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Method for preparing mono-disperse tungsten disulfide nano slices

A tungsten disulfide, nanosheet technology, applied in nanostructure fabrication, chemical instruments and methods, nanotechnology, etc., can solve the problems of inability to laterally divide and refine the basal plane, limit catalytic performance, etc.

Inactive Publication Date: 2010-06-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Tye et al. from the University of British Columbia (UBC) prepared a monolayer of molybdenum disulfide by exfoliation technology and studied its catalytic performance. The results showed that the monolayer structure can effectively improve the catalytic activity, but the exfoliation technology is only for longitudinal structural solution. Therefore, the preparation of nano-scale monodisperse sheet-like nanostructures has become a bottleneck that limits the further improvement of its catalytic performance.

Method used

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  • Method for preparing mono-disperse tungsten disulfide nano slices
  • Method for preparing mono-disperse tungsten disulfide nano slices
  • Method for preparing mono-disperse tungsten disulfide nano slices

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Mix 5g of tungsten oxide and 10g of sulfur into a stainless steel ball milling jar, pass in argon as a protective gas, use stainless steel balls as a ball milling medium with a ball-to-material ratio of 60:1, and mill at 400rpm for 24h. Take 1g of the activated product from ball milling and put it into a porcelain boat, and take another porcelain boat and fill it with 2g of sulfur; the tube furnace is pre-filled with argon to exhaust the air, and heated to 600°C, then place the above two boats in the heating zone , where the porcelain boat filled with sulfur is placed at the upstream of the gas as a supplementary sulfur source; after being kept at a constant temperature for 0.5h in an argon atmosphere, it is cooled to 250°C with the furnace in a hydrogen atmosphere, the porcelain boat is taken out, and the black powder is collected to obtain Monodisperse tungsten disulfide nanosheets with a thickness of about 4nm. figure 1 It is a field emission scanning electron micros...

Embodiment 2

[0015] Mix 5g of tungsten oxide and 10g of sulfur into a stainless steel ball milling tank, pass in argon as a protective gas, use stainless steel balls as a ball milling medium with a ball-to-material ratio of 60:1, and mill at 400rmp for 24h. Take 1g of the activated product from ball milling and put it into a porcelain boat. The tube furnace is filled with argon gas to exhaust the air, and heated to 600°C. Then place the porcelain boat in the heating zone without supplementary sulfur source; under argon atmosphere After constant temperature for 2 hours, cool down to 200°C with the furnace in a hydrogen atmosphere, take out the porcelain boat, collect black powder, and use XRD for detection. The results show that the product contains tungsten disulfide and partial tungsten oxide, indicating that the vulcanization is not complete, so it must be pre- Supplementary sulfur source.

Embodiment 3

[0017] Mix 5g of tungsten oxide and 10g of sulfur into a stainless steel ball milling tank, pass in argon as a protective gas, use stainless steel balls as a ball milling medium with a ball-to-material ratio of 60:1, and mill at 400rmp for 24h. Take 1g of the activated product from the ball mill and put it into a porcelain boat, and take another porcelain boat and fill it with 2g of sulfur; the tube furnace is pre-filled with argon to exhaust the air, and heated to 500°C, and then put the above two boats in the heating zone , where the porcelain boat filled with sulfur was placed in the upstream of the gas as a supplementary sulfur source; after being kept at a constant temperature for 2 hours in an argon atmosphere, it was cooled to 200°C with the furnace, the porcelain boat was taken out, and the black powder was collected. The experimental results showed that the product was not fully vulcanized. , only a small amount of flaky tungsten disulfide is generated.

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Abstract

The invention discloses a method for preparing mono-disperse tungsten disulfide nano slices. The method comprises the following steps: ball-milling, mixing and activating tungsten oxide and sulfur serving as raw materials, and annealing for 30 to 120 minutes at the constant temperature of between 600 and 700 DEG C in a protective atmosphere; during annealing at the constant temperature, preposing a part of sulfur powder as a complementary sulfur source, wherein the mass ratio of the complementary sulfur powder to the reaction mixture is between 0.05 and 10; and then, cooling a reaction product to below 250 DEG C along with a furnace in the protective atmosphere to obtain the mono-disperse tungsten disulfide nano slices. The method prepares a large amount of mono-disperse slice tungsten disulfide material by a simple and effective chemical synthesis method; and the method is simple and quick, has low production cost, and can be widely used in the aspects of lubrication and catalysis.

Description

technical field [0001] The invention relates to a preparation method in the field of nanomaterials, in particular to a preparation method of monodisperse sheet-like tungsten disulfide nanomaterials. Background technique [0002] Nano tungsten disulfide (WS 2 ) has broad application prospects in electronic probes, petroleum catalysis, hydrogen storage materials, friction lubrication, and solar cells due to its high specific surface area and good optical, electrical, lubricating, and catalytic properties. At present, the methods for preparing tungsten disulfide nanomaterials mainly include high-temperature gas-solid reaction method, thermal decomposition method, hydrothermal method, electrochemical method, chemical vapor deposition method and so on. The morphology and structure of prepared tungsten disulfide nanomaterials are also different, including nanotubes, nanowires, nanorods, nanoflowers, hollow nanospheres and inorganic fullerene structures, but there are few reports ...

Claims

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Application Information

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IPC IPC(8): C01G41/00B82B3/00
Inventor 王德志吴壮志孙翺魁汪异
Owner CENT SOUTH UNIV
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