CN104846434B - Two chalcogenide monocrystalline of a kind of two-dimentional transition metal and its preparation method and application - Google Patents
Two chalcogenide monocrystalline of a kind of two-dimentional transition metal and its preparation method and application Download PDFInfo
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Abstract
The invention discloses two chalcogenide monocrystalline of a kind of two-dimentional transition metal and its preparation method and application.In an inert atmosphere, can be with sulfur family simple substance (S by common, Se the concentration of S or Se in the metal for) reacting and hydrogen assist control system, to reach the purpose of the sulfuration of control transition metal layer or selenizing degree, controllably grows TMDs monocrystalline using chemical gaseous phase depositing process；By temperature control during deposition for 750 DEG C to 850 DEG C, and sedimentation time is controlled to 5 to 15 minutes, completes the preparation of TMDs monocrystalline；Wherein by substrate sputter processing method, sulfur family elemental powders consumption, the optimization for inhaling the preparation parameter such as S/Se metallic areas and species, density of hydrogen, growth temperature, growth time, realizing the strict control to high-quality two dimension two chalcogenide mono-crystalline structures of transition metal.
Description
Technical field
The invention belongs to two-dimensional film technical field of material, is related to a kind of two chalcogenide list of two-dimentional transition metal
Crystalline substance and its preparation method and application.
Background technology
Two chalcogenides of transition metal (TMDs) has similar structure, but the photoelectricity with oneself uniqueness with Graphene
Property, due to the presence of its band gap, and has preferable mobility value and on-off ratio simultaneously, in photoelectric device and P-N junction half
There is outstanding performance in conductor, so receiving the favor of numerous researcheres.In recent years, it has been found that two-dimentional transition metal two
Chalcogenide (TMDs), such as molybdenum bisuphide (MoS2), tungsten disulfide (WS2), two selenizing molybdenum (MoSe2) and two tungsten selenides
(WSe2) etc., the advantage represented at aspects such as metallicity, semiconductive and superconductivity is particularly evident.At the same time, TMDs partly leads
The band gap and property of body changes also with the change of the number of plies, can pass through accordingly to control its number of plies, multiple with other two-dimensional materials
Close, realize more application.
The field-effect transistor (FET) of the monolayer TMDs thin film obtained based on mechanical stripping has been shown one and very high has been opened
Ratio and a good mobility value is closed, two chalcogenide of several transition metal is mutually combined the P-N junction for obtaining in photoelectricity
Also excellent property is shown in the application such as device.In addition, TMDs thin film may be applied to inverter and light
In transistor.For example there is researcher recently by WSe being covered with metals such as Pt, Ru2Crystal, has obtained the high property of hydrogen production potential
Energy optoelectronic pole, with high using value.As can be seen here, two chalcogenide of transition metal will be before one kind extremely has application
The new material of scape.But the TMDs areas obtained in mechanical stripping are little and the number of plies is uncontrollable, while also cannot control well
The distribution of the TMDs that system is peeled off, this preparation method process are loaded down with trivial details and costly, it is impossible to prepare TMDs in a large number, cannot more enter
Applied research of the row based on high-quality TMDs.Therefore, how research grows that to obtain high quality monolayer TMDs be an inexorable trend.
