CN113337807A - Method for preparing two-dimensional material - Google Patents
Method for preparing two-dimensional material Download PDFInfo
- Publication number
- CN113337807A CN113337807A CN202110517464.XA CN202110517464A CN113337807A CN 113337807 A CN113337807 A CN 113337807A CN 202110517464 A CN202110517464 A CN 202110517464A CN 113337807 A CN113337807 A CN 113337807A
- Authority
- CN
- China
- Prior art keywords
- substrate
- dimensional material
- temperature
- temperature zone
- zone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000758 substrate Substances 0.000 claims abstract description 78
- 230000004048 modification Effects 0.000 claims abstract description 25
- 238000012986 modification Methods 0.000 claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 43
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 43
- 229910052594 sapphire Inorganic materials 0.000 claims description 18
- 239000010980 sapphire Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 13
- -1 polydimethylsiloxane Polymers 0.000 claims description 13
- 150000004770 chalcogenides Chemical class 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 10
- 230000007704 transition Effects 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 4
- ROUIDRHELGULJS-UHFFFAOYSA-N bis(selanylidene)tungsten Chemical compound [Se]=[W]=[Se] ROUIDRHELGULJS-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000002356 single layer Substances 0.000 description 13
- 239000010408 film Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000005693 optoelectronics Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C23C16/02—Pretreatment of the material to be coated
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0209—Pretreatment of the material to be coated by heating
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a method for preparing a two-dimensional material, comprising: (1): placing the substrate in a chemical vapor deposition system, and annealing the substrate at a high temperature; (2): adhering a surface modifying material to the surface of the annealed substrate; (3): removing the surface modifying material; (4): placing a substance for forming a two-dimensional material and a substrate subjected to surface modification treatment in a first temperature zone, a second temperature zone and a third temperature zone of a three-temperature-zone chemical vapor deposition system in sequence to form the two-dimensional material; (5): stopping introducing oxygen, stopping heating, naturally cooling to room temperature, and taking out the sample; (6): and separating the two-dimensional material from the substrate to obtain a target product. The invention can realize easy peeling of the two-dimensional material and the substrate, avoid introduction of pollutants and defects and effectively ensure the quality of a sample.
Description
Technical Field
The present invention relates to a method for preparing a two-dimensional material, and more particularly, to a method for preparing a two-dimensional material having a weak bonding force with a substrate.
Background
Since the discovery of graphene in 2004, two-dimensional materials have attracted considerable attention from researchers. Among them, transition group metal chalcogenides are ideal materials for constructing next-generation miniaturized, flexible, and transparent electronic and optoelectronic devices because of their thickness of a monoatomic layer and excellent physical properties as two-dimensional semiconductor materials.
Transition group metal chalcogenide has wide electrical application, in particular to molybdenum disulfide, which is a typical transition group metal chalcogenide, has high thermal stability and chemical stability, and good mechanical strength, flexibility and transparency, and a single layer of molybdenum disulfide has a direct band gap of 2.1 electron volts, and is suitable for preparing electronic and optoelectronic devices. At present, the preparation of the wafer-level molybdenum disulfide single-layer film is realized by methods such as chemical vapor deposition, physical vapor transmission, molecular beam epitaxy, atomic layer deposition, magnetron sputtering and the like.
However, to achieve practical applications of a single layer of molybdenum disulfide, the thin film is usually stripped from the original substrate and then transferred to a target substrate with a dielectric layer for later device processing. However, the two-dimensional material with large area is difficult to be peeled from the substrate without damage due to the strong bonding force between the two-dimensional material and the originally grown substrate, which limits the large-scale application thereof, and therefore the non-destructive transfer of the two-dimensional material with large area has been a scientific problem to be solved.
The most common two-dimensional material transfer method at present utilizes alkaline solution to corrode the substrate, so as to achieve the purpose of peeling the two-dimensional material from the substrate. However, in this method, the sample is soaked in the solution for a long time, and contaminants and defects are inevitably introduced, so that the quality of the sample is degraded.
