Method for preparing Te nanobelt by decomposing Sb2Te3 powder

Abstract

The invention relates to the technical field of nano material preparation, provides a method for preparing a Te nanobelt by decomposing Sb2Te3 powder, and solves the problems that the currently prepared one-dimensional Te nano material is low in preparation quality and the prepared structure and morphology do not meet the application demand. The method comprises the following steps: 1) placing antimony telluride powder in a quartz boat, placing at the heating center of a horizontal tube furnace, and placing above a quartz boat containing antimony telluride powder as a substrate; (2) introducing hydrogen and argon which are used as material reaction growth atmosphere into a quartz tube in a horizontal tube furnace for reaction, adjusting the gas mixing ratio and flow velocity, setting the heating temperature and time, starting the tube furnace, performing vapor deposition reaction in the quartz tube, taking out the substrate after the tube furnace procedure is finished, and drying the substrate to obtain the high-temperature-resistant gas-phase deposition material. The surface of the substrate is the grown Te nanobelt.

Description

Technical Field

[0001] The present invention relates to the technical field of nano material preparation, in particular to a method for preparing nano materials by decomposing Sb 2 Te 3 Method for preparing Te nanobelts from powder. Background Art

[0002] Tellurium (Te) is a typical p-type semiconductor with a special chain structure. It has many excellent properties, such as thickness-dependent band gap (0.35eV-1eV), high carrier mobility, excellent thermoelectricity, anisotropic lattice thermal conductivity and room temperature ferroelectricity, etc. It is widely used in high-density storage, catalysis and photoelectric detection.

[0003] Due to the quantum confinement effect, nanoscale materials exhibit many physical and chemical properties that are different from bulk materials, and have potential value in micro-optoelectronic devices, nano-optoelectronics, and stealth materials. Therefore, the synthesis and application of Te also show a trend of low-dimensionality, especially one-dimensional Te nanomaterials show strong anisotropy, and their application in the field of polarized optoelectronics has attracted more and more attention, so its related synthesis methods have also attracted much attention.

[0004] At present, the synthesis methods of one-dimensional tellurium nanomaterials mainly include microwave-assisted synthesis, solvothermal method, thermal evaporation and chemical vapor deposition. However, some of these methods require harsh reaction conditions, such as high temperature and high pressure, cumbersome experimental steps, expensive experimental instruments and long reaction time. Some also need to use volatile ionic liquids and organic solvents, and even need to add some templates, polymer additives and a variety of substrates. The tellurium nanomaterials obtained by the existing synthesis methods will inevitably have residual solvents or additives, thereby reducing the excellent optoelectronic properties of semiconductor materials, and the addition of substrates will produce secondary pollution during material transfer, thus limiting the wide application of tellurium nanomaterials. In contrast, chemical vapor deposition can react at normal pressure or low pressure, and has the advantages of high product purity and simple deposition process. In addition, by consciously adjusting variables such as precursors, deposition parameters and substrates, the composition, composition and morphology of the product can be flexibly controlled. However, when Te powder is used as a precursor, hexagonal Te nanosheets are easily obtained by direct deposition, and such highly symmetric Te nanosheets will limit their application in the field of polarized optoelectronics.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] Therefore, in view of the above problems, the present invention provides a method for decomposing Sb 2 Te 3The method for preparing Te nanobelts from powder solves the problems that the currently prepared one-dimensional Te nanomaterials have low preparation quality and the prepared structural morphology does not meet application requirements.

[0007] To achieve the above object, the present invention adopts the following technical scheme: a method of decomposing Sb 2 Te 3 The method for preparing Te nanobelts from powder comprises the following steps:

[0008] (1) A quartz boat containing antimony telluride powder is placed at the heating center of a horizontal tube furnace, and a substrate is placed on the quartz boat containing antimony telluride powder;

[0009] (2) Hydrogen and argon are introduced into the quartz tube of the horizontal tube furnace as the atmosphere for material reaction growth, and the gas flow rate is adjusted. The tube furnace is turned on to allow the vapor deposition reaction to take place in the quartz tube. After the tube furnace program is completed, the substrate is taken out, and the surface of the substrate is the grown Te nanobelt.

[0010] Furthermore, the substrate in step (1) is a fluorpho-mica sheet, which is cut into a rectangle with a size of 1 cm*1 cm, and the natural mica sheet is naturally cleaved from the interlayer into two thin sheets, and the new cleavage surface is selected as the growth surface.

