CN110983249A - Preparation method of large-area continuous layered molybdenum sulfide - Google Patents
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Abstract
The invention discloses a preparation method of a large-area continuous layered molybdenum sulfide film, which comprises the following steps: s1, preparing MoO with the thickness of 10-20 nm on the surface of the substrate3Film, MoO3The film is in a grid structure or a lattice structure S2, and the substrate with the film is placed in a CVD furnace for vulcanization to obtain a continuous layered molybdenum sulfide film; magnetron sputtering using a templateOr atomic deposition, firstly preparing MoO with the thickness of 10-20 nm on a substrate3Film, and then MoO is formed by high temperature CVD method3Sulfurizing the film in high-temperature sulfur steam atmosphere to obtain layered continuous molybdenum sulfide film, and regulating MoO3The thickness of the film and the size of meshes and lattices in the template realize the control of the layer number and the continuity of the molybdenum sulfide film, and the high-quality large-area continuous layered molybdenum sulfide film is prepared.
Description
Technical Field
The invention relates to the technical field of preparation of special functional films, in particular to a preparation method of a large-area continuous layered molybdenum sulfide film.
Background
MoS2Is a material with a graphite-like structure, belongs to Transition-metal dichalcogenides (TMD), can be prepared into a single-layer or few-layer structure with a graphene-like structure, and the bulk material of the material is an indirect band gap semiconductor with 1.29eV, while the single-layer MoS is a single-layer MoS2A direct band gap characteristic is exhibited with a forbidden band width of 1.9 eV. The layered molybdenum sulfide can be used in the field of novel semiconductor electronic devices and optoelectronic devices. In addition, the catalyst has the characteristic of large specific surface area, and can be used as an electrochemical hydrogen evolution catalyst, a gas sensor and the like. In addition, due to its large layer spacing (MoS)2Interlayer spacing of about 0.65 nm) can introduce foreign atoms or molecules between the layers by an intercalation method, and the transition metal binary sulfide can be used as an electrode material intercalation main body which is well applied to a high-energy-density battery.
For the scale application of semiconductor electronic devices and optoelectronic devices, there are many methods for preparing single-layer or few-layer binary transition metal sulfides, including the conventional mechanical stripping method, lithium ion intercalation method and Chemical Vapor Deposition (CVD) method, and the conventional stripping method has a small product size, and the intercalation of lithium ions can cause the destruction of crystal structure, which affects the electrical and optical properties of the material. The limitation of the existing method is that only a crystal layer with a small area can be prepared, and the growth of a large surface cannot be realized.
Disclosure of Invention
The invention aims to provide a preparation method of a large-area continuous layered molybdenum sulfide film, which can be used for preparing a large-area continuous transition metal binary sulfide few-layer structure and realizing application in the aspect of semiconductor electronic devices.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a large-area continuous layered molybdenum sulfide film comprises the following steps:
s1, preparing MoO with the thickness of 10-20 nm on the surface of the substrate3Film, MoO3The film is in a grid structure or a lattice structure;
and S2, putting the substrate with the prepared film into a CVD furnace for sulfurization to obtain the continuous layered molybdenum sulfide film.
Further, the mesh size of the mesh structure in step S1 is 0.5 to 1000 μm.
Further, the dot diameter of the dot matrix structure in the step S1 is 0.5 to 1000 μm, and the distance between two adjacent dots is 0.5 to 1000 μm.
Further, step S1 is performed by using a mask, a photoresist or a PS colloidal particle template, and using a magnetron sputtering or atomic deposition process.
Further, the vulcanization in the step S2 includes a high temperature region and a low temperature region, and the high temperature region is sequentially heated or cooled at four stages of room temperature to 500 ℃, 500 ℃ to constant temperature, constant temperature heat preservation, and constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature area is 600-750 ℃, and the constant temperature of the low-temperature area is 200 DEG C
Further, in the step S5, the temperature rise rate of the high-temperature zone in the temperature-500 ℃ stage is 10 ℃/min, the temperature rise rate of the high-temperature zone in the temperature-500 ℃ stage is 5-10 ℃/min, and the time of the constant-temperature heat preservation stage of the high-temperature zone is 20-40 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 5-10 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20-40 min;
the stages from constant temperature to room temperature of the high-temperature area and the low-temperature area are naturally cooled.
