CN104846434A - Two-dimensional transition metal disulfides monocrystalline, and preparation method and applications thereof - Google Patents

Two-dimensional transition metal disulfides monocrystalline, and preparation method and applications thereof Download PDF

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CN104846434A
CN104846434A CN201510174079.4A CN201510174079A CN104846434A CN 104846434 A CN104846434 A CN 104846434A CN 201510174079 A CN201510174079 A CN 201510174079A CN 104846434 A CN104846434 A CN 104846434A
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transition metal
monocrystalline
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chalcogenide
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CN104846434B (en
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刘津欣
王凌翔
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Wuhan University WHU
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Abstract

The invention discloses a two-dimensional transition metal disulfides (TMDs) monocrystalline, and a preparation method and applications thereof. According to the preparation method, in an inert atmosphere, assist control of the concentration of S or Se in a system is realized with common metal which is capable of reacting with sulfur family elementary substance (S, Se) and hydrogen so as to control sulfuration degree or selenylation degree of a transition metal layer, and controllable growth of TMDs monocrystalline is realized via chemical vapor deposition; deposition temperature is controlled to be 750 to 850 DEG C, and deposition time is controlled to be 5 to 15min so as to complete TMDs monocrystalline preparation; wherein, strict control on high-quality two-dimensional transition metal disulfides monocrystalline is realized via optimization of preparation parameters such as substrate sputtering treatment method, sulfur family elementary substance powder using amount, absorbed S/Se metal area and kinds, hydrogen concentration, growth temperature, and growth time.

Description

A kind of two-dimentional transition metal two chalcogenide monocrystalline and its preparation method and application
Technical field
The invention belongs to two-dimensional film technical field of material, relate to a kind of two-dimentional transition metal two chalcogenide monocrystalline and its preparation method and application.
Background technology
Transition metal two chalcogenide (TMDs) and Graphene have similar structure, but there is the photoelectric property of oneself uniqueness, due to the existence of its band gap, and there is good mobility value and on-off ratio simultaneously, outstanding performance is had, so receive the favor of numerous investigator in photoelectric device and P-N junction semi-conductor.In recent years, it is found that two-dimentional transition metal two chalcogenide (TMDs), as molybdenumdisulphide (MoS 2), tungsten disulfide (WS 2), two selenizing molybdenum (MoSe 2) and two tungsten selenide (WSe 2) etc., the advantage represented in metallicity, semiconductive and supraconductivity etc. is particularly evident.Meanwhile, band gap and the character of TMDs semi-conductor also change along with the change of the number of plies, can, by controlling its number of plies, with other two-dimensional material compounds, realize more applying accordingly.
The field-effect transistor (FET) of the individual layer TMDs film obtained based on mechanically peel has shown a very high on-off ratio and a good mobility value, and the P-N junction that the mutual compound of several transition metal two chalcogenide obtains also shows excellent character in the application such as photoelectric device.In addition, TMDs film can also be applied in transverter and lighting transistor.Investigator is such as had to pass through to cover WSe with metals such as Pt, Ru recently 2crystal, obtains the high-performance optical electrode of hydrogen production potential, has high using value.As can be seen here, transition metal two chalcogenide will be a kind of type material extremely having application prospect.But the TMDs area obtained in mechanically peel is little and the number of plies is uncontrollable, also cannot control the distribution of the TMDs peeled off well, this preparation method's process is loaded down with trivial details simultaneously, and costly, TMDs cannot be prepared in a large number, more cannot carry out the applied research based on high quality TMDs.Therefore, how research grows that to obtain high quality monolayer TMDs be an inexorable trend.
