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A method for ultrasonically exfoliating black phosphorus to prepare few-layer black scales

An ultrasonic peeling and black phosphorus flake technology is applied in the preparation of functional materials and the field of optoelectronic materials, which can solve the problems of high atmospheric pressure, high temperature, high energy consumption, and low purity of black phosphorus, and achieve the effects of less impurities, simple operation and high quality.

Active Publication Date: 2017-03-15
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The research results were published online in the journal "Nature Nanotechnology" (Nature Nanotechnology 2014, 9, 372–377). Under a pressure of 10kbar, they heated red phosphorus to 1000°C and then dropped it to 600°C at a cooling rate of 100°C / h. °C to obtain a few-layer black phosphorus material (in the industry, the number of layers is less than 10 is defined as a few-layer black phosphorus sheet); this method requires high atmospheric pressure and high temperature, high energy consumption, and low purity of black phosphorus

Method used

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  • A method for ultrasonically exfoliating black phosphorus to prepare few-layer black scales
  • A method for ultrasonically exfoliating black phosphorus to prepare few-layer black scales
  • A method for ultrasonically exfoliating black phosphorus to prepare few-layer black scales

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Effect test

Embodiment 1

[0028] Put the black phosphorus powder and the intercalation agent into N-cyclohexyl-2-pyrrolidone (CHP) according to the mass ratio of 1:0.5, wherein the size of the black phosphorus powder is 50 μm, the intercalation agent is naphthalene, and the intercalation agent The concentration is controlled at 5mg / mL; the oxygen content and water content in the mixed solution are controlled to be lower than 20ppm, and the stripping reaction temperature is 40°C for 2 hours of ultrasonic reaction; the pore diameter of the vacuum filter membrane obtained by ultrasonic stripping is 0.1μm After vacuum filtration at 60°C, few-layer black phosphorus flakes can be obtained by vacuum drying.

Embodiment 2

[0030] Put the black phosphorus powder and the intercalation agent into N-cyclohexyl-2-pyrrolidone (CHP) according to the mass ratio of 1:1, wherein the size of the black phosphorus powder is 50 μm, the intercalation agent is naphthalene, and the intercalation agent The concentration is controlled at 10mg / mL; the oxygen content and water content in the mixed solution are controlled to be lower than 20ppm, and the stripping reaction temperature is 40°C for 1 hour of ultrasonic reaction; the pore diameter of the vacuum filter membrane obtained by ultrasonic stripping is 0.1μm After vacuum filtration at 60°C, few-layer black phosphorus flakes can be obtained by vacuum drying.

Embodiment 3

[0032] Put the black phosphorus powder and the intercalation agent into N-cyclohexyl-2-pyrrolidone (CHP) according to the mass ratio of 1:0.5, wherein the size of the black phosphorus powder is 50 μm, the intercalation agent is naphthalene, and the intercalation agent The concentration is controlled at 5 mg / mL; the oxygen content and water content in the mixed solution are controlled to be lower than 20 ppm, and the stripping reaction temperature is 60 ° C for 1 hour of ultrasonic reaction; the pore diameter of the vacuum filter membrane obtained by ultrasonic stripping is 0.1 μm After vacuum filtration at 60°C, few-layer black phosphorus flakes can be obtained by vacuum drying.

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Abstract

The invention relates to a method for preparing few-layer black scales by ultrasonically stripping a black scale. The method comprises the steps of uniformly mixing black scale powder and an intercalator in an organic solvent according to a given ratio to obtain a mixture, insulating the air, ultrasonically treating the mixture in water bath, and carrying out vacuum suction filtration and vacuum drying to obtain a few-layer black scale material. A series of compounds such as cetyl trimethyl ammonium bromide, phenanthrene and naphthalene are used as the intercalator to prepare the few-layer black scale. Compared with the prior art, the prepared few-layer black scale has advantages of few defects, few impurities, high quality and the like. Meanwhile, the process is simple to operate and low in cost, and the prepared few-layer black scale is expected to substitute the graphene material to be applied to the field of a photoelectric material.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional materials, and relates to a method for ultrasonically exfoliating black phosphorus to prepare few-layer black scales, and the prepared few-layer black phosphorus flakes can be applied to the field of photoelectric materials. Background technique [0002] Black phosphorus is a crystal with metallic luster, which can be formed by transforming white phosphorus under high pressure and temperature. It has a sheet structure similar to graphite and has good electrical conductivity. One of the focuses of new two-dimensional semiconductor research. Compared with graphene, few-layer black phosphorus flakes have more obvious advantages in the field of optoelectronic materials: first, graphene has no semiconductor band gap, that is to say, it is difficult to complete the conversion between conductors and insulators, and cannot realize digital circuits. Logical on and off, and black phosphor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/02
Inventor 马守龙李缜
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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