CN109183156A - A kind of disulphide monocrystalline and its preparation method and application - Google Patents
A kind of disulphide monocrystalline and its preparation method and application Download PDFInfo
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- CN109183156A CN109183156A CN201811324860.5A CN201811324860A CN109183156A CN 109183156 A CN109183156 A CN 109183156A CN 201811324860 A CN201811324860 A CN 201811324860A CN 109183156 A CN109183156 A CN 109183156A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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Abstract
The present invention relates to a kind of disulphide monocrystalline and its preparation method and application, the preparation method includes: (1) in the tube furnace that middle part has heating device, along the direction of air-flow, sulfur family simple substance source and the transition metal oxide source for being mixed with sodium chloride are being accounted at the 25~35% of tube furnace total length and placed at 45~55% apart from tube furnace inlet end distance respectively；Growth substrate is placed with above the transition metal oxide source；(2) it is passed through protective gas into the tube furnace, the temperature that tube furnace is warming up to chemical vapor deposition is then subjected to chemical vapor deposition.The disulphide monocrystalline of highly crystalline quality, super large crystal domain size is obtained by the method.The disulphide monocrystalline is applied to any one in nano-device, optical device and on piece laser or at least two combinations.
Description
Technical field
The present invention relates to electronics and field of photoelectric technology more particularly to a kind of disulphide monocrystalline and preparation method thereof and use
On the way.
Background technique
Transition-metal dichalcogenide (TMDs) has similar structure with graphene, but has oneself unique photo electric
Matter due to the presence of its band gap, and has preferable mobility value and on-off ratio simultaneously, partly leads in photoelectric device and P-N junction
There is outstanding performance in body, so receiving the favor of numerous researchers.In recent years, it has been found that two-dimentional transition metal sulfur family
Compound includes molybdenum disulfide, tungsten disulfide, two selenizing molybdenums, two tungsten selenides, two selenizing niobiums etc., metallicity, semiconductive and
The advantage that superconductivity etc. shows is particularly evident, has in nano-device, optical device and on piece laser wide
Application prospect.
The performance of the high quality Transition-metal dichalcogenide of super large crystal domain size is more excellent, therefore, controls super large ruler
The synthesis of very little two dimension disulphide monocrystalline is the key that it carries out subsequent basic research and device application, and to its energy band knot
The research of the physical characteristics such as structure, energy valley has important value to condensed state physics and opto-electronics.But at present also
There is some challenges, that is, hardly result in the disulphide monocrystalline of super large crystal domain size.
CN108118395A discloses a kind of method that chemical vapor deposition prepares two tungsten selenide monocrystal thin films, this method packet
Include: using the oxide powder of tungsten, halide salt, selenium powder as raw material, inert gas is carrier gas, and raw material is flashed to gaseous state and is transported to
Deposition on substrate grows two selenizing W films.Pass through the means such as control raw material proportioning, growth temperature, growth time, carrier gas flux
Control film thickness.Using the method, can under hydrogen free environment, under 600~800 degrees Celsius growth obtain 50 μm with
Two selenizing W films upper, the number of plies is controllable, but the size of two obtained tungsten selenide monocrystalline is only 50 μm, and it is brilliant that super large is not implemented
The preparation of the disulphide monocrystalline of farmland size.
CN105002476A discloses a kind of side of the chemical gas-phase method growing large-size single layer molybdenum disulfide of substrate modification
Method.To vulcanize ammonia as substrate surface dressing agent, controlled by means such as the concentration, soaking time, cleaning method of controlled modification agent
Nucleation rate controls film thickness by means such as growth temperature, growth time, the throughputs of control chemical vapor deposition.It utilizes
The present invention can on the basis of original growth chemical vapor depsotition equipment, under the conditions of relatively low growth temperature, efficiently
Growing large-size single-layer molybdenum disulfide film, but the full-size of the single-layer molybdenum disulfide film is only 100 μm.
CN104846434A discloses two chalcogenide monocrystalline of a kind of two-dimentional transition metal and its preparation method and application.
