CN114182351B - Tetragonal phase cuprous telluride and synthesis method thereof - Google Patents
Tetragonal phase cuprous telluride and synthesis method thereof Download PDFInfo
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Abstract
The invention discloses tetragonal-phase cuprous telluride and a method for synthesizing tetragonal-phase and hexagonal-phase cuprous telluride in a phase-controllable manner. The method comprises the following steps: providing a copper source, tellurium powder and a substrate; placing the copper source, the tellurium powder and the substrate in a chemical vapor deposition reaction chamber, and introducing transport gas; generating tetragonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 660-690 ℃; or generating the hexagonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 700-800 ℃. The method for synthesizing the square-phase and hexagonal-phase cuprous telluride with controllable phases, provided by the invention, has the advantages that the phases of the compound can be regulated and controlled by regulating and controlling the growth temperature by adopting a chemical vapor deposition method, and a large-size two-dimensional cuprous telluride single crystal can be controllably grown; and the method can synthesize the tetragonal-phase cuprous telluride, and the tetragonal-phase structure is a brand new atomic-phase structure of the cuprous telluride.
Description
Technical Field
The invention relates to the field of materials, in particular to tetragonal-phase cuprous telluride and a synthetic method thereof.
Background
Cuprous telluride is one of the important members of vacancy doped semiconductors (e.g., copper chalcogenide) and is of increasing interest due to its tunable localized surface plasmon resonance. Meanwhile, cuprous telluride is commonly used for forming a back contact layer so as to improve the performance of the thin film solar cell. Since the copper-tellurium material system is a multi-phase system, there are currently known a copper-telluride (cuprous telluride), a copper-heptatelluride, a copper-tetratelluride, a copper-ditelluride, a copper-telluride (copper telluride), a copper-ditelluride, and so on. Therefore, the growth of cuprous telluride on the phase-controllable material is difficult.
Therefore, it is necessary to provide a method for synthesizing tetragonal-phase cuprous telluride in view of the problems in the prior art.
Disclosure of Invention
The invention aims to provide a method for synthesizing tetragonal-phase cuprous telluride, which can realize phase-controllable synthesis of large-size tetragonal-phase two-dimensional cuprous telluride single crystal.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
in a first aspect, the present invention provides a method for synthesizing tetragonal-phase two-dimensional cuprous telluride, comprising:
providing a copper source, tellurium powder and a substrate; placing the copper source, the tellurium powder and the substrate in a chemical vapor deposition reaction chamber, and introducing transport gas; and generating tetragonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 660-690 ℃.
In one or more embodiments of the invention, the copper source comprises a mixture of copper powder and a halide or a copper salt.
In one or more embodiments of the present invention, the halide includes at least one of sodium chloride, potassium chloride, sodium iodide, potassium iodide; the copper salt includes at least one of copper sulfate, copper nitrate, copper chloride, copper bromide and copper iodide.
In one or more embodiments of the present invention, the tetragonal two-dimensional cuprous telluride is produced by heating to a growth temperature of 660 to 690 ℃ within 15 to 20min, and maintaining the temperature at the growth temperature for 30 to 60min.
In one or more embodiments of the invention, the passing the transport gas comprises:
and introducing the transport gas at the ventilation flow of 600sccm for 5-10 min to clean the chemical vapor deposition reaction chamber, and then introducing the transport gas at the ventilation flow of 60-100 sccm.
In one or more embodiments of the invention, the transport gas is one of argon, nitrogen, a mixture of hydrogen and argon, or a mixture of hydrogen and nitrogen.
In one or more embodiments of the invention, in the chemical vapor deposition reaction chamber, the tellurium powder is 15-25 cm away from and upstream of the copper source, and the substrate is positioned above the copper source.
In a second aspect, the invention provides tetragonal cuprous telluride, which is generated from a copper source and tellurium powder by a chemical vapor deposition method at a growth temperature of 660-690 ℃.
Compared with the prior art, the method for synthesizing the tetragonal-phase cuprous telluride, provided by the invention, adopts a chemical vapor deposition method, can regulate and control the phase of a compound through regulating and controlling the growth temperature, and can controllably grow the large-size tetragonal-phase two-dimensional cuprous telluride single crystal; and the method can synthesize the tetragonal-phase two-dimensional cuprous telluride, and the tetragonal-phase structure is a brand new atomic-phase structure of the cuprous telluride.
