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Two-dimensional black phosphorus nanosheet and liquid-phase peeling preparation method thereof

A liquid phase exfoliation and nanosheet technology, applied in the preparation of phosphorus, nanotechnology, nanotechnology and other directions, can solve the problems of difficult removal of organic solvents, small size, high yield of liquid phase exfoliation, and achieve high stability.

Active Publication Date: 2017-05-24
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above three methods all have some disadvantages: although the two-dimensional black phosphorus nanosheets obtained by the mechanical exfoliation method have large size and small defects, the yield and yield are low; while the liquid phase exfoliation method has high yield but small size, and organic solvents are difficult to remove. ; The size of the black phosphorus film obtained by the pulsed laser deposition method is large but the product is amorphous

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  • Two-dimensional black phosphorus nanosheet and liquid-phase peeling preparation method thereof
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  • Two-dimensional black phosphorus nanosheet and liquid-phase peeling preparation method thereof

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Embodiment 1

[0036] A preparation method for liquid phase exfoliation of two-dimensional black phosphorus nanosheets, comprising the following steps:

[0037] Step (1): drying tri-n-butyl(methyl)phosphine hexafluorophosphate in vacuum at 100°C for 48 hours;

[0038] Step (2): Add 10 mg of block black phosphorus and 5 mg of dried tri-n-butyl(methyl)phosphine hexafluorophosphate into 40 mL of N-methylpyrrolidone in a weight ratio of 1:0.5 , to obtain a mixed solution, wherein the concentration of black phosphorus in N-methylpyrrolidone is 0.25mg / mL, and the probe is ultrasonicated for 3h with a power of 900W under the sealed condition, and the temperature is controlled at 5°C during the entire probe ultrasonic process. °C; and then ultrasonicated in a water bath at a power of 500W for 3h, and the temperature was kept at 5 °C during the entire process of ultrasonication in a water bath. Then, it was left to stand overnight, and the supernatant was taken for centrifugation at 7000 rpm to obta...

Embodiment 2

[0040] A preparation method for liquid phase exfoliation of two-dimensional black phosphorus nanosheets, comprising the following steps:

[0041] Step (1): drying tri-n-butyl(methyl)phosphine hexafluorophosphate in vacuum at 100°C for 48 hours;

[0042] Step (2): Add 10 mg of block black phosphorus and 50 mg of dried tri-n-butyl(methyl)phosphine hexafluorophosphate into 2 mL of N-methylpyrrolidone in a weight ratio of 1:5 (NMP) to obtain the mixed solution, wherein the concentration of black phosphorus in N-methylpyrrolidone is 5mg / mL, and the probe ultrasonic 3h is carried out with the power of 900W under the sealed condition, and the temperature is controlled during the whole probe ultrasonic process to keep at 5°C; then perform ultrasonication in a water bath with a power of 500W for 3h, and keep the temperature at 5°C during the entire process of ultrasonication in a water bath. Then, it was left to stand overnight, and the supernatant was taken for centrifugation at 7000...

Embodiment 3

[0044] A preparation method for liquid phase exfoliation of two-dimensional black phosphorus nanosheets, comprising the following steps:

[0045] Step (1): drying tri-n-butyl(methyl)phosphine hexafluorophosphate in vacuum at 100°C for 48 hours;

[0046] Step (2): Add 10mg of block black phosphorus and 75mg of dried tri-n-butyl(methyl)phosphine hexafluorophosphate to 0.2mL of N-methylpyrrolidone in a weight ratio of 1:7.5 (NMP) to obtain a mixed solution, wherein the concentration of black phosphorus in N-methylpyrrolidone is 50mg / mL, and the probe is ultrasonicated for 3h with a power of 900W under a sealed condition, and the temperature is controlled during the entire probe ultrasonic process Keep it at 5°C; then conduct ultrasonication in a water bath with a power of 500W for 3h, and keep the temperature at 5°C during the whole process of ultrasonication in a water bath. Then, it was left to stand overnight, and the supernatant was taken for centrifugation at 7000 rpm to ob...

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Abstract

The invention provides a liquid-phase peeling preparation method of two-dimensional black phosphorus nanosheets. The liquid-phase peeling preparation method comprises the following steps: adding blocky black phosphorus and a phosphorus-containing ionic liquid into an organic solvent in a mass ratio of 1:(0.5-100) so as to obtain a mixed liquid, under an anaerobic condition of 0-10 DEG C, performing probe ultrasonic treatment on the mixed liquid for 3-7 hours, performing water bath ultrasonic treatment for 1-10 hours, leaving to stand, and performing centrifugal separation on supernate, thereby obtaining the two-dimensional black phosphorus nanosheets. Due to a synergistic effect of the phosphorus-containing ionic liquid and the organic solvent, the purpose of peeling the blocky black phosphorus into large-size two-dimensional black phosphorus nanosheets with high efficiency and low cost can be achieved. The invention further provides the two-dimensional black phosphorus nanosheets which is prepared by using the liquid-phase peeling preparation method.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic nanomaterials, in particular to a two-dimensional black phosphorus nanosheet and a liquid phase exfoliation preparation method thereof. Background technique [0002] Black phosphorus is a new type of two-dimensional material with a direct band gap. Its band gap can be adjusted from 0.3eV (bulk state) to 1.5eV (single layer) through the number of layers, so it can absorb wavelengths ranging from visible light to infrared for communication. light, coupled with its high carrier mobility (up to 1000cm at a thickness of 10nm 2 ˙v -1 ˙s -1 ) and higher on-off ratio (10 4 ), which shows great potential advantages in the fields of semiconductor, optoelectronics and photothermal. [0003] At present, there are three main ways to prepare black phosphorus with atomic layer thickness (ie, two-dimensional black phosphorus nanosheets): (1) mechanical exfoliation method; (2) liquid phase exf...

Claims

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Application Information

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IPC IPC(8): C01B25/02B82Y30/00B82Y40/00
CPCC01B25/02C01P2002/01C01P2002/20C01P2004/04C01P2004/61C01P2006/16Y02P20/54
Inventor 张晗邢晨阳张家宜
Owner SHENZHEN UNIV
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