Preparation method of tungsten disulfide nanotube

A tungsten disulfide and nanotube technology, applied in chemical instruments and methods, nanotechnology, tungsten compounds, etc., to achieve the effects of low temperature, simple and easy-to-control production process, and uniform diameter

Inactive Publication Date: 2011-07-27
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of tungsten disulfide nanotubes, the method aims to solve the size and size distribution of tungsten disulfide nanotubes, and the prepared tungsten disulfide nanotubes have a certain size and growth orientation. Good consistency and pure product

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  • Preparation method of tungsten disulfide nanotube
  • Preparation method of tungsten disulfide nanotube
  • Preparation method of tungsten disulfide nanotube

Examples

Experimental program
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Effect test

Embodiment 1

[0020] A porous alumina template with a pore diameter of about 100 nm and uniform size was prepared by a secondary anodic oxidation method. Dissolve 0.35 g of ammonium tetrathiotungstate in 5 mL of dimethyl sulfoxide, and magnetically stir to prepare a 0.2 mol / L precursor solution. The prepared AAO template was immersed in the precursor solution for 30 min, and then the AAO template was placed in an oven at 70°C to fully volatilize the dimethyl sulfoxide solvent. This process was repeated three times. Put the AAO template loaded with the precursor into a horizontal tubular heating furnace, and feed H at a flow rate of 50 mL / min. 2 / N 2 Mixed gas (H 2 and N 2 The volume ratio is 1:9), and at the same time, heat the tube furnace to 550°C at a heating rate of 10°C / min, keep it warm for 1-2h to fully react, and then cool to room temperature with the furnace to obtain blue-black tungsten disulfide nanotube.

[0021] figure 1 It is a transmission electron microscope (TEM) phot...

Embodiment 2

[0023] A porous alumina template with a pore diameter of about 100 nm and uniform size was prepared by a secondary anodic oxidation method. Dissolve 0.35 g of ammonium tetrathiotungstate in 5 mL of dimethyl sulfoxide, and magnetically stir to prepare a 0.2 mol / L precursor solution. The precursor solution was introduced into the AAO template by suction filtration, and then the AAO template was placed in an oven at 70°C to fully volatilize the dimethyl sulfoxide solvent. Put the AAO template loaded with the precursor into a horizontal tubular heating furnace, and feed H at a flow rate of 50 mL / min. 2 / N 2 Mixed gas (H 2 and N 2 The volume ratio is 1:9), while heating the tube furnace to 550°C at a heating rate of 10°C / min, keeping it warm for 1-2h to fully react, and then cooling to room temperature with the furnace to obtain tungsten disulfide nanotubes.

[0024] figure 2 It is a transmission (TEM) photo of the tungsten disulfide nanotubes prepared in this embodiment. It...

Embodiment 3

[0026] A porous alumina template with a pore diameter of about 100 nm and uniform size was prepared by a secondary anodic oxidation method. Dissolve 0.54 g of ammonium tetrathiotungstate in 5 mL of dimethyl sulfoxide, and magnetically stir to prepare a 0.3 mol / L precursor solution. The prepared AAO template was immersed in the precursor solution for 2 days, and then the AAO template was placed in an oven at 70° C. to fully volatilize the dimethyl sulfoxide solvent. Put the AAO template soaked in the solution into a horizontal tubular heating furnace, and pass H at a flow rate of 50mL / min. 2 / N 2 Mixed gas (H 2 and N 2 The volume ratio is 1:9), and at the same time, heat the tube furnace to 550°C at a heating rate of 10°C / min, keep it warm for 1-2h to fully react, and then cool to room temperature with the furnace to obtain blue-black tungsten disulfide nanotube.

[0027] image 3 It is a transmission (TEM) photo of the tungsten disulfide nanotubes prepared in this embodi...

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Abstract

The invention relates to a preparation method of a tungsten disulfide nanotube, comprising the following steps of: with (NH4)2WS4 as a raw material, preparing, soaking, pyrolyzing and separating a template. The preparation method of the tungsten disulfide nanotube is characterized by comprising the following steps of: soaking the AAO (Anodic Aluminum Oxide) template into a DMSO (Dimethylsulfoxide) solution of the (NH4)2WS4 with the concentration of 0.2-0.4 mol/L for at least half hour; taking out the AAO template, volatilizing solvent DMSO, then placing in a reducing atmosphere and calcining at 500-600 DEG C for 1-2 hours; and cooling, and then separating to obtain the WS2 nanotube from the AAO template. The preparation method has a simple process; and in addition, the prepared WS2 nanotube has uniform, consistent and controllable diameter.

Description

1. Technical field [0001] The present invention relates to a kind of preparation method of inorganic nano material, specifically a kind of tungsten disulfide (WS 2 ) Nanotube preparation method. 2. Background technology [0002] Tungsten disulfide has a layered structure similar to graphite, with weak van der Waals force between layers, and metal W atoms and S atoms in the layer are combined with strong covalent bonds. But under the influence of the outside world, WS 2 The dangling bonds at the edge of the sheet are easily destabilized and coiled to form nanotube or fullerene structures. WS of fullerene structure 2 Due to the absence of dangling bonds, nanomaterials have lower surface energy and higher chemical stability, making their friction properties far better than those of traditional layered 2H-WS. 2 . WS 2 Due to their unique structure and properties, nanotubes can be applied to solid lubricants (especially under high vacuum and high load), electrode materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00B82Y40/00
Inventor 凤仪朱艳芳张学斌李斌余东波刘慧强
Owner HEFEI UNIV OF TECH
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