The method has the beneficial effects that the substrate is modified by utilizing the template), and the MoO with the thickness of 10-20 nm is prepared on the substrate firstly by combining a magnetron sputtering or atomic deposition method3Film, and then MoO is formed by high temperature CVD method3Sulfurizing the film in high-temperature sulfur steam atmosphere to obtain layered continuous molybdenum sulfide film, and regulating MoO3Thickness of thin film and MoO3The size of the grid or the lattice realizes the control of the layer number and the continuity of the molybdenum sulfide film, and the high-quality large-area continuous layered molybdenum sulfide film is prepared.
Drawings
The invention is further illustrated with reference to the following figures and examples:
FIG. 1 is an optical microscope photograph of a layered molybdenum sulfide thin film prepared according to one embodiment of the present invention;
FIG. 2 is a Raman spectrum of a layered molybdenum sulfide thin film prepared according to a first embodiment of the present invention;
FIG. 3 is an optical microscope photograph of a layered molybdenum sulfide thin film prepared in example III of the present invention;
FIG. 4 is a Raman spectrum of a single-layer molybdenum sulfide thin film prepared in example III of the present invention;
fig. 5 is a raman spectrum of the double-layered molybdenum sulfide thin film prepared in example three of the present invention.
Detailed Description
Example one
The invention provides a preparation method of a large-area continuous layered molybdenum sulfide film, which comprises the following steps:
s1, taking a quartz plate with the size of 3cm by 3cm as a substrate, ultrasonically cleaning the substrate for 5 minutes by using a mixed solution of alcohol and acetone, then cleaning the substrate by using deionized water, and drying the substrate by using nitrogen;
fixing a stainless steel mask plate with the size slightly larger than that of the substrate and the aperture of 1000 mu m on the surface of the substrate, and then integrally placing the mask plate on a substrate fixing frame in a magnetron sputtering coating chamber;
the magnetron sputtering takes molybdenum as a target material, Ar and oxygen are respectively introduced into the target material at the flow rates of 30sccm and 6sccm, and chamber gasThe pressure is 1.0Pa, the sputtering power is 60W, the film coating is carried out on the surface of the substrate, the film coating time is controlled, and MoO with the thickness of 20nm is prepared3A film; taking out a sample wafer after film coating is finished, and taking down the stainless steel mask plate to obtain the lattice structure MoO3A film;
s2, placing the substrate with the prepared film in a high-temperature area of a CVD tube furnace, and placing elemental sulfur powder in a low-temperature area;
the tube furnace is vacuumized and N is introduced2As a carrier gas, the carrier gas flows through 300sccm, and the pressure in the tube is maintained to be slightly higher than the atmospheric pressure by 10-100 kPa;
the high-temperature area is sequentially heated and cooled according to four stages of room temperature to 500 ℃, constant temperature heat preservation, constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature area is 650 ℃, and the constant temperature of the low-temperature area is 200 ℃;
the temperature rise rate of the high-temperature region at the room temperature-500 ℃ stage is 10 ℃/min, the temperature rise rate of the high-temperature region at the 500-constant temperature stage is 5 ℃/min, and the time of the high-temperature region at the constant temperature heat preservation stage is 20 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 6 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20 min;
the stages of constant temperature to room temperature of the high-temperature area and the low-temperature area are naturally cooled, the vulcanization process is finished after cooling, the obtained layered molybdenum sulfide film is taken out, and the appearance, Raman spectrum and other representations are carried out, and the results are shown in the figure 1 and the figure 2.