[0011] Furthermore, the diameter of the quartz tube in step (1) is 1 inch.

[0012] Furthermore, the substrate in step (1) is a fluorpho-mica sheet, which is cut into a rectangle with a size of 1 cm*1 cm, and the natural mica sheet is naturally cleaved from the interlayer into two thin sheets, and the new cleavage surface is selected as the growth surface.

[0013] Furthermore, the reaction in step (2) is carried out under normal pressure.

[0014] Furthermore, the suitable gas described in step (2) is a mixed gas of hydrogen and argon, the mixing ratio of hydrogen to argon is 1:15-1:19, the gas flow rate is controlled to be 200sccm, the heating temperature is set to 660-670°C, and the reaction time is set to 5-10min.

[0015] Furthermore, the Te nanobelt described in step (2) is one-dimensional and has high crystal quality and orientation arrangement characteristics.

[0016] By adopting the above technical solution, the beneficial effects of the present invention are: based on the chemical vapor deposition method, by decomposing Sb 2 Te 3The powder was used to prepare highly anisotropic Te nanobelts, which have high crystal quality and specific orientation arrangement, and the angles between the nanobelts are mostly 60° or 120°. In addition, my country has abundant reserves of Sb and Te elements, and the precursor source is relatively easy to obtain. This method has the characteristics of high production efficiency, good repeatability, high quality of prepared products, and easy promotion. It is of great value for the controllable preparation of highly anisotropic Te nanobelts, the exploration of their basic physical properties, and their further research in the field of polarization photoelectric detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 An optical image of a tellurium nanoribbon prepared according to an embodiment of the present invention is shown.

[0018] Figure 2 The XRD pattern of the tellurium nanoribbon prepared in the embodiment of the present invention is shown.

[0019] Figure 3 An AFM image of a tellurium nanoribbon prepared according to an embodiment of the present invention is shown.

[0020] Figure 4 The Raman spectrum and Raman mapping diagram of the tellurium nanoribbon prepared in the embodiment of the present invention are shown.

[0021] Figure 5 The X-ray photoelectron spectrum (XPS) of the tellurium nanoribbon prepared in the embodiment of the present invention is shown.

[0022] Figure 6 The transmission electron microscopy (TEM) characterization results of the tellurium nanobelts prepared in the embodiments of the present invention are shown. A low-magnification TEM image (a) of a single tellurium nanobelt on a copper grid, a corresponding selected area electron diffraction (SAED) image (b), a high-resolution TEM (HRTEM) image (c), and an energy dispersive analysis (EDX) spectrum (d). DETAILED DESCRIPTION

[0023] In order to further understand the content of the present invention, the present invention is further described below in conjunction with examples.

[0024] Example

[0025] One method is to decompose Sb 2 Te 3 The method for preparing Te nanobelts from powder comprises the following steps:

[0026] (1) Preparation of fluorphlogopite mica substrate: Use pointed tweezers to naturally dissociate a 1 cm*1 cm fluorphlogopite mica sheet from the middle of the layer into two pieces, and use the newly dissociated clean side as the growth substrate;

[0027] (2) Using a quartz boat to hold about 30 mg of antimony telluride powder, and placing it at the center of the heating source of a horizontal tube furnace, and placing fluorphlogopite as a substrate on top of the quartz boat containing the antimony telluride powder;

[0028] (3) Argon gas is introduced into a quartz tube with a diameter of 1 inch in the furnace and purged for 10 minutes to disperse excess oxygen and water vapor in the tube, and then hydrogen gas is introduced into the quartz tube as a catalyst together with argon gas as an atmosphere for material reaction growth, and the mixing ratio of hydrogen and argon is controlled to be 1:15, and the flow rate of the mixed gas is also adjusted to 200 sccm; wherein, in other embodiments, the mixing ratio of hydrogen and argon gas is controlled to be 1:15-1:19 to achieve the purpose of the present invention;

[0029] (4) The heating temperature is set to 660°C, the heating rate is maintained at 10°C / min, and the reaction time is set to 5 min; then the tubular furnace is turned on and the program is run to allow the vapor deposition reaction to proceed in the quartz tube. After the tubular furnace program is completed, the substrate is taken out, and the surface of the substrate is the grown Te nanobelt.

[0030] Figure 1 Shown is an optical image of the Te nanobelt prepared by the present invention, with a scale length of 50 μm. The OM image shows that the length of the nanobelt is at least 20 μm, and the nanobelts are highly oriented, with the angles between the Te nanobelts being 60° or 120°.

