SiO2 / MoS2 chemical vapor deposition preparation method
By depositing SiO2 films on silicon wafer substrates and controlling their morphology, and preparing MoS2 on SiO2 in combination with chemical vapor deposition technology, the complex problem of MoS2 morphology control in the prior art is solved, and a simple and controllable large-scale production is achieved, suitable for a variety of electronic and optoelectronic device applications.
Patent Information
- Application Number
- CN202411828606.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-12
- Publication Date
- 2025-03-18
AI Technical Summary
The prior art has complex and cumbersome control process on the MoS2 morphology in chemical vapor deposition, and the substrate thickness has an impact on visible optical absorption, making it difficult to achieve simple and controllable large-scale production.
A SiO2/MoS2 chemical vapor deposition preparation method is adopted. By depositing SiO2 film on the silicon wafer substrate and dividing the reaction chamber into multiple separate spatial areas using the silicon plate substrate in the soft plasma reaction chamber, the morphology of the SiO2 film is controlled, and then MoS2 deposition is performed on the SiO2 film to achieve MoS2 preparation with different morphology.
The operation steps are simplified, the preparation efficiency is improved, the materials are easy to obtain, the production cost is low, the reaction conditions are simple and controllable, the demand for instruments and equipment is low, and the prepared SiO2/MoS2 has a periodic layered morphology, which is suitable for electronic and optoelectronic devices.
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Figure CN119640230A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of nanomaterials, and in particular to a SiO2 / MoS2 chemical vapor deposition preparation method. Background Art
[0002] Transition Metal Dichalcogenides (TMDs) are a class of materials with a layered structure, consisting of two layers of chalcogen atoms (S, Se or Te) sandwiched by a layer of transition metal atoms (such as Ti, Zr, Hf, Mo, W, etc.), forming a sandwich-like structure. Transition metal dichalcogenides are MX2-type semiconductors. Where M is a transition metal atom, such as Mo, W, etc.; X is a chalcogen atom, such as S, Se, Te, etc. Transition metal dichalcogenides have atomic-level thickness, strong spin-orbit coupling, and good electronic and mechanical properties. Among these transition metal dichalcogenides, MoS2 has attracted much attention due to its unique structure and excellent properties.
[0003] MoS2 is a typical representative of transition metal sulfides, and its layers are connected by van der Waals forces; the band gap of MoS2 changes with the number of layers. Its bulk MoS2 has an indirect band gap of 1.29eV, the valence band top (VBM) is located at the Γ point, and the conduction band bottom (CBM) is located at the low symmetry point of the Brillouin zone. In the case of a single layer of MoS2, the VBM and CBM are located at the same κ position, so the single layer of MoS2 is a direct band gap with a band gap of 1.9eV. Due to the unique structure and properties of MoS2, it is often used to study its visible light absorption characteristics. MoS2 is abundant in reserves and low in cost. A wide variety of MoS2 with different surface microstructures and layers can be obtained. Its different number of layers and morphologies have different effects on the absorption of visible light. Therefore, studying the effects of its surface structure and number of layers on optical absorption has an important impact on solving the energy crisis.
[0004] The research on the optical properties of two-dimensional materials includes light absorption, photoluminescence, optical enhancement, modulation and control, nonlinear effects, sensing and detection, waveguides and resonant cavities, etc. These studies provide theoretical basis and practical guidance for the application of two-dimensional materials in optoelectronics, optical communications, sensor technology and other fields, and promote the development of related technologies. Two-dimensional materials such as MoS2 have become a hot spot in optical research due to their unique structure and properties, and have brought new possibilities for the development of future optical devices and systems. Although MoS2 has application prospects in many fields, the research on its periodic surface structure is relatively small. Current research mainly focuses on the characterization of atomic-level flatness of MoS2 single crystal surface, the application potential of the surface in fields such as photocatalysis and optoelectronic devices, and the study of surface defects, doping and heterostructures to optimize its performance.
[0005] At present, chemical vapor deposition has been proven to be the most effective method for preparing crystalline TMDs. The morphology of MoS2 is generally focused on the study of the visible light absorption of MoS2 with natural unique morphology or MoS2 with morphology controlled by chemical vapor deposition. However, the process of controlling the morphology of MoS2 in chemical vapor deposition is relatively complicated and tedious, and the thickness of the substrate also affects the visible optical absorption of MoS2.