Drawings
FIG. 1 is an optical diagram of tetragonal phase two-dimensional cuprous telluride obtained in example 1 of the present invention;
FIG. 2 is a spherical aberration electron microscope image of a tetragonal two-dimensional cuprous telluride plane obtained in example 1 of the present invention;
FIG. 3 is a spherical aberration electron microscope image of a tetragonal two-dimensional cuprous telluride cross-section obtained in example 1 of the present invention;
FIG. 4 is a Raman spectrum analysis chart of tetragonal-phase two-dimensional cuprous telluride obtained in example 1 of the present invention;
FIG. 5 is a scanning energy spectrum of a copper element surface of tetragonal phase two-dimensional cuprous telluride obtained in example 1 of the present invention;
fig. 6 is a tellurium element surface scanning energy spectrum of the tetragonal phase two-dimensional cuprous telluride obtained in example 1 of the present invention;
fig. 7 is a diagram of an energy spectrum of tetragonal-phase two-dimensional cuprous telluride obtained in example 1 of the present invention;
FIG. 8 is an optical diagram of hexagonal-phase two-dimensional cuprous telluride obtained in example 2 of the present invention;
FIG. 9 is a spherical aberration electron microscope image of a hexagonal phase two-dimensional cuprous telluride plane obtained in example 2 of the present invention;
FIG. 10 is a spherical aberration electron microscope image of a hexagonal phase two-dimensional cuprous telluride cross section obtained in example 2 of the present invention;
fig. 11 is a raman spectrum analysis chart of hexagonal phase two-dimensional cuprous telluride obtained in example 2 of the present invention.
FIG. 12 is a copper element surface scanning energy spectrum of hexagonal phase two-dimensional cuprous telluride obtained in example 2 of the present invention;
fig. 13 is a tellurium element plane-scan energy spectrum of hexagonal phase two-dimensional cuprous telluride obtained in example 2 of the present invention;
fig. 14 is a diagram of an energy spectrum of hexagonal-phase two-dimensional cuprous telluride obtained in example 2 of the present invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
It is noted that, unless otherwise indicated, all numbers expressing feature sizes, quantities, and physical characteristics used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the foregoing specification and attached claims are approximations that can be suitably varied by those skilled in the art in seeking to obtain the desired properties utilizing the teachings disclosed herein. The use of numerical ranges by endpoints includes all numbers within that range and any range within that range, for example, 1 to 5 includes 1, 1.2, 1.4, 1.55, 2, 2.75, 3, 3.80, 4, and 5, and the like.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus; the term "preferred" refers to a preferred alternative, but is not limited to only the selected alternative.
At present, a solid phase reaction method, a cosolvent method, a solution method and the like are mostly used for the growth of cuprous telluride, and the obtained products are mostly bulk materials or nanoparticles. As for the direct growth in the two-dimensional form, there are a few of the growth of cuprous telluride by molecular beam epitaxy, the growth of two-dimensional cuprous telluride alloy by deposition annealing, and the like. But the size of the obtained product is extremely small or is alloy, and the two-dimensional large-size cuprous telluride single crystal is difficult to obtain.
Therefore, the invention provides a method for synthesizing tetragonal-phase and hexagonal-phase two-dimensional cuprous telluride in a phase-controllable manner, which comprises the following steps:
providing a copper source, tellurium powder and a substrate;
placing the copper source, the tellurium powder and the substrate in a chemical vapor deposition reaction chamber, and introducing transport gas; generating tetragonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 660-690 ℃; or
And generating hexagonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 700-800 ℃.
The method for synthesizing the square-phase and hexagonal-phase two-dimensional cuprous telluride with controllable phases, which is provided by the invention, can controllably grow large-size square-phase and hexagonal-phase two-dimensional cuprous telluride single crystals by adopting a chemical vapor deposition method and regulating and controlling the growth temperature.
In an exemplary embodiment, the copper source may be a mixture of copper powder and a halide, a copper salt, copper oxide, copper hydroxide, or the like. Wherein, the halide can be at least one of sodium chloride, potassium chloride, sodium iodide and potassium iodide; the copper salt may be at least one of copper sulfate, copper nitrate, copper chloride, copper bromide and copper iodide.
In an exemplary embodiment, when the tetragonal two-dimensional cuprous telluride is generated, the temperature is raised to the growth temperature of 660-690 ℃ within 15-20 min, and the temperature is kept at the growth temperature (660-690 ℃) for 30-60 min.
In an exemplary embodiment, when the hexagonal-phase two-dimensional cuprous telluride is generated, the temperature is raised to the growth temperature of 700-800 ℃ within 15-20 min, and the temperature is kept at the growth temperature for 30-60 min.