Early in last century, just there are a lot of researcheres to study the preparation method of TMDs.With regard to WSe2For, earliest
It is by thermal evaporation WSe2Powder, or thermal decomposition WSe3The method of powder prepares WSe2Crystal, later, has developed some new again
Method, such as heating W (or WO3) and Se (or H2Se mixture), and with the metal-oxide of W (such as W (CO)6, WCl5, WOCl5
Deng) WSe is obtained with methods such as the compound reactions of Se2Granule or crystal, but it is not strict monolayer WSe2Thin film.Right
In the preparation of other several TMDs monocrystalline, method and effect are also essentially identical, therefore how controllably to prepare high-quality TMDs mono-
Crystalline substance becomes the problem that researchers pay close attention to jointly.And chemical vapour deposition technique (CVD) prepares tow -dimensions atom material as one kind
The classical way of material, has begun to extensively be applied by researcheres.The method of main flow is with S powder and Se powder, MoO at present3Powder
And WO3Powder is presoma, is reacted to each other at high temperature deposition by CVD, finally direct growth on a dielectric base, respectively
The MoS of monolayer can be obtained2、WS2、MoSe2And WSe2.But oxide (the MoO for introducing in this process3And WO3) can remain
On the surface of gained sample, so as to have a huge impact to the quality of the TMDs monocrystalline for obtaining and application.There is researcher
By presoma is changed to the TMDs powder for having synthesized, the introducing of oxide is avoided, but so cannot but pass through to control gold
Category is controlled than carrying out the long TMDs films for obtaining of opposite with the amount of the material of sulfur family simple substance, result in the drop of product controllable degree
Low；Also there is researcher that presoma is changed to gas reactant, can so improve the controllability for generating TMDs monocrystalline, but this
Method is difficult to obtain large-area TMDs crystal regions under very big growth window.At present, how high-quality is controllably prepared
Large-area monolayer TMDs becomes the problem that researchers pay close attention to jointly.
Content of the invention
The purpose of the present invention is to overcome defect present in prior art, there is provided a kind of large-area high-quality two dimension transition gold
Belong to two chalcogenide monocrystalline, in an inert atmosphere, by the common metal that can be reacted with sulfur family simple substance (S, Se) and hydrogen
The concentration of S or Se in assist control system, to reach the purpose of the sulfuration of control transition metal layer or selenizing degree, using chemical gas
Phase deposition process controllably grows TMDs monocrystalline.By temperature control during deposition for 750 DEG C to 850 DEG C, and sedimentation time control
It is made as 5 to 15 minutes, completes the preparation of the TMDs monocrystalline.Wherein by substrate sputter processing method, sulfur family elemental powders
Consumption, the optimization for inhaling the preparation parameter such as S/Se metallic areas and species, density of hydrogen, growth temperature, growth time, realize to height
The strict control of mass transfer metal dichalcogenides mono-crystalline structures.
The technical scheme that the present invention is provided is specific as follows：
A kind of preparation method of two chalcogenide monocrystalline of two-dimentional transition metal (TMDs monocrystalline), comprises the steps：
(1), under high vacuum condition, one layer of transition metal nanoparticles layer is sputtered in dielectric base after cleaning；
(2) dielectric base that sputtering has transition metal nanoparticles layer is placed on the high-temperature region of CVD stoves, by sulfur family simple substance and
The metal for absorbing sulfur family simple substance is placed on low-temperature space；
(3), in atmosphere of inert gases, the high-temperature region of CVD stoves is heated with 15 DEG C/min～45 DEG C/min of heating rate
To 750 DEG C～850 DEG C, while the heating rate control low-temperature space temperature with 15 DEG C/min～45 DEG C/min synchronously arrives at 700
DEG C～780 DEG C, wherein, the temperature difference of high-temperature region and low-temperature space is 50～70 DEG C；High-purity hydrogen is then passed to, flow is maintained at
5sccm～20sccm, maintains 5 minutes～20 minutes；After reaction terminates, sulfur family simple substance source and dielectric base and transition gold is controlled
The temperature of category nanoparticle layers, makes three be cooled to 650 DEG C～750 DEG C in 2 minutes～8 minutes；Treat that CVD furnace temperatures are down to
650 DEG C～750 DEG C, regulation and control rate of temperature fall makes which be cooled to 150 DEG C～250 DEG C in 10 minutes～20 minutes；
(4) treat that room temperature is down to naturally by whole CVD stoves, that is, obtain two chalcogenide monocrystalline of two-dimentional transition metal.
A kind of two chalcogenide monocrystalline of two-dimentional transition metal, by two chalcogenide monocrystalline of above-mentioned two-dimentional transition metal
Preparation method is prepared.