As far back as last century, the preparation method of a lot of investigators to TMDs is just had to be studied.With regard to WSe 2, be by thermal evaporation WSe the earliest 2powder, or thermolysis WSe 3the method of powder prepares WSe 2crystal, afterwards, had developed again some novel methods, as heating W (or WO 3) and Se (or H 2se) mixture, and with the metal oxide of W (as W (CO) 6, WCl 5, WOCl 5deng) obtain WSe with the method such as the compound reaction of Se 2particle or crystal, but not strict individual layer WSe 2film.For the preparation of other several TMDs monocrystalline, method and effect are also substantially identical, and therefore how controllably preparing high quality TMDs monocrystalline becomes the common problem paid close attention to of investigators.And chemical Vapor deposition process (CVD) is as a kind of classical way preparing tow-dimensions atom material, start studied persons' widespread use.The method of current main flow is with S powder and Se powder, MoO 3powder and WO 3powder is presoma, at high temperature to be reacted to each other deposition by CVD, finally direct growth on a dielectric base, can obtain the MoS of individual layer respectively 2, WS 2, MoSe 2and WSe 2.But the oxide compound (MoO introduced in this process 3and WO 3) surface of gained sample can be remained in, thus can have a huge impact the quality of the TMDs monocrystalline obtained and application.There is investigator by presoma being changed into the TMDs powder synthesized, avoid the introducing of oxide compound, but so but cannot control than to growing the TMDs film obtained with the amount of substance of sulfur family simple substance by controlling metal, result in the reduction of product controllable degree; Also there is investigator to change presoma into gas reactant, the controllability generating TMDs monocrystalline can be improved like this, but this method is difficult under very large growth window, obtain large-area TMDs crystal region.At present, how controllably to prepare the large-area individual layer TMDs of high quality and become the common problem paid close attention to of investigators.
Summary of the invention
The object of the invention is to overcome the defect existed in prior art, a kind of large-area high-quality two dimension transition metal two chalcogenide monocrystalline is provided, in an inert atmosphere, by common can with sulfur family simple substance (S, Se) concentration of S or Se in the metal reacted and hydrogen subcontrol system, to reach the object controlling transition metal layer sulfuration or selenizing degree, chemical gaseous phase depositing process is utilized controllably to grow TMDs monocrystalline.Temperature during deposition is controlled to be 750 DEG C to 850 DEG C, and depositing time controls to be 5 to 15 minutes, completes the preparation of described TMDs monocrystalline.Wherein by the optimization to substrate sputter treatment process, sulfur family elemental powders consumption, preparation parameter such as suction S/Se metallic area and kind, density of hydrogen, growth temperature, growth time etc., realize the strict control to high quality transition metal two chalcogenide single crystal structure.
Technical scheme provided by the invention is specific as follows:
A kind of preparation method of two-dimentional transition metal two chalcogenide monocrystalline (TMDs monocrystalline), comprises the steps:
(1), under high vacuum condition, dielectric base after cleaning sputters one deck transition metal nanoparticles layer;
(2) there is the dielectric base of transition metal nanoparticles layer to be placed on the high-temperature zone of CVD stove sputtering, the metal of sulfur family simple substance and absorption sulfur family simple substance is placed on cold zone;
(3) in atmosphere of inert gases, with the temperature rise rate of 15 DEG C/min ~ 45 DEG C/min, the high-temperature zone of CVD stove is heated to 750 DEG C ~ 850 DEG C, control cold zone temperature with the temperature rise rate of 15 DEG C/min ~ 45 DEG C/min simultaneously and synchronously arrive 700 DEG C ~ 780 DEG C, wherein, the temperature head of high-temperature zone and cold zone is 50 ~ 70 DEG C; Then pass into high-purity hydrogen, flow remains on 5sccm ~ 20sccm, maintains 5 minutes ~ 20 minutes; After reaction terminates, control the temperature of sulfur family simple substance source and dielectric base and transition metal nanoparticles layer, make three be cooled to 650 DEG C ~ 750 DEG C in 2 minutes ~ 8 minutes; Treat that CVD furnace temperature is down to 650 DEG C ~ 750 DEG C, regulation and control rate of temperature fall makes it in 10 minutes ~ 20 minutes, be cooled to 150 DEG C ~ 250 DEG C;
(4) treat that whole CVD stove is down to room temperature naturally, namely obtain two-dimentional transition metal two chalcogenide monocrystalline.
A kind of two-dimentional transition metal two chalcogenide monocrystalline, is prepared by the preparation method of above-mentioned two-dimentional transition metal two chalcogenide monocrystalline.
Described two-dimentional transition metal two chalcogenide monocrystalline is as the application of two-dimensional film material.
Described TMDs monocrystalline is individual layer, wherein adopt chemical Vapor deposition process, to sputter at the metal simple-substance on dielectric base surface and sulfur family elemental powders as presoma, and with the metal of common absorption sulfur family simple substance and hydrogen assisted reaction, at substrate surface deposition TMDs monocrystalline, wherein temperature during deposition is controlled to be 750 DEG C to 850 DEG C, and depositing time controls to be 5 to 15 minutes.
Described transition metal is Mo and W, derives from bulk, sheet, thread or powdered elemental etc. that its purity is more than or equal to 99.95%.The sputtering time of the transition metal layer in dielectric base controls to be 5 to 25 seconds, preferably 5 to 15 seconds, most preferably 7 to 10 seconds.
