CN110344025B - Two-dimensional Zn-doped Ca2Si nano film and chemical vapor deposition method thereof - Google Patents

Two-dimensional Zn-doped Ca2Si nano film and chemical vapor deposition method thereof Download PDF

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CN110344025B
CN110344025B CN201910816710.4A CN201910816710A CN110344025B CN 110344025 B CN110344025 B CN 110344025B CN 201910816710 A CN201910816710 A CN 201910816710A CN 110344025 B CN110344025 B CN 110344025B
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温翠莲
彭建邦
余新江
萨百晟
蔡书畅
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Fuzhou University
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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
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    • 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
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/42—Silicides
    • 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
    • C23C16/44—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 method of coating
    • C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • 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
    • C23C16/56—After-treatment

Abstract

The invention belongs to the field of low-dimensional nano film materials, and particularly relates to two-dimensional Zn-doped Ca2Si nano-film and chemical vapor deposition method thereof. Placing the quartz capsule filled with Ca powder in the front end region of the three-temperature-region high-temperature tube furnace, placing the quartz capsule filled with Zn powder in the middle region of the three-temperature-region high-temperature tube furnace, and placing the pretreated glass substrate in the end region of the three-temperature-region high-temperature tube furnace. Under argon and SiH4Heating the front end, the middle and the tail end regions of the three-temperature-zone tube furnace at a certain heating rate under the carrier gas, reacting for a period of time, depositing reaction products on a glass substrate, and then carrying out in-situ annealing treatment on the reaction products in the tube furnace to obtain the two-dimensional Zn-doped Ca2A thin layer of Si material. The method has simple preparation process and high product purity, and is expected to realize large-scale and high-quality two-dimensional Zn-doped Ca2The production of the Si nano film has good industrialization prospect.

