Preparation method of non-water-soluble transition metal disulphide nanosheets

A transition metal and disulfide technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as uneven thickness distribution of nanosheets, strict process requirements, and sensitive reaction conditions. Achieve the effect of excellent shape, low preparation cost and controllable number of layers

Inactive Publication Date: 2015-12-09
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The exfoliation method generally uses commercial water-insoluble transition metal dichalcogenide bulk powders as raw materials, and obtains water-insoluble transition metal dichalcogenide nanosheets (Acc. Chem.Res.2014,47,1067-1075)(Adv.Mater.2012,24,772-775)(J.Am.Chem.Soc.2013,135,10274-10277); although the method is simple and direct, the preparation However, there are problems such as serious uneven thickness distribution, poor dispersion, easy agglomeration, easy damage, and poor quality of nanosheets. At the same time, it is accompanied by serious noise pollution and chemical pollution caused by the peeling process.
The chemical synthesis method generally uses transition metal salts and sulfur-conta

Method used

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  • Preparation method of non-water-soluble transition metal disulphide nanosheets
  • Preparation method of non-water-soluble transition metal disulphide nanosheets
  • Preparation method of non-water-soluble transition metal disulphide nanosheets

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Weigh 0.3531g ammonium molybdate, 0.3654g thiourea and 17.55g sodium chloride, dissolve the mixture in 100ml of deionized water, stir and dissolve to form a solution with a magnetic stirrer with a stirring speed of 300r / min, and then Sonicate with a 400W sonicator for 15 minutes and mix well. Put the mixture in the refrigerator for 12 hours to freeze, and then place it in a freeze dryer at -50°C for vacuum drying until the mixture is dried. Grind the mixture and pass through a 150-mesh sieve, take 10g of powder and place it in the ark, put the ark in a tube furnace, pass through the Ar inert gas of 200ml / min to remove the air, then use the Ar inert gas of 200ml / min, and use 10 The heating rate of ℃ / min is raised to 750 ℃, and the temperature is kept for 2 hours for chemical vapor deposition. After the reaction is completed, it is cooled to room temperature under the protection of Ar atmosphere to obtain the calcined product A, which is collected, ground and washed with ...

Embodiment 2

[0032]Take by weighing 0.3531g ammonium molybdate, 0.3654g thiourea and 35.1g sodium chloride, dissolve the mixture in 150ml of deionized water, stir and dissolve to form a solution with a magnetic stirrer with a stirring speed of 300r / min, and then Sonicate with a 400W sonicator for 15 minutes and mix well. Put the mixture in the refrigerator for 12 hours to freeze, and then place it in a freeze dryer at -50°C for vacuum drying until the mixture is dried. Grind the mixture and pass through a 100-mesh sieve, take 10g of powder and place it in the ark, put the ark into the tube furnace, pass through the Ar inert gas of 200ml / min to remove the air, then use the Ar inert gas of 200ml / min, and use 10 The heating rate of ℃ / min is raised to 600 ℃, and the temperature is kept for 3 hours for chemical vapor deposition. After the reaction is completed, it is cooled to room temperature under the protection of Ar atmosphere to obtain the calcined product A, which is collected, ground and...

Embodiment 3

[0034] Weigh 0.2463g ammonium metatungstate, 0.1827g thiourea and 23.4g sodium chloride, dissolve the mixture in 100ml of deionized water, stir and dissolve with a magnetic stirrer at a stirring speed of 300r / min to form a solution, and then Ultrasound with a power of 400W for 15 minutes, and mix well. Put the mixture in the refrigerator for 12 hours to freeze, and then place it in a freeze dryer for vacuum drying at -40°C until the mixture is dried. Grind the mixture and pass through a 150-mesh sieve, take 10g of powder and place it in the ark, put the ark in a tube furnace, pass through the Ar inert gas of 200ml / min to remove the air, then use the Ar inert gas of 200ml / min, and use 10 The heating rate of ℃ / min is raised to 750 ℃, and the temperature is kept for 2 hours for chemical vapor deposition. After the reaction is completed, it is cooled to room temperature under the protection of Ar atmosphere to obtain the calcined product B, which is collected, ground and washed wi...

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Abstract

The invention relates to a preparation method of non-water-soluble transition metal disulphide nanosheets. The preparation method comprises the following steps that water-soluble salts containing transition metal elements are used as transition metal sources; thiourea is used as a sulphur source; the transition metal sources, the sulphur source and NaCl are added into deionized water to be dissolved according to the mol ratio of transition metal elements in the transition metal sources to the sulphur element in the sulphur source being 1: (1.8 to 2.5) and according to the mol ratio of the transition elements in the transition metal source to the NaCl being 1:(150 to 600); then, freezing and vacuum drying are performed to obtain a mixture; the prepared mixture is ground into powder; the powder is put into a tubular furnace constant-temperature region for calcination and chemical vapor deposition to obtain products; water washing and vacuum drying are carried out; the disulphide nanosheets are obtained. The disulphide nanosheets with the characteristics of high quality, uniform dimension, relatively controllable layer number, higher yield, lower relative preparing cost and the like can be obtained.

Description

technical field [0001] The invention relates to a universal preparation method of water-insoluble transition metal disulfide nanosheets, which can be applied to and not limited to the field of lithium-ion secondary battery electrode materials. Background technique [0002] The nanoscale two-dimensional structure of graphene has more special and magical physical and chemical properties different from the macroscopic two-dimensional structure. Such unique properties have gradually attracted scientists' attention and research on other nanoscale two-dimensional structures. [0003] Monolayer and multilayer water-insoluble transition metal dichalcogenides such as MoS 2 , W 2 , VS 2 , FeS 2 ,CoS 2 etc. Because of its close-packed hexagonal structure and sheet stacking method similar to graphene, it has aroused great research interest of scientists in recent years. Transition metal dichalcogenide nanosheets with two-dimensional structure and ultrathin thickness exhibit unusual...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/1397H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/1397H01M4/5815H01M10/0525Y02E60/10
Inventor 何春年周静雯赵乃勤师春生刘恩佐李家俊
Owner TIANJIN UNIV
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