Therefore, a new preparation method of the two-dimensional material is sought, so that the binding force of the two-dimensional material and the substrate is reduced, the corrosion time of the sample in the solution can be shortened, even the sample transfer can be carried out only by using water without the participation of the solution, and the quality of the sample is effectively ensured.
Disclosure of Invention
In view of the above problems, according to an embodiment of the present invention, there is provided a method for preparing a two-dimensional material, which is effective to reduce a bonding force of the two-dimensional material to a substrate, so that the resultant two-dimensional material can be completely separated from the substrate with high ease, specifically, the method comprising the steps of:
step (1): placing a substrate in a chemical vapor deposition system, introducing argon-oxygen mixed gas or high-purity oxygen, and annealing the substrate at a high temperature to enable the substrate to generate periodic steps;
step (2): adhering a surface modification material on the surface of the annealed substrate, and carrying out surface modification treatment on the surface modification material;
and (3): removing the surface modification material from the surface of the surface modification treated substrate;
and (4): placing a substance for forming the two-dimensional material and the substrate subjected to surface modification treatment in a first temperature zone, a second temperature zone and a third temperature zone of a three-temperature-zone chemical vapor deposition system in sequence to form the two-dimensional material;
and (5): stopping introducing oxygen after the two-dimensional material grows, stopping heating in all three temperature areas, naturally cooling to room temperature, and taking out a sample;
and (6): and separating the two-dimensional material from the substrate to obtain a target product.
According to a preferred embodiment of the invention, the substrate is one of sapphire, silicon dioxide, glass, quartz, mica.
According to a preferred embodiment of the invention, the annealing temperature is in the range of 900 ℃ to 1000 ℃.
According to a preferred embodiment of the invention, the surface modifying material is polydimethylsiloxane.
According to a preferred embodiment of the present invention, the temperature of the first temperature zone is 100 ℃ to 150 ℃, the temperature of the second temperature zone is 450 ℃ to 650 ℃, and the temperature of the third temperature zone is 800 ℃ to 1000 ℃.
According to a preferred embodiment of the present invention, the chamber pressure of the chemical vapor deposition is maintained at about 1torr, and the temperature zones of the first temperature zone, the second temperature zone and the third temperature zone are maintained for about 40 minutes.
According to a preferred embodiment of the invention, the two-dimensional material is a transition group metal chalcogenide.
According to a preferred embodiment of the present invention, the transition group metal chalcogenide is one of molybdenum disulfide, tungsten disulfide, molybdenum diselenide, tungsten diselenide.
According to a preferred embodiment of the invention, the transition group metal chalcogenide is molybdenum disulfide.
According to a preferred embodiment of the present invention, the substance for forming the two-dimensional material is sulfur powder and molybdenum trioxide.
The invention provides a method for preparing a two-dimensional material, which realizes the reduction of the bonding force between the two-dimensional material and a substrate. The method for regulating and controlling the binding force provided by the invention is simple and quick, has low cost, ensures that the grown two-dimensional material and the transferred two-dimensional material are clean and lossless, has excellent properties, and can be used for preparing high-performance electronic devices and optoelectronic devices.
The foregoing and other features and advantages of the present application will become apparent from the following description of exemplary embodiments.
Drawings
The above and other objects, features and advantages of the present application will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings. The accompanying drawings are included to provide a further understanding of the embodiments of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. In the drawings, like reference numbers generally represent like parts or steps.