Example two
The invention provides a preparation method of a large-area continuous layered molybdenum sulfide film, which comprises the following steps:
s1, taking a quartz plate with the size of 3cm by 3cm as a substrate, ultrasonically cleaning the substrate for 5 minutes by using a mixed solution of alcohol and acetone, then cleaning the substrate by using deionized water, and drying the substrate by using nitrogen;
fixing a lattice-shaped hole structure stainless steel mask plate which is slightly larger than the substrate in size, has the aperture of 1000 mu m and the hole spacing of 2000 mu m on the surface of the substrate, sticking the part of the mask plate extending out of the substrate on a substrate frame by using a high-temperature adhesive tape, and then integrally placing the mask plate on a substrate fixing frame in a magnetron sputtering coating chamber;
the magnetron sputtering takes molybdenum as a target material, Ar and oxygen are respectively introduced into the target material at the flow rates of 30sccm and 6sccm, the air pressure of a chamber is 1.0Pa, the sputtering power is 60W, the surface of the substrate is coated, the coating time is controlled, and MoO with the thickness of 20nm is prepared3A film; taking out a sample wafer after film coating is finished, and taking down the stainless steel mask plate to obtain the lattice structure MoO3A film;
s2, placing the substrate with the prepared film in a high-temperature area of a CVD tube furnace, and placing elemental sulfur powder in a low-temperature area;
the tube furnace is vacuumized and N is introduced2As a carrier gas, the carrier gas flows through 300sccm, and the pressure in the tube is maintained to be slightly higher than the atmospheric pressure by 10-100 kPa;
the high-temperature area is sequentially heated and cooled according to four stages of room temperature to 500 ℃, constant temperature heat preservation, constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature region is 680 ℃, and the constant temperature of the low-temperature region is 200 ℃.
The temperature rise rate of the high-temperature region at the room temperature-500 ℃ stage is 10 ℃/min, the temperature rise rate of the high-temperature region at the 500-constant temperature stage is 5 ℃/min, and the time of the high-temperature region at the constant temperature heat preservation stage is 20 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 6 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20 min;
and naturally cooling the high-temperature area and the low-temperature area at the constant temperature-room temperature stage, finishing the vulcanization process after cooling, and taking out the obtained layered molybdenum sulfide film.
EXAMPLE III
The invention provides a preparation method of a large-area continuous layered molybdenum sulfide film, which comprises the following steps:
s1, taking a quartz plate with the size of 3cm by 3cm as a substrate, ultrasonically cleaning the substrate for 5 minutes by using a mixed solution of alcohol and acetone, then cleaning the substrate by using deionized water, and drying the substrate by using nitrogen;
fixing a stainless steel mask plate with the size slightly larger than that of the substrate and the aperture of 1000 mu m on the surface of the substrate, and then integrally placing the mask plate on a substrate fixing frame in a magnetron sputtering coating chamber;
the magnetron sputtering takes molybdenum as a target material, Ar and oxygen are respectively introduced into the target material at the flow rates of 30sccm and 6sccm, the air pressure of a chamber is 1.0Pa, the sputtering power is 60W, the surface of the substrate is coated, the coating time is controlled, and MoO with the thickness of 20nm is prepared3A film; taking out a sample wafer after film coating is finished, and taking down the stainless steel mask plate to obtain the lattice structure MoO3A film;
s2, placing the substrate with the prepared film in a high-temperature area of a CVD tube furnace, and placing elemental sulfur powder in a low-temperature area;
the tube furnace is vacuumized and N is introduced2As a carrier gas, the carrier gas flows through 300sccm, and the pressure in the tube is maintained to be slightly higher than the atmospheric pressure by 10-100 kPa;
the high-temperature area is sequentially heated and cooled according to four stages of room temperature to 500 ℃, constant temperature heat preservation, constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature region is 700 ℃, and the constant temperature of the low-temperature region is 200 ℃.
The temperature rise rate of the high-temperature region at the room temperature-500 ℃ stage is 10 ℃/min, the temperature rise rate of the high-temperature region at the 500-constant temperature stage is 5 ℃/min, and the time of the high-temperature region at the constant temperature heat preservation stage is 20 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 6 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20 min;
the stages of constant temperature to room temperature of the high-temperature area and the low-temperature area are naturally cooled, the vulcanization process is finished after cooling, the obtained layered molybdenum sulfide film is taken out, and the appearance, Raman spectrum and other representations are carried out, and the results are shown in figures 3 to 5.
