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A stripping solution for preparing two-dimensional nanomaterials and its application

A two-dimensional nanomaterial and solution technology, applied in the fields of nanocarbon, nanotechnology, phosphorus preparation, etc., can solve the damage of graphene electronic structure and crystal integrity, limit application and industrialization development, process condition control conditions, etc. problem, to achieve the effect of easy industrial application, avoid secondary aggregation, avoid strong acid and strong corrosive chemical reagents

Active Publication Date: 2019-12-27
北京华科讯能石墨烯新技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The CVD method is a method of depositing graphene on a solid film substrate through a gas phase reaction at a high temperature. This method can prepare high-quality, large-area graphene, but it has high costs, complicated processes, and harsh process conditions. restricted its development
Currently the most commonly used redox method, the basic principle is to treat graphite with a strong protonic acid to form a graphite interlayer compound, and then add a strong oxidant to oxidize it to form graphene oxide, which can be further reduced to obtain reduced graphene oxide, but In the production process of this method, strong acids and strong oxidants that are highly corrosive and oxidizing to chemical equipment are used, which are harmful to the environment, and the electronic structure and crystal integrity of graphene are seriously damaged. , the electrical conductivity is significantly reduced, which limits its application and industrialization in the fields of energy and electronics
The method of liquid phase mechanical exfoliation can prepare high-quality graphene and graphene-like two-dimensional nanomaterials, but its efficiency is low and the cost is high. For example, the exfoliation efficiency in pure water is relatively low, and the exfoliation efficiency in some pure organic solvents is relatively low. Although relatively high, the use of organic solvents has the characteristics of flammability, explosion, and high cost, which limits its industrial application

Method used

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  • A stripping solution for preparing two-dimensional nanomaterials and its application
  • A stripping solution for preparing two-dimensional nanomaterials and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] First, add 10ml of ethanol, 10ml of isobutanol, 15ml of tert-butanol, and 100ml of glycerol into 1L of deionized water; Methylpyrrolidone, 0.05g of 9-anthracene carboxylic acid, and 0.01g of pyrene-1-sulfonic acid sodium salt were added to the above aqueous solution, and after uniform stirring, the stripping solution was obtained.

[0037] Stir and disperse 100g of flake graphite in the above solution. After mechanical shearing and ultrasonic stripping, graphene with a thickness of about 3nm and complete crystal structure can be obtained. The atomic force microscope and scanning electron microscope microscopic pictures are as follows: figure 1 , figure 2 shown.

[0038] Mechanical shearing and ultrasonic stripping are performed as follows:

[0039] (1) Submerge the cutter head of the emulsification cutting machine under the liquid surface, and cut the mixed solution for 2 hours under the condition of 40°C water bath, keeping the cutter head rotation speed at 8000rpm....

Embodiment 2

[0056] First, add 10ml of ethanol, 100ml of isopropanol, 10ml of n-butanol, 50ml of tert-butanol, and 20ml of glycerol into 1L of deionized water; Add sulfoxide, 0.3ml nitrogen-methylpyrrolidone, 0.02g 9-anthracene carboxylic acid, and 0.05g pyrene-1-sulfonic acid sodium salt into the above-mentioned aqueous solution, and stir to obtain a peeling solution. 100g molybdenum disulfide The powder is stirred and dispersed in the above solution, and after mechanical shearing and ultrasonic stripping, molybdenum disulfide nanosheets with a thickness of 1-10 nm and good crystallinity can be obtained. Compared with pure aqueous solution, molybdenum disulfide prepared by this solution The yield of nanosheets was increased by about 2 times.

Embodiment 3

[0058] First, add 10ml of ethanol, 10ml of n-propanol, 20ml of isopropanol, 15ml of tert-butanol, and 100ml of sec-butanol into 1L of deionized water; Dimethyl formamide, 1ml dimethyl sulfoxide, 0.1g 9-anthracene carboxylic acid, 0.06g pyrene-1-sulfonic acid sodium salt were added to the above aqueous solution, and after stirring evenly, the peeling solution was obtained. 30g black phosphorus powder Stirring and dispersing in the above solution, after mechanical shearing and ultrasonic stripping, black phosphorus nanosheets with a thickness of 1-10 nm can be obtained. Compared with pure aqueous solution, the yield of black phosphorus nanosheets prepared by this solution is increased by about 3 times.

[0059] In the peeling solution developed by the present invention, and under the composite action of mechanical shear and ultrasound, the layered solid powder can be efficiently and cleanly peeled into two-dimensional nano-sheets, such as graphene, molybdenum disulfide, black ph...

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Abstract

The invention provides a stripping solution for preparing a two-dimensional nanomaterial and application thereof. The stripping solution comprises the following components: an alcohol substance with the volume content of 0.05-59%, a methyl-containing organic solvent with the volume content of 0.03-8%, a fused ring compound with the concentration of 0.01mg / L-1g / L and the balance of water. The invention further provides application of the stripping solution. The stripping solution provided by the invention uses liquid water as a main body, so that the defects that the organic solvent is flammable and explosive are avoided, the cost is reduced, and use of strong acids and strong corrosive chemical reagents is avoided; layered solid particles are dispersed in the stripping solution, and underthe actions of mechanical shearing and ultrasonic, stripping of the layered solid particles into two-dimensional nanoflakes can be effectively accelerated, so that secondary aggregation of the two-dimensional nanoflakes is avoided.

Description

technical field [0001] The invention belongs to the field of preparation of two-dimensional nanometer materials, and in particular relates to a solution used in a liquid phase preparation method. Background technique [0002] The ideal graphene is a two-dimensional monoatomic layer graphite, which has a high specific surface area, excellent chemical and thermal stability, good electrical and thermal conductivity, excellent mechanical properties and other properties, from Geim of the University of Manchester in the United Kingdom. Since the group synthesized graphene by micro-mechanical exfoliation in 2004, it has triggered an upsurge of research on graphene and its composite materials, making graphene have great application prospects in the fields of catalysis, electronics, energy, biomedicine, and materials. At the same time, graphene-like two-dimensional nanomaterials, such as molybdenum disulfide nanoflakes and black phosphorus nanoflakes, have good catalytic hydrogen evo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01G39/06C01B25/02B82Y40/00
Inventor 杨树斌
Owner 北京华科讯能石墨烯新技术研究院有限公司
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