It in an inert atmosphere, can be with S or Se in sulfur family simple substance (S, Se) metal reacted and hydrogen auxiliary control system by common
Concentration, with achieve the purpose that control transition metal layer vulcanization or selenizing degree, controllably given birth to using chemical vapor deposition method
Long monocrystalline；It is 750 DEG C to 850 DEG C by temperature control when depositing, and sedimentation time control is 5 to 15 minutes, completes TMDs
The preparation of monocrystalline；Wherein by substrate sputter processing method, sulfur family elemental powders dosage and S/Se metallic area and type,
The optimization of the preparation parameters such as density of hydrogen, growth temperature, growth time is realized to two sulfur family chemical combination of high quality two dimension transition metal
The strict control of object mono-crystalline structures, but the size of obtained TMDs monocrystalline only has 20 μm or so, and size is smaller.
Therefore, large scale how is obtained, the disulphide monocrystalline of high quality becomes the field urgent problem to be solved.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of preparation sides of disulphide monocrystalline
Method, the preparation method include the following steps:
(1) in the tube furnace that middle part has heating device, along the direction of air-flow, sulfur family simple substance source and transition are placed respectively
Metal oxide source；Growth substrate is placed with above the transition metal oxide source；In the transition metal oxide source
It is mixed with sodium chloride；
(2) it is passed through protective gas into the tube furnace, then tube furnace is warming up to the temperature of chemical vapor deposition
Carry out deposition growing；
In the tube furnace, sulfur family simple substance source accounted at a distance from tube furnace inlet end tube furnace total length 25~
35%, such as 26%, 28%, 30%, 32% etc., it is total that transition metal oxide source accounts for tube furnace at a distance from tube furnace inlet end
Length 45~55%, such as 48%, 50%, 52% etc..
It is accounting at the 45~55% of tube furnace total length apart from tube furnace inlet end distance and is being placed at 25~35% respectively
Transition metal oxide source and sulfur family simple substance source, so that the temperature and sulfur family of deposition growing occur at transition metal oxide source
The transmission range that optimum temperature difference and sulfur family simple substance are formed between the temperature of simple substance source evaporation, is conducive to disulphide monocrystalline
Growth.
The present invention, which is reacted using NaCl with transition metal oxide, generates lower melting-point oxychloride offer continuous transition
Source metal supply, to be conducive to the extension of crystal domain size, can obtain the single-layer or multi-layer two of super large crystal domain size, high quality
Sulfide single crystal.
Preferably, the temperature of the chemical vapor deposition is 800~1150 DEG C, such as 800 DEG C, 850 DEG C, 900 DEG C, 950
DEG C, 1000 DEG C, 1100 DEG C etc..
Preferably, the temperature of the chemical vapor deposition is 1000~1150 DEG C.
The temperature of the chemical vapor deposition is the temperature at transition metal oxide source, which can be equal to tubular type
The temperature of furnace.
The temperature of chemical vapor deposition is set as 800~1150 DEG C, especially 1000~1150 DEG C, is cooperated sulfur family simple substance
Source, which is placed in, to be accounted at the 25~35% of tube furnace total length apart from tube furnace inlet end distance, places transition metal oxide source
Accounted at the 45~55% of tube furnace total length in apart from tube furnace inlet end distance, the effect that can be optimal, be due to compared with
High temperature is easier source amount volatilization, while providing higher energy, cooperation transition metal oxide source and sulfur family simple substance source
Preference temperature difference and sulfur family simple substance transmission range, the growth of disulphide monocrystalline is more advantageous to, thus two sulphur made
Compound monocrystalline has biggish crystal domain size (reaching as high as 0.57mm) and higher edge sharpness, and temperature is lower than 800 DEG C, source amount
Volatilization is difficult, and the size of obtained disulphide monocrystalline is smaller, but when temperature is higher than 1150 DEG C, excessively high temperature may band
Carry out some side reactions.
Preferably, the heating rate of the tube furnace be 25~35 DEG C/min, such as 26 DEG C/min, 28 DEG C/min, 30 DEG C/
Min, 33 DEG C/min etc..
Preferably, in the transition metal oxide source, the mass ratio of transition metal oxide and sodium chloride is 5~15:
1, such as 5:1,6:1,7:1,8:1,9:1,10:1,11:1,12:1,13:1,14:1 etc., preferably 9:1.
