CN110670125A - Preparation method of molybdenum sulfide two-dimensional material grown on sapphire substrate - Google Patents
Preparation method of molybdenum sulfide two-dimensional material grown on sapphire substrate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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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- 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
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- C23C16/305—Sulfides, selenides, or tellurides
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- 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
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Abstract
The invention discloses a MoS grown on a sapphire substrate2The preparation method of the two-dimensional material comprises the following steps: substrate preparation: adopting a Sapphire substrate without any pretreatment; preparing raw materials: delivering the Sapphire substrate to a quartz table in an MOCVD (metal organic chemical vapor deposition) cavity, controlling the pressure in the cavity at 20Torr, and introducing N into the cavity all the time220 slm; adopting a chemical vapor deposition method to carry out reaction: increasing the temperature in the cavity to the growth temperature, and introducing H2S source gas, Mo (CO)6Carrying out constant-temperature growth, cooling to room temperature, taking out a sample, and obtaining the MoS grown on the Sapphire substrate2A two-dimensional material. The method can effectively control MoS2Nucleation density, uniformity, and grain orientation, and has the advantage of high feasibility.
Description
Technical Field
The invention relates to MoS2The technical field of two-dimensional materials, in particular to a preparation method of a molybdenum sulfide two-dimensional material grown on a sapphire substrate.
Background
Single-layer transition metal chalcogenides have attracted considerable attention in recent years because of their excellent properties in the fundamental physics of mechanics, heat, optics, electricity, etc. Among them, molybdenum disulfide monolayer is the most typical transition metal chalcogenide, and has been studied more because of its wide source and good relative stability. To date, it has been discovered that a single layer of the semiconductor molybdenum disulfide can be used to fabricate piezoelectric transistors, generators, ultrasensitive photodetectors, chiral light emitting transistors, high performance integrated circuits, and the like. The practical application of the devices is realized, and the most basic is the large-scale controllable preparation of a high-quality single-layer molybdenum disulfide sample and the manufacture of the sample into a structure required by the devices.
Currently, various methods for preparing molybdenum disulfide have been developed, and we can broadly classify these methods into chemical stripping, mechanical stripping, physical deposition, and chemical vapor deposition. Although the stripping method is simple to operate, the obtained sample is irregular in shape and size, the sample is difficult to strip to a single layer, and residual glue introduced in the stripping process has great influence on later-stage device preparation and performance; the physical vapor transport adopts a powder molybdenum sulfide source, which has been proved to grow a single-layer molybdenum disulfide sample of a micron-scale single crystal with high optical quality, but the grown single crystal has smaller size generally. In contrast, the MOCVD (Metal-organic Chemical Vapor Deposition) method is the best method for preparing large-sized uniform two-dimensional materials. Meanwhile, the physical and chemical properties of the two-dimensional material can be realized by changing the conditions of chemical vapor deposition, so that the MOS is prepared by the MOCVD method2A two-dimensional material. Desire to grow MoS with controllable thickness and high quality on a large scale2Lattice matching of the material, substrate is critical, and MoS is the same time2The nucleation stage of (a) is most critical. Nucleation density, size, and grain orientation are currently under investigation.
Disclosure of Invention
To overcome the above-mentioned disadvantages and shortcomings of the prior art, it is an object of the present invention to provide a MoS grown on Sapphire substrate2(SulfurMolybdenum sulfide) two-dimensional material and a preparation method thereof. The method can effectively control MoS2Nucleation density, uniformity, and grain orientation, and has the advantage of high feasibility.
