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Molybdenum disulfide nano-sheet preparation method based on sodium chloride template

A molybdenum disulfide and nanosheet technology, applied in the field of molybdenum disulfide nanosheet materials and preparation thereof, can solve the problems of difficulty in obtaining dispersed molybdenum disulfide nanosheets, uneven size and thickness distribution, and easy damage to the nanosheets. , to achieve the effect of excellent morphology, low cost and high crystallinity

Inactive Publication Date: 2016-01-06
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The exfoliation method is the most important and mature method for preparing molybdenum disulfide nanosheets in recent years. Generally, commercialized molybdenum disulfide bulk powder is used as raw material to prepare molybdenum disulfide nanosheets by ultrasonic degradation or chemical exfoliation. (Adv.Mater.2012,24,772–775)(J.Am.Chem.Soc.2013,135,10274-10277); Although the exfoliation method is simple and direct, there are certain problems, such as the nanosheets are easily damaged and the quality Low height, uneven size and thickness distribution, long preparation time, easy to cause noise pollution and chemical pollution, etc.
The synthesis method can obtain molybdenum disulfide nanostructures with high crystallinity and good quality, but due to the large specific surface area of ​​the nanosheet itself, it will spontaneously tend to stack and agglomerate to reduce the Gibbs free energy of the system, so to So far, the method of synthesis is often to obtain a flower-like structure (Electrochim.Acta.2014, 115, 165-169) (RSCAdv.2015, 5, 7938-7943), it is difficult to obtain good dispersion and quality Higher, uniform size molybdenum disulfide nanosheets

Method used

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  • Molybdenum disulfide nano-sheet preparation method based on sodium chloride template
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  • Molybdenum disulfide nano-sheet preparation method based on sodium chloride template

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take by weighing 0.3531g ammonium molybdate, 0.3654g thiourea and 35.1g sodium chloride, dissolve the mixture in 200ml 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 wa...

Embodiment 2

[0025] Weigh 0.1765g ammonium molybdate, 0.1827g thiourea and 17.55g 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 washed w...

Embodiment 3

[0027] Take by weighing 0.1765g sodium molybdate, 0.1827g thiourea and 26.325g sodium chloride, dissolve the mixture in 200ml 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 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 A, which is collected, ground and wa...

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Abstract

The invention relates to a molybdenum disulfide nano-sheet preparation method based on a sodium chloride template. The method comprises the following steps: one or a mixture of two selected from ammonium molybdate and sodium molybdate is adopted as a molybdenum source; thiourea is adopted as a sulfur source; the molybdenum source, the sulfur source and NaCl are dissolved in deionized water according to a molar ratio that molybdenum in the molybdenum source to sulfur in the sulfur source is 1:(1.8-2.5) and according to that the molar ratio of molybdenum in the molybdenum source to NaCl is 1:(150-600); freezing and vacuum drying are carried out, such that a mixture is obtained; the prepared mixture is ground into powder; the powder is sieved and is laid in a square boat; the powder is placed in a tubular furnace thermostatic zone, and is subjected to calcining and chemical vapor deposition, such that a product A is obtained; the product A is washed and vacuum-dried, such that the molybdenum disulfide nano-sheets are obtained. with the method provided by the invention, molybdenum disulfide nano-sheets with characteristics of high quality, uniform dimension, relatively controllable layer number, relatively high yield and relatively low preparation cost can be obtained.

Description

technical field [0001] The invention relates to a molybdenum disulfide nanosheet material and a preparation method thereof, which can be applied to and not limited to the field of electrode materials for lithium-ion secondary batteries. Background technique [0002] Molybdenum disulfide is a typical transition metal dichalcogenide, and its unique physical and chemical properties have aroused widespread interest of scientists and received a lot of research in recent years. Molybdenum disulfide has a close-packed hexagonal structure similar to graphene, and a similar sheet stacking method; a single molybdenum disulfide molecular layer consists of two layers of S atomic layers, one layer of Mo atomic layers, and a sandwich of S-Mo-S. Composed of valence bonds, Molybdenum disulfide molecular layers are combined with weaker van der Waals forces. Compared with graphene, molybdenum disulfide has a larger (002) interplanar spacing with a width of 0.62nm, which enables it to store m...

Claims

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Application Information

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IPC IPC(8): C01G39/06
CPCC01G39/06B82Y40/00
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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