[0006] Wu Peng, Tan Tan and others proposed to prepare large-area MoS2 thin films by CVD. First, the Si / SiO2 wafer was cut into 5x5 mm square pieces, cleaned with acetone and isopropanol respectively, and then blown dry for use. Next, 50 mg MoO3 was dispersed in 10 ml of anhydrous ethanol and evenly dispersed using ultrasound for 10 minutes. Next, the Si / SiO2 substrate was placed upside down on the Si dripped with MoO3 dispersion to form a confined space, and argon was used as a carrier gas to ensure that the S source entered the confined space. Before the experiment began, the S powder was placed in a quartz boat under the carbon cloth heat source so that S could obtain enough heat to reach the evaporation temperature and react chemically with the MoO3 oxide on the Si substrate. During the entire growth process, 10 sccm argon was used as a carrier gas and the experiment was carried out under normal pressure. The experiment was divided into two stages. The first stage was the sulfurization stage. The temperature of the carbon cloth was raised to 550°C to keep the S precursor evaporated and ensure that there was enough S in the environment. The second stage is the growth stage, where the temperature of the carbon cloth is raised to 750°C and maintained for 900 seconds, during which MoO3 and S react chemically in the confined space. After the experiment, the carbon cloth is gradually cooled to room temperature. (Wu Peng, Tan Tan, Li Wei, et al. Preparation of large-area monolayer MoS2 and its photoelectric properties [J]. Acta Physica Sinica, 2023, 72(11): 302-308.).
[0007] The patent with publication number CN117276310A discloses a large-area two-dimensional material and a preparation method thereof, the preparation method comprising: providing a single crystal substrate; forming a single crystal thermal conductive layer on the single crystal substrate, the thermal conductivity of the single crystal thermal conductive layer being at least greater than the thermal conductivity of the sapphire substrate; and forming a two-dimensional material layer on the single crystal thermal conductive layer.
[0008] The patent with publication number CN220099176U discloses a gas transmission device for large-area preparation of two-dimensional materials. The device can control the corresponding gas transmission ratio when synthesizing two-dimensional materials, avoid the wrong proportion of synthetic materials due to atomic ratio imbalance, and enhance the preparation effect.
[0009] The above existing technologies mostly rely on complex, multi-step deposition methods for chemical vapor deposition of MoS2, and the method steps for controlling the surface morphology deposition are cumbersome and complex, usually requiring large equipment and harsh reaction conditions. Therefore, it is urgent to seek a new method for preparing SiO2 / MoS2 with simple and controllable reaction conditions, low demand for instruments and equipment, and large-scale production and application. Summary of the invention
[0010] The purpose of the present invention is to provide a SiO2 / MoS2 chemical vapor deposition preparation method, which can prepare MoS2 with different morphologies, the materials used are easy to obtain, the reaction conditions are simple and controllable, the requirements for instruments and equipment are low, and it can be used in large-scale production.
[0011] To achieve the above-mentioned purpose of the invention, the technical solution adopted by the present invention is: a SiO2 / MoS2 chemical vapor deposition preparation method, comprising the following steps:
[0012] S1, select a silicon wafer, clean it to remove impurities, dry it, and then polish it to obtain a uniform and flat silicon wafer as a deposition substrate; fix the deposition substrate at one end of the gas outlet of the soft plasma reaction chamber;
[0013] S2. Under room temperature, TEOS is placed in a quartz boat in a reaction chamber, and precursor nitrogen is introduced to blow TEOS onto a deposition substrate. Then, a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS, and the reaction deposition is performed at a temperature of 100 to 500° C. for 10 to 60 minutes to obtain a flat SiO2 film of a certain thickness.
[0014] S3, a plurality of silicon plate substrates are horizontally arranged in a soft plasma reaction chamber to divide the space in the soft plasma reaction chamber into several separate space areas, and one end of all silicon plate substrates close to the gas outlet is in contact with the SiO2 film on the substrate deposited in step S2; a quartz boat is placed on each silicon plate substrate; SiO2 deposition is performed separately in each separate space area by controlling the position of the air inlet pipe, and SiO2 films with different morphologies are obtained on the deposition substrate by changing the amount of TEOS added to the quartz boat; the specific deposition process is: at room temperature, TEOS is placed in all quartz boats on the silicon plate substrate, precursor nitrogen is introduced to blow TEOS onto the deposition substrate, and then a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS, and deposition is performed at a temperature of 100 to 500° C. for 10 to 60 minutes. After the deposition is completed, the movably arranged silicon-based substrate is removed to make the soft plasma reaction chamber an integral space area, and SiO2 films with different shapes are formed on the deposition substrate;
[0015] S4, after the chemical vapor deposition is completed and SiO2 is annealed, MoS2 is chemically vapor deposited on the SiO2 thin film substrate, and the specific steps are: introduce argon gas, place sulfur powder in the quartz boat near the air inlet, and then place a mixture of MoO3 and NaCl in the quartz boat near the air outlet, wherein NaCl is used as a combustion aid to promote the growth and accumulation of MoS2; the quartz boat near the air inlet is heated to 190°C, and the quartz boat near the air outlet is heated to 760°C, and maintained at atmospheric pressure for 10-60 minutes, sulfur powder, MoO3 and NaCl flow together with argon gas to react to obtain MoS2, and MoS2 is deposited on the SiO2 film obtained in step S3, and after annealing, SiO2 / MoS2 with a periodic layered morphology is obtained.
