CN111188024A - Method for preparing niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition - Google Patents
Method for preparing niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition Download PDFInfo
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- CXRFFSKFQFGBOT-UHFFFAOYSA-N bis(selanylidene)niobium Chemical compound [Se]=[Nb]=[Se] CXRFFSKFQFGBOT-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002135 nanosheet Substances 0.000 title claims abstract description 44
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 22
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 238000001878 scanning electron micrograph Methods 0.000 description 7
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- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
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- 238000005411 Van der Waals force Methods 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
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- 238000001069 Raman spectroscopy Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- ROUIDRHELGULJS-UHFFFAOYSA-N bis(selanylidene)tungsten Chemical compound [Se]=[W]=[Se] ROUIDRHELGULJS-UHFFFAOYSA-N 0.000 description 1
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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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a method for preparing a niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition, which takes niobium pentoxide powder and selenium powder as raw materials and grows the high-quality niobium diselenide nanosheet array on a silicon oxide substrate through one-step normal-pressure chemical vapor deposition. The invention has the characteristics of simple and convenient growth, large area and high efficiency, and the prepared material has good ultraviolet-visible light absorption performance and good stability and has high response speed of light detection.
Description
Technical Field
The invention relates to a photoelectric response characteristic material, in particular to a method for preparing a niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition, and belongs to the field of electronic materials and devices.
Background
Two-dimensional materials consist of a single or multiple layers of atoms or molecules,has unique properties and functions due to its unique two-dimensional structure. Inspired by graphene research, people have increasingly strong interest in other two-dimensional nanocrystals. Wherein the ultra-thin transition metal dichalcogenide comprises MoS2、ReS2、WS2、WSe2、PtSe2、NbSe2Etc., are considered to be important members of the two-dimensional nanomaterial family consisting of single-or multi-layered hexagonal systems. Each molecular film is composed of one metal atom and two atoms of a sulfur-based element. Although the X-M-X overlaps are connected by weak van der Waals forces, strong covalent interactions exist between the layers. The unique optoelectronic properties of transition metal dichalcogenides have given rise to a worldwide hot trend of research over the last few years. The materials have completely different energy band structures and excellent properties in the fields of electricity, optics, thermoelectricity, piezoelectricity, magnetic fields and the like. By superposing different two-dimensional materials, a material system with stronger function can be constructed. In the near infrared band, the material has the characteristic of strong exciton luminescence generated by strong coulomb effect, and provides a new material choice for the construction of novel luminescent devices (such as LEDs, photodetectors, lasers, solar cells and the like).
Niobium diselenide has become a very important material due to the physical properties of its charge density wave transition and superconducting transition. Niobium diselenide is hexagonal in structure, consisting of tightly packed, tightly coupled molecular layers, interacting with weak van der waals forces, resulting in a high degree of anisotropy. Niobium diselenide has a layered crystal structure, and the unit cell is 2H type and is composed of double layers of niobium diselenide. Because of the difficulty in sample preparation, less experimental research has been conducted on size-related properties. Niobium diselenide is essentially a two-dimensional metal with superconductor properties. The thin niobium diselenide layer can also be obtained by mechanical or organic solvent liquid phase stripping, by providing high energy to overcome the van der waals forces between the niobium diselenide layers, the latter method having the advantage of relatively low reaction temperature, but the thickness and size of the obtained niobium diselenide cannot be controlled. Of course, common methods for preparing niobium diselenide materials include lithium ion intercalation, Pulsed Laser Deposition (PLD), and the like, but these methods cannot prepare materials having good morphology and good crystallinity.
