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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AI-Extracted Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing molybdenum disulfide nanosheets by ultra...
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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.

Application Domain

Material nanotechnologyMolybdenum sulfides

Technology Topic

Butyl lithiumUltrasonic assisted +10

Image

  • 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(4)

Example Embodiment

[0027] Example 1
[0028] (a) Ultrasound assisted lithium intercalation
[0029] Add 200mg of molybdenum disulfide powder to 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 minutes.
[0030] (b) Stripping of molybdenum disulfide
[0031] Stop the reaction, let it stand for 30 minutes to remove the unreacted n-butyl lithium, add 5 ml of pre-deoxygenated ultrapure water into the reaction tube, continue the reaction under ultrasonic conditions for 0.5 hours, and peel off to obtain the crude product of molybdenum disulfide nanosheets.
[0032] (c) Ethanol cleaning
[0033] Measure 5 ml of absolute ethanol and mix with the obtained molybdenum disulfide nanosheet suspension. Centrifuge at 12000rpm for 10min to discard the supernatant, collect the bottom product of the centrifuge tube; then use 10ml of absolute ethanol to make a 20mg/ml suspension, centrifuge at 12000rpm for 5min, discard the supernatant, and keep the centrifuge Tube bottom product.
[0034] (d) Centrifugal purification
[0035] Measure 50ml of ultrapure water, mix with the molybdenum disulfide nanosheets obtained in (c) to make a 4mg/ml suspension, centrifuge at 5000rpm for 40min, discard the precipitate, centrifuge the upper product at 12000rpm for 60min, Discard the supernatant and keep the separated product at the bottom. The product was dispersed in a certain amount of ultrapure water, and the above centrifugal purification step was repeated to obtain the final product with a yield of 8.53%. The product transmission electron microscope photos are as figure 1 Shown.

Example Embodiment

[0036] Example 2
[0037] (a) Ultrasound assisted lithium intercalation
[0038] Add 200mg of molybdenum disulfide powder to 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 1h.
[0039] (b) Stripping of molybdenum disulfide
[0040] Stop the reaction and let it stand for 30 minutes to remove unreacted n-butyl lithium. Add 10 ml of pre-deoxygenated ultrapure water to the reaction tube, continue the reaction for 0.5 hours under ultrasonic conditions, and peel off to obtain a crude product of molybdenum disulfide nanosheets.
[0041] (c) Ethanol cleaning
[0042] Measure 10 ml of absolute ethanol and mix with the obtained molybdenum disulfide nanosheet suspension. Centrifuge at 10000rpm for 20min to discard the supernatant, and collect the bottom product of the centrifuge tube; then use 20ml of absolute ethanol to make a 10mg/ml suspension, centrifuge at 10000rpm for 5min, discard the supernatant, and save the centrifuge tube The bottom product.
[0043] (d) Centrifugal purification
[0044] Measure 20ml of ultrapure water, mix with the molybdenum disulfide nanosheets obtained in (c) to form a 10mg/ml suspension, centrifuge at 2000rpm for 40min, discard the precipitate, centrifuge the upper product at 10000rpm for 100min, discard Remove the supernatant and keep the separated product at the bottom. The product was dispersed in 20 ml of ultrapure water, centrifuged at 5000 rpm for 30 min, the precipitate was discarded, the upper product was centrifuged at 12,000 rpm for 30 min, and the bottom separated product was retained as the final product. The yield was 9.05%. The product transmission electron microscope photos are as figure 2 Shown.

Example Embodiment

[0045] Example 3
[0046] (a) Ultrasound assisted lithium intercalation
[0047] Add 200mg of molybdenum disulfide powder to 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 to remove the unreacted n-butyl lithium, add 10 ml of pre-deoxygenated ultrapure water into the reaction tube, continue the reaction under ultrasonic conditions for 0.5 hours, and peel off to obtain the crude product of the molybdenum disulfide nanosheets.
[0050] (c) Ethanol cleaning
[0051] Measure 10 ml of absolute ethanol and mix with the obtained molybdenum disulfide nanosheet suspension. Centrifuge at 11000rpm for 15min to discard the supernatant, collect the bottom product of the centrifuge tube; then use 20ml of absolute ethanol to make a 10mg/ml suspension, centrifuge at 10000rpm for 5min, discard the supernatant, and keep the centrifuge Tube bottom product.
[0052] (d) Centrifugal purification
[0053] Measure 50ml of ultrapure water, mix with the molybdenum disulfide nanosheets obtained in (c) into a 4mg/ml suspension, centrifuge at 5000rpm for 30min, discard the precipitate, centrifuge the upper product at 14000rpm for 30min, Discard the supernatant and keep the separated product at the bottom. The product was dispersed in a certain amount of ultrapure water, and the above centrifugal purification steps were repeated to obtain the final product with a yield of 16.68%. The product transmission electron microscope photos are as image 3 Shown.
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Description & Claims & Application Information

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