Application of the described two chalcogenide monocrystalline of two-dimentional transition metal as two-dimensional film material.
The TMDs monocrystalline is monolayer, wherein adopts chemical vapour deposition technique, to sputter at the gold on dielectric base surface
Category simple substance and sulfur family elemental powders are used as presoma, and the metal and hydrogen assisted reaction with common absorption sulfur family simple substance,
Substrate surface deposits TMDs monocrystalline, and wherein by temperature control during deposition for 750 DEG C to 850 DEG C, and sedimentation time is controlled to 5
To 15 minutes.
The transition metal is Mo and W, bulk, lamellar from its purity more than or equal to 99.95%, thread or powder
Last shape simple substance etc..The sputtering time of the transition metal layer in dielectric base is controlled to 5 to 25 seconds, preferably 5 to 15 seconds, and most preferably 7
To 10 seconds.
The sulfur family elemental powders are S and Se, the S powder and Se powder from purity more than or equal to 99.5%, S powder consumptions
For 0.04 to 0.12 gram, preferably 0.06 to 0.10 gram, most preferably 0.08 gram；Se powder consumption be 0.02 to 0.10 gram, preferably 0.04
To 0.08 gram, most preferably 0.06 gram.
Described absorb sulfur family simple substance metal be nickel, cobalt, ferrum, aluminum, gold, silver, copper, zinc, molybdenum, tungsten, titanium, vanadium, chromium, ruthenium, rhodium,
At least one at least one in platinum, palladium and iridium, preferably nickel, ferrum and copper；The selected metal for absorbing sulfur family simple substance for block,
Strip, lamellar, ring-type and netted, preferably ring-type and netted.The metallic area of selected absorption sulfur family simple substance is 1～10cm2, excellent
Select 4～7cm2, most preferably 6cm2.
The dielectric base is that surfacing is clean, fusing point is higher than 850 DEG C, and is difficult and the atomic reactions such as W, Mo, S, Se
Solid material, such as silicon chip, piezoid, sapphire or mica sheet etc..
The sulfur family simple substance source and the metal of sulfur family simple substance is absorbed in low-temperature space, substrate and splash-proofing sputtering metal layer are in high-temperature region.
High-temperature region temperature is 750 DEG C to 850 DEG C, preferably 790 DEG C to 810 DEG C, most preferably 800 DEG C.Low-temperature space temperature is 700 DEG C to 780
DEG C, preferably 740 DEG C to 770 DEG C, most preferably 760 DEG C.High-temperature region is 15 DEG C/min to 45 DEG C/minute with the heating rate of low-temperature space
Clock, preferably 25 DEG C/min to 35 DEG C/min, most preferably 30 DEG C/min.
Deposition process is carried out in inertia protective gas, is such as carried out in argon, nitrogen etc., preferably argon.Argon
Flow be 50sccm to 200sccm, preferably 100sccm to 150sccm, most preferably 100sccm.Hydrogen flowing quantity used by assisted reaction
For 5sccm to 20sccm, most preferably preferably 10sccm to 15sccm, 10sccm.The time of hydrogen assisted reaction is 5 to 20 points
Clock, preferably 5 to 15 minutes, most preferably 10 minutes.After reaction terminates, for the dielectric base and splash-proofing sputtering metal layer carry out two
Step cooling.The time of first step cooling is 2 minutes to 8 minutes, preferably 3 minutes to 5 minutes, most preferably 4 minutes.The first step is lowered the temperature
Temperature afterwards is 650 DEG C to 750 DEG C, preferably 680 DEG C to 720 DEG C, most preferably 700 DEG C.The time of second step cooling is 10 points
Clock to 20 minutes, preferably 12 minutes to 18 minutes, most preferably 15 minutes.Temperature after second step cooling terminates is 150 DEG C to 250
DEG C, preferably 180 DEG C to 220 DEG C, most preferably 200 DEG C.