When the mass ratio of transition metal oxide and sodium chloride is within the scope of 5~15:1, when especially for 9:1, provide
Transition metal oxide source vapour pressure is suitable, is conducive to the transmission and diffusion in source, thus promote the nucleation and growth of disulphide,
The disulphide monocrystalline that crystal domain size is up to 0.57mm can be obtained, the ratio of sodium chloride is excessive, the transiting metal oxidation provided
Material resource is excessive, causes nucleation excessive, inhibits the growth of large scale farmland area crystal, forms thick-layer sample；Sodium chloride ratio is too small, no
Enough transition metal oxide sources are enough to provide, it is slow so as to cause the transmission and diffusion in source, it is unfavorable for forming large scale crystalline substance
Body.
Preferably, the transition metal oxide includes WO3、MoO3、Ta2O5And Nb2O5In any one, preferably WO3。
Preferably, the WO3Powder 80~500 mesh of partial size, such as 90 mesh, 100 mesh, 120 mesh, 200 mesh, 300 mesh,
400 mesh, 500 mesh etc., preferably 100 mesh.
Preferably, the transition metal oxide source is placed in cube crucible, and the growth substrate is covered at described cube
The top of body crucible, and retain gap, enter for air-flow.
Preferably, the area in the gap accounts for the 10~20% of cube crucible open area, for example, 11%, 12%, 15%,
18% etc..
Preferably, the protective gas includes hydrogen and/or argon gas, preferably argon gas and hydrogen.
Preferably, the flow of the argon gas be 20~50sccm, such as 21sccm, 25sccm, 30sccm, 35sccm,
40sccm、45sccm、48sccm。
Preferably, the flow of the hydrogen is 5~15sccm, such as 6sccm, 8sccm, 10sccm, 12sccm, 14sccm
Deng preferably 5sccm.
Preferably, the sulfur family simple substance includes Se simple substance and/or S simple substance, preferably Se simple substance.
Preferably, the diameter of particle of the sulfur family simple substance is 100~300 mesh, such as 120 mesh, 150 mesh, 200 mesh, 250 mesh
Deng.
Preferably, the protective gas includes argon gas and hydrogen, and the flow of the hydrogen is 5~15sccm, such as
6sccm, 8sccm, 10sccm, 12sccm, 14sccm etc., preferably 5sccm, the flow of the argon gas are 20~50sccm.
Preferably, the transition metal oxide is WO3, the sulfur family simple substance is Se simple substance, the chemical vapor deposition
Temperature be 800-1050 DEG C, such as 800 DEG C, 820 DEG C, 850 DEG C, 1000 DEG C etc., preferably 1000~1050 DEG C.
When transition metal oxide is WO3, when sulfur family simple substance is Se simple substance, the temperature of chemical vapor deposition is controlled 800
Within the scope of~1050 DEG C, this is because the temperature range is conducive to provide transition more appropriate under the premise of NaCl auxiliary
Metal oxide source vapour pressure can reach optimal effect at this time, can obtain the single-layer or multi-layer of oversize, high quality
WSe2Monocrystalline.
The protective gas includes argon gas and hydrogen, and the flow of the hydrogen is 5~15sccm, such as 6sccm,
8sccm, 10sccm, 12sccm, 14sccm etc., preferably 5sccm, the flow of the argon gas are 20~50sccm, such as 21sccm,
25sccm, 30sccm, 35sccm, 40sccm, 45sccm, 48sccm etc.；
The partial size of the powder of the Se simple substance is 200 mesh；
The WO3Powder partial size be 100 mesh.
Preferably, the protective gas includes hydrogen and/or argon gas, preferably hydrogen and argon gas.
Preferably, in the tube furnace, placing the temperature at sulfur family simple substance source is 120~350 DEG C, such as 125 DEG C, 150
DEG C, 200 DEG C, 250 DEG C, 300 DEG C, 330 DEG C etc..
Preferably, the sulfur family simple substance is Se simple substance, and the temperature placed at sulfur family simple substance source is 220~350 DEG C, example
Such as 250 DEG C, 300 DEG C, 330 DEG C, preferably 300 DEG C.
Preferably, the cube crucible includes cube ceramic crucible.
Preferably, the sulfur family simple substance is placed in cube silica crucible.
Preferably, the growth substrate includes that one layer of amorphous Si O is contained on surface2Silicon wafer.
Preferably, the SiO2With a thickness of 220~300nm, such as 230nm, 240nm, 250nm, 270nm, 300nm
Deng preferably 300nm.