In recent years, Chemical Vapor Deposition (CVD) has been widely used for synthesizing transition metal dichalcogenides such as molybdenum disulfide and tungsten diselenide. Of course, a method of producing a high-quality niobium diselenide thin film by CVD has been reported. CVD techniques have great potential for high quality, large area, large size, phase/thickness controlled two-dimensional transition metal dichalcogenide growth. Various shapes are known to be synthesized, such as triangles, hexagons, triangular stars and hexagonal stars. Different growth parameters such as reaction temperature, carrier gas flow, reactant mass, distance between the substrate and the evaporation source material, and the like all influence the growth morphology and nucleation density of the nano material. The exploration of reaction conditions to obtain high-quality single crystal niobium diselenide nano materials with different morphologies has important research value.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition, and aims to solve the problem of preparing a vertically grown niobium diselenide nanosheet array material with good photoelectric response characteristic and quick response time through exploration and improvement of reaction conditions.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing a niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition is characterized by comprising the following steps:
1) cleaning a substrate by using a silicon oxide wafer as the substrate, and then putting the substrate into ozone for treatment for 30 minutes;
2) cleaning the tubular furnace by argon to ensure that no oxygen is mixed in the reaction process, and then introducing argon to maintain the normal pressure in the tubular furnace; mixing 0.1 g-0.2 g niobium pentoxide powder and 0.02 g-0.05 g sodium chloride, placing the mixture in a first quartz boat, inverting the silicon oxide wafer above the center of the first quartz boat, and then placing the first quartz boat in a central heating zone of a tube furnace; placing 1 g-2 g of selenium powder in a second quartz boat, then placing the second quartz boat in a tube furnace and locating the second quartz boat at the upstream of the first quartz boat;
3) heating the tube furnace to 850-900 ℃, then replacing argon with argon-hydrogen mixed gas, and carrying out heat preservation growth for 2-30 minutes at normal pressure;
4) after the growth is finished, opening a furnace cover for quick cooling, and replacing argon-hydrogen mixed gas with argon; and cooling to room temperature, and taking out to obtain the silicon oxide wafer with the niobium diselenide nanosheet array.
Further, in the step 1), the cleaning is sequentially performed by acetone, ethanol and deionized water.
Further, the second quartz boat is located at a distance from the first quartz boat in step 2), and the temperature of the second quartz boat is 450-500 ℃ when the first quartz boat is heated to 850-900 ℃ in step 3).
Further, in the step 3), the temperature rise rate of the tube furnace is 12 ℃/min.
Further, in the step 3), the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 10%, and the flow rate of the argon-hydrogen mixed gas is 100 sccm.
The invention has the beneficial effects that:
1. the niobium diselenide nanosheet array material prepared based on chemical vapor deposition has good photoelectric response characteristic under ultraviolet irradiation and high response speed.
2. The preparation method has the characteristics of simple and convenient growth, large area and high efficiency, overcomes the defects of the traditional mechanical stripping method and the like, and the obtained product has uniform and regular appearance which is beneficial to improving the light absorption capacity.
3. According to the invention, niobium pentoxide and sodium chloride mixed powder is used as a precursor, based on an optimized CVD (chemical vapor deposition) process, a niobium diselenide nanosheet array with the diameter of 40-60 mu m and the thickness of 80-500 nm is successfully synthesized on a silicon oxide wafer substrate in a large area, and the shape and size of the obtained nanosheet are changed along with the change of growth time and temperature. The invention provides a controllable method for directly synthesizing a large-scale and high-quality two-dimensional nanosheet system on a traditional substrate, and opens up a new research field for optoelectronics based on two-dimensional materials.
Drawings
FIG. 1 is a schematic view of the growth of a niobium diselenide nanosheet array prepared in accordance with the present invention.
Fig. 2 is a scanning electron micrograph of an array of niobium diselenide nanosheets obtained in examples 1, 2 and 3, the scanning electron micrograph showing the progression of niobium diselenide from nucleation to growth and densification, wherein fig. 2(a) corresponds to the product obtained in example 1, fig. 2(b) corresponds to the product obtained in example 2, and fig. 2(c) and 2(d) correspond to the product obtained in example 3.
Fig. 3 is a high resolution transmission scanning electron micrograph (fig. 3(a), inset in lower left is the corresponding SAED image) and HRTEM (fig. 3(b)) of the niobium diselenide nanosheet array obtained in example 3.
FIG. 4 is an X-ray diffraction pattern of the niobium diselenide nanosheet array obtained in example 3.
Fig. 5 is a raman spectrum of the niobium diselenide nanosheet array obtained in example 3.
Fig. 6 is an ultraviolet-visible absorption spectrum of the niobium diselenide nanosheet array obtained in example 3.
Fig. 7 is a voltage-current characteristic curve diagram of a device manufactured based on the niobium diselenide nanosheet array of example 3 under ultraviolet irradiation at a wavelength of 254nm, a wavelength of 365nm and dark, respectively.
Fig. 8 is a current-time plot of a device fabricated based on the niobium diselenide nanosheet array of example 3 under uv irradiation at a wavelength of 254nm and a bias voltage of 0.3V.
Detailed Description
The following embodiments of the present invention will be described in detail with reference to the accompanying drawings, which are provided for implementing the technical solution of the present invention, and provide detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following embodiments.