The cleaning step of described dielectric base is：It is cleaned by ultrasonic 20 by each in acetone, ethanol, water successively for dielectric base
Minute, then deionized water is cleaned up, and is dried up with nitrogen.
The present invention has following characteristics and advantage relative to prior art：
1st, the present invention is disclosed for the first time and prepares the side of TMDs monocrystalline using elemental metals layer is sputtered on a dielectric base
Method, and the concentration by S or Se in common suction S/Se metals and hydrogen assist control system, to reach the sulfur of control metal level
Change or the purpose of selenizing degree, controllably prepare strict uniform TMDs monocrystalline.In insulation when the method is sputtered using source metal
Substrate surface forms nanoparticle, and in an inert atmosphere, being allowed to volatilization to the heating of sulfur family simple substance source becomes gaseous state, profit during this
Part S or Se are absorbed with metals such as copper, reduce the nucleating point of TMDs, while making the atmosphere of S or Se in downstream more equal
Even obtaining uniform TMDs monocrystalline.After system reaches reaction temperature, the activity that hydrogen improves S/Se is passed through, area is obtained
Bigger TMDs monocrystalline.The method is reached by the strict control of usage amount and existence form to presoma in system
The purpose of its concentration is controlled, it is achieved thereby that the growth of high-quality two dimension two chalcogenide monocrystalline of transition metal.
2nd, this method has universality, for most of two chalcogenides of two-dimentional transition metal, by adjusting experiment ginseng
Number, is prepared using chemical vapour deposition technique.
3rd, method disclosed by the invention, the preparation for changing to innovative two chalcogenide monocrystalline of two-dimentional transition metal are existing
Shape.Other preparation methoies are compared, the nucleation of TMDs has been better controled over, the strict uniform TMDs for obtaining certain size is mono-
Crystalline substance, on the other hand, it also avoid the oxide residual in traditional preparation methods, and introduces metal as adjuvant, propose
A kind of new growth mechanism and theoretical model.
The method of the preparation two chalcogenide monocrystalline of two-dimentional transition metal that the 4th, the present invention is provided, condition are simple, without the need for severe
The conditions such as control programming rate, growth temperature, system pressure and cooling rate are carved, the directivity of substrate need not be more considered.Experiment
Preparation parameter (such as programming rate, growth temperature, system pressure and cooling rate etc.) control fault-tolerance is strong, prepares gained TMDs tight
Lattice are uniform, product reproducible, substrate is cheap and easy to get, is particularly suitable for industrialized production, be particularly suited for monolayer or
The controllable standby of few layer TMDs.
Description of the drawings
Preparation facilitiess schematic diagrams of the Fig. 1 for two chalcogenide monocrystalline of transition metal.
The flow chart that Fig. 2 prepares two chalcogenide monocrystalline of transition metal for chemical vapor deposition.
Fig. 3 is the optical photograph for depositing two tungsten selenide monocrystalline of monolayer on a quartz substrate in embodiment 1.
Fig. 4 is the Raman spectrogram for depositing two tungsten selenide monocrystalline of monolayer on a quartz substrate in embodiment 1.
Fig. 5 is the photoluminescence spectra figure for depositing two tungsten selenide monocrystalline of monolayer on a quartz substrate in embodiment 1.
Fig. 6 is the atomic force microscope images for depositing two tungsten selenide monocrystalline of monolayer on a quartz substrate in embodiment 1.
Fig. 7 is the Raman spectrogram for depositing two tungsten selenide of bilayer on a quartz substrate in embodiment 2.
Fig. 8 is the photoluminescence spectra figure for depositing two tungsten selenide of bilayer on a quartz substrate in embodiment 2.
Fig. 9 is the Raman spectrogram for depositing monolayer molybdenum bisuphide monocrystalline on a quartz substrate in embodiment 3.
Figure 10 is the photoluminescence spectra figure for depositing monolayer molybdenum bisuphide monocrystalline on a quartz substrate in embodiment 3.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
State method and be conventional method if no special instructions.The material can be obtained from open commercial sources if no special instructions.