Preferably, the time of the chemical vapor deposition be 3~15min, such as 4min, 5min, 6min, 7min, 8min,
9min, 10min, 11min, 12min, 15min etc..
Preferably, the mass ratio of the sulfur family simple substance and the transition metal oxide and sodium chloride mixed-powder be 4~
6:1, such as 4.5:1,5:1,5.5:1 etc., preferably 5:1.
Preferably, the preparation method includes the following steps:
(1) middle part have heating device tube furnace in, along the direction of air-flow, respectively apart from tube furnace inlet end away from
The silica crucible for the Se simple substance powder that partial size is 200 mesh is placed at account for tube furnace total length 25~35%, with a distance from
Tube furnace inlet end distance accounts at tube furnace total length 45~55% WO for being placed with that the partial size containing sodium chloride is 100 mesh3
The growth substrate is covered the top in the cube ceramic crucible by the cube ceramic crucible of powder, and is retained and accounted for cube
10~20% gap of body ceramic crucible open area enters for air-flow；
The mass ratio of the transition metal oxide and sodium chloride is 9:1；
The mass ratio of the sulfur family simple substance and the transition metal oxide and sodium chloride mixed-powder is 4~6:1；
(2) hydrogen that flow is 5~15sccm is passed through into the tube furnace, by tube furnace with 25~35 DEG C/min rate
1000~1150 DEG C are warming up to, 3~15min of chemical vapor deposition is carried out；It is described place Se simple substance source at temperature be 220~
350℃。
The second object of the present invention is to provide a kind of disulphide that the preparation method according to the first purpose obtains
Monocrystalline, 0.1mm≤disulphide monocrystalline crystal domain size≤0.57mm, such as 0.15mm, 0.18mm, 0.20mm,
0.25mm, 0.30mm, 0.35mm, 0.40mm, 0.45mm, 0.50mm, 0.56mm etc..
The disulphide monocrystalline has biggish crystal domain size, and photoelectric properties are more excellent.
Preferably, the disulphide monocrystalline with a thickness of 0.7~5.8nm, such as 0.8nm, 1.5nm, 2.1nm,
2.7nm, 3.5nm, 4.3nm, 5.1nm etc..
It is single layer disulphide monocrystalline when thickness is within the scope of 0.7~0.9nm, is multilayer two as thickness 1.2nm
Sulfide single crystal.
Preferably, the disulphide monocrystalline includes single layer disulphide monocrystalline and multilayer disulphide monocrystalline, preferably singly
Layer disulphide monocrystalline.
Preferably, the disulphide monocrystalline includes WSe2Monocrystalline, WS2Monocrystalline, MoS2Monocrystalline, MoSe2Monocrystalline, TaS2It is single
Brilliant, TaSe2Monocrystalline, NbS2Monocrystalline or NbSe2Any one in monocrystalline.
Preferably, the disulphide monocrystalline includes single layer WSe2Monocrystalline.
The third object of the present invention is to provide a kind of purposes of disulphide monocrystalline described in the second purpose, two sulphur
Compound monocrystalline is used for any one in nano-device, optical device and on piece laser or at least two combinations.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention respectively account at the 45~55% of tube furnace total length apart from tube furnace inlet end distance with 25~
Transition metal oxide source and sulfur family simple substance source are placed at 35%, so that deposition growing occurs at transition metal oxide source
The transmission range of optimum temperature difference and sulfur family simple substance is formed between temperature and the temperature of sulfur family simple substance source evaporation, cooperation utilizes
NaCl is reacted with transition metal oxide generates lower melting-point oxychloride offer continuous transition source metal supply, thus favorably
In the extension of crystal domain size, super large crystal domain size (reaching as high as 0.57mm), edge sharpness higher single layer or more can be obtained
Layer disulphide monocrystalline.
(2) in a preferred approach, the temperature of chemical vapor deposition is set as 800~1150 DEG C, especially 1000~1150
DEG C, higher temperature is easier source amount volatilization, while providing higher energy, cooperates selected sulfur family simple substance source and transition metal
The placement location of oxide source reaches more preferably effect, so that the disulphide monocrystalline made has biggish crystal domain size
(reaching as high as 0.57mm) and higher edge sharpness.