The purpose of the invention is realized by the following technical scheme:
MoS grown on Sapphire substrate2The preparation method of the (molybdenum sulfide) two-dimensional material comprises the following steps:
(1) adopting a sapphire substrate;
(2) placing the sapphire substrate in a MOCVD equipment cavity, and introducing protective gas;
(3) heating the MOCVD equipment cavity to the growth temperature of 900-1100 ℃, keeping the constant temperature for 2-15 minutes, and introducing H2S as source of sulfur gas, H2Introducing S for 5-20 minutes, and then introducing 2X 10-5～9×10-5slm Mo(CO)6Gas source while maintaining H2Introducing S, and MoS is carried out at the growth temperature of 900-1100 DEG C2Growing for 2-20 minutes at constant temperature, and obtaining MoS grown on Sapphire substrate after the constant temperature growth is finished2(molybdenum sulphide) two-dimensional material.
In the step (1), the epitaxial growth surface of the sapphire substrate is alpha-Al2O3And the metal oxide film is not pretreated outside the deposition cavity, and is subsequently sent into the MOCVD cavity for in-situ pretreatment. In addition, conventional methods subject the Sapphire substrate to high temperature O2The pretreatment is carried out for several hours, and the method only needs to be carried out in the MOCVD deposition chamber for 10 minutes H2And S is subjected to in-situ pretreatment, so that the time is greatly saved.
In the step (2), the protective gas is N2. The pressure intensity in the MOCVD equipment cavity is controlled to be 15 Torr-25 Torr, and the N is2The introduction amount of (2) is 15to 25 slm. Most preferably, the pressure in the MOCVD equipment cavity is controlled at 20 Torr. N in the MOCVD equipment cavity2The throughput of (2) was 20slm (standard lithium per minute, 1L flow per minute under standard conditions), and the chamber pressure was maintained at 20 Torr.
In the step (3), the temperature of the MOCVD equipment cavity is increased to 900-1100 ℃, the temperature is kept constant for 2-15 minutes, further preferably, the temperature of the MOCVD equipment cavity is slowly increased to 950-1050 ℃ for 8-11 minutes, the temperature is kept constant for 4-8 minutes, most preferably, the temperature of the MOCVD equipment cavity is slowly increased to 1000 ℃ for 10 minutes, and the temperature is kept constant for 5 minutes.
Firstly introducing H2S as a source of sulfur gas, said H2The introduction amount of S is 0.05-0.5 slm, and H2S is introduced for 5-15 minutes and then Mo (CO) is introduced6Gas source, most preferably, H is first introduced2S as a source of sulfur gas, said H2The amount of S introduced was 0.1slm, H2And introducing a gas source after the S is introduced for 10 minutes so as to passivate the surface of the Sapphire substrate. Firstly with H2S as a source of sulfur gas, compare to (C)2H5) And the S gas source reduces the pollution of the carbon atoms after thermal decomposition to the surface of the substrate. Simultaneous conventional growth of MoS2The vulcanization is carried out by pre-depositing Mo metal or by using MoOx powder and pushing the Mo metal into a CVD cavity in advance. This can result in the Mo source material dose not being freely adjustable. And the invention utilizes H2S gas source, firstly carrying out high-temperature in-situ passivation on the sapphire substrate, then introducing a Mo gas source for chemical vapor deposition, wherein the flow of the gas source can be independently and randomly controlled, and the pollution caused by the exposure of air after the pretreatment of the substrate is also avoided. Meanwhile, experiments prove that the product is subjected to H2The high-temperature in-situ passivation pretreatment of S can change the surface appearance of Sapphire, thereby being beneficial to the subsequent MoS2The orientation of the crystal grains is consistent, so that the crystal grain boundaries caused by the stitching of the crystal grains with different orientations are avoided. The existence of grain boundaries can seriously affect the optical and electrical properties of the film.