Described sulfur family elemental powders is S and Se, and derive from S powder and Se powder that purity is more than or equal to 99.5%, S powder consumption is 0.04 to 0.12 gram, preferably 0.06 to 0.10 gram, most preferably 0.08 gram; Se powder consumption is 0.02 to 0.10 gram, preferably 0.04 to 0.08 gram, most preferably 0.06 gram.
The metal of described absorption sulfur family simple substance is at least one in nickel, cobalt, iron, aluminium, gold and silver, copper, zinc, molybdenum, tungsten, titanium, vanadium, chromium, ruthenium, rhodium, platinum, palladium and iridium, at least one in preferred nickel, iron and copper; The selected metal absorbing sulfur family simple substance is bulk, strip, sheet, ring-type and netted, preferred ring-type and netted.The metallic area of selected absorption sulfur family simple substance is 1 ~ 10cm 2, preferably 4 ~ 7cm 2, most preferably 6cm 2.
Described dielectric base is that surfacing is clean, fusing point higher than 850 DEG C, and not easily with the solid material of the atomic reaction such as W, Mo, S, Se, as silicon chip, quartz plate, sapphire or sheet mica etc.
The metal of described sulfur family simple substance source and absorption sulfur family simple substance is in cold zone, and substrate and splash-proofing sputtering metal layer are in high-temperature zone.High-temperature zone temperature is 750 DEG C to 850 DEG C, preferably 790 DEG C to 810 DEG C, most preferably 800 DEG C.Cold zone temperature is 700 DEG C to 780 DEG C, preferably 740 DEG C to 770 DEG C, most preferably 760 DEG C.The temperature rise rate of high-temperature zone and cold zone is 15 DEG C/min to 45 DEG C/min, 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, as carried out in argon gas, nitrogen etc., and preferred argon gas.The flow of argon gas is 50sccm to 200sccm, preferred 100sccm to 150sccm, most preferably 100sccm.Assisted reaction hydrogen flowing quantity used is 5sccm to 20sccm, preferred 10sccm to 15sccm, most preferably 10sccm.The time of hydrogen assisted reaction is 5 to 20 minutes, preferably 5 to 15 minutes, most preferably 10 minutes.After reaction terminates, two step-down temperature are carried out for described dielectric base and splash-proofing sputtering metal layer.The time of the first step cooling is 2 minutes to 8 minutes, preferably 3 minutes to 5 minutes, most preferably 4 minutes.Temperature after the first step cooling 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 minutes 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: by dielectric base each ultrasonic cleaning 20 minutes in acetone, ethanol, water successively, then clean by washed with de-ionized water, and dries up with nitrogen.
The present invention has following characteristics and advantage relative to prior art:
1, the present invention discloses utilization and sputter elemental metals layer on a dielectric base to prepare the method for TMDs monocrystalline first time, and by the concentration of S or Se in common suction S/Se metal and hydrogen subcontrol system, the sulfuration of metal level or the object of selenizing degree is controlled, controllably the strict uniform TMDs monocrystalline of preparation to reach.Nanoparticle is formed on dielectric base surface when the method utilizes source metal to sputter, in an inert atmosphere, volatilization is made it to the heating of sulfur family simple substance source and becomes gaseous state, the metal pair part S or Se such as copper are utilized to absorb in this process, reduce the nucleation site of TMDs, make the atmosphere of S or Se in downstream more even to obtain uniform TMDs monocrystalline simultaneously.After system reaches temperature of reaction, pass into the activity that hydrogen improves S/Se, obtain the TMDs monocrystalline that area is larger.This method, by the usage quantity of presoma in system and the strict control of existence form, reaches the object controlling its concentration, thus achieves the growth of high quality two dimension transition metal two chalcogenide monocrystalline.
2, present method has universality, for most of two-dimentional transition metal two chalcogenide, by regulating experiment parameter, chemical Vapor deposition process all can be utilized to be prepared.
3, method disclosed by the invention, changes to innovative the preparation present situation of two-dimentional transition metal two chalcogenide monocrystalline.Compare other preparation method, control the nucleation of TMDs better, obtain the strict uniform TMDs monocrystalline of certain size, on the other hand, the oxide compound that it also avoid in traditional preparation methods remains, and introduces metal as auxiliary, proposes a kind of new growth mechanism and theoretical model.
