CN105839072A - Method for preparing rhenium disulfide thin film through chemical vapor deposition - Google Patents
Method for preparing rhenium disulfide thin film through chemical vapor deposition Download PDFInfo
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- CN105839072A CN105839072A CN201610243559.6A CN201610243559A CN105839072A CN 105839072 A CN105839072 A CN 105839072A CN 201610243559 A CN201610243559 A CN 201610243559A CN 105839072 A CN105839072 A CN 105839072A
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- rhenium
- thin film
- rhenium disulfide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing a rhenium disulfide thin film through chemical vapor deposition. According to the method, a two-element eutectoid alloy formed by a mixture of rhenium powder and tellurium powder is used as a rhenium source, powdered sulfur is used as a sulfur source, mica is used as a growth substrate, and the two-dimensional rhenium disulfide thin film grows under the argon atmosphere at the temperature ranging from 500 DEG C to 900 DEG C. Compared with an existing rhenium disulfide preparation method, the requirement for device conditions is low, the operation process is simple, the method has the beneficial effects of being low in reaction temperature, high in growth efficiency, even in layer number, high in lattice quality of the obtained product and good in controllability, large-area, high-quality and layer-number-controllable controlled growth of rhenium disulfide is achieved, and a reliable sample preparation method is provided for application of rhenium disulfide in the field of electronic and photoelectron devices.
Description
Technical field
The invention belongs to two-dimension nano materials preparing technical field, be specifically related to a kind of side preparing rhenium disulfide thin film
Method.
Background technology
Optics, electricity, calorifics and the mechanical property of two-dimensional atomic crystal material excellence make it at future electronic, photoelectricity
The fields such as son, energy storage device and catalysis are with a wide range of applications, and rapidly become the study hotspot of Material Field.
Wherein, anisotropy two-dimensional material rhenium disulfide (ReS2) it is " nova " of two-dimensional material family in recent years.
ReS2Unique lattice structure imparts its many outstanding character, and Density function theory shows, monolayer
ReS2For the 1T phase of distortion, this special structure makes this material have anisotropy, and can produce Pei Ersi
Distortion, this distortion will stop ReS2Orderly accumulation, and the overlapping of interlayer electron wave function is minimized,
Thus cause interlayer uncoupling.Research shows, from multilamellar to monolayer, and ReS2Remain direct band gap, band gap magnitude
Change the least, and Raman spectrum also will not have significant change with the change of the number of plies.The character of these excellences makes it
In fields such as future chips, information storage and photoelectric devices, there is good application prospect.
At present, overwhelming majority research work is all to use micromechanics stripping method and liquid phase chemical stripping method to prepare two dimension
ReS2Thin film.Though these methods are obtained in that ReS2Thin film, but the ReS obtained2Film dimensions is little, and size and
THICKNESS CONTROL is poor, it is impossible to realize following extensive device application.Chemical gaseous phase deposition (CVD) is considered as
A kind of effective technology preparing large-area high-quality two-dimensional material, but due to ReS2The particularity of material self is logical
Cross traditional CVD technology to prepare this material and there is also a lot of difficulty.The whole world only has two work to utilize at present
CVD technology has prepared two-dimentional ReS2Material, and all there is the biggest problem in prepared sample.One is with height
Rehenic acid amine (NH4ReO4) it is that Re source grows ReS2, but the by-product that this presoma decomposes generation is more, causes
Prepared ReS2Film lattice quality is excessively poor, and electricity mobility is extremely low.Another is
Source growth ReS2, but because of the fusing point of Re powder high (3180 DEG C), in general growth temperature range (500～
1000 DEG C) vapour pressure of Re is extremely low, causes the method growth efficiency the lowest, it is impossible to realize the big face of this material
Long-pending preparation.Especially because ReS2The interlaminar action power that material is weak, and the silicon dioxide substrate used by above method
Because surface atom diffusion barrier is bigger so that this material the most easily grows thick-layer, it is difficult to obtain
The uniform sample of the number of plies.Therefore, the uniform ReS of large area, high-quality and the number of plies2The controlled preparation of thin film is still
There is the biggest challenge.