Example 1
As shown in fig. 1, the niobium diselenide nanosheet array grows in a horizontal tube furnace by atmospheric pressure chemical vapor deposition, and the specific steps are as follows:
1) taking a silicon oxide wafer (20mm multiplied by 20mm in size and the thickness of a silicon oxide layer is 300nm) as a substrate, cleaning the substrate by acetone, ethanol and deionized water in sequence, and then placing the substrate into ozone for treatment for 30 minutes;
2) cleaning the tubular furnace by using argon to ensure that no oxygen is doped in the reaction process, and then keeping introducing 120sccm argon to maintain the normal pressure in the tubular furnace; mixing 0.1g of niobium pentoxide powder and 0.02g of sodium chloride, placing the mixture in a first quartz boat, inverting a silicon oxide wafer above the center of the first quartz boat (namely, a silicon oxide layer faces downwards), and then placing the first quartz boat in a central heating zone of a tube furnace; 1g of selenium powder is placed in a second quartz boat and then placed in a tube furnace, and is positioned at the upstream (interval of 10cm) of the first quartz boat;
3) heating the tube furnace to 850 ℃ at the heating rate of 12 ℃/min (the temperature of the first quartz boat is 850 ℃ and the temperature of the second quartz boat is 500 ℃), then replacing argon with 100sccm argon-hydrogen mixed gas, and carrying out heat preservation growth for 2 minutes at normal pressure;
4) after the growth is finished, opening a furnace cover for rapid cooling, and replacing argon-hydrogen mixed gas with 120sccm argon to prevent high-temperature oxidation; and cooling to room temperature, and taking out to obtain the silicon oxide wafer with the niobium diselenide nanosheet array.
Fig. 2(a) is a scanning electron micrograph of the product obtained in this example, and it can be seen that the substrate surface is a distribution of individual spheres, which indicates that several precursors reach the melting point and begin to evaporate, with signs of primary nucleation.
Example 2
As shown in fig. 1, the niobium diselenide nanosheet array grows in a horizontal tube furnace by atmospheric pressure chemical vapor deposition, and the specific steps are as follows:
1) taking a silicon oxide wafer (20mm multiplied by 20mm in size and the thickness of a silicon oxide layer is 300nm) as a substrate, cleaning the substrate by acetone, ethanol and deionized water in sequence, and then placing the substrate into ozone for treatment for 30 minutes;
2) cleaning the tubular furnace by using argon to ensure that no oxygen is doped in the reaction process, and then keeping introducing 120sccm argon to maintain the normal pressure in the tubular furnace; mixing 0.1g of niobium pentoxide powder and 0.02g of sodium chloride, placing the mixture in a first quartz boat, inverting a silicon oxide wafer above the center of the first quartz boat (namely, a silicon oxide layer faces downwards), and then placing the first quartz boat in a central heating zone of a tube furnace; 1g of selenium powder is placed in a second quartz boat and then placed in a tube furnace, and is positioned at the upstream (interval of 12cm) of the first quartz boat;
3) heating the tube furnace to 900 ℃ at the heating rate of 12 ℃/min (the temperature of the first quartz boat is 900 ℃ at the moment, and the temperature of the second quartz boat is 500 ℃ at the moment), then replacing argon with 100sccm argon-hydrogen mixed gas, and keeping the temperature at normal pressure for growth for 20 minutes;
4) after the growth is finished, opening a furnace cover for rapid cooling, and replacing argon-hydrogen mixed gas with 120sccm argon to prevent high-temperature oxidation; and cooling to room temperature, and taking out to obtain the silicon oxide wafer with the niobium diselenide nanosheet array.
Fig. 2(b) is a scanning electron micrograph of the product obtained in this example, and it can be seen that the substrate surface is petal-shaped distributed one by one, indicating that the precursor interaction has already indicated that vertical growth has begun.