Description

Two-dimensional Zn-doped Ca2Si nano film and chemical vapor deposition method thereof
Technical Field
The invention belongs to the field of low-dimensional nano film materials, and particularly relates to two-dimensional Zn-doped Ca2A Si nano-film and a preparation method of a chemical vapor deposition method.
Background
Two-dimensional materials are confined to two-dimensional planes due to their carrier transport and thermal diffusion, making such materials exhibit many unique properties. The adjustable band gap characteristic of the band gap is widely applied in the fields of field effect tubes, photoelectric devices, thermoelectric devices and the like; the controllability of the spin degree of freedom and the valley degree of freedom thereof has led to intensive research in the fields of spintronics and valley electronics; due to the special properties of the crystal structure, different two-dimensional materials have anisotropy of different electrical properties or optical properties, including anisotropy of properties such as Raman spectrum, photoluminescence spectrum, second-order harmonic spectrum, light absorption spectrum, thermal conductivity and electric conductivity, and have great development potential in the fields of polarized photoelectric devices, polarized thermoelectric devices, bionic devices, polarized light detection and the like.
Alkaline earth metal silicide Ca2The Si material has a direct band gap of about 0.31 eV, is composed of Ca and Si elements with extremely long resource life, can be recycled, has no pollution to the earth, and is characterized in that Ca is a calcium-silicon compound2Si has excellent compatibility with the existing silicon-based technology, is considered to be a promising novel environment-friendly semiconductor material, and has potential application prospects in the fields of solar cells, thermoelectric conversion and the like. Compared with a block material, the two-dimensional material has more advantages, such as better flexibility and high transparency, and therefore, the two-dimensional material has wide application prospects in the corresponding fields. Two-dimensional CaC2The phase transition under high pressure has attracted higher attention, and physical properties such as excellent conductivity and superconductivity of the phase transition are researched; CaP3The nano film is a new predicted two-dimensional functional material, not only has a direct band gap of 1.15 eV, but also has a band gap as high as 19930 cm2·V-1·s-1Is a highly desirable functional material for nanoelectronic applications. Two-dimensional Ca2Si has good stability under ambient conditions and exhibits anisotropic carrier mobility in different directions, such high carrier mobility indicating two-dimensional Ca2The Si nano film has good prospect for high-efficiency solar cells and other applications.
The electronic structure and the electrical property of the material can be effectively changed by element doping. Since Zn element has properties similar to those of alkaline earth metals and the radius of Zn ion is smaller than that of Ca ion, when Zn element is doped with Ca2After Si, Zn ions easily substitute for Ca ions and enter the lattice structure to be doped as donors, providing conductive electrons as carriers.In addition, the doping of Zn ions can enable more vacancies to be formed in the semiconductor, thereby improving the electrical conductivity and the thermoelectric property of the material. At present, Ca is doped with Zn2Si thermoelectric materials have not been reported yet.
In addition, the size and thickness of the two-dimensional nano-film prepared by the stripping method cannot be effectively controlled, and the yield is low. The two-dimensional nano film obtained by the sputtering method has poor crystallinity, small grain size and easy metal residue. In contrast, the two-dimensional nano film prepared by chemical vapor deposition has larger size and higher crystallinity, and can realize high-quality growth of single-layer, double-layer and few-layer film samples, so the two-dimensional Zn-doped Ca is prepared by the chemical vapor deposition method2And (3) a Si nano film.
Disclosure of Invention
The invention aims to provide two-dimensional Zn-doped Ca2Si nano-film and chemical vapor deposition method thereof. The preparation method is to grow high-quality two-dimensional Zn-doped Ca on the glass substrate by using a chemical vapor deposition synthesis method2And (3) a Si nano film.
In order to achieve the purpose, the invention adopts the following technical scheme:
two-dimensional Zn-doped Ca2A chemical vapor deposition method of a Si nano-film, the method comprising the steps of:
(1) pretreating the glass substrate to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 0.5-3 of Ca powder and Zn powder, placing a quartz capsule filled with the Ca powder in the front end region of the three-temperature-region high-temperature tube furnace, placing the quartz capsule filled with the Zn powder in the middle region of the three-temperature-region high-temperature tube furnace, and placing the pretreated glass substrate in the tail end region of the three-temperature-region high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 40-60 sccm to exhaust the air in the furnace; repeating the steps for 2-4 times to completely replace the air in the furnace by argon;
(4) introducing argon into the tube furnace at a certain speedAnd SiH4Heating the front end region of the three-temperature-region high-temperature tubular furnace to 600-700 ℃ at a heating rate of 25-35 ℃/min, simultaneously heating the middle region of the three-temperature-region high-temperature tubular furnace to 400-500 ℃ at a heating rate of 15-25 ℃/min, heating the end region where the glass substrate is located to 500-600 ℃ at a heating rate of 35-45 ℃/min, reacting for 20-60 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace to obtain the two-dimensional Zn-doped Ca2A thin layer of Si material.
The method for pretreating the glass substrate in the step (1) comprises the following steps: and sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively.
The purity of the Ca powder in the step (2) is 99.9 percent, and the purity of the Zn powder is 99.9 percent.
Introducing argon gas with the flow rate of 40-60 sccm and SiH in the step (4)4The gas flow rate is 15-30 sccm.
The annealing temperature in the step (4) is 400-500 ℃, and the annealing time is 0.5-5 h.
The invention has the beneficial effects that: two-dimensional Zn-doped Ca prepared by chemical vapor deposition method2Compared with other preparation methods, the Si nano film has simple preparation process, can prepare large-area and high-purity nano films, has high product purity, and is expected to realize large-scale and high-quality two-dimensional Zn-doped Ca2The production of the Si nano film has good industrialization prospect.
Drawings
FIG. 1 is a chemical vapor deposition method for preparing two-dimensional Zn-doped Ca2A flow diagram of the Si nano-film;
FIG. 2 shows two-dimensional Zn-doped Ca obtained in example 22XRD pattern of Si nano-film;
FIG. 3 shows two-dimensional Zn-doped Ca obtained in example 22Scanning electron microscope images of the Si nano-film.