[0016] Furthermore, in step S3, a frame device with holes of different shapes in the middle is arranged in each separate space area perpendicular to the silicon-based substrate and close to the gas outlet of the soft plasma reaction chamber; the frame device is removed after the SiO2 deposition is completed.
[0017] Preferably, in step S2 and step S3, the nitrogen flow rate is 0.1-5.0 slm; the ozone volume concentration in the mixed gas is controlled at 1-5%; and the partial pressure of TEOS is 0.5-5 Torr.
[0018] Furthermore, in step S3, 2-3 silicon plates are placed in the reaction chamber.
[0019] Preferably, in step S4, the volume flow rate of argon gas is 40-200 sccm.
[0020] Furthermore, in step S1, the silicon wafer is ultrasonically cleaned with acetone, anhydrous ethanol and deionized water in sequence, each time for 5 minutes.
[0021] The preparation process of chemical vapor deposition (CVD) periodic morphology SiO2 / MoS2 is mainly divided into three steps: first, a flat SiO2 film of a certain thickness is deposited on the deposition substrate by chemical vapor deposition; this flat SiO2 has good thermal and chemical stability, and the thickness of the substrate affects the material's absorption of visible light; the deposition of SiO2 provides preparation for the subsequent deposition of morphology on its surface. Next, the reaction chamber is divided into several areas by a silicon plate substrate, so that each area can be subjected to separate chemical vapor deposition. By changing the amount of TEOS added to the quartz boat and adding a frame device with holes of different shapes, SiO2 films of different thicknesses and morphologies are deposited in each area. This step can control the morphology of the material surface and prepare for the next step of depositing MoS2 with different morphologies; finally, the silicon plate substrate used to divide the area is removed, and MoS2 is deposited on SiO2 by chemical vapor deposition. Since the required surface morphology has been formed in the second step, MoS2 can be directly deposited on the SiO2 surface in the last step. The morphology of MoS2 has different effects on the absorption of visible light, so this method can obtain SiO2 / MoS2 with periodic morphology. This structure has unique electrical properties and interface characteristics and is suitable for various electronic and optoelectronic device applications.
[0022] Compared with the prior art, the present invention has the following beneficial effects:
[0023] The present invention discloses a method for depositing molybdenum disulfide of different morphologies on silicon dioxide. The method first forms silicon dioxide layers of different thicknesses on the surface of a deposition substrate by finely controlling the process of chemical vapor deposition, and these layers can exhibit specific geometric morphologies, that is, controllable growth and morphology design of silicon dioxide are achieved by precisely controlling the deposition conditions; and then molybdenum disulfide is deposited by chemical vapor deposition. The method simplifies the operation steps and improves the preparation efficiency by realizing the control of the SiO2 morphology on the MoS2 surface morphology in a single reaction chamber; in addition, the materials used in the method of the present invention are easy to obtain, the production cost is low, the reaction conditions are simple and controllable, the demand for instruments and equipment is low, and it has the potential for large-scale production and application. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 A schematic diagram of a chemical vapor deposition apparatus used in Example 1 of the present invention;
[0025] Figure 2 A schematic diagram of a chemical vapor deposition apparatus used in Example 2 of the present invention;
[0026] Figure 3 are the absorption curves of the samples prepared in Examples 1-2 of the present invention in the visible light range;
[0027] Figure 4 This is a SEM image of MoS2 with a convex morphology prepared in Example 1 of the present invention;
[0028] Figure 5 This is a SEM image of MoS2 with a cylindrical morphology prepared in Example 2 of the present invention;
[0029] In the figure, 1. soft plasma reaction chamber, 2. silicon-based substrate, 3. quartz boat, 4. deposition substrate, 5. frame equipment. DETAILED DESCRIPTION
[0030] The present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.