FIG. 1 is a flow chart of a method of preparing a two-dimensional material having a weak bonding force with a substrate according to the present invention;
FIG. 2 is a photograph of (a) polydimethylsiloxane and sapphire substrate used in the present invention, (b) polydimethylsiloxane mounted on the surface of the sapphire substrate, and (c) a single layer of molybdenum disulfide on the grown wafer-level sized sapphire substrate;
FIG. 3 is (a) an optical microscope image, (b) an atomic force microscope image, (c) a Raman spectrum, and (d) a fluorescence spectrum of a monolayer of molybdenum disulfide sample prepared by the method of the present invention;
FIG. 4 is a photograph comparing (a) a strong binding molybdenum disulfide sample with (b) a weak binding molybdenum disulfide sample grown in accordance with the present invention in a process of peeling in deionized water and (c) two different binding samples before and after peeling;
fig. 5 is a graph of the lateral force versus lateral displacement for (a) a strong binding molybdenum disulfide sample and (b) a weak binding molybdenum disulfide sample prepared by the present invention, obtained by a scratch test of a nanoindenter;
fig. 6 is a photograph of a sample of a monolayer of molybdenum disulfide prepared according to the present invention having a weak bonding force with a substrate transferred to (a) a silica substrate and (b) a polydimethylsiloxane substrate.
Detailed Description
FIG. 1 is a flow chart of the present invention for preparing a two-dimensional material with weak bonding force with an original substrate, which specifically comprises the following steps:
step (1): placing a substrate in a chemical vapor deposition system, introducing argon-oxygen mixed gas or high-purity oxygen, and annealing the substrate at high temperature to enable the substrate to generate periodic steps, which is beneficial to nucleation at the initial growth stage; the substrate is one of sapphire, silicon dioxide, glass, quartz and mica, and is preferably sapphire; the annealing temperature is 900-1000 ℃.
Step (2): and pasting a surface modification material on the surface of the annealed substrate, and performing surface modification treatment on the annealed substrate, wherein the surface modification material is preferably polydimethylsiloxane, but is not limited to the polydimethylsiloxane.
And (3): removing the surface modification material from the surface of the surface modification treated substrate.
And (4): placing a substance for forming the two-dimensional material and the substrate subjected to surface modification treatment in a first temperature zone, a second temperature zone and a third temperature zone of a three-temperature-zone chemical vapor deposition system in sequence to form the two-dimensional material, wherein preferably, the temperature of the first temperature zone is 100-150 ℃, the temperature of the second temperature zone is 450-650 ℃, and the temperature of the third temperature zone is 800-1000 ℃; maintaining the pressure of the chemical vapor deposition chamber at about 1torr, and maintaining the temperature zones of the first temperature zone, the second temperature zone and the third temperature zone for about 40 minutes; however, the method is not limited to this, and may be appropriately adjusted according to the production amount.
And (5): and stopping introducing oxygen after the two-dimensional material grows, stopping heating in all three temperature areas, naturally cooling to room temperature, and taking out the sample.
And (6): and separating the two-dimensional material from the substrate to obtain a target product.
In the present invention, the two-dimensional material is a transition group metal chalcogenide, such as one of molybdenum disulfide, tungsten disulfide, molybdenum diselenide, tungsten diselenide, preferably molybdenum disulfide; when the two-dimensional material is molybdenum disulfide, the substances for forming the two-dimensional material may be sulfur powder and molybdenum trioxide, but is not limited thereto, and other substances capable of generating molybdenum disulfide may also be used.
In the invention, when the molybdenum disulfide two-dimensional material is formed, sulfur powder, molybdenum trioxide and the annealed sapphire wafer can be sequentially placed in the first temperature zone, the second temperature zone and the third temperature zone of the three-temperature-zone chemical vapor deposition system. And introducing carrier gas (argon and oxygen) and keeping the pressure of the cavity at about 1 torr. The temperature of the three temperature zones is respectively raised to a certain temperature, and the temperature zones are respectively as follows: 100-150 ℃, 450-650 ℃ and 800-1000 ℃ for about 40 minutes, during which the molybdenum disulfide undergoes nucleation and film formation.
After the two-dimensional material growth is completed, the technical effect of the invention compared with the prior art can be compared with the sample without the substrate modification treatment through the difficulty of the process of peeling the two-dimensional material from the substrate by the sample.