(3) in a preferred approach, when the mass ratio of transition metal oxide and sodium chloride is 5~15:1, specifically for 9:1
When, the cooperation of NaCl and transition metal oxide reaches optimum efficiency, and super large crystal domain size can be prepared and (reach as high as
Disulphide monocrystalline 0.57mm).
Detailed description of the invention
Fig. 1 is single layer WSe prepared by embodiment 12The optical picture of sample.
Fig. 2 is few layer of WSe prepared by embodiment 12The optical picture of sample.
Fig. 3 is single layer WSe prepared by embodiment 12The AFM of sample schemes.
Fig. 4 is WSe prepared by comparative example 12The optical picture of sample.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
Prepare disulphide monocrystalline:
(1) middle part have heating device tube furnace in, along the direction of air-flow, respectively apart from tube furnace inlet end away from
The silica crucible for the Se simple substance powder that 50mg partial size is 200 mesh is placed at account for tube furnace total length 30%, with a distance from
Tube furnace inlet end distance accounts at tube furnace total length 50% WO for being placed with that the partial size containing sodium chloride is 100 mesh3Powder
(wherein, sodium chloride 1mg, WO3Surface is contained one layer of 300nm and is altogether unjustifiable crystalline state S by cube ceramic crucible 9mg)iO2Silicon substrate
Bottom cover retains 15% gap for accounting for cube crucible open area in the top of the cube ceramic crucible, is used for air-flow
Into；
(2) be passed through into the tube furnace flow be 5sccm hydrogen and 20sccm argon gas, by tube furnace with 30 DEG C/
The rate of min is warming up to 1050 DEG C, makes 300 DEG C of temperature at Se simple substance source, keeps temperature 15min, carries out chemical gaseous phase
Deposition.After, using polymethyl methacrylate (PMMA) by WSe2Sample is transferred on copper mesh, to carry out subsequent table
Sign.
Fig. 1, Fig. 3 are the WSe of the present embodiment2The optical picture of monocrystalline, Fig. 1 are single layer WSe2Monocrystalline, Fig. 3 are few layer WSe2It is single
Crystalline substance, as seen from the figure WSe2The size of monocrystalline all has higher edge sharpness up to 0.57mm.
Fig. 2 is the WSe for being the present embodiment2The AFM of monocrystalline schemes, and afm image height is 0.80nm, it was demonstrated that the WSe2Monocrystalline is
Single layer structure.
Embodiment 2
The difference from embodiment 1 is that tube furnace is warming up to 1150 DEG C.
Embodiment 3
The difference from embodiment 1 is that tube furnace is warming up to 800 DEG C
Embodiment 4
The difference from embodiment 1 is that tube furnace is warming up to 1000 DEG C.
Embodiment 5
The difference from embodiment 1 is that sodium chloride 1.65mg, WO3For 8.35mg.
Embodiment 6
The difference from embodiment 1 is that sodium chloride 0.6mg, WO3For 9.4mg.
Embodiment 7
The difference from embodiment 1 is that sodium chloride 3mg, WO3For 7mg.
Embodiment 8
The difference from embodiment 1 is that sodium chloride 0.45mg, WO3For 9.55mg.
Embodiment 9
The difference from embodiment 1 is that the partial size of the powder of Se simple substance is 100 mesh, WO3Powder partial size be 80 mesh.
Embodiment 10
The difference from embodiment 1 is that the partial size of the powder of Se simple substance is 300 mesh, WO3Powder partial size be 500 mesh.
Embodiment 11
Prepare disulphide monocrystalline:
(1) middle part have heating device tube furnace in, along the direction of air-flow, respectively apart from tube furnace inlet end away from
It is placed with the silica crucible for the S simple substance powder that 40mg partial size is 100 mesh at account for tube furnace total length 25%, is managed with a distance from
Formula furnace inlet end distance accounts at the 45% of tube furnace total length the MoO for being placed with that the partial size containing sodium chloride is 400 mesh3Powder
(wherein, sodium chloride 1mg, MoO3Cube ceramic crucible 9mg) will be covered with the S of one layer of 220nm thicknessiO2Silicon substrate bottom cover
In the top of the cube ceramic crucible, and retain 10% gap for accounting for cube crucible open area, enters for air-flow；
(2) it is passed through the argon gas that flow is 60sccm into the tube furnace, tube furnace is heated up with the rate of 25 DEG C/min
To 800 DEG C, make 120 DEG C of temperature at S simple substance source, keep temperature 3min, carries out chemical vapor deposition.After, it utilizes
Polymethyl methacrylate (PMMA) is by MoO3Sample is transferred on copper mesh, to carry out subsequent characterization.