[0031] The sulfur powder used in the following examples was purchased through the McLean Reagent Network, with a CAS number of 7704-34-9, a molecular weight of 32.07, a size of 50G, and a purity of 99.98% as a powder sample; TEOS was purchased through the McLean Reagent Network, with a CAS number of 78-10-4, a molecular weight of 208.33, a size of 25ml, and a purity of 90% as a liquid sample; MoO3 was purchased through the McLean Reagent Network, with a CAS number of 1313-27-5, a size of 5G, a molecular weight of 143.94, and a purity of 99.97 as a powder sample.
[0032] Embodiment 1
[0033] A method for preparing SiO2 / MoS2 by chemical vapor deposition, a schematic diagram of a chemical vapor deposition device used in the method is shown in FIG. Figure 1 As shown, the following steps are included:
[0034] S1. Select a silicon wafer with a size of 6cm*6cm, clean it with acetone, anhydrous ethanol and deionized water to remove impurities, dry the surface of the silicon wafer with a drying gun, and then polish it to obtain a uniform and flat silicon wafer as a deposition substrate 4; fix the deposition substrate 4 at one end of the gas outlet of the soft plasma reaction chamber 1;
[0035] S2. Chemical vapor deposition of SiO2 depends on the reaction efficiency and the utilization rate of TEOS. It can be concluded from the formula: m = density * area * thickness that if the deposition substrate 4 has an area of 6cm * 6cm and a thickness of 100nm, at least 0.729mg of TEOS is required. However, in the actual reaction, since the efficiency cannot reach 100% conversion, at least 0.99mg is required. Under room temperature, 1.mg TEOS is placed in the quartz boat 3 in the reaction chamber, and the precursor nitrogen gas is introduced to blow TEOS onto the deposition substrate 4. Then, 0.5slm of a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS. The volume concentration of ozone in the mixed gas is controlled at 5%. The reaction is deposited at a temperature of 100°C for 20min to obtain a 100nm thick flat SiO2 film.
[0036] S3, two silicon plate substrates 2 are arranged horizontally and movably in the soft plasma reaction chamber 1, and the soft plasma reaction chamber 1 is equally divided into three separate space areas, and one end of all silicon plate substrates 2 close to the gas outlet is in contact with the SiO2 film on the substrate 4 deposited in step S2; a quartz boat 3 is placed on each silicon plate substrate 2; by controlling the position of the air inlet pipe, chemical vapor deposition is performed again in the middle space area, and chemical vapor deposition is not performed in the other two space areas; according to the formula of step S2, at least 0.264 mg of TEOS is calculated, and 0.3 mg of TEOS is placed in the quartz boat 3 in the middle area, and chemical vapor deposition of 10 nm thick planar SiO2 is performed again, and 0.5 slm O3 / O2 is introduced in this process, and the volume concentration of ozone in the mixed gas is controlled at 5%, and the reaction deposition is carried out at a temperature of 100°C for 20 minutes; after the deposition is completed, the two silicon-based substrates 2 that are arranged movably are removed, so that the soft plasma reaction chamber 1 is an integral space area, and a SiO2 film in the shape of a convex character is formed on the deposition substrate 4;
[0037] S4, after the chemical vapor deposition is completed and SiO2 is annealed, MoS2 is chemically vapor deposited on the SiO2 thin film substrate, and the specific steps are: introduce argon gas (40sccm), place 0.8mg sulfur powder in the quartz boat 3 near the air inlet, and then place a mixture of 3.5mg MoO3 and 3.5mg NaCl in the quartz boat 3 near the air outlet, wherein NaCl is used as a combustion aid to promote the growth and accumulation of MoS2; the vicinity of the quartz boat 3 near the air inlet is heated to 190°C within 25min, and the vicinity of the quartz boat 3 near the air outlet is heated to 760°C within 25min, and maintained at atmospheric pressure for 15min, sulfur powder, MoO3 and NaCl flow together with argon gas to react to obtain MoS2, and MoS2 is deposited on the SiO2 film obtained in step S3, and after waiting for annealing, a film with a thickness of 10nm and an area of 36cm 2 The convex shape of MoS2 (such as Figure 4shown).
