downstream flat-temperature zone, obtained product reaction is fully and regular shape, crystallinity are high.
In the present invention, by the selection of the substrate in vapor deposition, preparation method of the present invention can be used in difference
VTe is prepared in substrate2Nanometer sheet material, to obtain that the material of different use demands can be met.
Preferably, the substrate is Si/SiO2Substrate, sapphire substrates or mica substrate；Further preferably
Si/285nm SiO2Substrate.
In the present invention, VTe is prepared2During nanometer sheet, under the preferred growth temperature and carrier gas flux,
It is 5-30min that growth time is kept the temperature under the depositing temperature；Preferably 5-25min；Further preferably 10-20min；More
Further preferably 10-15min.
A kind of preferred VTe of the present invention2The preparation method of two-dimensional material, by Te powder and VCl3With 1: 1~3: 1 mass ratio
It is blended under 580-620 DEG C of temperature, the carrier gas flux of 40-80sccm (Ar) by chemical vapour deposition technique, in Si/285nm
SiO2Substrate surface constant temperature deposits 10-20min, and VTe is prepared2Nanometer sheet.
One kind of the invention more preferably prepares ultra-thin VTe2The method of nanometer sheet, preferred raw material (Te：VCl3) quality
Than being 1: 1~3: 1；Preferred growth temperature is 600-620 DEG C；Preferred carrier gas flux is 60-80 sccm (Ar)；It is excellent at this
Under the growth temperature of choosing and the collaboration of carrier gas flux, good topography uniformity, good crystallinity and thickness can be made and can be controlled in and receive
The VTe of meter level2, nanometer sheet.
Preparation VTe still more preferably2The method of nanometer sheet, raw material (Te：VCl3) mass ratio be 3: 1, growth temperature
It is 600-610 DEG C；Carrier gas flux is by chemical vapor deposition under 60-80sccm (Ar) flow rate of carrier gas in Si/285nm SiO2
Substrate surface constant temperature deposits 10-20min, to form VTe in substrate surface2Nanometer sheet.
The present invention also provides using VTe made from the preparation method2The thickness of nanometer sheet is 8-360 nm, size
It is 2-30 μm.Pattern is mostly regular hexagonal or triangle, and better crystallinity degree, is monocrystalline and quality is high.
Preferably, VTe2The thickness of nanometer sheet is 8-100nm, and size is 2-10 μm.
Further preferably, VTe2The thickness of nanometer sheet is 8-30nm, and size is 3-10 μm.
Most preferably, the thickness of VTe2 nanometer sheets is 8-15nm, and size is 3-10 μm.
VTe has successfully been prepared with chemical vapour deposition technique for the first time in the present invention2Nanometer sheet, thickness is up to 8nm, originally
Invent the VTe prepared2Nanometer sheet is to probe into their properties special on two-dimentional scale to provide the foundation, and grind for theory
The reliability studied carefully provides proof.And the method for the present invention is easy to operate, the nanometer sheet thickness being prepared is controllable, regular shape,
It is high quality single crystal.
The invention also includes a kind of VTe obtained2The application of two-dimensional material, is applied to electricity device
In preparation and magnetic research.
Preferably, by the VTe obtained by the present invention2Nanometer sheet is used to prepare VTe2Field-effect transistor.
Preferably, the VTe2The preparation method of field-effect transistor is：In the VTe that CVD method is prepared2Nanometer
On piece obtains VTe with electron beam exposure deposited metal2Field-effect transistor.This method operating process is simple, reproducible.
Preferably, by vacuum coating equipment in VTe2Deposited metal in two-dimensional material；
Preferably, the metal is Ti and/or Au.
Preferably, the thickness of the metal Ti is 5nm, and the thickness of Au is 100nm.
Preferably, by the VTe obtained by the present invention2Nanometer sheet is used for VTe2Magnetic property is studied.