Embodiment 12
Prepare disulphide monocrystalline:
(1) middle part have heating device tube furnace in, along the direction of air-flow, respectively apart from tube furnace inlet end away from
The silica crucible for the Se simple substance powder that 60mg partial size is 200 mesh is placed at account for tube furnace total length 35%, with a distance from
Tube furnace inlet end distance accounts at the 55% of tube furnace total length the Nb for being placed with that the partial size containing sodium chloride is 300 mesh2O5Powder
Body (wherein, sodium chloride 1mg, Nb2O5Cube ceramic crucible 9mg) will be covered with the S of one layer of 300nm thicknessiO2Silicon base
Cover the top in the cube ceramic crucible, and retain 20% gap for accounting for cube crucible open area, for air-flow into
Enter；
(2) be passed through into the tube furnace flow be 15sccm hydrogen and 50sccm argon gas, by tube furnace with 35 DEG C/
The rate of min is warming up to 1000 DEG C, makes 220 DEG C of temperature at Se simple substance source, keeps temperature 15min, carries out chemical gaseous phase
Deposition.After, using polymethyl methacrylate (PMMA) by NbSe2Sample is transferred on copper mesh, subsequent to carry out
Characterization.
Embodiment 13
Prepare disulphide monocrystalline:
(1) middle part have heating device tube furnace in, along the direction of air-flow, respectively apart from tube furnace inlet end away from
The silica crucible for the Se simple substance powder that 60mg partial size is 200 mesh is placed at account for tube furnace total length 25%, with a distance from
Tube furnace inlet end distance accounts at the 55% of tube furnace total length the Nb for being placed with that the partial size containing sodium chloride is 300 mesh2O5Powder
Body (wherein, sodium chloride 1mg, Nb2O5Cube ceramic crucible 9mg) will be covered with the SiO of one layer of 270nm thickness2Silicon base
Cover the top in the cube ceramic crucible, and retain 20% gap for accounting for cube crucible open area, for air-flow into
Enter；
(2) be passed through into the tube furnace flow be 10sccm hydrogen and 50sccm argon gas, by tube furnace with 35 DEG C/
The rate of min is warming up to 1100 DEG C, makes 350 DEG C of temperature at Se simple substance source, keeps temperature 20min, carries out chemical gaseous phase
Deposition.After, using polymethyl methacrylate (PMMA) by NbSe2Sample is transferred on copper mesh, subsequent to carry out
Characterization.
Comparative example 1
The difference from embodiment 1 is that not adding sodium chloride.
The WSe that this comparative example obtains2The optical picture of sample as shown in figure 4, it can be seen from the figure that the size of the monocrystalline compared with
It is small, about 15 μm or so, and it is in irregular shape, edge sharpness is lower, and single layer accounting is seldom, and the sample of preparation is mostly thick-layer.
Comparative example 2
The difference from embodiment 1 is that accounted for apart from tube furnace inlet end distance tube furnace total length 23% at place
It is placed with the silica crucible for the Se simple substance powder that 50mg partial size is 200 mesh.
Comparative example 3
The difference from embodiment 1 is that being put being accounted at tube furnace total length 58% apart from tube furnace inlet end distance
Having the partial size containing sodium chloride is the WO of 100 mesh3The cube ceramic crucible of powder.
Performance test
(1) pattern of prepared disulphide single crystal samples is characterized using Olympus BX51 optical microscopy.
(2) thickness of Bruker ICON atomic force microscope characterization disulphide single crystal samples is utilized.
The performance test results are as shown in table 1.