Example 3
As shown in fig. 1, the niobium diselenide nanosheet array grows in a horizontal tube furnace by atmospheric pressure chemical vapor deposition, and the specific steps are as follows:
1) taking a silicon oxide wafer (20mm multiplied by 20mm in size and the thickness of a silicon oxide layer is 300nm) as a substrate, cleaning the substrate by acetone, ethanol and deionized water in sequence, and then placing the substrate into ozone for treatment for 30 minutes;
2) cleaning the tubular furnace by using argon to ensure that no oxygen is doped in the reaction process, and then keeping introducing 120sccm argon to maintain the normal pressure in the tubular furnace; mixing 0.2g of niobium pentoxide powder and 0.05g of sodium chloride, placing the mixture in a first quartz boat, inverting a silicon oxide wafer above the center of the first quartz boat (namely, a silicon oxide layer faces downwards), and then placing the first quartz boat in a central heating zone of a tube furnace; 2g of selenium powder is placed in a second quartz boat and then placed in a tube furnace, and is positioned at the upstream (interval of 12cm) of the first quartz boat;
3) heating the tube furnace to 900 ℃ (the temperature of the first quartz boat is 900 ℃ and the temperature of the second quartz boat is 500 ℃) at the heating rate of 12 ℃/min, then replacing argon with 100sccm argon-hydrogen mixed gas, and carrying out heat preservation growth for 30 minutes at normal pressure;
4) after the growth is finished, opening a furnace cover for rapid cooling, and replacing argon-hydrogen mixed gas with 120sccm argon to prevent high-temperature oxidation; and cooling to room temperature, and taking out to obtain the silicon oxide wafer with the niobium diselenide nanosheet array.
Fig. 2(c) and 2(d) are scanning electron micrographs of the product obtained in this example, and it can be seen that the surface of the substrate is in the form of uniformly distributed discs, which are more dense and uniform and have a larger scale than that of example 2. This embodiment is a condition for optimal growth.
Fig. 3 is a high-resolution transmission scanning electron micrograph (fig. 3(a), the lower left inset is a corresponding SAED image) and a HRTEM (fig. 3(b)) of the niobium diselenide nanosheet array obtained in this example. Fig. 3(a) is taken from a typical niobium diselenide nanosheet, with diffraction rings of polycrystalline material visible in the SAED plot in the lower left, and a distinct lattice fringe belonging to niobium diselenide visible in fig. 3 (b). The interparticle spacing was 0.29nm relative to the plane of the niobium diselenide (102), which can be seen to be a single crystal nanoplate. However, there are also niobium diselenide (108) and (0012) crystal surfaces with grain spacings of 0.217nm and 0.21nm in the upper and lower right corners of the image. Thus, the product is an array of polycrystalline niobium diselenide nanosheets consisting of a plurality of single crystal nanosheets, which also correspond to the previous SAED image.
Fig. 4 is an X-ray diffraction pattern of the niobium diselenide nanosheet array obtained in the present example, and the reflection observed from the pattern conforms to the 2H-type niobium diselenide reference spectrum (JCPDS document No. 72-1621). The niobium diselenide crystal has good orientation in the (102), (105), (108), (0012), (110), (0016), and (206) crystal planes. Furthermore, comparing the (102) and (110) crystal faces with the PDF cards with the strongest peaks of 30.8 ° and 53.2 ° qualitatively reveals that the nanosheet arrays prepared at 900 ℃ are highly crystalline. In addition, the back base was subtracted by the jade software to obtain the peak width at half maximum, and then the average grain size was estimated using the FWHM value in the Scherrer equation. Three major peaks (30.8 °, 34.9 ° and 53.2 °) were taken, with an average grain size of 161 nm. XRD diffraction results further demonstrate the successful preparation of niobium diselenide, and the major peaks in the XRD pattern also correspond to those in the previous HRTEM pattern.
Fig. 5 is a raman spectrum of the niobium diselenide nanosheet array obtained in this example. The data show that two phonon peaks A of the niobium diselenide nanosheet array1gAnd E2gAre respectively positioned at 225cm-1And 238cm-1. Two high energy peaks are associated with planar phonons. 190cm-1Are designated as nearby broad functional soft modes, including two phonon frequencies ω 0- Γ M (2/3) of a second order scattering process wave vector. Raman spectroscopy has been used to measure the thickness of niobium diselenide flakes. Certainly, since the vertical structure of the niobium diselenide is grown in the embodiment, the peak height is similar to that of a membrane Raman spectrum, which further proves that the method can grow the large-area and high-quality niobium diselenide nanosheet array.
Fig. 6 is an ultraviolet-visible absorption spectrum of the niobium diselenide nanosheet array obtained in this example. It can be seen that the UV-visible absorption spectrum has strong absorption peaks at 208nm, 263nm and 361nm, indicating that the device may have photoresponse to UV light.