Preferably, the magnetic required VTe of the measurement2The preparation method of nanometer sheet is：By Te powder and VCl3With 3: 1
Mass ratio be blended under 610 DEG C of temperature, the carrier gas flux of 50sccm (Ar) through chemical vapour deposition technique, constant temperature
30min, in Si/285nm SiO2VTe is prepared in substrate surface2Nanometer sheet.
By the method for the invention, VTe made from the method for the present invention is found2Two-dimensional material has room-temperature ferromagnetic and metal
Property.
Advantageous effect
The present invention under the collaboration of preferred growth temperature and carrier gas flux, can be made by aumospheric pressure cvd
Pattern is uniform, thickness is controllable, the VTe of good crystallinity2Nanometer sheet.
VTe prepared by the present invention2Nanometer sheet thickness is up to 8nm, and size is at 2-30 μm, and pattern is good, rule hexagon
Or triangle, better crystallinity degree, quality are high.VTe can be prepared with this method2Field-effect transistor.What the present invention was prepared
Ultra-thin VTe2Nanometer sheet is that they provide the foundation in the electricity of two-dimentional scale, magnetic research, and are expected to be applied to spin electricity
Son is learned, the fields such as nano electron device.
Use without complex operations step and expensive raw material in preparation process of the present invention, equipment is simple, and operates letter
Single easy, favorable reproducibility.
The present invention has obtained monocrystalline VTe of the thickness up to 8nm by simple aumospheric pressure cvd method2Nanometer
Piece, size are monocrystalline at 2-30 μm, and quality is high, and thickness is controllable, favorable reproducibility, the preparation method simple possible, is other
The preparation of two-dimensional gold attribute material provides reference.Also, the ultra-thin VTe that the present invention is prepared2Nanometer sheet is nanoelectronic
It learns, the research of the magnetic fields of two-dimentional scale provides new possibility.
Description of the drawings
Fig. 1 prepares VTe2The aumospheric pressure cvd schematic device of nanometer sheet；
Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8 are respectively embodiment 1, embodiment 2, embodiment 3, embodiment 4, reality
Apply example 5, embodiment 6, VTe made from embodiment 72The optical schematic diagram of nanometer sheet；
Fig. 9, Figure 10, Figure 11, Figure 12, Figure 13, Figure 14, Figure 15, Figure 16, Figure 17 are respectively to compare case 1, compare case
2, case 3 is compared, case 4 is compared, compares case 5, compares case 6, compares case 7, compares case 8, is prepared by comparison case 9
Obtained VTe2The optical schematic diagram of nanometer sheet；
Figure 18 is VTe prepared by case study on implementation 82Field-effect transistor；
Figure 19 is VTe in case study on implementation 82The electricity of field-effect transistor exports and transfer characteristic curve.
Figure 20 is VTe needed for the Magnetic Test of the preparation of case study on implementation 92Optical schematic diagram；
Figure 21 is VTe prepared by case study on implementation 92The relevant magnetization curve in magnetic field and the relevant null field of temperature of nanometer sheet
Cooling magnetization curve.
Figure 22 is VTe prepared by case study on implementation 12The Raman spectrum (a) of nanometer sheet, Raman image (b) and XRD spectrum
(c)。
Specific implementation method：
Below by case study on implementation, the present invention is further described, but present disclosure is not limited solely in following
Hold.
Prepare VTe2The vapor phase growing apparatus schematic diagram of nanometer sheet is shown in Fig. 1, including quartz ampoule 1, the quartz ampoule 1
Left side side cavity is that (left side flat-temperature zone is also referred to as upstream flat-temperature zone to high-temperature constant warm area 2/3；Right side flat-temperature zone is also referred to as downstream
Flat-temperature zone), it is mounted with Te and VCl3The porcelain boat 4 of raw material powder is placed on high-temperature constant warm area 2, and the device, which is additionally provided with, to be added
The heating device of the heat high-temperature constant warm area；The porcelain boat 5 for being mounted with substrate is placed on high-temperature constant warm area 3；
1 two end of quartz ampoule is both provided with stomata, wherein the stomata close to high-temperature constant warm area 2 is air admission hole, is leaned on
The stomata of nearly high-temperature constant warm area 3 is venthole.