Detailed Description
The present invention will be further explained below by way of specific examples, but the present invention is not limited to these examples.
Example 1
Two-dimensional Zn-doped Ca prepared by chemical vapor deposition2The method for preparing the Si nano film comprises the following specific steps:
(1) sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 0.5 g of Ca powder and Zn powder, placing a quartz capsule filled with 3.5 g of Ca powder with the purity of 99.9 percent in the front end area of the three-temperature-area high-temperature tube furnace, placing a quartz capsule filled with 0.1 g of Zn powder with the purity of 99.9 percent in the middle area of the three-temperature-area high-temperature tube furnace, and placing the pretreated glass substrate in the end area of the three-temperature-area high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 40 sccm to exhaust the air in the furnace; repeating the step for 3 times to completely replace the air in the furnace by argon;
(4) introducing argon and SiH into the tubular furnace at a certain speed4The flow rate of the introduced argon gas was 40 sccm and SiH was added to the mixed gas of (1)4The gas flow rate is 15 sccm; heating the front end region of the three-temperature-region high-temperature tube furnace to 600 ℃ at the heating rate of 25 ℃/min, simultaneously heating the middle region of the three-temperature-region high-temperature tube furnace to 400 ℃ at the heating rate of 15 ℃/min, heating the end region where the glass substrate is located to 500 ℃ at the heating rate of 35 ℃/min, reacting for 60 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace at the annealing temperature of 400 ℃ for 5 h to obtain Ca2A thin layer of Si material.
Example 2
Two-dimensional Zn-doped Ca prepared by chemical vapor deposition2The method for preparing the Si nano film comprises the following specific steps:
(1) sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 3, placing a quartz capsule filled with 3.5 g of Ca powder with the purity of 99.9% in the front end area of the three-temperature-zone high-temperature tube furnace, placing a quartz capsule filled with 0.5 g of Zn powder with the purity of 99.9% in the middle area of the three-temperature-zone high-temperature tube furnace, and placing the pretreated glass substrate in the end area of the three-temperature-zone high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 40 sccm to exhaust the air in the furnace; repeating the step for 3 times to completely replace the air in the furnace by argon;
(4) introducing argon and SiH into the tubular furnace at a certain speed4The flow rate of the introduced argon gas was 40 sccm and SiH was added to the mixed gas of (1)4The gas flow rate is 30 sccm; heating the front end region of the three-temperature-region high-temperature tube furnace to 660 ℃ at the heating rate of 30 ℃/min, simultaneously heating the middle region of the three-temperature-region high-temperature tube furnace to 500 ℃ at the heating rate of 25 ℃/min, heating the end region of the glass substrate to 560 ℃ at the heating rate of 40 ℃/min, reacting for 30 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace at the annealing temperature of 500 ℃ for 0.5 h to obtain Ca2A thin layer of Si material.
Example 3
Two-dimensional Zn-doped Ca prepared by chemical vapor deposition2The method for preparing the Si nano film comprises the following specific steps:
(1) sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 2.5 of Ca powder and Zn powder, placing a quartz capsule of 2.3 g of Ca powder with the purity of 99.9 percent in the front end area of the three-temperature-area high-temperature tube furnace, placing a quartz capsule filled with 0.3 g of Zn powder with the purity of 99.9 percent in the middle area of the three-temperature-area high-temperature tube furnace, and placing the pretreated glass substrate in the end area of the three-temperature-area high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 60 sccm to exhaust the air in the furnace; repeating the step for 3 times to completely replace the air in the furnace by argon;
(4) introducing argon and SiH into the tubular furnace at a certain speed4The flow rate of the introduced argon gas is 60 sccm, and SiH is added to the mixed gas4The gas flow rate is 15 sccm; heating the front end region of the three-temperature-region high-temperature tube furnace to 700 ℃ at the heating rate of 35 ℃/min, simultaneously heating the middle region of the three-temperature-region high-temperature tube furnace to 450 ℃ at the heating rate of 25 ℃/min, heating the end region of the glass substrate to 600 ℃ at the heating rate of 45 ℃/min, reacting for 40 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace at the annealing temperature of 400 ℃ for 5 h to obtain Ca2A thin layer of Si material.
Example 4
Two-dimensional Zn-doped Ca prepared by chemical vapor deposition2The method for preparing the Si nano film comprises the following specific steps:
(1) sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 1.5 of Ca powder and Zn powder, placing a quartz capsule of 4.5 g of Ca powder with the purity of 99.9 percent in the front end area of the three-temperature-area high-temperature tube furnace, placing a quartz capsule filled with 0.3 g of Zn powder with the purity of 99.9 percent in the middle area of the three-temperature-area high-temperature tube furnace, and placing the pretreated glass substrate in the end area of the three-temperature-area high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 60 sccm to exhaust the air in the furnace; repeating the step for 3 times to completely replace the air in the furnace by argon;
(4) introducing argon and SiH into the tubular furnace at a certain speed4The flow rate of the introduced argon gas is 60 sccm, and SiH is added to the mixed gas4The gas flow rate is 30 sccm; heating the front end region of the three-temperature-region high-temperature tube furnace to 700 ℃ at the heating rate of 35 ℃/min, and simultaneously heating the three temperatures at the heating rate of 25 ℃/minHeating the middle area of the zone high-temperature tube furnace to 500 ℃, heating the end area of the glass substrate to 600 ℃ at the heating rate of 45 ℃/min, reacting for 40 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace at the annealing temperature of 500 ℃ for 1 h to obtain Ca2A thin layer of Si material.
Table 1 shows two-dimensional Zn-doped Ca calculated in examples 1 to 42The Si nano-film has the characteristics of atomic ratio, carrier concentration, carrier mobility and the like.
TABLE 1 two-dimensional Zn doping with Ca2Atomic ratio, carrier concentration and carrier mobility of Si nano-film
Figure DEST_PATH_IMAGE001
As can be seen from Table 1, compared to undoped Ca2Si nano-film, Ca after Zn doping2The carrier concentration of the Si nano film is improved by 1-2 orders of magnitude, and the carrier mobility can reach 9879.56 cm at most2·V-1 ·s-1This high carrier concentration and high carrier mobility indicate two-dimensional Zn-doped Ca2The Si nano film has good prospect for the application of high-efficiency solar cells and nano electronic devices.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (6)

