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Macroscopic-quantity preparation method of phosphorene

A phosphorene and macro-scale technology, applied in the field of macro-scale preparation of phosphorene, can solve the problems of difficulty in obtaining large-scale phosphorene, difficulty in large-scale production, complicated operations, etc., and achieves good peeling effect, high equipment utilization, The effect of easy automation

Inactive Publication Date: 2017-08-18
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical exfoliation method is a traditional method for preparing two-dimensional materials from bulk layered crystals, mainly by sticking a piece of tape on one side of the block material, and sticking the other side to another piece of tape, and then tearing off one piece of tape. Thinner flake materials can be obtained by operation. Although this preparation method can guarantee the original performance of the material, the operation is complicated, time-consuming and labor-intensive, and it is difficult to carry out large-scale production.
Ultrasonic liquid phase exfoliation is a widely used method for preparing ultra-thin two-dimensional materials from bulk materials. The bulk material is directly ultrasonically treated in an organic solvent. The biggest defect of this method is that the ultrasonic treatment takes a long time, and The yield is low, and it is difficult to obtain phosphorene with a large size

Method used

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  • Macroscopic-quantity preparation method of phosphorene
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  • Macroscopic-quantity preparation method of phosphorene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Weigh 0.2g of orthorhombic black phosphorus crystal with a balance (XRD pattern as figure 1 shown) into the reagent bottle, then use a graduated cylinder to measure 200mL of organic solvent NMP (N-methylpyrrolidone) and pour it into the reagent bottle, and mix well to obtain a mixed solution after sealing;

[0023] (2) Evacuate the air in the high-pressure homogenizer with argon, pour the mixed liquid prepared in step (1) into the hopper of the high-pressure homogenizer, turn on the power, turn on the high-pressure homogenizer, and set the working pressure to 1500bar, make the mixed liquid pass through the homogenization chamber of the high-pressure homogenizer at high speed, and obtain a suspension with good peeling effect after 5 minutes;

[0024] (3) Centrifuge the suspension obtained in step (2) at a rotational speed of 2000 rpm, filter the supernatant with a polytetrafluoroethylene membrane, and wash repeatedly with deionized water and absolute ethanol to obtai...

Embodiment 2

[0027] (1) Weigh 2g of orthorhombic black phosphorus crystals with a balance (XRD pattern as figure 1 shown) into the reagent bottle, then use a graduated cylinder to measure 200mL of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate, pour it into the reagent bottle, and mix evenly to obtain a mixed solution after sealing;

[0028] (2) Evacuate the air in the high-pressure homogenizer with helium, pour the mixed solution prepared in step (1) into the hopper of the high-pressure homogenizer, turn on the power, turn on the high-pressure homogenizer, and set the working pressure to 1600bar, make the mixed liquid pass through the homogenization chamber of the high-pressure homogenizer at high speed, and obtain a suspension with good peeling effect after 30 minutes;

[0029] (3) Centrifuge the suspension obtained in step (2) at a rotational speed of 4000 rpm, filter the supernatant with a polypropylene membrane, and wash repeatedly with deionized water and absolute ethan...

Embodiment 3

[0031] (1) Weigh 10g of orthorhombic black phosphorus crystals with a balance (XRD pattern as figure 1 shown) into the reagent bottle, then use a measuring cylinder to measure 200mL deionized water into the reagent bottle, and mix well after sealing;

[0032] (2) Evacuate the air in the high-pressure homogenizer with nitrogen, pour the prepared mixed solution into the hopper of the high-pressure homogenizer, turn on the power, turn on the high-pressure homogenizer, set the working pressure to 1700bar, and make the mixed solution Pass through the homogenization chamber of the high-pressure homogenizer at high speed, and obtain a suspension with good peeling effect after 60 minutes;

[0033] (3) Centrifuge the suspension obtained in step (2) at a rotational speed of 8000 rpm, filter the supernatant with a nitrocellulose membrane, and wash repeatedly with deionized water and absolute ethanol to obtain phosphorene.

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Abstract

The invention discloses a macroscopic-quantity preparation method of phosphorene. The macroscopic-quantity preparation method comprises the following steps: (1) preparing liquid; (2) peeling; (3) centrifugally separating; and (4) filtering and washing. For the existing dilemma of difficulty in large-scale preparation of non-defective phosphorene, the method uses equipment with continuous operation, namely high-pressure homogenizer, so that when passing through a homogenizing cavity, materials are acted by mechanical forces such as high-speed shearing, high-frequency oscillation and convection impact and corresponding heat effect simultaneously, so that the peeling effect is good. The method has the characteristics of high equipment utilization rate, large productivity, stable process parameters, easiness in implementation of automatic operation and the like, can guarantee the product quality and also can realize industrial-scale preparation. The phosphorene prepared by adopting the method has good application prospect in the fields of photoelectron, energy storage, catalysis and the like.

Description

technical field [0001] The invention relates to a macro-preparation method of phosphorene, which belongs to the technical field of phosphorene preparation. Background technique [0002] In nature, the allotropes of phosphorus mainly include white phosphorus, red phosphorus and black phosphorus. Compared with white phosphorus and red phosphorus, black phosphorus is the most stable allotrope of phosphorus. The crystal forms of black phosphorus mainly include orthorhombic, rhombic, simple cubic and amorphous. Orthorhombic black phosphorus has a layered structure, and the layers are combined by van der Waals force. Therefore, it can be chemically and The physical method breaks this interlayer force, thereby obtaining few-layer or single-layer black phosphorene. Black phosphorene has many excellent properties that bulk black phosphorus does not have, such as high specific surface area, adjustable direct band gap and good photoelectric performance, etc. These advantages make it v...

Claims

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Application Information

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IPC IPC(8): C01B25/02
CPCC01B25/02C01P2002/01C01P2002/82C01P2002/72Y02P20/54
Inventor 廉培超王波叶云王倩李海宁
Owner KUNMING UNIV OF SCI & TECH
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