In the present embodiment, unless specified or limited otherwise, the distance of flat-temperature zone 1 and 2 is 23cm.
Embodiment 1
VTe2The preparation of nanometer sheet：
Te powder and VCl that mass ratio is 3: 1 will be filled3The porcelain boat of powder is placed on the flat-temperature zone 2 of tube furnace, a piece of Si/
285nm SiO2As VTe2Growth substrate it is bright be placed on up be placed on another porcelain boat the flat-temperature zone 3 of tube furnace with
Obtain crystal growth temperature appropriate.Before heating, the air in quartz ampoule is discharged with the argon gas of larger flow.Then make
It heats and is increased to 600 DEG C of (growth temperatures in flat-temperature zone 2,3；Mixed raw material and the depositing temperature in substrate are 600
DEG C), and argon flow amount is 70sccm, constant temperature 10min just has monocrystalline VTe on silicon chip2Nanometer sheet generates.VTe2Nanometer
The Experimental equipment of piece is as shown in Figure 1, the VTe prepared2The optical photograph of nanometer sheet is as shown in Figure 2.
Fig. 2 is the VTe prepared2The optical schematic diagram of nanometer sheet, Si/SiO2Substrate is light red, white, pale red, dark red
Hexagon/triangle represent the VTe of different-thickness2(by thick to thin), the VTe obtained under this condition2Nanometer sheet crystallinity
Good, thickness 8-100nm, size is 2-10 μm.Scale in Fig. 2 is 10 μm.
Figure 22 distinguishes VTe prepared by case study on implementation 12The Raman spectrum (a) of nanometer sheet, Raman image (b) and XRD light
It composes (c).Wherein Raman spectrum (a) is respectively A there are two very strong spike1gAnd E2gVibration mode, it was demonstrated that system of the present invention
Standby VTe2Sample quality is high, better crystallinity degree.Entire VTe2The color contrast of nanometer sheet Raman image (b) is consistent, shows sample
Product surface is highly uniform.XRD spectrum (c) display there are four main crystal face diffraction maximum (001), (002), (003), (004),
Spacing between adjacent two crystal face is almost the same, and half-peak breadth is very narrow, diffraction peak intensity is high, prepared by this surface present invention
VTe2For monocrystalline, quality is high, and crystallinity is very good.
Embodiment 2
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 80sccm, sedimentation time 10min.Fig. 3 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is lilac, and the hexagon of darkviolet, purple and white represents different-thickness
VTe2(by thin to thickness).Scale in Fig. 3 is 10 μm；VTe made from the present embodiment2Nanometer sheet good crystallinity, thickness 8-
50nm, size are 3-15 μm.
Embodiment 3
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 1: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 80sccm, sedimentation time 10min.Fig. 4 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is light red, and the hexagon of peony, red and white represents different thickness
VTe2(by thin to thickness).Scale in Fig. 4 is 10 μm, and that obtain under this condition is mostly thin VTe2Nanometer sheet, and good crystallinity.
VTe made from the present embodiment2Nanometer sheet good crystallinity, thickness 8-15nm, size are 3-8 μm.
Embodiment 4
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 40sccm, sedimentation time 10min.Fig. 5 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is light red, and the hexagon of peony, red and white represents different thickness
VTe2(by thin to thickness).Scale in Fig. 5 is 10 μm, the VTe obtained under this condition2Nanometer sheet density is small, and size is more than 10 μm,
It is suitble to do electricity device.VTe made from the present embodiment2Nanometer sheet good crystallinity, thickness 9-30nm, size are 10-15 μm.
Embodiment 5
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 580 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 60sccm, sedimentation time 10min.Fig. 6 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is light red, and peony, the triangle of red and white, hexagon represent
Different thick VTe2(by thin to thickness).Scale in Fig. 6 is 10 μm, under this condition mostly thin VTe2Nanometer sheet and shape rule
Then, good crystallinity, thickness 8-30nm, size are 3-10 μm.
