CN107934926B - Preparation method of molybdenum diselenide nanotube - Google Patents
Preparation method of molybdenum diselenide nanotube Download PDFInfo
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- CN107934926B CN107934926B CN201711443092.0A CN201711443092A CN107934926B CN 107934926 B CN107934926 B CN 107934926B CN 201711443092 A CN201711443092 A CN 201711443092A CN 107934926 B CN107934926 B CN 107934926B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The invention discloses a preparation method of a molybdenum diselenide nanotube, which comprises the following process steps: 1) paving molybdenum hexacarbonyl at the bottom of a ceramic crucible, then placing a porous anodic aluminum oxide template with an opening downward above the molybdenum hexacarbonyl, sealing the crucible, placing the crucible in a tubular furnace, carrying out low-temperature sublimation deposition under the protection of gas, and continuously heating for pyrolysis; 2) after the temperature of the vacuum tube furnace is reduced to room temperature, the opening of the template is downwards placed in a ceramic crucible filled with selenium powder, and the temperature is raised after the crucible is sealed, so that elemental selenium and metal molybdenum are directly reacted; 3) removing the porous alumina template and the redundant selenium by using a dilute acid solution, then carrying out suction filtration treatment, and drying to obtain a finished product. The method has simple steps, no environmental pollution and no need of complex equipment, and the prepared molybdenum diselenide nanotube powder material has strong size controllability, good crystallinity and uniform nanotube wall morphology, thereby greatly improving the comprehensive performance of the finished product of the molybdenum diselenide nanotube powder material. The invention has wide applicability and is beneficial to large-scale industrial production.
Description
Technical Field
The invention relates to the field of semiconductor nano materials, in particular to a preparation method of a semiconductor nano tube.
Background
Two-dimensional semiconductor materials have been increasingly studied because of their inherently large band gaps. However, graphene has great research value in electronics due to its remarkable carrier mobility, but its application in optoelectronics is greatly limited due to the lack of band gap. Molybdenum diselenide is a transition metal selenide, has a two-dimensional layered structure with a band gap, and is formed by stacking hexagonal X-M-X sandwich units, metal elements and selenium group elements are combined into a single sandwich unit through covalent bonds, and different units are combined through weak van der Waals force. The unique energy band structure determines that the material has abundant electronic states, so that the material is very suitable for application in the fields of electronics, photonics and the like. In addition, the molybdenum diselenide single-layer sheet is of a three-dimensional porous structure, has good structural rigidity, and can remarkably improve the thermal property, the mechanical property and other properties of the device. Therefore, the molybdenum diselenide two-dimensional crystal has wide application prospect in the fields of solar cells, photocatalysts, phototransistors, light emitting diodes, light modulators and the like. The current research reports mainly focus on the preparation and performance research of multilayer molybdenum diselenide, and the research on one-dimensional materials is less, especially the preparation method.
Disclosure of Invention
The invention aims to provide a preparation method of a molybdenum diselenide nanotube aiming at the defects of the prior art, and the obtained molybdenum diselenide nanotube powder material has wide applicability and excellent comprehensive performance and can be applied to electronic devices.
The technical scheme adopted by the invention is as follows: a preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) taking molybdenum hexacarbonyl as a raw material and porous anodic aluminum oxide as a template, paving the raw material at the bottom of a ceramic crucible, then placing the porous anodic aluminum oxide template with an opening downward above the raw material, sealing the crucible, placing the crucible in a vacuum tube furnace, heating under the protection of gas, sublimating at low temperature to sublimate and deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template, continuously heating to deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template for thermal decomposition to obtain metal molybdenum deposit;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the alumina template, placing the alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating the vacuum tube furnace under the protection of gas to ensure that elemental selenium and metal molybdenum directly react, stopping heating, and cooling the crucible to room temperature along with the furnace;
3) removing the porous alumina template and the redundant selenium by using a dilute acid solution, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product.
As a further improvement of the scheme, the pore diameter of the porous anodic alumina template in the step 1) is within the range of 10-200 nm. In particular, the shape controllability of the nanotube can be stronger by limiting the pore diameter of the porous anodic alumina template.
As a further improvement of the scheme, the low-temperature sublimation temperature in the step 1) is 50-150 ℃, and the sublimation time is 30-200 min. The invention directly obtains the deposit through low-temperature sublimation, and the limit of the sublimation temperature and the heat preservation time can ensure that the molybdenum hexacarbonyl is more fully deposited.
As a further improvement of the scheme, the thermal decomposition temperature in the step 1) is 200-420 ℃, and the thermal decomposition time is 30-100 min. In particular, the limitation of the pyrolysis temperature and the pyrolysis time can effectively improve the crystallinity of the metal molybdenum in the alumina template.
As a further improvement of the scheme, in the step 2), the reaction temperature of the elemental selenium and the metal molybdenum is 500-750 ℃, and the reaction time is 30-120 min. In particular, the reaction temperature and the reaction time of the molybdenum diselenide are limited by the invention, so that the reaction is more complete.
As a further improvement of the scheme, the dilute acid solution in the step 3) is a phosphoric acid solution with the concentration of 0.1-3 mol/L. In particular, further definition of dilute acid solution allows for more efficient removal of the alumina template.
As a further improvement of the scheme, the gas in the step 1) and the step 2) is argon or nitrogen, the gas purity is 99.999%, and the gas flow rate of the gas protection is 10-500 SCCM.
