CN114182230A - Chemical vapor deposition method for preparing two-dimensional tellurine film - Google Patents
Chemical vapor deposition method for preparing two-dimensional tellurine film Download PDFInfo
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- CN114182230A CN114182230A CN202111425591.3A CN202111425591A CN114182230A CN 114182230 A CN114182230 A CN 114182230A CN 202111425591 A CN202111425591 A CN 202111425591A CN 114182230 A CN114182230 A CN 114182230A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/28—Deposition of only one other non-metal element
Abstract
The invention discloses a chemical vapor deposition method for preparing a two-dimensional tellurium alkene film, which comprises the following steps: placing a growth substrate and an auxiliary substrate in a chemical vapor deposition furnace, wherein the auxiliary substrate is positioned below the growth substrate, introducing inert gas into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate; wherein the auxiliary substrate is a metal substrate, and the metal is capable of forming an alloy with tellurium. The invention utilizes a chemical vapor deposition method, and aims to uniformly and controllably provide tellurium sources from the eutectic body in the whole growth process after tellurium and metal form a solid solution in the growth process by introducing a metal substrate, so that a high-quality two-dimensional telluroene film is finally prepared. The invention can avoid the problem of nonuniform time-space distribution of the solid precursor adopted in the traditional vapor deposition method in the growth process, and avoids the thickness nonuniformity of the final product.
Description
Technical Field
The invention relates to the technical field of two-dimensional materials, in particular to a chemical vapor deposition method for preparing a two-dimensional telluroene film.
Background
In recent years, two-dimensional atomic crystals have been widely used in various fields such as photoelectrons, energy sources, and catalysis due to their excellent properties in various aspects such as optics, electricity, and mechanics, and have become a new research hotspot in the field of semiconductor materials. Among them, the telluritene of the sixth main group is gradually another emerging hot material besides the elementary materials of phosphuritene, stannene, etc. due to its novel structure and properties. Tellurium is one of the members of chalcogen, crystal tellurium is a P-type narrow band gap semiconductor, the band gap size is about 0.33ev at room temperature, the crystal tellurium can be used in various fields of electrons, photoelectrons, thermoelectricity, piezoelectricity and the like, and the wide application of the crystal tellurium is attributed to the unique configuration of the tellurium, the crystal tellurium is a chain structure formed by a spiral chain and a hexagonal framework, wherein each spiral chain is formed by closely packing tellurium atoms, and the spiral chains further form the hexagonal framework to finally form the tellurium. Due to this unique configuration, tellurium-based materials exhibit some anisotropy during synthesis, and thus controlled growth of two-dimensional telluridines remains a significant challenge.
At present, most of two-dimensional tellurine synthesis methods are prepared by adopting a traditional liquid phase method, and although the liquid phase method can obtain a thin layer or even a single layer of two-dimensional tellurine, the defects of a final product are more and the device performance is difficult to improve. In addition, some subjects adopt molecular beam epitaxy and physical vapor deposition to obtain the telluroene, but the thickness and the size of a synthetic product are limited to a certain extent, and the large-scale application cannot be realized.
Accordingly, the prior art remains to be improved and developed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a chemical vapor deposition method for preparing a two-dimensional telluroene film, aiming at solving the problem of uneven thickness of the two-dimensional telluroene film prepared by the existing method.
The technical scheme of the invention is as follows:
a chemical vapor deposition method for preparing a two-dimensional tellurine film, comprising the steps of: placing a growth substrate and an auxiliary substrate in a chemical vapor deposition furnace, wherein the auxiliary substrate is positioned below the growth substrate, introducing inert gas into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate; wherein the auxiliary substrate is a metal substrate, and the metal is capable of forming an alloy with tellurium.
Optionally, the growth substrate is one of a mica substrate and a sapphire substrate.
Further optionally, the growth substrate is a mica substrate.
Optionally, the auxiliary substrate is a copper foil.
Optionally, the chemical vapor deposition furnace is a single temperature zone tube furnace.
Optionally, the growth temperature is 500 ℃ to 700 ℃.
Optionally, the growth time is from 5 minutes to 30 minutes.
Optionally, the flow rate of the inert gas is 50sccm to 200 sccm.
Optionally, the inert gas is argon or nitrogen.
Optionally, the method specifically includes the steps of: and placing the mica substrate and the copper foil in a tube furnace, wherein the copper foil is positioned below the mica substrate, introducing argon into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate.
Compared with the existing method for growing the two-dimensional telluroene, the method has the following beneficial effects:
(1) the method adopted by the invention has lower requirements on experimental equipment, simple operation flow and high feasibility of specific implementation.