Embodiment 6
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 620 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 70sccm, sedimentation time 10min.Fig. 7 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is peony, and the hexagon of pink and white is VTe2.Scale in Fig. 7
It is 10 μm, the VTe obtained under this condition2Nanometer sheet thickness is uniform, regular shape, good crystallinity, thickness 10-15nm, size
It is 6-10 μm.
Embodiment 7
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, source temperature 610, growth temperature
For 600 DEG C (temperature of volatility of raw material and deposition is 600 DEG C), flow 60sccm, sedimentation time 10min.Fig. 8 is
The VTe of preparation2The optical schematic diagram of nanometer sheet, Si/SiO2Substrate is peony, and the hexagon of pink and white is
VTe2.Scale in Fig. 8 is 10 μm, and that obtain under this condition is thin VTe2Nanometer sheet, regular shape, density is smaller, thick
Degree is 8-15nm, and size is 5-10 μm.
Compare case 1
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 100sccm, sedimentation time 10min.Fig. 9 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is lilac, and darkviolet and white small triangle are relatively thin VTe2；This is right
VTe made from ratio2Nanometer sheet is mostly triangle, and density is larger, and size is small (being not suitable for doing electricity device), thickness 8-
60nm, size are 1-3 μm.Scale in Fig. 9 is 10 μm.
Compare case 2
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 30sccm, sedimentation time 10min.Figure 10 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is light red, and red and white triangle/hexagon is VTe2Nanometer sheet obtains
The product quality arrived is not high, surface irregularity, and there are many folds.Scale in Figure 10 is 10 μm.
Compare case 3
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 650 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 70sccm, sedimentation time 10min.Figure 11 is the VTe prepared2It receives
The optical schematic diagram of rice piece, Si/SiO2Substrate is purple, and the hexagon of white, grey and golden yellow is VTe2.Present case obtains
VTe2It is too thick, and the portion of product and silicon chip that deposit are angled.Scale in Figure 11 is 10 μm.
Compare case 4
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 570 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 70sccm, sedimentation time 10min.Figure 12 is to obtain under this condition
Optical schematic diagram, Si/SiO2Substrate is lilac, and colored hexagon is Te and VCl3The product not exclusively obtained is reacted, it should
The X-ray energy spectrogram of product shows that its ingredient contains Te, V and a small amount of Cl.Scale in Figure 12 is 10 μm.
Compare case 5
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 0.8: 1, and growth temperature is 600 DEG C (former
The temperature of material volatilization and deposition is 600 DEG C), flow 70sccm, sedimentation time is 10 min.Figure 13 is to obtain under this condition
The optical schematic diagram obtained, Si/SiO2Substrate is light red, there is no to obtain VTe2 nanometer sheets on silicon chip.Mark in Figure 13
Ruler is 10 μm.
Compare case 6
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 4: 1, and growth temperature is 600 DEG C of (raw materials
The temperature of volatilization and deposition is 600 DEG C), flow 70sccm, sedimentation time 10min.Figure 14 is to obtain under this condition
Optical schematic diagram, Si/SiO2Substrate is lilac, and red, white hexagon is VTe2Nanometer sheet has part nanometer sheet tight
It etches again, only a remaining part.Scale in Figure 14 is 10 μm.
Compare case 7
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality is than still for 3: 1 still by Te powder and VCl3It separates
It is placed on left side flat-temperature zone, growth temperature is 600 DEG C, flow 70sccm, sedimentation time 10min.Figure 15 is under this condition
The optical schematic diagram of acquisition, Si/SiO2Substrate is pink, and red, white hexagon is VTe2Nanometer sheet, it can be seen that work as original
When material is placed respectively, insufficient, obtained VTe is reacted2Nanometer sheet amount is considerably less.Scale in Figure 15 is 10 μm.