[0031] Figure 2 The X-ray diffraction (XRD) data of the Te nanobelt prepared by the present invention is shown. In the XRD spectrum, there is only one peak except the peak from the natural mica sheet, and this peak is located at 23.03°, corresponding to the (100) crystal plane of Te (PDF#36-1452), which indicates that the growth of the Te nanobelt is based on the (100) crystal plane.

[0032] Figure 3 The atomic force microscope (AFM) image and height information of the Te nanobelt prepared by the present invention are shown.

[0033] Figure 4 The Raman spectrum and Raman mapping diagram of the antimony telluride two-dimensional single crystal nanosheet prepared in the embodiment of the present invention are shown. Figure 4 (a) shows an optical image of a single Te nanoribbon selected when collecting Raman signals in the present invention. Figure 4 (b) shows the Raman spectrum of the nanoribbon, where A 1 and E 2 The characteristic peaks prove that the obtained nanoribbons are Te. Figure 4 (c) and (d) show the Raman mapping images of the typical vibration modes of the nanoribbon.

[0034] Figure 5 The X-ray photoelectron (XPS) spectrum of Te prepared in the embodiment of the present invention is shown, specifically, the 3d orbital peak fitting diagram of Te.

[0035] Figure 6 The transmission electron microscopy (TEM) characterization results of the Te single crystal nanobelts prepared in the embodiment of the present invention are shown. The low-magnification TEM image (a), the corresponding selected area electron diffraction (SAED) image (b), the high-resolution TEM (HRTEM) image (c) and the energy spectrum analysis (EDX) spectrum (d) of a single Te nanobelt on a copper grid. The diffraction spots shown in the selected area electron diffraction (SAED) image support the proof that these Te nanobelts have a high-quality single crystal orthorhombic structure, among which the perfect orthorhombic lattice has no obvious defects in the high-resolution TEM (HRTEM) image (c). The measured fringe space is approximately 0.59nm and 0.22nm, corresponding to the (0001) plane and the (1-210) plane, respectively. (d) Energy spectrum analysis (EDX) shows that this nanosheet contains only tellurium, further proving that this nanobelt is Te.

[0036] Although the present invention has been specifically shown and described in conjunction with the preferred embodiments, it should be understood by those skilled in the art that various changes may be made to the present invention in form and details without departing from the spirit and scope of the present invention as defined by the appended claims, all of which are within the scope of protection of the present invention.

Claims

1. A method for preparing Te nanobelts by decomposing Sb2Te3 powder, characterized in that: The method comprises the following steps: 1) using a quartz boat to hold antimony telluride powder and placing it at the heating center of a horizontal tube furnace, and placing a substrate on the quartz boat holding the antimony telluride powder; 2) Hydrogen and argon are introduced together as the atmosphere for material reaction growth into the quartz tube in the horizontal tube furnace for reaction, and the gas mixing ratio and flow rate are adjusted, the heating temperature and time are set, and the tube furnace is turned on to allow the vapor deposition reaction to proceed in the quartz tube. After the tube furnace program is completed, the substrate is taken out, and the surface of the substrate is the grown Te nanobelt.

2. The method for preparing Te nanobelts by decomposing Sb2Te3 powder according to claim 1, characterized in that: The quartz tube described in step (1) has a diameter of 1 inch.

3. The method for preparing Te nanobelts by decomposing Sb2Te3 powder according to claim 1, characterized in that: The substrate described in step (1) is a fluorpho-mica sheet, the size of which is a 1 cm*1 cm square. The fluorpho-mica sheet is naturally cleaved from the interlayer into two thin sheets, and a new cleavage surface is selected as the growth surface.

4. The method for preparing Te nanobelts by decomposing Sb2Te3 powder according to claim 1, characterized in that: The reaction in step (2) is carried out under normal pressure.

5. The method for preparing Te nanobelts by decomposing Sb2Te3 powder according to claim 1, characterized in that: In step (2), the mixing ratio of hydrogen to argon is 1:15-1:19, the gas flow rate is controlled to be 200 sccm, the heating temperature is set to 660-670°C, and the reaction time is set to 5-10 min.

6. The method for preparing Te nanobelts by decomposing Sb2Te3 powder according to claim 1, characterized in that: The prepared Te nanoribbons are one-dimensional and have high crystal quality and oriented arrangement characteristics.

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