(2) The method adopted by the invention introduces the metal substrate as an auxiliary substrate, forms the eutectic body by metal and tellurium, so that tellurium can be controlled and uniformly provided by the eutectic body in the whole growth process, the growth substrate is used as a substrate for epitaxial growth, and finally the high-quality direction-controllable two-dimensional tellurium-alkene film is prepared.
(3) The substrate is placed in a special mode, the growth substrate is buckled on the auxiliary substrate in an inverted mode to form a reaction micro-cavity, and the tellurium sources are distributed in the reaction micro-cavity in a small difference in time and space, so that the two-dimensional tellurium-alkene film with uniform thickness can be obtained. And the reaction microcavity formed by the growth substrate and the auxiliary substrate can limit the growth of the tellurite in the three-dimensional direction, so that the two-dimensional tellurite film with controllable size and thickness can be obtained.
Drawings
Fig. 1 is an optical microscope photograph of the mica substrate in example 1.
Fig. 2 is an optical microscope photograph of the mica substrate in example 2.
Fig. 3 is a raman spectrum photograph of the two-dimensional tellurine deposited on the surface of the mica substrate in example 2.
FIG. 4 is an atomic force microscope photograph of the two-dimensional tellurine deposited on the surface of the mica substrate in example 2.
FIG. 5 is an electron diffraction photograph of the two-dimensional tellurine deposited on the surface of the mica substrate in example 2.
FIG. 6 is a high resolution atomic image of two-dimensional tellurine deposited on the surface of a mica substrate in example 2.
Fig. 7 is a photograph of the copper foil before and after growth in example 2.
Fig. 8 is an energy dispersive X-ray spectroscopy plot of the copper foil after growth in example 2.
Fig. 9 is an optical microscope photograph of the sapphire substrate in example 3.
FIG. 10 is a schematic diagram of the chemical vapor deposition of two-dimensional telluriene in examples 1-3.
Detailed Description
The invention provides a chemical vapor deposition method for preparing a two-dimensional tellurium alkene film, and in order to make the purpose, the technical scheme and the effect of the invention clearer and clearer, the invention is further described in detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a chemical vapor deposition method for preparing a two-dimensional tellurium alkene film, which comprises the following steps: placing a growth substrate and an auxiliary substrate in a chemical vapor deposition furnace, wherein the auxiliary substrate is positioned below the growth substrate, introducing inert gas into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate; wherein the auxiliary substrate is a metal substrate, and the metal is capable of forming an alloy with tellurium.
The conventional chemical vapor deposition method is a technique for efficiently synthesizing a two-dimensional material, but there are still many difficulties in actual synthesis due to the intrinsic structure of tellurine. In this embodiment, an auxiliary substrate (metal substrate) is introduced as an intermediate of a tellurium source by using a chemical vapor deposition method, and the purpose is to uniformly and controllably provide the tellurium source from the eutectic body in the whole growth process after tellurium and metal form a solid solution in the growth process, the growth substrate is used as a substrate for epitaxial growth, and finally, a high-quality direction-controllable two-dimensional tellurium-alkene thin film is prepared. The chemical vapor deposition method can avoid the problem of nonuniform time and space distribution of the solid precursor adopted in the traditional vapor deposition method in the growth process, and avoids the thickness nonuniformity of the final product.
Compared with the existing method for growing two-dimensional telluroene, the method has the following beneficial effects:
(1) the method adopted by the embodiment has low requirements on experimental equipment, simple operation flow and high feasibility of specific implementation.
(2) The method adopted by the embodiment introduces a metal substrate as an auxiliary substrate, and the metal can form a eutectic body with tellurium, so that tellurium can be uniformly and controllably provided by the eutectic body in the whole growth process through forming the eutectic body with tellurium.
(3) The substrate is placed in a special mode, the growth substrate is buckled on the auxiliary substrate in an inverted mode to form a reaction micro-cavity, and the tellurium sources are distributed in the reaction micro-cavity in a small difference in time and space, so that the two-dimensional tellurium-alkene film with uniform thickness can be obtained.
In the embodiment, the high-quality two-dimensional telluroene film is prepared by adopting the chemical vapor deposition method, and the purpose of further improving the quality of the two-dimensional telluroene film can be achieved by optimizing growth parameters. The growth parameters that can be optimized are growth temperature, growth time, carrier gas atmosphere and flow rate, and growth substrate and auxiliary substrate.
In one embodiment, the growth substrate is a mica substrate, a sapphire substrate or other substrates with certain symmetry, and the oriented substrate provides good epitaxial effect on deposition and growth of materials, so that a large-area single crystal film can be obtained.