The present invention using the elemental metals source and sulfur family simple substance source being splashed in dielectric base, using chemical vapor deposition
Method, on the surface of the substrate two chalcogenide monocrystalline of direct growth transition metal.The dielectric base of metal level will specifically have been sputtered
The high-temperature region (750～850 DEG C) of CVD stoves is placed on, sulfur family simple substance source and absorption S/Se metals are placed on low-temperature space (650～750 DEG C)；
Before preparing, system does not need special evacuation；In preparation process, inertia protective gas is passed through, keeps normal pressure, while being passed through hydrogen
Gas assisting growth；By controlling growth conditionss (such as temperature, growth time etc.), high-quality mistake can be grown on the surface of the substrate
Cross metal dichalcogenides monocrystalline.The preparation method is using cost and method simple economy, it is easy to control, and can prepare big
Area and high quality two dimension two chalcogenide monocrystalline of transition metal.
Embodiment 1：Prepare two tungsten selenide monocrystalline of monolayer
(1) piezoid is cut into silicon knife the square of 10 × 10mm, is respectively cleaned by ultrasonic in acetone, ethanol, water successively
20 minutes, then deionized water was cleaned up, and was dried up with nitrogen.
(2) the piezoid magnetron sputtering after cleaning is sputtered in front, tungsten layer sputtering electronic anesthetic vaporizer (ULVAC, ACS-
4000-C4) under a high vacuum, the tungsten target with purity more than 99.95%, sputtering time are 7 seconds.
(3) will be equipped with the selenium powder that purity is that 99.5%, quality is 0.03g and be put into a new quartz boat, and by the quartz boat
The low-temperature space (the Single port position of CVD stoves) of CVD stoves one end is placed on, as shown in Figure 1.
(4) piezoid for having sputtered tungsten layer is put in quartz boat, quartz boat is pushed into the high-temperature region of CVD stove quartz ampoules
(middle part of CVD stoves), as shown in Figure 1.
(5) absorb selenium used by copper sheet be placed on selenium powder and sputtered tungsten layer piezoid between, area is 1cm2, such as Fig. 1
Shown.
(6) high-purity argon gas are passed through in quartz ampoule, flow is maintained at 100sccm.
(7) CVD stoves high-temperature region was heated to 800 DEG C in 25 minutes, now low-temperature space temperature synchronously arrives at 760 DEG C.?
Under conditions of 760 DEG C of 800 DEG C of high-temperature region and low-temperature space, high-purity hydrogen is passed through, flow is maintained at 10sccm, maintains 10 minutes.Instead
The temperature of selenium source and quartz substrate and sputtering tungsten layer after should terminating, is controlled, and is allowed to 700 DEG C were cooled in 4 minutes.
(8) treat that CVD furnace temperatures are down to 700 DEG C, open tube furnace lid regulation and control rate of temperature fall, be allowed to lower the temperature in 15 minutes
To 200 DEG C.
(9) treat that room temperature is down to naturally by whole quartz ampoule, take out sample.
Sample characterization is carried out using optical microscope, Raman spectrum, fluorescence spectrum and atomic force microscope.Can be with from Fig. 3
Find out, the two tungsten selenide monocrystalline for obtaining on a quartz substrate are triangular in shape, and triangle average side length is up to more than 20 μm.Scheme simultaneously
In 4 Raman spectrum, 248cm-1And 259cm-1Nearby there is the characteristic peak of two tungsten selenides, in 306cm-1Nearby there is not two-layer
Or the characteristic peak of multilamellar, it was demonstrated that it is two tungsten selenide of monolayer.There is a very strong peak at 780nm in the photoluminescence spectra of Fig. 5, be
The characteristic peak of two tungsten selenide of monolayer.During the atomic force microscope of Fig. 6 is characterized, delta-shaped region is relatively significantly shown.These
Data all show that prepared sample is two tungsten selenide crystal of high-quality monolayer.
