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Method for quickly synthesizing tungsten sulphide nanometer powder

A nano-powder, tungsten sulfide technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of long synthesis cycle, poor crystallinity, and small yield, and achieve fast reaction speed, high conversion rate, and high yield. Effect

Active Publication Date: 2016-12-07
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Others use non-toxic sulfur powder as a sulfur source, whether tungsten powder or tungsten oxide is used as a tungsten source, the reaction mechanism is as described above, and there are disadvantages such as long synthesis period, low purity, poor crystallinity, and small output. Failed to replace ammonium thiotungstate method

Method used

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  • Method for quickly synthesizing tungsten sulphide nanometer powder
  • Method for quickly synthesizing tungsten sulphide nanometer powder
  • Method for quickly synthesizing tungsten sulphide nanometer powder

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The method for rapidly synthesizing tungsten sulfide nanopowder of the present invention comprises the following steps:

[0023] Step 1, put 0.1g of tungstic acid powder in the quartz boat, and place it in the constant temperature zone of the openable tube furnace, put excess sulfur powder in the quartz boat, and place it in the tube furnace In the upstream area of ​​the carrier gas, a separate heating jacket is added to control the temperature separately to ensure a constant evaporation rate of sulfur;

[0024] Step 2, first evacuate the quartz tube, and when the vacuum degree of the vacuum chamber is below 4Pa, pass the carrier gas argon (introduction speed 0.2L / min) and air (introduction speed 80mL / min) into the quartz tube , adjust the pressure in the quartz tube to be stable at 5KPa, start the heating program of the tube furnace and a separate heating mantle to control the velocity of sulfur evaporation, and increase the temperature of the constant temperature zone...

Embodiment 2

[0028] The method for rapidly synthesizing tungsten sulfide nanopowder of the present invention comprises the following steps:

[0029]Step 1, put 1g of tungstic acid powder in the quartz boat, and place it in the constant temperature zone of the openable tube furnace, put excess sulfur powder in the quartz boat, and place it in the tube furnace In the upstream area of ​​the gas, a separate heating jacket is added to control the temperature separately to ensure a constant evaporation rate of sulfur;

[0030] Step 2, first evacuate the quartz tube, and when the vacuum degree of the vacuum chamber is below 4Pa, pass the carrier gas argon into the quartz tube (passing speed 0.2L / min), and adjust the pressure in the quartz tube to stabilize at 5KPa , start the heating program of the tube furnace and a separate external heating mantle to control the velocity of sulfur evaporation, raise the constant temperature zone of the tube furnace to 600 °C at a rate of 30 °C / min, and the cont...

Embodiment 3

[0034] The method for rapidly synthesizing tungsten sulfide nanopowder of the present invention comprises the following steps:

[0035] Step 1, put 1g of tungstic acid powder in the quartz boat, and place it in the constant temperature zone of the openable tube furnace, put excess sulfur powder in the quartz boat, and place it in the tube furnace In the upstream area of ​​the gas, a separate heating jacket is added to control the temperature separately to ensure a constant evaporation rate of sulfur;

[0036] Step 2, first evacuate the quartz tube, and when the vacuum degree of the vacuum chamber is below 4Pa, pass the carrier gas argon into the quartz tube (passing speed 0.2L / min), and adjust the pressure in the quartz tube to stabilize at 5KPa , start the heating program of the tube furnace and a separate external heating mantle to control the velocity of sulfur evaporation, raise the constant temperature zone of the tube furnace to 600 °C at a rate of 30 °C / min, and the con...

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Abstract

The invention discloses a method for quickly synthesizing tungsten sulphide nanometer powder. According to the method disclosed by the invention, tungstic acid and elemental sulfur are used as raw materials, and under the condition of protective atmosphere of 600-750 DEG C, a reaction is performed for 5-30 minutes, so that the tungsten disulfide nanometer powder which is large in specific surface area, high in crystalinity and good in dispersibility is obtained. A gas phase synthesis technique adopted by the method disclosed by the invention is applied to the synthesis of the tungsten sulphide nanometer materials, and compared with a conventional method for industrial production of WS2, the method disclosed by the invention has the advantages of being milder in reaction conditions, lower in cost of raw materials, more environmental-friendly, higher in reaction speed, higher in conversion rate and higher in yield; and in small-batch synthesis, the heat preservation time can be shortened to 5 minutes, but 95% or above of the conversion rate of the tungsten sulphide can also be maintained, and the method can be suitable for industrial large-scale production of high-grade tungsten sulphide.

Description

technical field [0001] The invention relates to a method for rapidly synthesizing tungsten sulfide nanopowder, which belongs to the field of nanomaterial preparation. Background technique [0002] Transition metal sulfides have a layered structure similar to graphite, and the layers are bonded by strong covalent bonds, while the layers are bonded by weak van der Waals forces, so the layers are easy to peel off, with good anisotropy and low coefficient of friction. Tungsten disulfide (WS 2 ), as a typical transition metal sulfide, has unique properties in many aspects such as optics, electricity, catalysis, and mechanics, and is widely used in various fields such as electrode materials, catalysts, and solid lubricants. Especially in terms of solid lubricants, it is not only suitable for general lubrication conditions, but also has a good lubrication effect in certain high temperature, high pressure, high vacuum, high load, radiation and corrosive environments. Excellent lu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00
CPCC01G41/00C01P2002/72C01P2004/03
Inventor 洪昆权葛兴
Owner SOUTHEAST UNIV
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