Preparation method of tungsten disulfide micron structure

A micron-structured tungsten disulfide technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of high reaction temperature, high toxicity, serious reaction pollution, etc., to reduce production costs, reduce toxicity, The effect of uniform product size

Inactive Publication Date: 2013-01-30
ZHEJIANG ORIENT CRYSTAL OPTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of preparation method, WS 2 The preparation of nanostructures mainly includes hydrothermal reaction method, chemical vapor deposition (CVD) method, ultrasonic oscillation method, microwave radiation method, WO 3 Reduction methods, etc., among which the more commonly used methods are hydrothermal method and CVD method, such as Y.D.Li et al. (JACS) prepared WS by hydrothermal method 2 nanotubes, but the preparation cycle of this method is long; Jifen Wu et al. (Material Lett.) prepared WS by hydrothermal method 2 Hollow spheres, but the use of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] with thiourea and WCl 6 As the reaction raw material, the tubular annealing furnace was used as the reaction system to prepare WS 2 micron tube.

[0011] First weigh a certain amount of thiourea and WCl 6 , making thiourea and WCl 6 The molar ratio is 9:1. Then put it in the reaction system, vacuumize the reaction system, and when it reaches about 10Pa, fill the system with high-purity argon with a purity of more than 99.99% to 1 atmosphere, and then vacuumize it again to 10Pa, and so on. , cyclic pumping and inflating three times, until the air in the system is basically completely eliminated, and the reaction system is sealed. The system was then ramped to 800°C over 50 minutes, where it was grown for 60 minutes before heating was turned off. The system was kept under vacuum throughout the reaction process. After the system naturally cools down to room temperature, take out the sample for structure and morphology characterization. After the reaction, collect the...

Embodiment 2

[0013] with thiourea and WCl 6 As the reaction raw material, the tubular annealing furnace was used as the reaction system to prepare WS 2 micron tube.

[0014] First weigh a certain amount of thiourea and WCl 6 , making thiourea and WCl 6 The molar ratio is 7:1. Then put it in the reaction system, vacuumize the reaction system, and when it reaches about 10Pa, fill the system with high-purity argon with a purity of more than 99.99% to 1 atmosphere, and then vacuumize it again to 10Pa, and so on. , cyclic pumping and inflating three times, until the air in the system is basically completely eliminated, and the reaction system is sealed. The system was then ramped to 850°C over 60 minutes, where it was grown for 60 minutes before heating was turned off. The system was kept under vacuum throughout the reaction process. After the system naturally cools down to room temperature, take out the sample for structure and morphology characterization. After the reaction, collect the...

Embodiment 3

[0016] with thiourea and WCl 6 As the reaction raw material, the tubular annealing furnace was used as the reaction system to prepare WS 2 micron tube.

[0017] First weigh a certain amount of thiourea and WCl 6 , making thiourea and WCl 6 The molar ratio is 6:1. Then put it in the reaction system, vacuumize the reaction system, and when it reaches about 10Pa, fill the system with high-purity argon with a purity of more than 99.99% to 1 atmosphere, and then vacuumize it again to 10Pa, and so on. , cyclic pumping and inflating three times, until the air in the system is basically completely eliminated, and the reaction system is sealed. The system was then ramped to 850°C over 60 minutes, where it was grown for 80 minutes before heating was turned off. The system was kept under vacuum throughout the reaction process. After the system naturally cools down to room temperature, take out the sample for structure and morphology characterization. After the reaction, collect the...

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Abstract

The invention belongs to the manufacturing field of semiconductor micron materials and particularly relates to a preparation method of a tungsten disulfide micron structure. The preparation method is characterized in that the chemical vapor deposition (CVD) method is adopted, thiourea and tungsten hexachloride (WC16) are taken as reaction sources, and the structure is obtained in a vacuum state at 750-950 DEG C. According to the preparation method, the thiourea and WC16 are placed in a constant temperature area and a low temperature area respectively, the reaction temperature of the WC16 is maintained at 750-950 DEG C, the temperature difference between the WC16 and the thiourea is maintained at 50-150 DEG C, the saturated vapor pressure is reached simultaneously at a specific temperature by using the temperature difference, and steam is generated for reaction. The preparation method has the advantages of being simple and easy to implement, environment-friendly, non-toxic and even in product size; particularly the non-toxic thiourea is used as the S source, the production cost and toxicity of S sources such as H2S are reduced, and the preparation method is economical and environment-friendly.

Description

technical field [0001] The invention belongs to the manufacturing category of semiconductor micron materials, in particular to a preparation method of tungsten disulfide micron structure, especially a preparation method of tungsten disulfide micron tube. Background technique [0002] The unique structure, excellent properties and many potential applications of inorganic fullerene nanomaterials have attracted widespread attention and research interest from scientists all over the world. Tungsten disulfide (WS 2 ) is usually a layered structure compound with a structure similar to graphite, which is WS 2 Layer stacking along the C axis (perpendicular to the sulfide layer), WS 2 In the layer is a strong covalent bond between the metal W atom and the S atom, and the WS 2 The layers are combined by weak van der Waals force. In addition, WS 2 As a semiconductor itself, it has important application potential in energy band engineering. More recently, scientists have proposed t...

Claims

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Application Information

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IPC IPC(8): C01G41/00
Inventor 李京波孟秀清李庆跃李凯池旭明夏建白
Owner ZHEJIANG ORIENT CRYSTAL OPTICS
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