Further, the growth substrate is a mica substrate. The surface atomic level flattening of the mica substrate and the high matching of the surface atomic level flattening and the tellurium alkene crystal lattice play a crucial role in the epitaxial growth of the two-dimensional tellurium alkene, the directional growth of the two-dimensional tellurium alkene is realized, and a reliable preparation method is provided for the field of optoelectronic devices of the two-dimensional tellurium alkene.
In one embodiment, the auxiliary substrate is a copper foil. The copper foil is used as an auxiliary substrate, the copper foil and tellurium can form a copper-tellurium alloy, and the copper-tellurium alloy is used as an intermediate of the next step of vapor deposition of the two-dimensional tellurium alkene, so that the tellurium can be uniformly and controllably provided by the copper-tellurium alloy in the whole growth process. Of course, not limited to copper foil, other metals that can be alloyed with tellurium can also be used as the auxiliary substrate.
In one embodiment, the chemical vapor deposition furnace is a tube furnace. Further, the tube furnace is a single-temperature-zone tube furnace. The single-temperature-zone tube furnace can simultaneously meet the temperature requirement of material growth and the heating requirement of the crystal tellurium precursor, and an independent heating device is not required to be provided for heating the precursor.
In one embodiment, the growth temperature is from 500 ℃ to 700 ℃. Further, the optimum growth temperature is 600 ℃. At the temperature, tellurium and copper foil can form a copper-tellurium alloy with specific components, the alloy can re-evaporate the gas-phase tellurium source uniformly and controllably, and then epitaxial growth is performed uniformly and controllably on the surface of a target substrate (growth substrate).
In one embodiment, the growth time is from 5 minutes to 30 minutes. Further, the optimal growth time is 10 minutes, and under the growth time, the two-dimensional telluriene film with controllable layer number and flat surface can be obtained.
In one embodiment, the inert gas (e.g., argon or nitrogen) is flowed at a rate of 50sccm to 200 sccm. Further, the flow rate of the inert gas is preferably 60 sccm. At this carrier gas flow rate, the gas-phase tellurium can be efficiently transferred to the target substrate.
In a specific embodiment, the chemical vapor deposition method for preparing the two-dimensional tellurine film specifically comprises the following steps: and placing the mica substrate and the copper foil in a tube furnace, wherein the copper foil is positioned below the mica substrate, introducing argon into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate.
In the embodiment, a chemical vapor deposition method is utilized, copper foil is introduced to serve as an intermediate of a tellurium source, the tellurium source is uniformly and controllably provided from the eutectic body in the whole growth process after tellurium and copper form a solid solution in the growth process, and mica serves as an epitaxial growth substrate, so that the high-quality direction-controllable two-dimensional tellurium-alkene film is finally prepared. The chemical vapor deposition method can avoid the problem of nonuniform time and space distribution of the solid precursor in the growth process in the traditional vapor deposition method, and avoids the thickness nonuniformity of the final product.
Compared with the existing method for growing two-dimensional telluroene, the method has the following beneficial effects:
(1) the method adopted by the embodiment has low requirements on experimental equipment, simple operation flow and high feasibility of specific implementation.
(2) The method adopted by the embodiment introduces the copper foil as an auxiliary substrate, and tellurium form a eutectic body, so that tellurium can be uniformly and controllably provided by the eutectic body in the whole growth process.
(3) According to the special placement mode of the substrate, the mica is reversely buckled on the copper foil to form a reaction micro-cavity, and the distribution of the tellurium sources in the reaction micro-cavity has smaller difference in time and space, so that the two-dimensional telluroene with uniform thickness can be obtained.
(4) The surface atomic level flattening of the mica substrate and the high matching of the surface atomic level flattening and the tellurium alkene crystal lattice play a crucial role in the epitaxial growth of the two-dimensional tellurium alkene, the directional growth of the two-dimensional tellurium alkene is realized, and a reliable preparation method is provided for the field of optoelectronic devices of the two-dimensional tellurium alkene.
The following specific examples are further provided to facilitate an understanding of the invention.
Example 1
Taking crystal tellurium as a precursor, mica as a growth substrate, taking high-purity argon as a growth atmosphere, controlling the gas flow to be 60sccm and the growth time to be 10 minutes, and naturally cooling the temperature of the tube furnace to room temperature to obtain the two-dimensional tellurium-alkene film deposited on the mica substrate.
Fig. 1 is an optical microscope photograph of the mica substrate of example 1, and it can be seen from fig. 1 that there is almost no deposition of the sample of two-dimensional tellurine on the mica substrate without the aid of the copper foil.