Compared with the prior art, the comparison method can prove that the bonding force between the two-dimensional material sample prepared by the method and the substrate is effectively reduced, so that the two-dimensional material sample can be completely and nondestructively stripped from the original substrate on which the two-dimensional material grows and transferred to any other substrate, and the uniform regulation and control of the bonding force between the two-dimensional material with wafer level size and the substrate can be realized.
Furthermore, according to the method, the polydimethylsiloxane surface modification treatment can be carried out on the two surfaces of the substrate, and then the substrate subjected to the two-surface modification treatment is vertically placed in the cavity, so that the two-dimensional material with weak binding force can be simultaneously grown on the front surface and the back surface of the substrate.
The two-dimensional semiconductor material grown by the method has excellent electrical property and optical property, for example, a field effect transistor prepared by the sample has very high current switching ratio and field effect mobility, and is suitable for preparing high-performance electronic devices and optoelectronic devices, and the product grown by the method and having weak binding force is beneficial to preparing laminated homogeneous/heterogeneous structures.
Examples
Specifically, the preparation of a monolayer molybdenum disulfide two-dimensional material is realized by the method, and the performances of various aspects of the monolayer molybdenum disulfide two-dimensional material are verified.
Firstly, a substrate is placed in a chemical vapor deposition system, argon-oxygen mixed gas is introduced, the substrate is annealed at high temperature, and then polydimethylsiloxane is removed from the surface of the substrate.
Then, 5g of sulfur powder, 5mg of molybdenum trioxide powder and the sapphire wafer are respectively placed in a first temperature zone, a second temperature zone and a third temperature zone of the three-temperature-zone chemical vapor deposition system.
Then, the chamber was sealed and evacuated, and 275sccm argon gas and a small amount of oxygen gas were introduced, and the chamber pressure was maintained at about 1 torr. The temperatures of the three temperature zones are 130 ℃, 530 ℃ and 900 ℃ respectively, and are maintained for about 40 minutes, during which the monolayer of molybdenum disulfide undergoes nucleation and film formation. And stopping introducing oxygen after the growth is finished, stopping heating in all three temperature areas, naturally cooling to room temperature, and taking out the sample.
In fig. 2, (a) is a photograph of the polydimethylsiloxane and the sapphire substrate used in the present invention, (b) is a photograph of the polydimethylsiloxane adhered to the surface of the sapphire substrate and the surface modification treatment is performed on the substrate, and fig. 2(c) is a photograph of a wafer-level-sized single-layer molybdenum disulfide sample obtained after growth, which shows that the entire sample surface is very clean and the sample uniformity is very good.
Figure 3 shows a picture of the surface topography of a sample of molybdenum disulfide after growth is completed. Wherein, (a) is an optical microscope image of molybdenum disulfide on a sapphire substrate; (b) is an atomic force microscope image of molybdenum disulfide on a sapphire substrate. The surface of the sample is very flat and clean, and the polydimethylsiloxane is pasted and cannot pollute the surface and the interface of the sample. (c) And (d) respectively showing the Raman spectrum and the fluorescence spectrum of the molybdenum disulfide film grown by the method. In Raman spectroscopy, molybdenum disulfide exhibits E2gAnd A1gTwo raman characteristic peaks, the difference in peak positions of the two characteristic peaks indicating that the molybdenum disulfide is a monolayer film; and in the fluorescence spectrum, molybdenum disulfide has a fluorescence peak at the wavelength of 658 nm.
FIG. 4 is a comparison of the stripping process of the weakly binding molybdenum disulfide film grown according to the present invention and the strongly binding molybdenum disulfide film used for comparison in deionized water. Wherein, the graphs (a) and (b) respectively show the peeling process of two different samples with strong bonding force and weak bonding force, namely, one corner of the sample is clamped by a pair of tweezers, the sample is slowly immersed into deionized water, and the peeling of the sample is realized by utilizing the difference of hydrophilicity and hydrophobicity between molybdenum disulfide and a sapphire substrate. (c) FIG. d is a photograph showing a comparison of the two samples before and after peeling. Therefore, the sample with strong bonding force is immersed in the deionized water, the sample cannot be stripped from the sapphire substrate due to the strong bonding force between the sample and the substrate, the sample with weak bonding force is immersed in the deionized water and can be completely stripped from the sapphire substrate, and the single-layer molybdenum disulfide film floats on the surface of the deionized water, so that the fact that the molybdenum disulfide grown by the method has very weak bonding force between the substrate and is easy to strip and transfer is qualitatively proved.