To test the opto-electrical properties of the array obtained in this example, the device was fabricated using conventional photolithography and electron beam evaporation techniques: electrodes were fabricated on the resulting array with a 5 μm spacing between the electrodes, each electrode consisting of 20nm thick titanium and 80nm thick gold, both grown by electron beam evaporation, and a thin titanium layer to improve the adhesion and electrical contact properties of the gold layer. Finally, the device was annealed in an argon atmosphere at 150 ℃ for 2 hours. The voltammetry of the devices was tested in dark and light conditions using a Keithley 2636 illuminant meter. The ultraviolet performance of the device was tested with a portable ultraviolet lamp at 254nm and 365nm wavelengths, respectively (these two ultraviolet rays also correspond to the two strong absorption peaks of the ultraviolet visible absorption spectrum). All measurements were performed at room temperature and atmospheric pressure.
FIG. 7 shows a device manufactured based on the niobium diselenide nanosheet array of the present embodiment under ultraviolet irradiation of darkness, 254nm wavelength and 365nm wavelength respectivelyVoltammetric profile. As can be seen from the figure, the prepared nanosheet array has good ohmic contact, and the device has obvious photoresponse under the irradiation of two beams of laser. The comparison of the curves under the dark condition and the ultraviolet irradiation condition shows that the resistance under the dark condition reaches 4k omega, and the lowest resistance under the ultraviolet irradiation is 1k omega. It is further demonstrated that niobium diselenide in the 2H form exhibits metallic properties. The performance of the device is further analyzed through the calculation of the resistivity, and the niobium diselenide nanosheet array is 2.5 x 10 under the dark condition-3Omega. m, and a resistivity of 7.5 x 10 under 365nm wavelength laser irradiation and 254nm wavelength laser irradiation, respectively-4Omega m and 6.7 x 10-4Omega.m. Its resistivity is similar to that of carbon and much lower than that of semiconductors such as silicon.
Fig. 8 is a current-time curve diagram of a device fabricated based on the niobium diselenide nanosheet array of the present embodiment under uv irradiation at a wavelength of 254nm and a bias voltage of 0.3V. When a bias of 0.3V was applied, the photocurrent was 1.8mA and the dark current was 0.4 mA. The reaction time for both the rise and fall was 7 milliseconds. It can be seen that the absorption response rate remains unchanged. The fast response speed of optical detection is due to the fact that the prepared niobium diselenide nanosheet has the characteristics of high-quality single crystal property and few defects. In conclusion, the invention has the characteristics of simple and convenient growth, large area and high efficiency, and the prepared material has good ultraviolet-visible light absorption performance and good stability and has quick response of light detection.
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for preparing a niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition is characterized by comprising the following steps:
1) cleaning a substrate by using a silicon oxide wafer as the substrate, and then putting the substrate into ozone for treatment for 30 minutes;
2) cleaning the tubular furnace by argon to ensure that no oxygen is mixed in the reaction process, and then introducing argon to maintain the normal pressure in the tubular furnace; mixing 0.1 g-0.2 g niobium pentoxide powder and 0.02 g-0.05 g sodium chloride, placing the mixture in a first quartz boat, inverting the silicon oxide wafer above the center of the first quartz boat, and then placing the first quartz boat in a central heating zone of a tube furnace; placing 1 g-2 g of selenium powder in a second quartz boat, then placing the second quartz boat in a tube furnace and locating the second quartz boat at the upstream of the first quartz boat;
3) heating the tube furnace to 850-900 ℃, then replacing argon with argon-hydrogen mixed gas, and carrying out heat preservation growth for 2-30 minutes at normal pressure;
4) after the growth is finished, opening a furnace cover for quick cooling, and replacing argon-hydrogen mixed gas with argon; and cooling to room temperature, and taking out to obtain the silicon oxide wafer with the niobium diselenide nanosheet array.
2. The method of claim 1, wherein: in the step 1), the cleaning is sequentially performed by acetone, ethanol and deionized water.
3. The method of claim 1, wherein: the distance between the second quartz boat and the first quartz boat in the step 2) should be ensured to be 450-500 ℃ when the position of the first quartz boat is heated to 850-900 ℃ in the step 3).
4. The method of claim 1, wherein: in the step 3), the temperature rise rate of the tube furnace is 12 ℃/min.
5. The method of claim 1, wherein: in the step 3), the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 10%, and the introducing flow of the argon-hydrogen mixed gas is 100 sccm.
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| CN102923777A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
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| CN108155028A (en) * | 2017-12-29 | 2018-06-12 | 安徽大学 | Preparation method of flower-like molybdenum disulfide high-performance supercapacitor electrode |
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