The Mo (CO)6The gas source is introduced at a rate of 2X 10-5～9×10-5slm, more preferably 4X 10-5～6×10-5slm, most preferably 5X 10-5slm Mo(CO)6。H2S is introduced for 5-15 minutes and then Mo (CO) is introduced6Gas source while maintaining H2Introducing S, and MoS is carried out at the growth temperature of 950-1050 DEG C2Isothermal growth for 3-15 minutes, most preferably, H2S10 minutes after the introduction of Mo (CO)6Gas source while maintaining H2Introduction of S at growth temperatureMoS at 1000 ℃2And 5 minutes of constant temperature growth. The invention can complete single-layer MoS within 20 minutes2The film growth, compared with the traditional method which takes several hours, greatly saves the cost. Due to the utilization of H2S carries out high-temperature in-situ passivation pretreatment on the sapphire substrate, and compared with the traditional method without pretreatment, the Raman spectrum characteristic of the single-layer film is improved, and the characteristic common peak E for representing the quality of the single crystal2gHas a full width at half maximum (FWHM) Raman shift of 2.99cm-1Improved to 2.66cm-1Characterizing the characteristic bimodal spectral intensity ratio E of the doping2g/A1gAlso from 0.82 to 1.1, indicating better electrical properties. And the C-AFM characterization proves that the compound is obtained by H2And the film current characteristic is improved from 22nA to 280nA by S pretreatment.
Stopping the Mo (CO) after the constant temperature growth is finished6Gas source, keeping introducing H2S gas source, then cooling, and stopping H2Introducing S gas source to obtain MoS grown on Sapphire substrate2(molybdenum sulphide) two-dimensional material.
Said stop H2S gas source, pressure is kept at 20Torr, N2The gas was maintained at 20slm and a single layer of MoS was taken out to a thickness of 1-22And (3) sampling.
Most preferably, a MoS grown on Sapphire substrate2The preparation method of the (molybdenum sulfide) two-dimensional material comprises the following steps:
(1) adopting a sapphire substrate;
(2) placing a sapphire substrate in a MOCVD (metal organic chemical vapor deposition) equipment cavity, and introducing protective gas, wherein the protective gas is N2Said N is2The introducing amount of the MOCVD equipment is 15-25 slm, and the pressure intensity in the cavity of the MOCVD equipment is controlled to be 15 Torr-25 Torr;
(3) slowly raising the temperature of the MOCVD equipment cavity to 1000 ℃ for 10 minutes, keeping the constant temperature for 5 minutes, and introducing H2S as a source of sulfur gas, said H2The amount of S introduced was 0.1slm, H2S10 minutes after the introduction of Mo (CO)6Gas source, said Mo (CO)6The gas source is introduced at 5X 10-5slm while maintaining H2Introduction of SMoS is carried out at a growth temperature of 1000 DEG C2The constant temperature growth is carried out for 5 minutes, and after the constant temperature growth is finished, the Mo (CO) is stopped6Gas source, keeping introducing H2S gas source, then cooling, and stopping H2Introducing S gas source to obtain MoS grown on Sapphire substrate2(molybdenum sulphide) two-dimensional material.
MoS grown on Sapphire substrate of the invention2The (molybdenum sulfide) two-dimensional material can be used for manufacturing piezoelectric transistors, generators, ultra-sensitive photodetectors, chiral light-emitting transistors, high-performance integrated circuits and the like.
The invention provides a MoS grown on a Sapphire substrate prepared by the preparation method2A two-dimensional material. The MOCVD method adopted by the invention has controllable reaction conditions and MoS2Controllable nucleation density and grain orientation, MoS2The thickness is controllable, and a stable and efficient MoS is provided2A method for growing two-dimensional nano materials.
Compared with the prior art, the invention has the following advantages and effects:
(1) the preparation method provided by the invention adopts a chemical vapor deposition process to carry out reaction and utilizes H2S、Mo(CO)6As an independent gas source, the method has high implementability, variable and controllable growth conditions, and large size and uniform thickness of the obtained sample;
(2) the preparation method provided by the invention uses Sapphire as a substrate and MoS2Lattice matching can effectively improve MoS2Quality of nucleation;
(3) the preparation method provided by the invention uses H firstly2S gas source firstly carries out in-situ passivation pretreatment on the Sapphire substrate, and then Mo (CO) is introduced6Performing MoS2And (5) growing the material. By H2S pretreatment, the morphology of the Sapphire substrate is improved, the step-shaped morphology edge is smoother, and MoS2The nucleation density is effectively reduced, and the uniformity of the grain orientation is obviously improved. Simultaneously, the pollution of the surface of the substrate and O caused by remote passivation are avoided2A time consuming process of high temperature pretreatment.