Compare case 8
This comparative example is inquired into, and H is adulterated in carrier gas2, specific as follows：
It is compared with embodiment 1, difference lies in Te and VCl3Powder quality ratio is 3: 1, and growth temperature is 600 DEG C, carrier gas
For Ar/H2Gaseous mixture, flow 80/5sccm, sedimentation time 10min.Figure 16 is the optical schematic diagram obtained under this condition,
Si/SiO2Substrate is light red, and red, white hexagon is VTe2Nanometer sheet, the VTe2 nanometer sheets obtained under this condition are not only close
Spend small, size is less than normal and in irregular shape.Scale in Figure 16 is 10 μm.
Compare case 9
Silicon chip substrate is placed into the central flat-temperature zone with single temperature zone tube furnace, Te and VCl3Powder is mixed with 3: 1 mass ratio
It closes and is uniformly positioned in the porcelain boat of substrate upstream (away from substrate 5cm), it is 600 DEG C that central warm area temperature, which is arranged, and carrier gas Ar throughputs are
80sccm, constant temperature time 10min.Figure 17 is the optical schematic diagram obtained under this condition, Si/SiO2Substrate is lilac, color
The hexagon of color is the compound of the unreacted element containing V and Cl.Scale in Figure 17 is 10 μm.
Embodiment 8
VTe2The preparation method of field-effect transistor, in the VTe that CVD method is prepared2It is exposed with electron beam in nanometer sheet
Light deposition metal Ti (5nm)/Au (100nm) obtains VTe2 field effect transistors.The picture for the VTe2 field-effect transistors prepared
As shown in figure 18.Obtained electricity output and transfer characteristic curve are tested as shown in Figure 19.
Si/SiO in Figure 182Substrate is mulberry, VTe2For blue or white hexagon, VTe2The long rectangle of gold on surface
It is respectively the metal Ti and Au of deposition with square, scale is 200 μm in figure.
Figure 19 a are VTe2The output characteristic curve of field-effect transistor；Figure 19 b are VTe2The transfer of field-effect transistor is special
Linearity curve；Demonstrate the VTe that the present invention is prepared2Nanometer sheet is metallic substance and electric conductivity is good.
Case study on implementation 9
Measure VTe needed for magnetism2The preparation of nanometer sheet：
Te powder and VCl that mass ratio is 3: 1 will be filled3The porcelain boat of powder is placed on the flat-temperature zone 2 of tube furnace, a piece of Si/
285nm SiO2As VTe2Growth substrate it is bright be placed on up be placed on another porcelain boat the flat-temperature zone 3 of tube furnace with
Obtain crystal growth temperature appropriate.Before heating, the air in quartz ampoule is discharged with the argon gas of larger flow.Then make
Flat-temperature zone 2,3, which heats, is increased to 620 DEG C, and argon flow amount is 50 sccm, and constant temperature 30min just has big face on silicon chip
Product monocrystalline VTe2Nanometer sheet generates.VTe2The Experimental equipment of nanometer sheet is as shown in Figure 1, the VTe prepared2The optics of nanometer sheet
Photo is as shown in figure 20.The obtained relevant magnetization curve in magnetic field and the relevant null field cooling magnetization curve of temperature are tested as schemed
Shown in 21.
Figure 20 is to prepare to measure magnetic required VTe2The optical schematic diagram of nanometer sheet, white hexagon and triangle
For VTe2Nanometer sheet, the VTe obtained under this condition2Nanometer sheet good crystallinity, density are big.Scale in Figure 20 is 10 μm.
Figure 21 a, 21b are respectively 10K, VTe under 300K2The relevant magnetization curve in nanometer sheet magnetic field, proves VTe2Nanometer sheet
With low temperature and room-temperature ferromagnetic；The VTe that Figure 21 c are measured under the conditions of being externally-applied magnetic field 5000Oe2Nanometer sheet temperature is relevant
Null field cools down magnetization curve, it was demonstrated that VTe2The Curie temperature of nanometer sheet is close to 300 K.
Claims (10)
1. a kind of VTe2The preparation method of two-dimensional material, it is characterised in that：By Te and VCl3The heated volatilization of mixed raw material, and
Carrier gas flux in 40-80sccm under the depositing temperature at 580-620 DEG C, grows to form VTe in substrate surface2Two-dimensional material；
The carrier gas is protection gas.