Figure 5 shows the lateral force versus lateral displacement for a molybdenum disulfide film with a weak binding force versus a molybdenum disulfide film with a strong binding force for the control. The measurement principle is as follows: and (3) utilizing a scratch test mode of a nano indenter, loading a load (380 mu N) with a certain magnitude on an indenter, scraping the surface of the sample by the indenter, stripping the molybdenum disulfide from the sapphire substrate, simultaneously measuring the magnitude of the lateral force, and giving a relation graph of the lateral force and the lateral displacement. The strength of the binding force between the molybdenum disulfide and the substrate can be reflected by the lateral force, and the stronger the binding force, the larger the lateral force. It can be seen from fig. 5 that the magnitude of the lateral force is approximately around 45 μ N for the samples with strong bonding force, while the value of the lateral force is about 30 μ N for the samples with weak bonding force, which quantitatively demonstrates the very weak bonding force between the grown molybdenum disulfide of the present invention and the substrate.
In fig. 6, (a) and (b) are photographs of a wafer-level single-layer molybdenum disulfide two-dimensional material having a weak bonding force prepared by the method of the present invention transferred onto a silicon dioxide substrate and a polydimethylsiloxane substrate, respectively, and it can be seen from (a) and (b) of fig. 6 that the peeling process does not damage the sample due to the reduced bonding force between the sample obtained by the method and the sapphire substrate, and the sample obtained after the transfer is still complete and clean.
The foregoing describes the general principles of the present application in conjunction with specific embodiments, however, it is noted that the advantages, effects, etc. mentioned in the present application are merely examples and are not limiting, and they should not be considered essential to the various embodiments of the present application. Furthermore, the foregoing disclosure of specific details is for the purpose of illustration and description and is not intended to be limiting, since the foregoing disclosure is not intended to be exhaustive or to limit the disclosure to the precise details disclosed.
The block diagrams of devices, apparatuses, systems referred to in this application are only given as illustrative examples and are not intended to require or imply that the connections, arrangements, configurations, etc. must be made in the manner shown in the block diagrams. These devices, apparatuses, devices, systems may be connected, arranged, configured in any manner, as will be appreciated by those skilled in the art. Words such as "including," "comprising," "having," and the like are open-ended words that mean "including, but not limited to," and are used interchangeably therewith. The words "or" and "as used herein mean, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
It should also be noted that in the devices, apparatuses, and methods of the present application, the components or steps may be decomposed and/or recombined. These decompositions and/or recombinations are to be considered as equivalents of the present application.
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, the description is not intended to limit embodiments of the application to the form disclosed herein. While a number of example aspects and embodiments have been discussed above, those of skill in the art will recognize certain variations, modifications, alterations, additions and sub-combinations thereof.
Claims (10)
1. A method for producing a two-dimensional material, characterized in that the method comprises the steps of:
step (1): placing a substrate in a chemical vapor deposition system, introducing argon-oxygen mixed gas or high-purity oxygen, and annealing the substrate at a high temperature to enable the substrate to generate periodic steps;
step (2): adhering a surface modification material on the surface of the annealed substrate, and carrying out surface modification treatment on the surface modification material;
and (3): removing the surface modification material from the surface of the surface modification treated substrate;
and (4): placing a substance for forming the two-dimensional material and the substrate subjected to surface modification treatment in a first temperature zone, a second temperature zone and a third temperature zone of a three-temperature-zone chemical vapor deposition system in sequence to form the two-dimensional material;
and (5): stopping introducing oxygen after the two-dimensional material grows, stopping heating in all three temperature areas, naturally cooling to room temperature, and taking out a sample;
and (6): and separating the two-dimensional material from the substrate to obtain a target product.
