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Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation

A molybdenum disulfide, nanosheet technology, applied in the direction of molybdenum sulfide, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of harsh conditions, slow speed, complicated operation, etc., and achieve good dispersion state and thickness. uniform effect

Inactive Publication Date: 2015-01-28
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation. Problems such as slow speed, low yield, harsh conditions and complicated operation

Method used

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  • Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation
  • Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation
  • Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (a) Ultrasound-assisted lithium intercalation

[0029] Add 200mg of molybdenum disulfide powder into a 25ml Schlenk tube, remove the air in the reaction tube with high-purity argon and then seal it, and slowly add 6.25ml of n-butyllithium (2.4M) solution dropwise. Ultrasonic reaction at room temperature for 40 min.

[0030] (b) Stripping of molybdenum disulfide

[0031] Stop the reaction, let it stand for 30 minutes, remove unreacted n-butyllithium, add 5ml of pre-deoxygenated ultrapure water to the reaction tube, continue the reaction under ultrasonic conditions for 0.5h, and peel off to obtain the crude product of molybdenum disulfide nanosheets.

[0032] (c) Ethanol cleaning

[0033] Measure 5ml of absolute ethanol and mix it with the obtained suspension of molybdenum disulfide nanosheets. Centrifuge at 12000rpm for 10min, discard the supernatant, and collect the product at the bottom of the centrifuge tube; use 10ml of absolute ethanol to make a 20mg / ml suspensio...

Embodiment 2

[0037] (a) Ultrasound-assisted lithium intercalation

[0038] Add 200mg of molybdenum disulfide powder into a 25ml Schlenk tube, remove the air in the reaction tube with high-purity argon and then seal it, and slowly add 1.04ml of n-butyllithium (2.4M) solution dropwise. Ultrasonic reaction at room temperature for 1 h.

[0039] (b) Stripping of molybdenum disulfide

[0040] Stop the reaction, let it stand for 30 minutes, remove unreacted n-butyllithium, add 10ml of pre-deoxygenated ultrapure water to the reaction tube, continue the reaction under ultrasonic conditions for 0.5h, and peel off to obtain the crude product of molybdenum disulfide nanosheets.

[0041] (c) Ethanol cleaning

[0042]Measure 10ml of absolute ethanol and mix it with the obtained suspension of molybdenum disulfide nanosheets. Centrifuge at 10,000rpm for 20min, discard the supernatant, and collect the product at the bottom of the centrifuge tube; use 20ml of absolute ethanol to make a 10mg / ml suspension...

Embodiment 3

[0046] (a) Ultrasound-assisted lithium intercalation

[0047] Add 200mg of molybdenum disulfide powder into a 25ml Schlenk tube, remove the air in the reaction tube with high-purity argon and then seal it, and slowly add 1.04ml of n-butyllithium (2.4M) solution dropwise. Ultrasonic reaction at room temperature for 3h.

[0048] (b) Stripping of molybdenum disulfide

[0049] Stop the reaction, let it stand for 30 minutes, remove unreacted n-butyllithium, add 10ml of pre-deoxygenated ultrapure water to the reaction tube, continue the reaction under ultrasonic conditions for 0.5h, and peel off to obtain the crude product of molybdenum disulfide nanosheets.

[0050] (c) Ethanol cleaning

[0051] Measure 10ml of absolute ethanol and mix it with the obtained suspension of molybdenum disulfide nanosheets. Centrifuge at 11000rpm for 15min, discard the supernatant, and collect the product at the bottom of the centrifuge tube; use 20ml of absolute ethanol to make a 10mg / ml suspension,...

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Abstract

The invention provides a method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation and belongs to the field of preparation of molybdenum disulfide nanosheets. The method provided by the invention comprises the following steps: performing ultrasonic reaction on molybdenum disulfide powder and n-butyl lithium under the protection of high-purity argon gas to obtain lithium-intercalated molybdenum disulfide; and adding ultra-pure water into a reactant, performing chemical stripping on a molybdenum disulfide bulk material to obtain single-layer molybdenum disulfide nanosheets, adding anhydrous ethanol for washing, and performing ultra-pure water dispersion and high-speed centrifugal separation so as to obtain a single-layer molybdenum disulfide nanosheet material which can be dispersed in water. Compared with the traditional method for preparing the molybdenum disulfide nanosheets by chemical intercalation, the method for preparing the molybdenum disulfide nanosheets, provided by the invention, has the characteristics of high reaction speed, high reaction yield, good stripping effect, simple operation, mild reaction conditions and easiness in large-scale production.

Description

technical field [0001] The invention relates to a method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation, which belongs to the preparation technology of nanometer materials, and in particular relates to a method for preparing molybdenum disulfide nanosheets through chemical intercalation. Background technique [0002] Molybdenum disulfide is a representative two-dimensional transition metal chalcogenide. This type of layered compound has a unique "sandwich" structure of chalcogen-metal elements-chalcogen, in which the metal atoms in the layer and the chalcogen atoms are bonded by strong covalent bonds, and the layers between layers Rely on weaker van der Waals forces to bind. Due to its unique physical and chemical properties, molybdenum disulfide is used in solid lubrication, hydrodesulfurization catalysis and other fields. [0003] Due to the two-dimensional layered structure of transition metal chalcogenides, when their geomet...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
CPCC01G39/06C01P2004/04C01P2004/20
Inventor 宇文力辉汪联辉于欢张琦张玉倩
Owner NANJING UNIV OF POSTS & TELECOMM
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