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 PDF

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CN108584888A
CN108584888A CN201810270126.9A CN201810270126A CN108584888A CN 108584888 A CN108584888 A CN 108584888A CN 201810270126 A CN201810270126 A CN 201810270126A CN 108584888 A CN108584888 A CN 108584888A
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段曦东
段镶锋
李佳
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Hunan University
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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

A kind of telluride vanadium two-dimensional material and its synthetic method and application
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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CN109629004A (en) * 2019-01-09 2019-04-16 湖南大学 The method that Van der Waals is epitaxially formed the thin transition metal tellurides two-dimensional metallic material of atom level in no dangling bonds substrate
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
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CN115101357A (en) * 2022-06-14 2022-09-23 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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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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CN109629004A (en) * 2019-01-09 2019-04-16 湖南大学 The method that Van der Waals is epitaxially formed the thin transition metal tellurides two-dimensional metallic material of atom level in no dangling bonds substrate
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
CN115231530B (en) * 2022-06-09 2023-10-10 四川大学 Room temperature ferromagnetic MoSe 2 Film material and preparation method thereof
CN115101357A (en) * 2022-06-14 2022-09-23 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
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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