Example four
The invention provides a preparation method of a large-area continuous layered molybdenum sulfide film, which comprises the following steps:
s1, taking a quartz plate with the size of 3cm by 3cm as a substrate, ultrasonically cleaning the substrate for 5 minutes by using a mixed solution of alcohol and acetone, then cleaning the substrate by using deionized water, and drying the substrate by using nitrogen;
fixing a stainless steel mask plate with the size slightly larger than that of the substrate and the aperture of 1000 mu m on the surface of the substrate, and then integrally placing the mask plate on a substrate fixing frame in a magnetron sputtering coating chamber;
the magnetron sputtering takes molybdenum as a target material, Ar and oxygen are respectively introduced into the target material at the flow rates of 30sccm and 6sccm, the air pressure of a chamber is 1.0Pa, the sputtering power is 60W, the surface of the substrate is coated, the coating time is controlled, and MoO with the thickness of 20nm is prepared3A film; taking out a sample wafer after film coating is finished, and taking down the stainless steel mask plate to obtain the lattice structure MoO3A film;
s2, placing the substrate with the prepared film in a high-temperature area of a CVD tube furnace, and placing elemental sulfur powder in a low-temperature area;
the tube furnace is vacuumized and N is introduced2As a carrier gas, the carrier gas flows through 300sccm, and the pressure in the tube is maintained to be slightly higher than the atmospheric pressure by 10-100 kPa;
the high-temperature area is sequentially heated and cooled according to four stages of room temperature to 500 ℃, constant temperature heat preservation, constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature region is 720 ℃, and the constant temperature of the low-temperature region is 200 ℃.
The temperature rise rate of the high-temperature region at the room temperature-500 ℃ stage is 10 ℃/min, the temperature rise rate of the high-temperature region at the 500-constant temperature stage is 5 ℃/min, and the time of the high-temperature region at the constant temperature heat preservation stage is 20 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 6 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20 min;
and naturally cooling the high-temperature area and the low-temperature area at the constant temperature-room temperature stage, finishing the vulcanization process after cooling, and taking out the obtained layered molybdenum sulfide film.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (6)
1. A preparation method of a large-area continuous layered molybdenum sulfide film is characterized by comprising the following steps:
s1, preparing MoO with the thickness of 10-20 nm on the surface of the substrate3Film, MoO3The film is in a grid structure or a lattice structure;
and S2, putting the substrate with the prepared film into a CVD furnace for sulfurization to obtain the continuous layered molybdenum sulfide film.
2. The method as claimed in claim 1, wherein the mesh size of the mesh structure in step S1 is 0.5-1000 μm.
3. The method as claimed in claim 1, wherein the dot diameter of the lattice structure in step S1 is 0.5-1000 μm, and the distance between two adjacent dots is 0.5-1000 μm.
4. The method for preparing a large-area continuous layered molybdenum sulfide film as claimed in claim 1, wherein step S1 is performed by magnetron sputtering or atomic deposition using a mask, a photoresist or a PS colloidal particle template.
5. The method for preparing a large-area continuous layered molybdenum sulfide film as claimed in claim 1, wherein the step S2 comprises a high temperature region and a low temperature region, wherein the high temperature region is sequentially heated or cooled at four stages of room temperature to 500 ℃, 500 ℃ to constant temperature, constant temperature heat preservation, and constant temperature to room temperature; the low-temperature area is heated and cooled sequentially according to three stages of room temperature-constant temperature, constant-temperature heat preservation and constant-temperature-room temperature; the constant temperature of the high-temperature region is 600-750 ℃, and the constant temperature of the low-temperature region is 200 ℃.
6. The method for preparing a large-area continuous layered molybdenum sulfide film according to claim 5, wherein the temperature rise rate in the stage from the high temperature zone to 500 ℃ in the step S5 is 10 ℃/min, the temperature rise rate in the stage from 500 ℃ to the constant temperature zone is 5-10 ℃/min, and the time in the constant temperature heat preservation stage in the high temperature zone is 20-40 min;
the temperature rise rate of the low-temperature region from room temperature to constant temperature is 5-10 ℃/min, and the time of the low-temperature region constant temperature heat preservation stage is 20-40 min.
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