1 the performance test results of table
| Crystal domain size/μm | The number of plies | Pattern | |
| Embodiment 1 | 570 | Single layer/few layer | Triangle |
| Embodiment 2 | 600 | Single layer/few layer | Triangle |
| Embodiment 3 | 50 | Single layer | Triangle |
| Embodiment 4 | 400 | Single layer/few layer | Triangle |
| Embodiment 5 | 100 | Single layer/few layer | Triangle |
| Embodiment 6 | 400 | Single layer/few layer | Triangle |
| Embodiment 7 | 50 | Few layer/thick-layer | Triangle |
| Embodiment 8 | 180 | Single layer/few layer/thick-layer | Triangle |
| Embodiment 9 | 500 | Single layer/few layer | Triangle |
| Embodiment 10 | 500 | Single layer/few layer | Triangle |
| Embodiment 11 | 280 | Single layer/few layer/thick-layer | Triangle |
| Embodiment 12 | 200 | Single layer/few layer | Triangle |
| Embodiment 13 | 450 | Single layer/few layer/thick-layer | Triangle |
| Comparative example 1 | 15 | Single layer/few layer/thick-layer | Triangle |
| Comparative example 2 | 40 | Single layer/few layer | Triangle |
| Comparative example 3 | 30 | Single layer/few layer | Triangle |
Note: single layer monocrystalline with a thickness of 0.6~1nm, few layer monocrystalline with a thickness of 1~10nm, the thickness of thick-layer monocrystalline is big
In 10nm.
As shown in Table 1, by comparing embodiment and comparative example it is found that disulphide single crystal domains ruler prepared by implementation column
Very little entirety is greater than comparative example, tends to the growth of single layer or few layer crystal body, and edge sharpness higher (Fig. 1 and Fig. 4) this be by
It is accounting at the 45~55% of tube furnace total length apart from tube furnace inlet end distance and is being placed at 25~35% respectively in the present invention
Transition metal oxide source and sulfur family simple substance source, so that the temperature and sulfur family of deposition growing occur at transition metal oxide source
The transmission range of optimum temperature difference and sulfur family simple substance is formed between the temperature of simple substance source evaporation, furthermore the presence of NaCl makes
The steam of transition metal oxide source supplies abundance, and the two collectively promotes nucleation and growth.Comparative example 1~4 is it is found that when temperature
When degree is 1000~1150 DEG C, the disulphide single crystal domains size of preparation is up to inferior centimeter order, this is because the temperature range
It is conducive to provide sufficient source supply, transmission and diffusion, to promote sample grown.Comparison example 1,5~8 is it is found that ratio is 5
When~15:1, the disulphide sample size of preparation is influenced by NaCl accounting, and when 9:1, obtained size is maximum, this is because should
Ratio can make the vapour pressure of transition metal oxide source be maintained at a suitable state, not only improve the transmission and expansion in source
It dissipates, and not will lead to source excessively to lead to the growth of thick-layer sample.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of preparation method of disulphide monocrystalline, which is characterized in that the preparation method includes the following steps:
(1) in the tube furnace that middle part has heating device, along the direction of air-flow, sulfur family simple substance source and transition metal are placed respectively
Oxide source；Growth substrate is placed with above the transition metal oxide source；It is mixed in the transition metal oxide source
Sodium chloride；
(2) it is passed through protective gas into the tube furnace, then carries out the temperature that tube furnace is warming up to chemical vapor deposition
Deposition growing；
In the tube furnace, sulfur family simple substance source accounts for the 25~35% of tube furnace total length, mistake at a distance from tube furnace inlet end
It crosses metal oxide source and accounts for tube furnace total length 45~55% at a distance from tube furnace inlet end.
2. preparation method according to claim 1, which is characterized in that the temperature of the chemical vapor deposition be 800~
1150℃；
Preferably, the temperature of the chemical vapor deposition is 1000~1150 DEG C；
Preferably, the heating rate of the tube furnace is 25~35 DEG C/min.
3. preparation method according to claim 1 or 2, which is characterized in that in the transition metal oxide source, transition gold
The mass ratio for belonging to oxide and sodium chloride is 5~15:1, preferably 9:1；
Preferably, the transition metal oxide includes WO3、MoO3、Ta2O5And Nb2O5In any one, preferably WO3；
Preferably, the WO3Powder partial size be 80~500 mesh, preferably 100 mesh；
Preferably, the transition metal oxide source is placed in cube crucible, and the growth substrate is covered in the cube earthenware
The top of crucible, and retain gap, enter for air-flow；
Preferably, the area in the gap accounts for the 10~20% of cube crucible open area.