Example 2
This example is different from example 1 in that a piece of copper foil is placed under mica, and the other conditions are the same as example 1.
Fig. 2 is an optical microscope photograph of the mica substrate in example 2, and it can be seen from fig. 2 that there are a large number of triangular samples of two-dimensional telluroene deposited on the mica substrate with the aid of copper foil, and that these triangles have a certain orientation.
Fig. 3 is a raman spectrum photograph of the two-dimensional tellurine deposited on the surface of the mica substrate in example 2, and it can be seen from fig. 3 that three raman vibration modes are consistent with those reported in the literature.
Fig. 4 is an atomic force microscope photograph of the two-dimensional tellurine deposited on the surface of the mica substrate in example 2, and it can be seen from fig. 4 that the thickness of the triangular two-dimensional tellurine sample is uniform and about 10 nm.
Fig. 5 is an electron diffraction photograph of the two-dimensional tellurite deposited on the surface of the mica substrate in example 2, and it can be seen from fig. 5 that the hexagonal diffraction spots of the single crystal confirm the hexagonal lattice structure of the two-dimensional tellurite.
FIG. 6 is a high resolution atomic image photograph of the two-dimensional telluroene deposited on the surface of the mica substrate in example 2. from FIG. 6, it can be seen that the (100) interplanar spacing of the two-dimensional telluroene is about 0.39nm, which is consistent with the values reported in the literature.
Fig. 7 is a photograph comparison of the copper foil before and after growth in example 2, and it can be seen from fig. 7 that the copper foil before growth is golden yellow and the copper foil after growth is blackened, indicating that the copper foil has undergone a chemical reaction during the growth.
Fig. 8 is an energy dispersive X-ray spectroscopy chart of the copper foil after growth in example 2, and it can be seen from fig. 8 that the elemental ratio of copper and tellurium is close to 2: 1, illustrating the formation of a eutectic with copper and tellurium.
Example 3
This example is different from example 1 in that the mica substrate was replaced with a c-plane sapphire substrate, and the other conditions were the same as example 1.
Fig. 9 is an optical microscope photograph of the sapphire substrate in example 3, and it can be seen from fig. 9 that, when the copper foil is used for assisting, a large number of triangular samples of two-dimensional telluroene are still deposited on the sapphire substrate, which illustrates that the method for copper foil assisted growth of two-dimensional telluroene is not only applicable to mica substrates, but is expected to be expanded to other more substrate types.
FIG. 10 is a schematic view of the chemical vapor deposition of two-dimensional telluroene according to examples 1-3, wherein the tellurium particles are placed in the upstream low temperature zone (greater than 450 degrees), the substrate is placed in the central high temperature zone, the upper substrate is mica or sapphire, and the lower substrate is copper foil, as can be seen from FIG. 10.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film is characterized by comprising the following steps: placing a growth substrate and an auxiliary substrate in a chemical vapor deposition furnace, wherein the auxiliary substrate is positioned below the growth substrate, introducing inert gas into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate; wherein the auxiliary substrate is a metal substrate, and the metal is capable of forming an alloy with tellurium.
2. The chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film as claimed in claim 1, wherein the growth substrate is one of a mica substrate and a sapphire substrate.
3. The chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film as claimed in claim 2, wherein the growth substrate is a mica substrate.
4. The chemical vapor deposition method for preparing a two-dimensional telluroene film according to claim 1, wherein the auxiliary substrate is a copper foil.
5. The chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film as claimed in claim 1, wherein the chemical vapor deposition furnace is a single temperature zone tube furnace.
6. The chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film as claimed in claim 1, wherein the growth temperature is 500 ℃ to 700 ℃.
7. The chemical vapor deposition method for producing a two-dimensional tellurine film according to claim 1, wherein the growth time is 5 to 30 minutes.
8. The chemical vapor deposition method for preparing a two-dimensional tellurium film as claimed in claim 1, wherein the inert gas has a flow rate of 50sccm to 200 sccm.
9. The chemical vapor deposition method for producing a two-dimensional tellurine film according to claim 1, wherein the inert gas is argon or nitrogen.
10. The chemical vapor deposition method for preparing a two-dimensional tellurium-alkene film as claimed in claim 1, which comprises the steps of: and placing the mica substrate and the copper foil in a tube furnace, wherein the copper foil is positioned below the mica substrate, introducing argon into the chemical vapor deposition furnace, adding crystal tellurium, and growing a two-dimensional telluroene film to obtain the two-dimensional telluroene film on the growth substrate.
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Cited By (1)
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