4, the method for preparation provided by the invention two-dimentional transition metal two chalcogenide monocrystalline, condition is simple, controls the conditions such as heat-up rate, growth temperature, system pressure and cooling rate, more without the need to considering the directivity of substrate without the need to harshness.It is strong that experiment preparation parameter (as heat-up rate, growth temperature, system pressure and cooling rate etc.) controls fault-tolerance, prepare gained TMDs strictly even, product reproducible, substrate is cheap and easy to get, be particularly suitable for suitability for industrialized production, be particularly useful for the controlled synthesis of individual layer or few layer TMDs.
Accompanying drawing explanation
Fig. 1 is the preparation facilities schematic diagram of transition metal two chalcogenide monocrystalline.
Fig. 2 is the schema that transition metal two chalcogenide monocrystalline is prepared in chemical vapour deposition.
Fig. 3 is the optical photograph of the individual layer two tungsten selenide monocrystalline deposited in embodiment 1 on a quartz substrate.
Fig. 4 is the Raman spectrogram of the individual layer two tungsten selenide monocrystalline deposited in embodiment 1 on a quartz substrate.
Fig. 5 is the photoluminescence spectra figure of the individual layer two tungsten selenide monocrystalline deposited in embodiment 1 on a quartz substrate.
Fig. 6 is the atomic force microscope images of the individual layer two tungsten selenide monocrystalline deposited in embodiment 1 on a quartz substrate.
Fig. 7 is the Raman spectrogram of bilayer two tungsten selenide deposited in embodiment 2 on a quartz substrate.
Fig. 8 is the photoluminescence spectra figure of bilayer two tungsten selenide deposited in embodiment 2 on a quartz substrate.
Fig. 9 is the Raman spectrogram of the individual layer molybdenumdisulphide monocrystalline deposited in embodiment 3 on a quartz substrate.
Figure 10 is the photoluminescence spectra figure of the individual layer molybdenumdisulphide monocrystalline deposited in embodiment 3 on a quartz substrate.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described material all can obtain from open commercial sources if no special instructions.
The present invention adopts the elemental metals source and sulfur family simple substance source that are splashed in dielectric base, adopts chemical Vapor deposition process, on the surface of the substrate direct growth transition metal two chalcogenide monocrystalline.Specifically the dielectric base sputtering metal level is placed on the high-temperature zone (750 ~ 850 DEG C) of CVD stove, sulfur family simple substance source and absorption S/Se metal are placed on cold zone (650 ~ 750 DEG C); Before preparation, system does not need to vacuumize specially; In preparation process, pass into inertia protective gas, keep normal pressure, pass into hydrogen assisting growth simultaneously; By controlling growth conditions (as temperature, growth time etc.), high-quality transition metal two chalcogenide monocrystalline can be grown on the surface of the substrate.This preparation method adopts cost and method simple economy, is easy to control, and can prepare large-area high-quality two dimension transition metal two chalcogenide monocrystalline.
Embodiment 1: prepare individual layer two tungsten selenide monocrystalline
(1) with silicon cutter, quartz plate is cut into the square of 10 × 10mm, each ultrasonic cleaning 20 minutes in acetone, ethanol, water successively, then clean by washed with de-ionized water, and dry up with nitrogen.
(2) the quartz plate magnetron sputtering after cleaning sputters in front, and tungsten layer sputtering uses electronic anesthetic vaporizer (ULVAC, ACS-4000-C4) under a high vacuum, and be greater than the tungsten target of 99.95% by purity, sputtering time is 7 seconds.
(3) put into a new quartz boat by being equipped with the selenium powder that purity is 99.5%, quality is 0.03g, and this quartz boat is placed on the cold zone (the Single port position of CVD stove) of CVD stove one end, as shown in Figure 1.
(4) quartz plate sputtering tungsten layer is put into quartz boat, quartz boat is pushed into the high-temperature zone (middle part of CVD stove) of CVD stove silica tube, as shown in Figure 1.
(5) copper sheet absorbing selenium used is placed on selenium powder and has sputtered between the quartz plate of tungsten layer, and area is 1cm 2, as shown in Figure 1.
(6) pass in silica tube by high-purity argon gas, flow remains on 100sccm.
(7) CVD stove high-temperature zone was heated to 800 DEG C in 25 minutes, now cold zone temperature synchronously arrives 760 DEG C.Under the condition of 800 DEG C, high-temperature zone with 760 DEG C, cold zone, pass into high-purity hydrogen, flow remains on 10sccm, maintains 10 minutes.After reaction terminates, control the temperature of selenium source and quartz substrate and sputtering tungsten layer, make it to be cooled to 700 DEG C in 4 minutes.