Drawings
FIG. 1 provides example 1 without passing through H2AFM (atomic force microscope) image of the morphology of the Sapphire substrate pretreated by S;
FIG. 2 is a pass H provided in example 12S, preprocessing an AFM (atomic force microscopy) picture of the Sapphire substrate morphology;
FIG. 3 is a pass H provided in example 12After S pretreatment, MoS2MoS after 5 min growth2Forming a nuclear AFM picture;
FIG. 4 is a graph of the temperature, pressure, and source gases in the MOCVD chamber provided in example 1 over time;
FIG. 5 shows the non-/Via H provided in example 12After S pretreatment, MoS2Raman (Raman spectrum) characterization after 20 min of growth, FIG. 5, with no H in the lower curve2MoS under S substrate pretreatment2A characteristic; the upper curve is through H2MoS after S substrate pretreatment2A characteristic;
FIG. 6 shows the non-/Via H provided in example 12After S pretreatment, MoS2Characterization of C-AFM (conductive atomic force microscope) after 20 min of growth, in FIG. 6, H is not shown on the left2MoS under S substrate pretreatment2A current characteristic representation; the right side is a pass H2MoS after S pretreatment2And (4) a current characteristic representation diagram.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, unless otherwise specified, are all implementable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated by the manufacturer, and are regarded as conventional products commercially available.
Example 1
(1) Using alpha-Al2O3Sapphire substrate (ZMKJ 2INCH A-axis) without any pretreatment, the substrate morphology is as shown in FIG. 1;
(2) delivering the Sapphire substrate to a quartz table in an MOCVD chamber, controlling the pressure in the chamber to be 20Torr, and introducing the chamber all the timeN220slm；
(3) Adopting a chemical vapor deposition method to carry out reaction: slowly raising the temperature in the MOCVD chamber to 1000 ℃ within 10 minutes, and keeping the constant temperature for 5 minutes; first, 0.1slm H was introduced2S, using an air source for 10 minutes to passivate the surface of the Sapphire substrate, wherein the shape and effect are shown in figure 2; then 5X 10 of gas is introduced-5slm Mo(CO)6Gas source while maintaining H2Introducing S, and MoS is carried out at the growth temperature of 1000 DEG C2Growing for 5 minutes at constant temperature; stopping the Mo (CO) after the constant temperature growth is finished6Gas source, keeping introducing H2S gas source, then cooling to room temperature of 25 ℃, and stopping H after cooling2Introducing an S gas source, and taking out a sample to obtain the MoS growing on the Sapphire substrate2Two-dimensional material, as shown in fig. 3.
As can be seen in FIG. 2, the Sapphire substrate passes through H2After the S passivation pretreatment, the appearance is improved compared with that of the graph 1, and the step type edge becomes smooth; as can be seen in FIG. 3, MoS occurred over 5 minutes2After growth, MoS2Uniform, regular triangular grains are formed with the grains oriented in a uniform or 0/60 orientation to each other. The regular grain turning has the function of inhibiting the grain boundary generated by the subsequent grain sewing. Temperature, pressure and H in MOCVD chamber during the whole growth process2S、Mo(CO)6The variation of the gas source over time can be seen in fig. 4.