2. A method of producing a two-dimensional material according to claim 1, wherein the substrate is one of sapphire, silicon, silica, glass, quartz, mica.
3. A method of producing a two-dimensional material according to claim 1 or 2, characterised in that the annealing temperature is 900-1000 ℃.
4. A method of producing a two-dimensional material according to claim 1 or 2, characterised in that the surface-modifying material is polydimethylsiloxane.
5. The method of claim 1 or 2, wherein the temperature of the first temperature zone is 100 ℃ to 150 ℃, the temperature of the second temperature zone is 450 ℃ to 650 ℃, and the temperature of the third temperature zone is 800 ℃ to 1000 ℃.
6. The method of claim 1 or 2, wherein a chamber pressure of the chemical vapor deposition is maintained at about 1torr, and the temperature zones of the first temperature zone, the second temperature zone, and the third temperature zone are maintained for about 40 minutes.
7. A method of producing a two-dimensional material according to claim 1 or 2, characterized in that the two-dimensional material is a transition group metal chalcogenide.
8. The method of claim 7, wherein the transition group metal chalcogenide is one of molybdenum disulfide, tungsten disulfide, molybdenum diselenide, and tungsten diselenide.
9. The method of claim 8, wherein the transition group metal chalcogenide is molybdenum disulfide.
10. The method of producing a two-dimensional material according to claim 1 or 2, wherein the substance for forming a two-dimensional material is sulfur powder and molybdenum trioxide.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110517464.XA CN113337807A (en) | 2021-05-12 | 2021-05-12 | Method for preparing two-dimensional material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110517464.XA CN113337807A (en) | 2021-05-12 | 2021-05-12 | Method for preparing two-dimensional material |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113337807A true CN113337807A (en) | 2021-09-03 |
Family
ID=77469276
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110517464.XA Pending CN113337807A (en) | 2021-05-12 | 2021-05-12 | Method for preparing two-dimensional material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113337807A (en) |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103572284A (en) * | 2012-08-06 | 2014-02-12 | 徐明生 | Method for transferring two-dimensional nano-film |
CN104960286A (en) * | 2015-05-28 | 2015-10-07 | 东南大学 | Controllable flexible transfer method of two-dimensional materials |
WO2017009526A1 (en) * | 2015-07-13 | 2017-01-19 | Nokia Technologies Oy | An apparatus and method for enabling transfer of two dimensional materials |
CN107299333A (en) * | 2017-05-26 | 2017-10-27 | 西安理工大学 | A kind of preparation method of single-layer molybdenum disulfide film |
CN107447200A (en) * | 2016-10-28 | 2017-12-08 | 北京大学 | A kind of method for preparing transient metal chalcogenide compound/two-dimensional layer material interlayer heterojunction structure using two step chemical vapour deposition techniques |
CN110055591A (en) * | 2019-05-17 | 2019-07-26 | 中国科学院物理研究所 | The preparation method of two-dimentional ternary atomic crystal |
US20190232630A1 (en) * | 2018-01-27 | 2019-08-01 | Tsinghua University | Method for transferring two-dimensional nanomaterials |
CN111874896A (en) * | 2020-06-17 | 2020-11-03 | 中国科学院合肥物质科学研究院 | Method for accurately transferring two-dimensional material and application thereof |
CN112501555A (en) * | 2020-11-19 | 2021-03-16 | 南京大学 | Preparation method of single-layer molybdenum disulfide film |
-
2021
- 2021-05-12 CN CN202110517464.XA patent/CN113337807A/en active Pending
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103572284A (en) * | 2012-08-06 | 2014-02-12 | 徐明生 | Method for transferring two-dimensional nano-film |