Embodiment 2：Prepare double-deck two tungsten selenide
(1) piezoid is cut into silicon knife the square of 10 × 10mm, is respectively cleaned by ultrasonic in acetone, ethanol, water successively
20 minutes, then deionized water was cleaned up, and was dried up with nitrogen.
(2) the piezoid magnetron sputtering after cleaning is sputtered in front, tungsten layer sputtering electronic anesthetic vaporizer (ULVAC, ACS-
4000-C4) under a high vacuum, the tungsten target with purity more than 99.95%, sputtering time are 10 seconds.
(3) will be equipped with the selenium powder that purity is that 99.5%, quality is 0.05g and be put into a new quartz boat, and by the quartz boat
The low-temperature space (the Single port position of CVD stoves) of CVD stoves one end is placed on, as shown in Figure 1.
(4) piezoid for having sputtered tungsten layer is put in quartz boat, quartz boat is pushed into the high-temperature region of CVD stove quartz ampoules
(middle part of CVD stoves), as shown in Figure 1.
(5) absorb the copper ring used by selenium to be placed between selenium powder and growth substrate, area is 5cm2.
(6) high-purity argon gas are passed through in quartz ampoule, flow is maintained at 150sccm.
(7) CVD stoves high-temperature region was heated to 810 DEG C in 30 minutes, now low-temperature space temperature synchronously arrives at 765 DEG C.?
Under conditions of 765 DEG C of 810 DEG C of high-temperature region and low-temperature space, high-purity hydrogen is passed through, flow is maintained at 10sccm, maintains 10 minutes.Instead
The temperature of selenium source and quartz substrate and sputtering tungsten layer after should terminating, is controlled, and is allowed to 700 DEG C were cooled in 5 minutes.
(8) treat that CVD furnace temperatures are down to 700 DEG C, open tube furnace lid regulation and control rate of temperature fall, be allowed to lower the temperature in 15 minutes
To 200 DEG C.
(9) treat that room temperature is down to naturally by whole quartz ampoule, take out sample.
Sample characterization is carried out using Raman spectrum and photoluminescence spectra.From the Raman spectrum of Fig. 7,248cm-1With
259cm-1Nearby there is the characteristic peak of two tungsten selenides, in 306cm-1Nearby there is the characteristic peak of two-layer or multilamellar, while Fig. 8
Photoluminescence spectra has a very strong peak at 800nm, is the characteristic peak of double-deck two tungsten selenide, it was demonstrated that be double-deck two tungsten selenide.
Embodiment 3：Prepare monolayer molybdenum bisuphide monocrystalline
(1) piezoid is cut into silicon knife the square of 10 × 10mm, is respectively cleaned by ultrasonic in acetone, ethanol, water successively
20 minutes, then deionized water was cleaned up, and was dried up with nitrogen.
(2) the piezoid magnetron sputtering after cleaning is sputtered in front, molybdenum layer sputtering electronic anesthetic vaporizer (ULVAC, ACS-
4000-C4) under a high vacuum, the molybdenum target with purity more than 99.95%, sputtering time are 7 seconds.
(3) will be equipped with the sulphur powder that purity is that 99.5%, quality is 0.08g and be put into a new quartz boat, and by the quartz boat
The low-temperature space (the Single port position of CVD stoves) of CVD stoves one end is placed on, as shown in Figure 1.
(4) piezoid for having sputtered molybdenum layer is put in quartz boat, quartz boat is pushed into the high-temperature region of CVD stove quartz ampoules
(middle part of CVD stoves), as shown in Figure 1.
(5) absorb the copper ring used by sulfur to be placed between sulphur powder and growth substrate, area is 7cm2.
(6) high-purity argon gas are passed through in quartz ampoule, flow is maintained at 80sccm.
(7) CVD stoves high-temperature region was heated to 790 DEG C in 25 minutes, now low-temperature space temperature synchronously arrives at 755 DEG C.?