In an exemplary embodiment, the specific manner of introducing the transport gas includes: and introducing the transport gas at the ventilation flow rate of 600sccm for 5-10 min to clean the chemical vapor deposition reaction chamber, and then maintaining the ventilation flow rate of 60-100 sccm. Wherein the transport gas may be one of argon, nitrogen, hydrogen-argon mixture or hydrogen-nitrogen mixture
In an exemplary embodiment, in the chemical vapor deposition reaction chamber, the tellurium powder is located 15 to 25cm from the copper source and upstream of the copper source (upstream in the flow direction of the transport gas), and the substrate is located above the copper source.
In an exemplary embodiment, the tellurium powder and the copper source are respectively placed in two quartz boats, then the substrate (mica sheet, sapphire, silicon-oxygen sheet or silicon wafer) is covered on the quartz boat containing the copper source, and then the quartz boat containing the copper source and the tellurium powder is sequentially placed in the chemical vapor deposition reaction chamber, and the transport gas is introduced. Wherein, the quartz boat containing the copper source is arranged in the central heating area of the chemical vapor deposition reaction chamber.
There is currently still controversy regarding the atomic structure of cuprous telluride. Although several structures have been proposed experimentally and theoretically, the position in the atomic structure has not been determined.
Therefore, the invention also provides tetragonal cuprous telluride which is generated by a copper source and tellurium powder at the growth temperature of 660-690 ℃ by a chemical vapor deposition method. The tetragonal two-dimensional cuprous telluride can be synthesized by adopting the method in any one of the previous embodiments. The tetragonal-phase two-dimensional cuprous telluride has a tetragonal-phase structure which is a brand new atomic-phase structure of cuprous telluride.
The present invention is further illustrated by the following specific examples.
Example 1
Weighing 0.1g of copper powder and 0.05g of sodium chloride, uniformly mixing, placing the mixture into a clean quartz boat, and covering the mica substrate on the quartz boat to enable the mica substrate to be positioned above the mixture of the copper powder and the sodium chloride; 0.2g of tellurium powder was weighed into another quartz boat which was cleaned.
Sequentially placing a quartz boat containing copper powder and sodium chloride and a quartz boat containing tellurium powder in a quartz tube reaction chamber of chemical vapor deposition equipment; the quartz boat containing copper powder and sodium chloride is positioned in the central heating area of the reaction chamber, and the quartz boat containing tellurium powder is positioned at the upstream of the quartz boat containing copper powder and sodium chloride and has a distance of 15-25 cm.
Before the reaction, introducing high-purity argon for 5min at the ventilation flow of 600sccm to clean the chemical vapor deposition reaction chamber; then, high-purity argon gas is continuously introduced at the normal pressure at a ventilation flow rate of 60-100 sccm.
And (3) heating the reaction chamber to 660-690 ℃ after 15-20 min by setting a temperature control program, preserving the temperature for 30-60 min at the temperature, and then cooling to room temperature along with the furnace to obtain the tetragonal-phase two-dimensional cuprous telluride.
Fig. 1 is an optical diagram of tetragonal two-dimensional cuprous telluride obtained in example 1. Fig. 2 is a spherical aberration electron microscope image of a tetragonal two-dimensional cuprous telluride plane obtained in example 1. FIG. 3 is a spherical aberration electron microscope image of a tetragonal two-dimensional cuprous telluride cross section obtained in example 1. Fig. 4 is a raman spectrum analysis chart of the tetragonal-phase two-dimensional cuprous telluride obtained in example 1. Fig. 5 is a scanning energy spectrum of a copper element surface of tetragonal two-dimensional cuprous telluride obtained in example 1 of the present invention. Fig. 6 is a tellurium element surface scanning energy spectrum of the tetragonal phase two-dimensional cuprous telluride obtained in example 1 of the present invention. Fig. 7 is a diagram of an energy spectrum of tetragonal two-dimensional cuprous telluride obtained in example 1 of the present invention.
Example 2
Weighing 0.1g of copper powder and 0.05g of sodium chloride, uniformly mixing, placing the mixture into a clean quartz boat, and covering the mica substrate on the quartz boat to enable the mica substrate to be positioned above the mixture of the copper powder and the sodium chloride; 0.2g of tellurium powder was weighed into another clean quartz boat.
Sequentially placing a quartz boat containing copper powder and sodium chloride and a quartz boat containing tellurium powder in a quartz tube reaction chamber of chemical vapor deposition equipment; the quartz boat containing the copper powder and the sodium chloride is positioned in the central heating area of the reaction chamber, and the quartz boat containing the tellurium powder is positioned at the upstream of the quartz boat containing the copper powder and the sodium chloride and is 15-25 cm away from the quartz boat containing the copper powder and the sodium chloride.
