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A preparation method of transition metal chalcogenide layered compound nanosheet material

A technology of layered compounds and transition metals, which is applied in the field of preparation of few-layer nanomaterials, can solve the problems of long preparation period, nanosheet defects, and harsh preparation conditions, and achieve less residual unstripped raw materials and intercalant residues. Less quantity, less cost, green effect

Active Publication Date: 2022-06-28
XIAMEN HONGLU TUNGSTEN MOLYBDENUM IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technical scheme disclosed in CN104495935B proposes to use the method of adding oxidant in organic solvent to obtain molybdenum disulfide nanosheet material with higher yield by stirring or ultrasonic method, but this method is easy to cause the defect of nanosheet layer, and the preparation cycle is long, it is difficult to realize the large-scale Implementation
The technical scheme disclosed in CN107720825A adopts magnesium chloride and sodium sulfide as intercalation agents, continues heating in a high-pressure reactor and ultrasonically exfoliates to obtain molybdenum disulfide nanosheets, but this method consumes a lot of energy and has low yield, and is not suitable for large-scale preparation
Some researchers used lithium ion electrochemical intercalation method combined with ultrasonic stripping method to obtain molybdenum disulfide, tungsten disulfide and other nanosheets, but the preparation conditions of this method are harsh and the preparation process is cumbersome, which limits its popularization and application.
In short, the existing preparation technology of transition metal chalcogenide flake nanomaterials such as molybdenum disulfide still has problems such as long preparation cycle, high energy consumption, low yield, and low purity.

Method used

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Effect test

Embodiment 1

[0036](1) The molybdenum disulfide powder with an average particle size of 10um and polyvinylpyrrolidone (K30) were uniformly mixed in a weight ratio of 98:2 to obtain 30.6g of powder mixture;

[0037] (2) 20 mL of an aqueous electrolyte solution with a concentration of 8 mg / mL was prepared, and the electrolyte was ammonium bicarbonate;

[0038] (3) uniformly dispersing the above-mentioned powder mixture in the above-mentioned aqueous electrolyte solution to obtain a first slurry;

[0039] (4) The above-mentioned first slurry is placed in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing the intercalation reaction product, and a square orbit uniform stirring system is introduced during the reaction to always ensure that the first slurry is 1. The slurry is in a state of uniform flow exchange;

[0040] The above-mentioned electrochemical reaction device includes a DC voltage stabilized power supply, a reaction po...

Embodiment 2

[0046] (1) the molybdenum disulfide powder with an average particle size of 20um and polyethylene glycol (relative molecular mass is 1500g / mol) are uniformly mixed in a weight ratio of 99:1 to obtain 30.3g powder mixture;

[0047] (2) 20 mL of an aqueous electrolyte solution with a concentration of 5 mg / mL was prepared, and the electrolyte was hydrogen peroxide;

[0048] (3) uniformly dispersing the above-mentioned powder mixture in the above-mentioned aqueous electrolyte solution to obtain a first slurry;

[0049] (4) The above-mentioned first slurry is placed in an electrochemical reaction device for electrochemical intercalation reaction to obtain a second slurry containing the intercalation reaction product, and a square orbit uniform stirring system is introduced during the reaction to always ensure that the first slurry is 1. The slurry is in a state of uniform flow exchange;

[0050] The above-mentioned electrochemical reaction device includes a DC voltage stabilized p...

Embodiment 3

[0056] (1) the molybdenum disulfide powder with an average particle size of 30um and the dodecyl trimethyl ammonium bromide are uniformly mixed in a weight ratio of 98:2 to obtain a 30.6g powder mixture;

[0057] (2) Prepare 15 mL of an electrolyte aqueous solution with a concentration of 12.5 mg / mL, and the electrolyte is ammonium hydrogen sulfate;

[0058] (3) uniformly dispersing the above-mentioned powder mixture in the above-mentioned aqueous electrolyte solution to obtain a first slurry;

[0059] (4) the above-mentioned first slurry is placed in an electrochemical reaction device to carry out an electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product, and a stirring system of uniform circular motion is introduced in the reaction process to ensure that the The first slurry is in a state of uniform flow exchange;

[0060] The above-mentioned electrochemical reaction device comprises a DC voltage stabilized power supply...

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Abstract

The invention discloses a preparation method of a transition metal chalcogenide layered compound nanosheet material. The invention combines an electrochemical intercalation method with a mechanical and physical stripping method, adopts two kinds of conductive material interlayers to make an electrochemical reaction electrode, and introduces materials Flow system, electrochemical intercalation in water system and physical exfoliation in water-organic solvent mixed solvent system with suitable surface tension to prepare few-layer transition metal chalcogenide layered nanomaterials, which can be carried out under normal temperature and pressure conditions , the yield of the obtained product is high, the residual amount of the intercalation agent is small, the amount of residual unstripped raw materials is small, the purity of the product is high, and the preparation efficiency is better than the traditional electrochemical method and the organic solvent liquid phase stripping method.

Description

technical field [0001] The invention belongs to the technical field of preparation of few-layer nanomaterials, and in particular relates to a preparation method of a transition metal chalcogenide layered compound nanosheet material. Background technique [0002] The transition metal chalcogenide layered compound materials mainly include molybdenum disulfide, tungsten disulfide, molybdenum diselenide, molybdenum ditelluride, thallium diselenide, niobium diselenide, nickel ditelluride and the like. Once these transition metal chalcogenide layered compounds can be exfoliated into two-dimensional sheet nanomaterials, they have shown many important applications in the fields of electronics, optoelectronics and energy storage. [0003] Bulk molybdenum disulfide is a typical transition metal chalcogenide layered structure material. It can be easily extracted and prepared from natural molybdenite, and has been applied in the fields of lubrication, catalysis and composite materials....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
CPCC01G39/06B82Y30/00B82Y40/00C01P2004/20C01P2004/64C01P2004/04C01P2002/84C01P2006/40C01P2006/80
Inventor 陈宜波郑艾龙黄丽枚黄志民
Owner XIAMEN HONGLU TUNGSTEN MOLYBDENUM IND CO LTD
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