[0038] like Figure 3 As shown in the figure, the convex morphology MoS2 has a very smooth and high absorption curve. The advantages of convex morphology MoS2 mainly include high surface / volume ratio, tunable surface chemistry and special electronic properties. These advantages make convex morphology MoS2 show excellent sensitivity in chemical gas sensor applications and show potential application value in fields such as electrochemical catalytic hydrogen evolution. However, the specific advantages still need to be comprehensively evaluated based on factors such as the specific morphology, size, preparation process and application field of MoS2.
[0039] Embodiment 2
[0040] A method for preparing SiO2 / MoS2 by chemical vapor deposition, a schematic diagram of a chemical vapor deposition device used in the method is shown in FIG. Figure 2 As shown, the following steps are included:
[0041] S1. Select a silicon wafer with a size of 9 cm*9 cm, clean it with acetone, anhydrous ethanol and deionized water to remove impurities, dry the surface of the silicon wafer with a drying gun, and then polish it to obtain a uniform and flat silicon wafer as a deposition substrate 4; fix the deposition substrate 4 at one end of the gas outlet of the soft plasma reaction chamber 1;
[0042] S2. Chemical vapor deposition of SiO2 depends on the reaction efficiency and the utilization rate of TEOS. It can be concluded from the formula: m = density * area * thickness that if the deposition substrate 4 has an area of 6cm * 6cm and a thickness of 100nm, at least 0.729mg of TEOS is required; under room temperature, 1mg of TEOS is placed in the quartz boat 3 in the reaction chamber, and the precursor nitrogen gas is introduced to blow TEOS onto the deposition substrate 4, and then 1.0slm of a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS, and the volume concentration of ozone in the mixed gas is controlled at 5%. The reaction and deposition are carried out at a temperature of 100°C for 40min to obtain a 200nm thick flat SiO2 film;
[0043] S3, two silicon plate substrates 2 are arranged horizontally and movably in the soft plasma reaction chamber 1, and the soft plasma reaction chamber 1 is equally divided into three separate spatial regions, and the ends of all silicon plate substrates 2 close to the gas outlet are in contact with the SiO2 film on the substrate 4 deposited in step S2; a quartz boat 3 is placed on each silicon plate substrate 2; in each separate spatial region, a square frame device 5 with a circular hole in the middle is arranged perpendicular to the silicon-based substrate 2 and close to the gas outlet of the soft plasma reaction chamber 1, and the radius of the circular hole is 1 cm; then, chemical vapor deposition of 10nm thick SiO2 is carried out in each region, and since there is a frame device 5 in each region to block the deposited SiO2, cylindrical SiO2 can be formed in each region; according to the formula of step S2, at least 0.0086mg TEOS is required to be placed in the quartz boat 3 in each spatial region, 0.01mg TEOS is placed in the quartz boat 3 in each spatial region, and 2.0slm O3 / O2, the ozone volume concentration in the mixed gas is controlled at 5%, and the reaction deposition is carried out at a temperature of 100°C for 20 minutes; after the deposition is completed, the two silicon-based substrates 2 that are set up and the frame device 5 are removed, so that the soft plasma reaction chamber 1 is an integral space area, and periodic cylindrical SiO2 is formed on the deposition substrate 4;
[0044] S4, after the chemical vapor deposition SiO2 is annealed, chemical vapor deposition of MoS2 is performed on the SiO2 thin film substrate, the specific steps are: introduce argon gas (40sccm), place 3.24mg sulfur powder in the quartz boat 3 near the air inlet, and then place a mixture of 14.5mg MoO3 and 3.0mg NaCl in the quartz boat 3 near the air outlet, wherein NaCl is used as a combustion aid to promote the growth and accumulation of MoS2; the vicinity of the quartz boat 3 near the air inlet is heated to 190°C within 25min, and the vicinity of the quartz boat 3 near the air outlet is heated to 760°C within 25min, and maintained at atmospheric pressure for 15min, sulfur powder, MoO3 and NaCl flow together with argon gas to react to obtain MoS2, and MoS2 is deposited on the SiO2 film obtained in step S3, and after waiting for annealing, cylindrical MoS2 (such as Figure 5 As shown), each cylinder has a radius of 1 cm and a thickness of 10 nm.
[0045] like Figure 3 As shown, the cylindrical shape increases the optical absorption at short wavelengths. MoS2 with cylindrical morphology has excellent charge transfer performance and a high specific surface area, which is beneficial to improving its performance advantages in electrochemical energy storage, catalysis, and sensing.