The invention has the beneficial effects that: the method has simple steps, realizes the direct reaction of the molybdenum metal and the selenium powder in a limited space to prepare the molybdenum diselenide nanotube powder material, has no environmental pollution, does not need complex equipment, and has strong size controllability, good crystallinity and uniform nanotube wall appearance of the prepared molybdenum diselenide nanotube powder material, thereby greatly improving the comprehensive performance of the finished product of the molybdenum diselenide nanotube powder material. The invention has wide applicability and is beneficial to large-scale industrial production.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercial products; the process steps or preparation methods not mentioned in detail are all process steps or preparation methods known to the person skilled in the art.
Example 1
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM argon to clean air in the furnace tube. Under the protection of 100SCCM argon, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 250 ℃ under the protection of 100SCCM argon gas, keeping the temperature for 60min, continuing heating to 650 ℃ and keeping the temperature for 90min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 1.
Example 2
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 10nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM argon to clean air in the furnace tube. Under the protection of 100SCCM argon, heating to 50 ℃ and preserving heat for 200min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 220 ℃ under the protection of 100SCCM argon gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product of the molybdenum diselenide nanotube powder material in the embodiment 2.
Example 3
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 200nm with an opening downward above the molybdenum hexacarbonyl, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM argon to clean air in the furnace tube. Under the protection of 100SCCM argon, heating to 150 ℃ and preserving heat for 30min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 220 ℃ under the protection of 100SCCM argon gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.1mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product of the molybdenum diselenide nanotube powder material in the embodiment 3.
Example 4
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 200 ℃ and preserving heat for 100min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 220 ℃ under the protection of 100SCCM nitrogen, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 4.
Example 5
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM argon to clean air in the furnace tube. Under the protection of 100SCCM argon, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 420 ℃ and preserving heat for 30min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 300 ℃ under the protection of 100SCCM argon gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 5.
Example 6
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM argon to clean air in the furnace tube. Under the protection of 100SCCM argon, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 300 ℃ under the protection of 100SCCM argon gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 6.
Example 7
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 10SCCM argon to clean air in the furnace tube. Under the protection of 10SCCM argon, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 220 ℃ under the protection of 10SCCM argon gas, keeping the temperature for 120min, continuing heating to 500 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 7.
Example 8
A preparation method of molybdenum diselenide nanotubes comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 500SCCM argon to clean air in the furnace tube. Under the protection of argon gas of 500SCCM, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 220 ℃ under the protection of 500SCCM argon gas, keeping the temperature for 60min, continuing heating to 750 ℃ and keeping the temperature for 30min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out a sample, removing the porous alumina template and the redundant selenium powder by using a phosphoric acid solution with the concentration of 0.3mol/L, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum diselenide nanotube powder material in the embodiment 8.
Example 9
The finished products of the molybdenum diselenide nanotube powder materials prepared in the above embodiments 1 to 8 are observed by a scanning electron microscope respectively, and the finished products are observed to form one-dimensional tubular structures with uniform tube wall appearance and uniform diameter, and have good crystallinity and strong controllability of nanotube appearance.
The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (4)
1. A preparation method of molybdenum diselenide nanotubes is characterized by comprising the following process steps:
1) taking molybdenum hexacarbonyl as a raw material and porous anodic aluminum oxide as a template, paving the raw material at the bottom of a ceramic crucible, then placing a porous anodic aluminum oxide template with an opening downward above the raw material, sealing the crucible, placing the crucible in a vacuum tube furnace, heating under the protection of gas, sublimating at low temperature to deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template, continuously heating to thermally decompose the molybdenum hexacarbonyl deposited in the porous anodic aluminum oxide template to obtain metal molybdenum deposit;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with selenium powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating under the protection of gas to enable elemental selenium to directly react with metal molybdenum, stopping heating after the reaction is finished, and cooling the crucible to the room temperature along with the furnace;
3) removing the porous alumina template and the redundant selenium by using a dilute acid solution, washing by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product;
the low-temperature sublimation in the step 1) is carried out at the temperature of 50-150 ℃ for 30-200 min; the thermal decomposition temperature in the step 1) is 200-420 ℃, and the thermal decomposition time is 30-100 min; in the step 2), the reaction temperature of the elemental selenium and the metal molybdenum is 500-750 ℃, and the reaction time is 30-120 min.
2. The method for preparing molybdenum diselenide nanotubes as claimed in claim 1, wherein: the aperture of the porous anodic alumina template in the step 1) is within the range of 10-200 nm.
3. The method for preparing molybdenum diselenide nanotubes as claimed in claim 1, wherein: the diluted acid solution in the step 3) is a phosphoric acid solution with the concentration of 0.1-3 mol/L.
4. The method for preparing molybdenum diselenide nanotubes as claimed in claim 1, wherein: in the step 1) and the step 2), the gas is argon or nitrogen, the gas purity is 99.999%, and the gas flow rate of the gas protection is 10-500 SCCM.
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| CN1669920A (en) * | 2004-12-29 | 2005-09-21 | 浙江大学 | Method for preparing one-dimensional nanostructure in anode alumina template |
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| 类石墨烯二硫化钨薄膜的化学气相沉积法制备及其应用;尤运城 等;《化学进展》;20151112;第27卷(第11期);第1578页摘要，第1580页第3.1节 * |
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