FIG. 5 is a graph showing the MoS after 20 minutes of isothermal growth2Thin film Raman Spectroscopy (Raman) characterization, where the bottom curve is not shown as H2MoS under S substrate pretreatment2Spectral characteristics, upper curve passing through H2MoS after S substrate pretreatment2Spectral characteristics. Due to the utilization of H2S carries out high-temperature in-situ passivation pretreatment on the sapphire substrate, and compared with the traditional method without pretreatment, the Raman spectrum characteristic of the single-layer film is improved, and the characteristic common peak E for representing the quality of the single crystal2gHas a full width at half maximum (FWHM) Raman shift of 2.99cm-1Improved to 2.66cm-1Characterizing the characteristic bimodal spectral intensity ratio E of the doping2g/A1gAlso from 0.82 to 1.1, indicating better electrical properties.
FIG. 6 is a graph showing the MoS after 20 minutes of isothermal growth2Thin film conductive atomic force microscope (C-AFM) characterization, left blank H2MoS under S substrate pretreatment2Current characteristic, right through H2MoS after S pretreatment2Current characteristics. By H2And the film current characteristic is improved from 22nA to 280nA by S pretreatment.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a molybdenum sulfide two-dimensional material grown on a sapphire substrate is characterized by comprising the following steps:
(1) adopting a sapphire substrate;
(2) placing the sapphire substrate in a MOCVD equipment cavity, and introducing protective gas;
(3) heating the MOCVD equipment cavity to the growth temperature of 900-1100 ℃, keeping the constant temperature for 2-15 minutes, and introducing H2S as source of sulfur gas, H2S is introduced for 5to 20 minutes and then Mo (CO) is introduced6Gas source while maintaining H2Introducing S, and MoS is carried out at the growth temperature of 900-1100 DEG C2And growing for 2-20 minutes at constant temperature, and obtaining the molybdenum sulfide two-dimensional material grown on the sapphire substrate after the constant-temperature growth is finished.
2. The method for preparing the molybdenum sulfide two-dimensional material grown on the sapphire substrate according to claim 1, wherein in the step (2), the protective gas is N2。
3. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 2, wherein in the step (2), N is2The introduction amount of (2) is 15to 25 slm.
4. The method for preparing the molybdenum sulfide two-dimensional material grown on the sapphire substrate according to claim 1, wherein in the step (2), the pressure in the MOCVD equipment chamber is controlled to be 15 Torr-25 Torr.
5. The method for preparing the molybdenum sulfide two-dimensional material grown on the sapphire substrate according to claim 1, wherein in the step (3), the MOCVD equipment cavity is slowly heated to the growth temperature of 950-1050 ℃ for 8-11 minutes, and is kept at the constant temperature for 4-8 minutes.
6. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 1, wherein in the step (3), H is2The introduction amount of S is 0.05-0.5 slm.
7. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 1, wherein in the step (3), H is2S is introduced for 5-15 minutes and then Mo (CO) is introduced6And (4) a gas source.
8. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 1, wherein in the step (3), Mo (CO)6The gas source is introduced at a rate of 2X 10-5～9×10-5slm。
9. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 1, wherein in the step (3), MoS is performed at a growth temperature of 950 to 1050 ℃2Growing for 3-15 minutes at constant temperature.
10. The method for preparing a molybdenum sulfide two-dimensional material grown on a sapphire substrate according to claim 1, wherein in the step (3), after the constant-temperature growth is completed, Mo (CO) is stopped6Gas source, keeping introducing H2S gas source, then cooling, and stopping H2The air source of the S is introduced into the reactor,and obtaining the molybdenum sulfide two-dimensional material grown on the sapphire substrate.
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| CN111254491A (en) * | 2020-03-19 | 2020-06-09 | 四川大学 | Preparation method of high-quality two-dimensional atomic layer film |
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| CN105002476A (en) * | 2015-07-07 | 2015-10-28 | 南京大学 | Method for growing substrate-modified large-size monolayer molybdenum disulfide film through chemical vapor deposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111254491A (en) * | 2020-03-19 | 2020-06-09 | 四川大学 | Preparation method of high-quality two-dimensional atomic layer film |
| CN111254491B (en) * | 2020-03-19 | 2021-08-10 | 四川大学 | Preparation method of high-quality two-dimensional atomic layer film |
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