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Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping

A technology of molybdenum disulfide and molybdenite, applied in the direction of molybdenum sulfide, nanotechnology, nanotechnology, etc., can solve the problem of long peeling cycle, difficulty in obtaining molybdenum disulfide nanosheet structure with high diameter-thickness ratio, and difficult control of product morphology, etc. problem, to achieve the effect of efficient stripping

Active Publication Date: 2016-10-26
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This intermittent method of grinding and ultrasonic separation has the disadvantages of long stripping cycle, low stripping efficiency, and high cost. At the same time, the morphology of the obtained product is not easy to control, and it is difficult to obtain a molybdenum disulfide nanosheet structure with a high aspect-thickness ratio and a high specific surface area.

Method used

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  • Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping
  • Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping
  • Method for preparing molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Ultrasonic-sand milling coupled to strip molybdenite to prepare molybdenum disulfide nanosheets, the steps are as follows:

[0042] Disperse 11.25 g of molybdenite fine powder in 250 mL of NMP (N-methylpyrrolidone, C 5 h 9NO) to form a suspension; 2) followed by the addition of 3.9 g PVP (polyvinylpyrrolidone, (C 6 h 9 NO)n), ultrasonic for 20 min to fully disperse; 3) then transferred into the reaction chamber of a sand mill (rotation speed 2250 rpm), and then under the action of high-energy ultrasonic (ultrasonic power 280 W), the sand mill-ultrasonic coupling stripping 6 h; 4) The exfoliated molybdenum disulfide nanosheet suspension was left to stand for about 24 h, and then centrifuged and graded at 1500 rpm, 8000 rpm, and 10000 rpm for 45 min. The solid content of the molybdenum disulfide nanosheets in the supernatant suspension after centrifugation at 1500 rpm for 45 min is used as an evaluation standard for evaluating the peeling yield: the relative concentrat...

Embodiment 2

[0055] Ultrasonic-sand milling coupled to strip molybdenite to prepare molybdenum disulfide nanosheets, the steps are as follows:

[0056] Disperse 11.25 g molybdenite fine powder in 250 mL ethanol solution (48%wt ethanol, C 2 h 5 OH) to form a suspension; 2) followed by the addition of 3.9 g of PVP (polyvinylpyrrolidone, (C 6 h 9 NO)n), ultrasonic for 20 min to fully disperse; 3) then transfer into the reaction chamber of a sand mill (2250 rpm), and then couple with each other under the action of ultrasonic (ultrasonic power 280 W) for 4 h; 4 ) Let the stripped suspension stand for about 2 h, centrifuge for classification, and centrifuge at 1500 rpm, 5000 rpm, and 8000 rpm for 45 min respectively. Subsequent processing is the same as in Example 1.

[0057] Figure 11 It is a graph of stripping yield and stripping rate of molybdenum disulfide nanosheets. With the extension of time, the stripping yield gradually increases. When ethanol solution is used as the solvent, the ...

Embodiment 3

[0059] Ultrasonic-sand milling coupled to strip molybdenite to prepare molybdenum disulfide nanosheets, the steps are as follows:

[0060] Disperse 6.25 g molybdenite fine powder in 250 mL NMP (N-methylpyrrolidone, C 5 h 9 NO) to form a suspension; 2) followed by the addition of 2.17 g of PVP (polyvinylpyrrolidone, (C 6 h 9 NO)n), sonicate for 20 min to fully disperse, and add salt (0.57gNaCl) or alkali (0.39gNaOH) stripping aid at the same time; Under the action (ultrasonic power 280 W), the mutual coupling was carried out for 4 h; 4) The stripped suspension was left to stand for about 24 h, centrifuged for grading, and centrifuged at 1500 rpm, 8000 rpm, and 10000 rpm for 45 min respectively. Subsequent processing is the same as in Example 1.

[0061] Figure 12 It is the stripping yield and rate analysis diagram of molybdenum disulfide nanosheets, NMP is the stripping solvent, and the effect of adding salt (NaCl) and alkali (NaOH) stripping aids on the stripping yield a...

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Abstract

The invention belongs to the technical field of nanometer material processing, and particularly relates to a method for preparing a molybdenum disulfide nano-sheet from molybdenite through ultrasonic-sanding coupling stripping. The method comprises following steps: 1), molybdenite micropowder is dispersed in a stripping solvent, and a suspension liquid is formed; 2), a dispersing agent and a stripping assistant are dissolved in the suspension liquid obtained in the step 1) and subjected to ultrasonic dispersion; 3), the suspension liquid after subjected to the ultrasonic dispersion in the step 2) is subjected to continuous stripping under the ultrasonic-sanding coupling action, and the molybdenum disulfide nano-sheet is obtained. According to the designed novel method for preparing the molybdenum disulfide nano-sheets in a large scale from the molybdenite micropowder through ultrasonic-sanding coupling stripping, green transformation from a natural mineral to a high-performance function material is realized, and the method has important application value and economic benefit.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial processing, and in particular relates to a method for preparing molybdenum disulfide nanosheets by stripping molybdenite through ultrasonic-sand mill coupling. Background technique [0002] MoS 2 Nanosheets and their composites have rich physical and chemical properties, and have important applications in the fields of catalysis, energy conversion and storage, environmental purification, and lubrication. Bulk MoS 2 is an indirect gap semiconductor ( E g =1.2 eV), while its monolayer structure becomes a direct gap semiconductor with an energy gap of 1.8 eV [ Nano Lett. 2011, 11, 5111-5116], has fluorescent properties, can be used as a biomarker, and is also an efficient solar light absorber. In particular, MoS 2 Nanocrystals have excellent catalytic performance for electrocatalytic hydrogen production, and are expected to partially replace noble metals such as Pt, which will greatly r...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G39/06C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2004/64
Inventor 陈德良董会娜张锐卢红霞许红亮王海龙范冰冰邵刚王志强王凯张绪圭荆慧娟荣晓茹
Owner ZHENGZHOU UNIV
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