2. VTe as described in claim 12The preparation method of two-dimensional material, it is characterised in that：In mixed raw material, Te and VCl3's
Mass ratio is 1: 1~3: 1.
3. VTe as described in claim 12The preparation method of two-dimensional material, it is characterised in that：The heating volatilization of mixed raw material
Temperature is 580-620 DEG C.
4. VTe as described in claim 12The preparation method of two-dimensional material, it is characterised in that：The flow of carrier gas is preferably 60-
80sccm；Depositing temperature is 590-620 DEG C.
5. VTe as described in claim 12The preparation method of two-dimensional material, it is characterised in that：Mixed raw material is at a distance from substrate
For 21~24cm；Preferably 23cm.
6. VTe as described in claim 12The preparation method of two-dimensional material, it is characterised in that：It is protected under the depositing temperature
Warm growth time is 5-30min.
7. such as claim 1~6 any one of them VTe2The preparation method of two-dimensional material implements the deposition of the preparation method
Device includes the quartz ampoule of sealing, and the entrance for inputting carrier gas into quartz ampoule chamber is arranged in one end of the quartz ampoule,
The other end is provided with the outlet for exporting quartz ampoule gas to chamber；According to carrier gas stream direction, by the chamber of the quartz ampoule
Room is divided into upstream flat-temperature zone and downstream flat-temperature zone；It is characterized in that, above-mentioned upstream flat-temperature zone and downstream flat-temperature zone is both provided with
Heating device is equipped with Te powder and VCl3Porcelain boat be placed on upstream flat-temperature zone, equipped with substrate porcelain boat be arranged downstream flat-temperature zone；On
The shortest distance for swimming flat-temperature zone and downstream flat-temperature zone is 21~24cm.
8. VTe made from a kind of claim 1~7 any one of them preparation method2Two-dimensional material, which is characterized in that be VTe2
Nanometer sheet, thickness 8-360nm, size are 2-30 μm.
9. a kind of VTe according to any one of claims 82The application of two-dimensional material, it is characterised in that：Preparation applied to electricity device；It is excellent
It selects the VTe2Two-dimensional material is used to prepare VTe2Field-effect transistor.
10. VTe as claimed in claim 92The application of two-dimensional material, it is characterised in that：There is VTe in growth2It is used in two-dimensional material
After electron beam exposure marks sample, then in its surface deposited metal, obtain VTe2Field-effect transistor；
Preferably, by vacuum coating equipment in VTe2Deposited metal in two-dimensional material；
Preferably, the metal is Ti and Au
Preferably, the thickness of the metal Ti is 5nm, and the thickness of Au is 100nm.
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| CN107445204A (en) * | 2016-11-30 | 2017-12-08 | 北京大学 | A kind of method for preparing transient metal chalcogenide compound nano flake and vanadium disulfide, two selenizing vanadium nano flakes |
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| CN107445204A (en) * | 2016-11-30 | 2017-12-08 | 北京大学 | A kind of method for preparing transient metal chalcogenide compound nano flake and vanadium disulfide, two selenizing vanadium nano flakes |
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| CN110294463A (en) * | 2019-07-26 | 2019-10-01 | 华东师范大学 | A kind of transition element doped room-temperature ferromagnetic two-dimensional material and preparation method |
| CN110294463B (en) * | 2019-07-26 | 2022-07-08 | 华东师范大学 | Transition group element doped room-temperature ferromagnetic two-dimensional material and preparation method thereof |
| CN110846621A (en) * | 2019-11-11 | 2020-02-28 | 中国科学院上海技术物理研究所 | Two-step gas phase method for preparing large-area single-layer vanadium ditelluride material |
| CN115231530A (en) * | 2022-06-09 | 2022-10-25 | 四川大学 | Room temperature ferromagnetism MoSe 2 Thin film material and preparation method thereof |
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| CN115101357B (en) * | 2022-06-14 | 2024-01-26 | 中国工程物理研究院激光聚变研究中心 | Preparation method and application of ternary nickel cobalt tungsten telluride composite material |
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