CN104960286A (en) * | 2015-05-28 | 2015-10-07 | 东南大学 | Controllable flexible transfer method of two-dimensional materials |
WO2017009526A1 (en) * | 2015-07-13 | 2017-01-19 | Nokia Technologies Oy | An apparatus and method for enabling transfer of two dimensional materials |
CN107447200A (en) * | 2016-10-28 | 2017-12-08 | 北京大学 | A kind of method for preparing transient metal chalcogenide compound/two-dimensional layer material interlayer heterojunction structure using two step chemical vapour deposition techniques |
CN107299333A (en) * | 2017-05-26 | 2017-10-27 | 西安理工大学 | A kind of preparation method of single-layer molybdenum disulfide film |
US20190232630A1 (en) * | 2018-01-27 | 2019-08-01 | Tsinghua University | Method for transferring two-dimensional nanomaterials |
CN110055591A (en) * | 2019-05-17 | 2019-07-26 | 中国科学院物理研究所 | The preparation method of two-dimentional ternary atomic crystal |
CN111874896A (en) * | 2020-06-17 | 2020-11-03 | 中国科学院合肥物质科学研究院 | Method for accurately transferring two-dimensional material and application thereof |
CN112501555A (en) * | 2020-11-19 | 2021-03-16 | 南京大学 | Preparation method of single-layer molybdenum disulfide film |
Non-Patent Citations (1)
Title |
---|
廖俊懿 等: ""二维材料的转移方法"", 《物理学报》 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Li et al. | Wafer-scale single-crystal monolayer graphene grown on sapphire substrate | |
US20210399146A1 (en) | Transition metal chalcogenide van der waals films, methods of making same, and apparatuses and devices comprising same | |
JP6116705B2 (en) | Ge quantum dot growth method, Ge quantum dot composite material and application thereof | |
CN110055591B (en) | Preparation method of two-dimensional ternary atomic crystal | |
US8859044B2 (en) | Method of preparing graphene layer | |
TW201637870A (en) | Graphene and polymer-free method for transferring CVD grown graphene onto hydrophobic substrates | |
CN112537796B (en) | Low-energy light-excited material nondestructive thinning method | |
US10889914B2 (en) | Location-specific growth and transfer of single crystalline TMD monolayer arrays | |
CN110055589B (en) | Large-size single-layer hexagonal boron nitride single crystal or film and preparation method thereof | |
CN113337807A (en) | Method for preparing two-dimensional material | |
CN117153694A (en) | High-mobility strain two-dimensional material transistor and preparation method thereof | |
KR101741313B1 (en) | Doping method of graphene based on a supporting layer with ion implantation | |
CN110042365B (en) | Atomic layer deposition method for growing aluminum oxide on surface of two-dimensional material | |
Chou et al. | Single-crystalline silver film grown on Si (100) substrate by using electron-gun evaporation and thermal treatment | |
US9935207B2 (en) | Tunneling diode using graphene-silicon quantum dot hybrid structure and method of manufacturing the same | |
US9673167B2 (en) | Method for bonding substrates | |
CN111235528B (en) | Preparation method of silicon-based germanium nanodots under normal pressure | |
CN115377196A (en) | Epitaxial GaN with diamond as substrate and preparation method thereof | |
CN115287750A (en) | Method for preparing two-dimensional non-layered wide band gap oxide based on Van der Waals epitaxy | |
CN111847432A (en) | Large-area multilayer graphene and preparation method thereof | |
CN110820047B (en) | Preparation method of two-dimensional atomic crystal molecular superlattice | |
CN114807897B (en) | 1T' MoTe 2 Preparation method of nano film | |
CN112110411B (en) | Method for preparing suspended lamellar metal chalcogenides | |
CN113690145A (en) | Two-dimensional Bi2O2Se film thickness regulating and controlling method | |
Yan et al. | Towards bubble-free, centimeter-sized bilayer graphene enabled by backside lamination |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210903 |