4. preparation method described in any one of claim 1 to 3, which is characterized in that the protective gas includes hydrogen
Gas and/or argon gas, preferably argon gas and hydrogen；
Preferably, the flow of the argon gas is 20~50sccm；
Preferably, the flow of the hydrogen is 5~15sccm, preferably 5sccm.
5. preparation method according to any one of claims 1 to 4, which is characterized in that the sulfur family simple substance includes Se mono-
Matter and/or S simple substance, preferably Se simple substance；
Preferably, the diameter of particle of the sulfur family simple substance is 100~300 mesh；
Preferably, the protective gas includes argon gas and hydrogen, and the flow of the hydrogen is 5~15sccm, preferably 5sccm,
The flow of the argon gas is 20~50sccm.
6. preparation method according to any one of claims 1 to 5, which is characterized in that the transition metal oxide is
WO3, the sulfur family simple substance is Se simple substance, and the temperature of the chemical vapor deposition is 800~1050 DEG C, preferably 1000~1050
℃；
The protective gas includes argon gas and hydrogen, and the flow of the hydrogen is 5~15sccm, preferably 5sccm, the argon gas
Flow be 20~50sccm；
The partial size of the powder of the Se simple substance is 200 mesh；
The WO3Powder partial size be 100 mesh.
7. preparation method described according to claim 1~any one of 6, which is characterized in that in the tube furnace, place sulfur family
Temperature at simple substance source is 120~350 DEG C；
Preferably, the sulfur family simple substance is Se simple substance, and the temperature placed at sulfur family simple substance source is 220~350 DEG C, preferably
300℃；
Preferably, the cube crucible includes cube ceramic crucible；
Preferably, the sulfur family simple substance is placed in cube silica crucible；
Preferably, the growth substrate includes that one layer of amorphous Si O is contained on surface2Silicon wafer；
Preferably, the SiO2With a thickness of 220~300nm, preferably 300nm；
Preferably, the time of the chemical vapor deposition is 3~15min, preferably 10min；
Preferably, the mass ratio of the sulfur family simple substance and the transition metal oxide and sodium chloride mixed-powder is 4~6:1,
It is preferred that 5:1.
8. preparation method according to any one of claims 1 to 7, which is characterized in that the preparation method includes as follows
Step:
(1) it in the tube furnace that middle part has heating device, along the direction of air-flow, is accounted for respectively apart from tube furnace inlet end distance
The silica crucible for the Se simple substance powder that partial size is 200 mesh is placed at the 25~35% of tube furnace total length, apart from tubular type
Furnace inlet end distance accounts at tube furnace total length 45~55% WO for being placed with that the partial size for being mixed with sodium chloride is 100 mesh3Powder
Cube ceramic crucible, the growth substrate is covered into the top in the cube ceramic crucible, and retain and account for cube pottery
10~20% gap of porcelain crucible open area enters for air-flow；
The mass ratio of the transition metal oxide and sodium chloride is 9:1；
The mass ratio of the sulfur family simple substance and the transition metal oxide and sodium chloride mixed-powder is 4~6:1；
(2) it is 20~50sccm that hydrogen that flow is 5~15sccm and flow are passed through into the tube furnace, by tube furnace with 25
~35 DEG C/min rate is warming up to 1000~1150 DEG C, carries out 3~15min of chemical vapor deposition, at placement Se simple substance source
Temperature be 220~350 DEG C.
9. it is a kind of according to claim 1~any one of 8 described in the obtained disulphide monocrystalline of preparation method, feature exists
In 0.1mm≤disulphide monocrystalline crystal domain size≤0.57mm；
Preferably, the disulphide monocrystalline with a thickness of 0.7~5.8nm；
Preferably, the disulphide monocrystalline includes single layer disulphide monocrystalline and multilayer disulphide monocrystalline, preferred single layer two
Sulfide single crystal；
Preferably, the disulphide monocrystalline includes WSe2Monocrystalline, WS2Monocrystalline, MoS2Monocrystalline, MoSe2Monocrystalline, TaS2Monocrystalline,
TaSe2Monocrystalline, NbS2Monocrystalline or NbSe2Any one in monocrystalline；
Preferably, the disulphide monocrystalline includes single layer WSe2Monocrystalline.
10. a kind of purposes of disulphide monocrystalline according to claim 9, which is characterized in that the disulphide monocrystalline
For in nano-device, optical device and on piece laser any one or at least two combination.
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