Before the reaction, introducing high-purity argon for 5min at the ventilation flow of 600sccm to clean the chemical vapor deposition reaction chamber; then, high-purity argon gas is continuously introduced at the normal pressure at a ventilation flow rate of 60-100 sccm.
And (3) heating the reaction chamber to 700-800 ℃ after 15-20 min by setting a temperature control program, keeping the temperature at the temperature for 30-60 min, and cooling the reaction chamber to room temperature along with the furnace to obtain the hexagonal-phase two-dimensional cuprous telluride.
Fig. 8 is an optical diagram of the hexagonal-phase two-dimensional cuprous telluride obtained in example 2. Fig. 9 is a spherical aberration electron microscope image of the hexagonal phase two-dimensional cuprous telluride plane obtained in example 2. Fig. 10 is a spherical aberration electron microscope image of the hexagonal phase two-dimensional cuprous telluride cross section obtained in example 2. Fig. 11 is a raman spectrum analysis chart of hexagonal-phase two-dimensional cuprous telluride obtained in example 2. Fig. 12 is a copper element surface scanning energy spectrum of hexagonal phase two-dimensional cuprous telluride obtained in example 2 of the present invention. Fig. 13 is a tellurium element plane-scan energy spectrum of hexagonal phase two-dimensional cuprous telluride obtained in example 2 of the present invention. FIG. 14 is a diagram of the spectrum of hexagonal-phase two-dimensional cuprous telluride obtained in example 2 of the present invention;
in conclusion, the method for synthesizing the tetragonal-phase and hexagonal-phase two-dimensional cuprous telluride with controllable phases, which is provided by the invention, can regulate and control the phases of the compound by regulating and controlling the growth temperature by adopting a chemical vapor deposition method, and can controllably grow large-size tetragonal-phase and hexagonal-phase two-dimensional cuprous telluride single crystals; the method can synthesize the tetragonal-phase two-dimensional cuprous telluride, and the tetragonal-phase structure is a brand new atomic-phase structure of the cuprous telluride.
The foregoing description of specific exemplary embodiments of the invention has been presented for the purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (8)
1. A method for synthesizing tetragonal-phase two-dimensional cuprous telluride is characterized by comprising the following steps:
providing a copper source, tellurium powder and a substrate;
placing the copper source, the tellurium powder and the substrate in a chemical vapor deposition reaction chamber, and introducing transport gas;
and generating the tetragonal-phase two-dimensional cuprous telluride on the substrate at the growth temperature of 660-690 ℃.
2. The method of synthesizing a tetragonal two-dimensional cuprous telluride of claim 1 wherein said copper source comprises a mixture of copper powder and halide or a copper salt.
3. A method of synthesizing square phase two dimensional cuprous telluride as in claim 2 wherein said halide comprises at least one of sodium chloride, potassium chloride, sodium iodide, potassium iodide; the copper salt includes at least one of copper sulfate, copper nitrate, copper chloride, copper bromide and copper iodide.
4. A method for synthesizing square-phase two-dimensional cuprous telluride as set forth in any one of claims 1 to 3, wherein the temperature of the produced square-phase two-dimensional cuprous telluride is raised to the growth temperature of 660 to 690 ℃ within 15 to 20min, and the temperature is maintained at the growth temperature for 30 to 60min.
5. The method for synthesizing square-phase two-dimensional cuprous telluride as in any one of claims 1-3, wherein said introducing transport gas comprises:
and introducing the transport gas at the ventilation flow rate of 600sccm for 5-10 min to clean the chemical vapor deposition reaction chamber, and then maintaining the ventilation flow rate of 60-100 sccm.
6. The method of synthesizing tetragonal two-dimensional cuprous telluride as in claim 5 wherein said transport gas is one of argon, nitrogen, hydrogen argon or hydrogen nitrogen.
7. The method for synthesizing tetragonal two-dimensional cuprous telluride according to any of claims 1 to 3 wherein in said chemical vapor deposition reaction chamber tellurium powder is 15-25 cm from and upstream of copper source and said substrate is above copper source.
8. The tetragonal cuprous telluride is characterized in that the tetragonal cuprous telluride is generated by a copper source and tellurium powder at the growth temperature of 660-690 ℃ by a chemical vapor deposition method.
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| CN108441963A (en) * | 2018-03-16 | 2018-08-24 | 湖南大学 | A kind of application in telluride platinum two-dimensional material, preparation and its electricity device |
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| CN108441963A (en) * | 2018-03-16 | 2018-08-24 | 湖南大学 | A kind of application in telluride platinum two-dimensional material, preparation and its electricity device |
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