(8) treat that CVD furnace temperature is down to 700 DEG C, open tube furnace lid regulation and control rate of temperature fall, make it to be cooled to 200 DEG C in 15 minutes.
(9) treat that whole silica tube is down to room temperature naturally, take out sample.
Opticmicroscope, Raman spectrum, fluorescence spectrum and atomic force microscope is adopted to carry out sample characterization.As can be seen from Figure 3, the two tungsten selenide monocrystalline obtained on a quartz substrate are triangular in shape, and trilateral average side length can reach more than 20 μm.In the Raman spectrum of simultaneously Fig. 4,248cm -1and 259cm -1the neighbouring characteristic peak occurring two tungsten selenide, at 306cm -1near there is not characteristic peak that is two-layer or multilayer, prove individual layer two tungsten selenide.Having a very strong peak at the photoluminescence spectra of Fig. 5 at 780nm place, is the characteristic peak of individual layer two tungsten selenide.In the atomic force microscope sign of Fig. 6, show delta-shaped region more significantly.These data all show, prepared sample is two tungsten selenide crystal of high-quality individual layer.
Embodiment 2: prepare double-deck two tungsten selenide
(1) with silicon cutter, quartz plate is cut into the square of 10 × 10mm, each ultrasonic cleaning 20 minutes in acetone, ethanol, water successively, then clean by washed with de-ionized water, and dry up with nitrogen.
(2) the quartz plate magnetron sputtering after cleaning sputters in front, and tungsten layer sputtering uses electronic anesthetic vaporizer (ULVAC, ACS-4000-C4) under a high vacuum, and be greater than the tungsten target of 99.95% by purity, sputtering time is 10 seconds.
(3) put into a new quartz boat by being equipped with the selenium powder that purity is 99.5%, quality is 0.05g, and this quartz boat is placed on the cold zone (the Single port position of CVD stove) of CVD stove one end, as shown in Figure 1.
(4) quartz plate sputtering tungsten layer is put into quartz boat, quartz boat is pushed into the high-temperature zone (middle part of CVD stove) of CVD stove silica tube, as shown in Figure 1.
(5) copper ring absorbing selenium used is placed between selenium powder and growth substrate, and area is 5cm 2.
(6) pass in silica tube by high-purity argon gas, flow remains on 150sccm.
(7) CVD stove high-temperature zone was heated to 810 DEG C in 30 minutes, now cold zone temperature synchronously arrives 765 DEG C.Under the condition of 810 DEG C, high-temperature zone with 765 DEG C, cold zone, pass into high-purity hydrogen, flow remains on 10sccm, maintains 10 minutes.After reaction terminates, control the temperature of selenium source and quartz substrate and sputtering tungsten layer, make it to be cooled to 700 DEG C in 5 minutes.
(8) treat that CVD furnace temperature is down to 700 DEG C, open tube furnace lid regulation and control rate of temperature fall, make it to be cooled to 200 DEG C in 15 minutes.
(9) treat that whole silica tube is down to room temperature naturally, take out sample.
Raman spectrum and photoluminescence spectra is adopted to carry out sample characterization.From the Raman spectrum of Fig. 7,248cm -1and 259cm -1the neighbouring characteristic peak occurring two tungsten selenide, at 306cm -1near there is the characteristic peak of two-layer or multilayer, the photoluminescence spectra of Fig. 8 has a very strong peak at 800nm place simultaneously, is the characteristic peak of double-deck two tungsten selenide, proves double-deck two tungsten selenide.
Embodiment 3: prepare individual layer molybdenumdisulphide monocrystalline
(1) with silicon cutter, quartz plate is cut into the square of 10 × 10mm, each ultrasonic cleaning 20 minutes in acetone, ethanol, water successively, then clean by washed with de-ionized water, and dry up with nitrogen.
(2) the quartz plate magnetron sputtering after cleaning sputters in front, and molybdenum layer sputtering uses electronic anesthetic vaporizer (ULVAC, ACS-4000-C4) under a high vacuum, and be greater than the molybdenum target of 99.95% by purity, sputtering time is 7 seconds.
(3) put into a new quartz boat by being equipped with the sulphur powder that purity is 99.5%, quality is 0.08g, and this quartz boat is placed on the cold zone (the Single port position of CVD stove) of CVD stove one end, as shown in Figure 1.
(4) quartz plate sputtering molybdenum layer is put into quartz boat, quartz boat is pushed into the high-temperature zone (middle part of CVD stove) of CVD stove silica tube, as shown in Figure 1.