Under conditions of 755 DEG C of 790 DEG C of high-temperature region and low-temperature space, high-purity hydrogen is passed through, flow is maintained at 10sccm, maintains 10 minutes.Instead
The temperature of sulphur source and quartz substrate and sputtering molybdenum layer after should terminating, is controlled, and is allowed to 680 DEG C were cooled in 7 minutes.
(8) treat that CVD furnace temperatures are down to 680 DEG C, open tube furnace lid regulation and control rate of temperature fall, be allowed to lower the temperature in 14 minutes
To 200 DEG C.
(9) treat that room temperature is down to naturally by whole quartz ampoule, take out sample.
Sample characterization is carried out using Raman spectrum and photoluminescence spectra.In the Raman spectrum of Fig. 9,385cm-1And 405cm-1Nearby there is the characteristic peak of monolayer molybdenum bisuphide monocrystalline, it was demonstrated that be monolayer molybdenum bisuphide monocrystalline.While the luminescence generated by light light of Figure 10
Spectrum has a very strong peak at 675nm, is the characteristic peak of monolayer molybdenum bisuphide monocrystalline, it was demonstrated that be monolayer molybdenum bisuphide monocrystalline.
Claims (5)
1. the preparation method of two chalcogenide monocrystalline of a kind of two-dimentional transition metal, it is characterised in that comprise the steps：
(1), under high vacuum condition, one layer of transition metal nanoparticles layer is sputtered in dielectric base after cleaning；Described transition
Metal is Mo or W；
(2) dielectric base that sputtering has transition metal nanoparticles layer is placed on the high-temperature region of CVD stoves, sulfur family simple substance and copper is put
In low-temperature space；Described sulfur family simple substance is S or Se；
(3), in atmosphere of inert gases, the high-temperature region of CVD stoves is heated to 15 DEG C/min～45 DEG C/min of heating rate
750 DEG C～850 DEG C, while the heating rate control low-temperature space temperature with 15 DEG C/min～45 DEG C/min synchronously arrives at 700 DEG C
～780 DEG C, wherein, the temperature difference of high-temperature region and low-temperature space is 50～70 DEG C；High-purity hydrogen is then passed to, flow is maintained at
5sccm～20sccm, maintains 5 minutes～20 minutes；After reaction terminates, sulfur family simple substance source and dielectric base and transition gold is controlled
The temperature of category nanoparticle layers, makes three be cooled to 650 DEG C～750 DEG C in 2 minutes～8 minutes；Treat that CVD furnace temperatures are down to
650 DEG C～750 DEG C, regulation and control rate of temperature fall makes which be cooled to 150 DEG C～250 DEG C in 10 minutes～20 minutes；
(4) treat that room temperature is down to naturally by whole CVD stoves, that is, obtain two chalcogenide monocrystalline of two-dimentional transition metal；Described two dimension
Two chalcogenide monocrystalline of transition metal is two tungsten selenide of monolayer, double-deck two tungsten selenide or monolayer molybdenum bisuphide monocrystalline.
2. the preparation method of two chalcogenide monocrystalline of two-dimentional transition metal according to claim 1, it is characterised in that：Institute
Dielectric base is stated for silicon chip, piezoid, sapphire or mica sheet.
3. the preparation method of two chalcogenide monocrystalline of two-dimentional transition metal according to claim 1, it is characterised in that：Institute
The sputtering mode that states is：Transition metal is sputtered under a high vacuum 5 to 25 seconds using electronic anesthetic vaporizer.
4. the preparation method of two chalcogenide monocrystalline of two-dimentional transition metal according to claim 1, it is characterised in that：High
Warm area is 30 DEG C/min with the heating rate of low-temperature space.
5. the preparation method of two chalcogenide monocrystalline of two-dimentional transition metal according to claim 1, it is characterised in that：Institute
The cleaning step of the dielectric base that states is：It is cleaned by ultrasonic 20 minutes by each in acetone, ethanol, water successively for dielectric base, then
Deionized water is cleaned up, and is dried up with nitrogen.
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