1. Two-dimensional Zn-doped Ca2The chemical vapor deposition method of the Si nano film is characterized in that:
the method comprises the following steps:
(1) pretreating the glass substrate to remove impurities on the surface of the substrate;
(2) taking the molar ratio of 40: 0.5-3 of Ca powder and Zn powder, placing a quartz capsule filled with the Ca powder in the front end region of the three-temperature-region high-temperature tube furnace, placing the quartz capsule filled with the Zn powder in the middle region of the three-temperature-region high-temperature tube furnace, and placing the pretreated glass substrate in the tail end region of the three-temperature-region high-temperature tube furnace;
(3) pumping the vacuum degree of the high-temperature tube furnace to be below 10 Pa, then closing a vacuum valve, and introducing argon at the flow rate of 40-60 sccm to exhaust the air in the furnace; repeating the steps for 2-4 times to completely replace the air in the furnace by argon;
(4) introducing argon and SiH into the tubular furnace at a certain speed4Heating the front end region of the three-temperature-region high-temperature tubular furnace to 600-700 ℃ at a heating rate of 25-35 ℃/min, simultaneously heating the middle region of the three-temperature-region high-temperature tubular furnace to 400-500 ℃ at a heating rate of 15-25 ℃/min, heating the end region where the glass substrate is located to 500-600 ℃ at a heating rate of 35-45 ℃/min, reacting for 20-60 min to ensure that the atomic ratio of Ca to Si is 2:1, and depositing a reaction product on the glass substrate; carrying out in-situ annealing treatment on the reaction product in a tube furnace to obtain the two-dimensional Zn-doped Ca2A thin layer of Si material.
2. Two-dimensional Zn-doped Ca according to claim 12The chemical vapor deposition method of the Si nano film is characterized in that the method for pretreating the glass substrate in the step (1) comprises the following steps: and sequentially putting the glass substrate into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 15min respectively.
3. Two-dimensional Zn-doped Ca according to claim 12The chemical vapor deposition method of the Si nano film is characterized in that the purity of the Ca powder in the step (2) is 99.9 percent, and the purity of the Zn powder is 99.9 percent.
4. Two-dimensional Zn-doped Ca according to claim 12The chemical vapor deposition method of the Si nano film is characterized in that the flow rate of the argon gas introduced in the step (4) is 40-60 sccm, and SiH is added4The gas flow rate is 15-30 sccm.
5. Two-dimensional Zn-doped Ca according to claim 12Si NaThe chemical vapor deposition method of the rice film is characterized in that the annealing temperature in the step (4) is 400-500 ℃, and the annealing time is 0.5-5 hours.
6. Two-dimensional Zn-doped Ca prepared by the method of any one of claims 1 to 52And (3) a Si nano film.
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