Summary of the invention
The technical problem to be solved is to provide a kind of chemical gaseous phase using eutectic to assist to deposit
Method prepares the method for the uniform rhenium disulfide of large area, high-quality and the number of plies.
Solve above-mentioned technical problem be the technical scheme is that with rhenium powder and tellurium powder mass ratio as 1:3～10 mixed
Compound be rhenium source, sulfur powder be sulfur source, Muscovitum be growth substrate, 500～900 DEG C of growths 5～20 under an argon atmosphere
Minute, obtain two dimension rhenium disulfide thin film.
The present invention preferably with rhenium powder and tellurium powder mass ratio as 1:7～9 mixture for rhenium source.
Above-mentioned rhenium powder is 1:60～100 with the mass ratio of sulfur powder, and described sulfur powder preferably adds at 150～250 DEG C
Heat volatilization.
The present invention further preferably the most under an argon atmosphere 600～800 DEG C grow 10 minutes.
The present invention uses the chemical gaseous phase depositing process that eutectic assists, by introducing a certain amount of tellurium in rhenium powder
Powder forms rhenium-tellurium binary eutectic alloy, can allow the fusing point of metal Re from 3180 DEG C be reduced to 500～
Within 1000 DEG C, thus improve the growth efficiency of rhenium disulfide, it is achieved prepared by its large area.Moreover, according to
Rhenium disulfide material interlayer uncoupling and anisotropic characteristic, the present invention selects have relatively low atomic surface migration energy
Mica sheet as growth substrate, promote the Van der Waals epitaxial growth of the number of plies uniform rhenium disulfide thin film, effectively keep away
The rhenium disulfide having exempted to grow in traditional silicon substrate is the petal-like problem that thickness is uneven.
The inventive method compares the existing method preparing rhenium disulfide, requires relatively low to appointed condition, operating process letter
Single, have that reaction temperature is low, growth efficiency is high, the number of plies is uniform, products obtained therefrom lattice quality height and controllability good
Feature, it is achieved that the control growth of the controlled rhenium disulfide of large area, high-quality and the number of plies, for rhenium disulfide at electronics
Application with field of optoelectronic devices provides reliable sample preparation methods.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 800 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Optical microscope photograph at the end.
Fig. 2 be in embodiment 1 800 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Raman spectrogram at the end.
Fig. 3 be in embodiment 1 800 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
High-resolution-ration transmission electric-lens photo at the end.
Fig. 4 be in embodiment 1 800 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
X-ray photoelectron energy spectrogram at the end.
Fig. 5 be in embodiment 2 900 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Optical microscope photograph at the end.
Fig. 6 be in embodiment 2 900 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Raman spectrogram at the end.
Fig. 7 be in embodiment 3 600 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Optical microscope photograph at the end.
Fig. 8 be in embodiment 3 600 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Raman spectrogram at the end.
Fig. 9 be in embodiment 4 500 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Optical microscope photograph at the end.
Figure 10 be in embodiment 4 500 DEG C be transferred to SiO at mica substrate superficial growth gained rhenium disulfide2/ Si base
Raman spectrogram at the end.
Figure 11 be in comparative example 1 800 DEG C at SiO2The Raman spectrogram of/Si substrate surface growth gained rhenium disulfide.
Figure 12 be in comparative example 1 800 DEG C at SiO2The optical microscope of/Si substrate surface growth gained rhenium disulfide
Photo.
Detailed description of the invention
The present invention is described in more detail with embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention not only limits
In these embodiments.
