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

Method used

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

Examples

Experimental program
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Effect test

Example Embodiment

[0021] Example 1:

[0022] Weigh 0.3531g of ammonium molybdate, 0.3654g of thiourea and 35.1g of sodium chloride, dissolve the mixture in 200ml of deionized water, stir and dissolve into a solution with a magnetic stirrer with a stirring speed of 300r / min, and then use the power Ultrasound for 15 minutes with a 400W ultrasonic device and mix well. Put the mixed solution in a refrigerator for 12 hours to freeze, and then place it in a freeze dryer at -50°C and vacuum dry 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 into the tube furnace. Pass in 200ml / min of Ar inert gas to remove the air, and then use 200ml / min of Ar inert gas and 10 The temperature rise rate is ℃ / min. The temperature is raised to 750℃ and kept for 2h for chemical vapor deposition. After the reaction, it is cooled to room temperature under the protection of Ar atmosphere to obtain calcined product A, which is collected, g...

Example Embodiment

[0024] Example 2:

[0025] Weigh 0.1765g of ammonium molybdate, 0.1827g of thiourea and 17.55g of sodium chloride, dissolve the mixture in 150ml of deionized water, stir and dissolve into a solution with a magnetic stirrer with a stirring speed of 300r / min, and then use the power Ultrasound for 15 minutes with a 400W ultrasonic device and mix well. Put the mixed solution in a refrigerator for 12 hours to freeze, and then place it in a freeze dryer at -50°C and vacuum dry until the mixture is dried. Grind the mixture and pass a 100-mesh sieve, take 10g of powder and place it in the ark, put the ark into the tube furnace, pass 200ml / min of Ar inert gas to remove the air, and then use 200ml / min of Ar inert gas and 10 The temperature rise rate is ℃ / min. The temperature is raised to 600℃ and kept for 3 hours for chemical vapor deposition. After the reaction, it is cooled to room temperature under the protection of Ar atmosphere to obtain calcined product A, which is collected, ground...

Example Embodiment

[0026] Example 3:

[0027] Weigh 0.1765g sodium molybdate, 0.1827g thiourea and 26.325g sodium chloride, dissolve the mixture in 200ml of deionized water, stir and dissolve the mixture into a solution with a magnetic stirrer with a stirring speed of 300r / min, and then use the power Ultrasound for 15 minutes with a 400W ultrasonic device and mix well. Put the mixture in a refrigerator for 12 hours to freeze, and then place it in a freeze dryer at -40°C and vacuum dry until it is dried to obtain a mixture. Grind the mixture and pass through a 150-mesh sieve. Take 10g of powder and place it in the Ark. Put the Ark into the tube furnace. Pass in 200ml / min of Ar inert gas to remove the air, and then use 200ml / min of Ar inert gas and 10 The temperature rise rate is ℃ / min. The temperature is raised to 750℃ and kept for 2h for chemical vapor deposition. After the reaction, it is cooled to room temperature under the protection of Ar atmosphere to obtain calcined product A, which is colle...

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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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