[0046] The above is only a preferred specific implementation manner of the present invention, and the protection scope of the present invention is not limited thereto. Any simple change or equivalent replacement of the technical solution that can be obviously obtained by any technician familiar with the technical field within the technical scope disclosed in the present invention falls within the protection scope of the present invention.
Claims
1. A SiO2 / MoS2 chemical vapor deposition preparation method, characterized in that: The following steps are involved: S1, selecting a silicon wafer, cleaning it to remove impurities, drying it, and then polishing it to obtain a uniform and flat silicon wafer as a deposition substrate (4); fixing the deposition substrate (4) at one end of the gas outlet of the soft plasma reaction chamber (1); S2. Under room temperature, TEOS is placed in a quartz boat (3) in a reaction chamber, and precursor nitrogen gas is introduced to blow TEOS onto a deposition substrate (4). Then, a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS, and the reaction deposition is performed at a temperature of 100 to 500° C. for 10 to 60 minutes to obtain a flat SiO2 film of a certain thickness; S3, a plurality of silicon plate substrates (2) are arranged horizontally and movably in the soft plasma reaction chamber (1), so as to divide the space in the soft plasma reaction chamber (1) into several separate space areas, and the ends of all silicon plate substrates (2) close to the gas outlet are in contact with the SiO2 film on the deposition substrate (4) in step S2; a quartz boat (3) is placed on each silicon plate substrate (2); SiO2 deposition is performed in each separate space area by controlling the position of the gas inlet pipe, and different amounts of TEOS added to the quartz boat (3) are obtained on the deposition substrate (4). SiO2 films of the same morphology; the specific deposition process is: at room temperature, TEOS is placed in all quartz boats on a silicon plate substrate (2), precursor nitrogen is introduced to blow TEOS onto a deposition substrate (4), and then a mixed gas of O3 and O2 is introduced into the reaction chamber to react with TEOS, and deposition is performed at a temperature of 100 to 500° C. for 10 to 60 minutes. After the deposition is completed, the movable silicon-based substrate (2) is removed, so that the soft plasma reaction chamber (1) is an integral space area, and SiO2 films of different shapes are formed on the deposition substrate (4); S4, after the chemical vapor deposition is completed and SiO2 is annealed, MoS2 is chemically vapor deposited on the SiO2 thin film substrate, and the specific steps are: introducing argon gas, placing sulfur powder in the quartz boat (3) near the air inlet, and then placing a mixture of MoO3 and NaCl in the quartz boat (3) near the air outlet, wherein NaCl is used as a combustion aid to promote the growth and accumulation of MoS2; the vicinity of the quartz boat (3) near the air inlet is heated to 190° C., and the vicinity of the quartz boat (3) near the air outlet is heated to 760° C., and maintained at atmospheric pressure for 10-60 minutes, sulfur powder, MoO3 and NaCl flow together with argon gas to react to obtain MoS2, and MoS2 is deposited on the SiO2 film obtained in step S3, and after annealing, a periodic layered morphology of SiO2 / MoS2 is obtained.
2. A SiO2 / MoS2 chemical vapor deposition preparation method according to claim 1, characterized in that: In step S3, a frame device (5) having holes of different shapes in the middle is arranged in each separate space area perpendicular to the silicon-based substrate (2) and close to the gas outlet of the soft plasma reaction chamber (1); and the frame device (5) is removed after the SiO2 deposition is completed.
3. A SiO2 / MoS2 chemical vapor deposition preparation method according to claim 1 or 2, characterized in that: In step S2 and step S3, the nitrogen flow rate is 0.1-5.0 slm; the ozone volume concentration in the mixed gas is controlled at 1-5%, and the partial pressure of TEOS is 0.5-5 Torr.
4. A SiO2 / MoS2 chemical vapor deposition preparation method according to claim 1 or 2, characterized in that: In step S3, 2-3 silicon plates are placed in the reaction chamber.
5. A SiO2 / MoS2 chemical vapor deposition preparation method according to claim 1 or 2, characterized in that: In step S4, the volume flow rate of argon gas is 40-200 sccm.
6. A SiO2 / MoS2 chemical vapor deposition preparation method according to claim 1 or 2, characterized in that: In step S1, the silicon wafer is ultrasonically cleaned with acetone, anhydrous ethanol and deionized water in sequence, each time for 5 minutes.
Citation Information
Patent Citations
Large-area two-dimensional material and preparation method thereof
CN117276310A
Gas transmission device for large-area preparation of two-dimensional material
CN220099176U