Embodiment 1
Pottery is put into after rhenium powder that 1mg purity is 99.99% and tellurium powder mix homogeneously that 8mg purity is 99.9%
Boat uniformly spreads out, then the mica sheet of fresh stripping is tipped upside down in ceramic boat, this ceramic boat is pushed into tube furnace
The middle position of the thermal treatment zone；The sulfur powder that 80mg purity is 99.8% is put in another ceramic boat, and by this pottery
Boat is also pushed in tube furnace；Under argon flow amount is 20sccm, furnace temperature was risen to 800 DEG C in 22 minutes,
The heating-up temperature controlling sulfur powder is 200 DEG C, and then constant temperature 10 minutes naturally cool to room temperature with stove, obtain two
Dimension rhenium disulfide thin film.As seen from Figure 1, gained sample thin film pattern, size and the number of plies are the most uniform, from optics
Contrast can be seen that it is monolayer.The Raman spectrum of Fig. 2 is at 162cm-1And 213cm-1Two peaks at place are two sulfur
Change the characteristic peak of rhenium, " diamond shaped " rhenium chain structure of rhenium disulfide feature in the high-resolution-ration transmission electric-lens photo of Fig. 3
High-visible, result above confirms that gained sample is rhenium disulfide thin film, and has high lattice quality.By Fig. 4
Visible, x-ray photoelectron power spectrum only have the characteristic peak of rhenium element and element sulphur occur, the not spy of tellurium element
Levy peak to occur, it was demonstrated that during this tellurium assisting growth, tellurium element will not be doped in rhenium disulfide lattice structure
Go.
Embodiment 2
Pottery is put into after rhenium powder that 1mg purity is 99.99% and tellurium powder mix homogeneously that 3mg purity is 99.9%
Boat uniformly spreads out, then the mica sheet of fresh stripping is tipped upside down in ceramic boat, this ceramic boat is pushed into tube furnace
The middle position of the thermal treatment zone；The sulfur powder that 100mg purity is 99.8% is put in another ceramic boat, and by this pottery
Porcelain boat is also pushed in tube furnace；Under argon flow amount is 20sccm, furnace temperature was risen to 900 DEG C in 25 minutes,
The heating-up temperature controlling sulfur powder is 200 DEG C, and then constant temperature 10 minutes naturally cool to room temperature with stove, obtain two
Dimension rhenium disulfide thin film.From Fig. 5～6, gained thickness of sample is uniform, and pattern is relatively regular, its Raman spectrum
Two characteristic peaks occur in 162cm-1And 213cm-1Place, it was demonstrated that gained sample is high-quality rhenium disulfide thin film.
Embodiment 3
Pottery is put into after rhenium powder that 1mg purity is 99.99% and tellurium powder mix homogeneously that 7mg purity is 99.9%
Boat uniformly spreads out, then the mica sheet of fresh stripping is tipped upside down in ceramic boat, this ceramic boat is pushed into tube furnace
The middle position of the thermal treatment zone；The sulfur powder that 60mg purity is 99.8% is put in another ceramic boat, and by this pottery
Boat is also pushed in tube furnace；Under argon flow amount is 20sccm, furnace temperature was risen to 600 DEG C in 20 minutes,
The heating-up temperature controlling sulfur powder is 200 DEG C, and then constant temperature 10 minutes naturally cool to room temperature with stove, obtain two
Dimension rhenium disulfide thin film.Uniform from Fig. 7～8, gained sample size and thickness, pattern is hexagon, its
Two characteristic peaks of Raman spectrum occur in 162cm-1And 213cm-1Place, it was demonstrated that gained sample is high-quality curing
Rhenium thin film.
Embodiment 4
Pottery is put into after rhenium powder that 1mg purity is 99.99% and tellurium powder mix homogeneously that 10mg purity is 99.9%
Porcelain boat uniformly spreads out, then the mica sheet of fresh stripping is tipped upside down in ceramic boat, this ceramic boat is pushed into tubular type
The middle position of the stove thermal treatment zone；The sulfur powder that 100mg purity is 99.8% is put in another ceramic boat, and should
Ceramic boat is also pushed in tube furnace；Under argon flow amount is 20sccm, furnace temperature was risen to 500 in 18 minutes
DEG C, the heating-up temperature controlling sulfur powder is 200 DEG C, and then constant temperature 10 minutes naturally cool to room temperature with stove,
To two dimension rhenium disulfide thin film.Uniform from Fig. 9～10, gained sample size and thickness, pattern is circular,
Two characteristic peaks of its Raman spectrum occur in 162cm-1And 213cm-1Place, it was demonstrated that gained sample is that rhenium disulfide is thin
Film.
