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Preparation method for 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, harsh preparation conditions, cumbersome preparation process, etc., and achieve the effects of green cost, excellent preparation efficiency and high product purity

Active Publication Date: 2020-02-11
XIAMEN HONGLU TUNGSTEN MOLYBDENUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Preparation method for transition metal chalcogenide layered compound nanosheet material
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  • Preparation method for transition metal chalcogenide layered compound nanosheet material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0037] (2) preparation concentration is 20mL of aqueous electrolyte solution of 8mg / mL, and this electrolyte is 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) Place the above-mentioned first slurry in an electrochemical reaction device to perform an electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product. During the reaction, a square track uniform stirring system is introduced to ensure that the first - The slurry is in a state of uniform flow and exchange;

[0040] The above electrochemical reaction device includes a DC stabilized power supply, a reaction cell and an electrode assembly. The reaction cell is a cuboid m...

Embodiment 2

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

[0047] (2) Preparation concentration is 20mL of aqueous electrolyte solution of 5mg / mL, and this electrolyte is 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) Place the above-mentioned first slurry in an electrochemical reaction device to perform an electrochemical intercalation reaction to obtain a second slurry containing an intercalation reaction product. During the reaction, a square track uniform stirring system is introduced to ensure that the first - The slurry is in a state of uniform flow and exchange;

[0050] The above electrochemical reaction device includes a DC stabilized power supply, a reaction cell and an electrode assembl...

Embodiment 3

[0056] (1) Mix molybdenum disulfide powder with an average particle size of 30um and dodecyltrimethylammonium bromide in a weight ratio of 98:2 to obtain a 30.6g powder mixture;

[0057] (2) preparation concentration is 15mL of aqueous electrolyte solution of 12.5mg / mL, and this electrolyte is ammonium bisulfate;

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

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

[0060] The above-mentioned electrochemical reaction device includes a DC stabilized power supply, a reaction cell and an electrode assembly,...

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Abstract

The invention discloses a preparation method for a transition metal chalcogenide layered compound nanosheet material. According to the method, an electrochemical intercalation method is combined witha mechanical physical peeling method, two electroconductive materials are used to prepare an electrochemical reaction electrode in an interlayer manner, a material flow system is introduced, electrochemical intercalation is performed in a water system and physical stripping is performed in a water-organic solvent mixed solvent system having a suitable surface tension to prepare the few-layer transition metal chalcogenide layered nanomaterial, the reaction can be performed at normal temperature and pressure, and the obtained product has a high yield, a small amount of residual intercalating agent, a small amount of residual un-stripped raw materials, high product purity, and preparation efficiency superior to that of a traditional electrochemical method and an 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] Transition metal chalcogenide layered compound materials mainly include molybdenum disulfide, tungsten disulfide, molybdenum diselenide, molybdenum ditelluride, thallium diselenide, niobium diselenide, nickel diselenide, etc. 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 conveniently extracted and prepared from natural molybdenite, and has been applied in the fields of lubrication, catalysis and composite materials. The ...

Claims

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Application Information

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Patent Type & Authority Applications(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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