(5) copper ring absorbing sulphur used is placed between sulphur powder and growth substrate, and area is 7cm 2.
(6) pass in silica tube by high-purity argon gas, flow remains on 80sccm.
(7) CVD stove high-temperature zone was heated to 790 DEG C in 25 minutes, now cold zone temperature synchronously arrives 755 DEG C.Under the condition of 790 DEG C, high-temperature zone with 755 DEG C, cold zone, pass into high-purity hydrogen, flow remains on 10sccm, maintains 10 minutes.After reaction terminates, control the temperature of sulphur source and quartz substrate and sputtering molybdenum layer, make it to be cooled to 680 DEG C in 7 minutes.
(8) treat that CVD furnace temperature is down to 680 DEG C, open tube furnace lid regulation and control rate of temperature fall, make it to be cooled to 200 DEG C in 14 minutes.
(9) treat that whole silica tube is down to room temperature naturally, take out sample.
Raman spectrum and photoluminescence spectra is adopted to carry out sample characterization.In the Raman spectrum of Fig. 9,385cm -1and 405cm -1near occur the characteristic peak of individual layer molybdenumdisulphide monocrystalline proving individual layer molybdenumdisulphide monocrystalline.The photoluminescence spectra of Figure 10 has a very strong peak at 675nm place simultaneously, is the characteristic peak of individual layer molybdenumdisulphide monocrystalline, proves individual layer molybdenumdisulphide monocrystalline.

Claims (10)

1. a preparation method for two-dimentional transition metal two chalcogenide monocrystalline, is characterized in that, comprise the steps:
(1), under high vacuum condition, dielectric base after cleaning sputters one deck transition metal nanoparticles layer;
(2) there is the dielectric base of transition metal nanoparticles layer to be placed on the high-temperature zone of CVD stove sputtering, the metal of sulfur family simple substance and absorption sulfur family simple substance is placed on cold zone;
(3) in atmosphere of inert gases, with the temperature rise rate of 15 DEG C/min ~ 45 DEG C/min, the high-temperature zone of CVD stove is heated to 750 DEG C ~ 850 DEG C, control cold zone temperature with the temperature rise rate of 15 DEG C/min ~ 45 DEG C/min simultaneously and synchronously arrive 700 DEG C ~ 780 DEG C, wherein, the temperature head of high-temperature zone and cold zone is 50 ~ 70 DEG C; Then pass into high-purity hydrogen, flow remains on 5sccm ~ 20sccm, maintains 5 minutes ~ 20 minutes; After reaction terminates, control the temperature of sulfur family simple substance source and dielectric base and transition metal nanoparticles layer, make three be cooled to 650 DEG C ~ 750 DEG C in 2 minutes ~ 8 minutes; Treat that CVD furnace temperature is down to 650 DEG C ~ 750 DEG C, regulation and control rate of temperature fall makes it in 10 minutes ~ 20 minutes, be cooled to 150 DEG C ~ 250 DEG C;
(4) treat that whole CVD stove is down to room temperature naturally, namely obtain two-dimentional transition metal two chalcogenide monocrystalline.
2. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: described dielectric base is silicon chip, quartz plate, sapphire or sheet mica.
3. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: described transition metal is Mo or W, its purity >=99.95%.
4. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: described sulfur family simple substance is S or Se.
5. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: described sputtering mode is: use electronic anesthetic vaporizer to sputter transition metal 5 to 25 seconds under a high vacuum.
6. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: the metal of described absorption sulfur family simple substance is at least one in nickel, cobalt, iron, aluminium, gold and silver, copper, zinc, molybdenum, tungsten, titanium, vanadium, chromium, ruthenium, rhodium, platinum, palladium, iridium.
7. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, is characterized in that: the temperature rise rate of high-temperature zone and cold zone is 30 DEG C/min.
8. the preparation method of two-dimentional transition metal two chalcogenide monocrystalline according to claim 1, it is characterized in that: the cleaning step of described dielectric base is: by dielectric base each ultrasonic cleaning 20 minutes in acetone, ethanol, water successively, then clean by washed with de-ionized water, and dry up with nitrogen.
9. a two-dimentional transition metal two chalcogenide monocrystalline, is characterized in that: prepared by the preparation method of the arbitrary described two-dimentional transition metal two chalcogenide monocrystalline of claim 1-8.
10. two-dimentional transition metal two chalcogenide monocrystalline according to claim 9 is as the application of two-dimensional film material.
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