Comparative example 1
In embodiment 1, the SiO after the mica sheet of fresh stripping being cleaned2/ Si substrate is replaced, other steps
Same as in Example 1.As seen from Figure 11, two characteristic peaks of Raman spectrum occur in 162cm-1And 213cm-1
Place, it was demonstrated that gained sample is rhenium disulfide.But as seen from Figure 12, gained sample is the thickest block, and not
Enough smooth, petal-shaped occurs, SiO is described2/ Si substrate is unsuitable for growing large-area, the uniform monolayer of the number of plies or few
Layer rhenium disulfide thin film.
Claims (5)
1. the method that a chemical gaseous phase deposition prepares rhenium disulfide thin film, it is characterised in that: with rhenium powder and tellurium powder
Mass ratio be the mixture of 1:3～10 be rhenium source, sulfur powder be sulfur source, Muscovitum be growth substrate, under an argon atmosphere
500～900 DEG C grow 5～20 minutes, obtain two dimension rhenium disulfide thin film.
The method that chemical gaseous phase deposition the most according to claim 1 prepares rhenium disulfide thin film, its feature exists
In: with rhenium powder and tellurium powder mass ratio as 1:7～9 mixture for rhenium source.
The method that chemical gaseous phase deposition the most according to claim 1 prepares rhenium disulfide thin film, its feature exists
In: described rhenium powder is 1:60～100 with the mass ratio of sulfur powder.
4. the method preparing rhenium disulfide thin film according to the chemical gaseous phase deposition described in claims 1 to 3 any one,
It is characterized in that: described sulfur powder heats volatilization at 150～250 DEG C.
The method that chemical gaseous phase deposition the most according to claim 4 prepares rhenium disulfide thin film, its feature exists
In: 600～800 DEG C grow 10 minutes under an argon atmosphere.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188220A (en) * | 2017-06-20 | 2017-09-22 | 华中科技大学 | A kind of two-dimensional nano Ga2In4S9The preparation method and product of crystalline material |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
| CN110205605A (en) * | 2019-06-17 | 2019-09-06 | 东南大学 | A kind of method of atomic layer deposition rhenium disulfide film |
| CN110467358A (en) * | 2019-07-09 | 2019-11-19 | 广东工业大学 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
| CN110838586A (en) * | 2018-08-15 | 2020-02-25 | 深圳国家能源新材料技术研发中心有限公司 | Rhenium sulfide nanotube and preparation method and application thereof |
| JP2022137083A (en) * | 2016-12-02 | 2022-09-21 | エーエスエム アイピー ホールディング ビー．ブイ． | Atomic layer deposition of rhenium containing thin film |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2022137083A (en) * | 2016-12-02 | 2022-09-21 | エーエスエム アイピー ホールディング ビー．ブイ． | Atomic layer deposition of rhenium containing thin film |
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| CN107188220B (en) * | 2017-06-20 | 2019-05-14 | 华中科技大学 | A kind of two-dimensional nano Ga2In4S9The preparation method and product of crystalline material |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
| CN110838586A (en) * | 2018-08-15 | 2020-02-25 | 深圳国家能源新材料技术研发中心有限公司 | Rhenium sulfide nanotube and preparation method and application thereof |
| CN110838586B (en) * | 2018-08-15 | 2023-02-10 | 深圳国家能源新材料技术研发中心有限公司 | Rhenium sulfide nano tube and preparation method and application thereof |
| CN110205605A (en) * | 2019-06-17 | 2019-09-06 | 东南大学 | A kind of method of atomic layer deposition rhenium disulfide film |
| CN110467358A (en) * | 2019-07-09 | 2019-11-19 | 广东工业大学 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
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