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Method for preparing nano-black phosphorus by electric field and microwave field co-assisted stripping of black phosphorus

A technology of microwave field and black phosphorus, applied in the direction of phosphorus preparation, nanotechnology, nanotechnology, etc., can solve the problems of slow liquid intercalation, long time required, complicated equipment and process, etc., and achieve simple operation and short time consumption , large size effect

Inactive Publication Date: 2018-12-21
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of mechanical stripping method is low, which is suitable for laboratory research; the equipment and process of vapor deposition method are complicated, and the conditions are harsh; ultrasonic liquid phase stripping or shear stripping liquid intercalation is slow and takes a long time, and long-term stripping will Destroy the crystal structure of black phosphorus; although electrochemical exfoliation can realize the intercalation of ions in a short time, resulting in the exfoliation of black phosphorus, but the nano black phosphorus layer obtained only by electrochemical exfoliation is relatively thick, and further ultrasonic treatment is required ; Although a single microwave stripping can obtain nano black phosphorus with thinner sheets and better quality in a short period of time, the liquid intercalation in the short microwave process is relatively slow, so the concentration of nano black phosphorus obtained is low

Method used

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  • Method for preparing nano-black phosphorus by electric field and microwave field co-assisted stripping of black phosphorus
  • Method for preparing nano-black phosphorus by electric field and microwave field co-assisted stripping of black phosphorus
  • Method for preparing nano-black phosphorus by electric field and microwave field co-assisted stripping of black phosphorus

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Effect test

Embodiment 1

[0025] Embodiment 1: A kind of method that electric field and microwave field synergistically assist exfoliate black phosphorus to prepare nanometer black phosphorus, concrete steps are:

[0026] (1) Fix the black phosphorus crystal on the metal rod with conductive glue as the working electrode, and the working electrode is the anode; use the platinum sheet as the counter electrode, place the working electrode and the counter electrode in parallel and vertically in the sulfuric acid electrolysis with a concentration of 1mol / L In the solution, the distance between the working electrode and the counter electrode is 2cm, and under the condition of voltage 3V, perform ion intercalation and exfoliate the black phosphorus sheet for 2h to obtain the intercalated black phosphorus dispersion A;

[0027] (2) Under a microwave power of 800W and an inert gas (argon) atmosphere, the intercalated black phosphorus dispersion A obtained in step (1) was subjected to microwave peeling treatment ...

Embodiment 2

[0031] Embodiment 2: A kind of electric field and microwave field assist the method for stripping black phosphorus to prepare nano black phosphorus, concrete steps are:

[0032] (1) Fix the black phosphorus crystal on the metal rod with conductive glue as the working electrode, and the working electrode is the anode; the platinum sheet is used as the counter electrode, and the working electrode and the counter electrode are placed in parallel and vertically on a dodecane with a concentration of 1mol / L. In the alkyl sodium sulfate electrolyte, the distance between the working electrode and the counter electrode is 3 cm, and under the condition of voltage 20V, perform ion intercalation and exfoliate the black phosphorus sheet for 0.5h to obtain the intercalated black phosphorus dispersion A;

[0033] (2) Under a microwave power of 300W and an inert gas (argon) atmosphere, the intercalated black phosphorus dispersion A obtained in step (1) was subjected to microwave peeling treatm...

Embodiment 3

[0035] Embodiment 3: A kind of method that electric field and microwave field synergistically assist exfoliate black phosphorus to prepare nanometer black phosphorus, concrete steps are:

[0036] (1) Fix the black phosphorus crystal on the metal rod with conductive glue as the working electrode, and the working electrode is the anode; use the platinum sheet as the counter electrode, place the working electrode and the counter electrode in parallel and vertically in the hydrogen phosphate with a concentration of 2mol / L In the diammonium electrolyte, the distance between the working electrode and the counter electrode is 5cm, and under the condition of a voltage of 10V, the ion intercalation and exfoliation of the black phosphorus sheet are carried out for 2 hours to obtain the intercalation black phosphorus dispersion A;

[0037] (2) Under a microwave power of 300W and an inert gas (argon) atmosphere, the intercalated black phosphorus dispersion A obtained in step (1) was subjec...

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Abstract

The invention relates to a method for preparing nano-black phosphorus by electric field and microwave field co-assisted stripping of black phosphorus, and belongs to the technical field of preparationof nano materials. The method comprises the following steps: fixing the black phosphorus on a metal rod by using conductive adhesive and taking the metal rod as a working electrode, wherein the working electrode is an anode or cathode; taking a platinum sheet as a counter electrode, vertically putting the working electrode and the counter electrode in electrolyte in parallel, wherein the distancebetween the working electrode and the counter electrode is 2 to 5cm; under the condition that the voltage is 2 to 20 V, carrying out ion intercalation on the black phosphorus for 0.5 to 2 hours to obtain intercalated black phosphorus dispersion liquid A; in the atmosphere of 100 to 800W microwave power and inert gas, carrying out microwave stripping treatment on the intercalated black phosphorusdispersion liquid A for 1 to 10 minutes to obtain black phosphorus dispersion liquid B; carrying out centrifugal separation on the black phosphorus dispersion liquid B to obtain the nano-black phosphorus.

Description

technical field [0001] The invention relates to a method for preparing nano black phosphorus by synergistically assisting an electric field and a microwave field to strip black phosphorus, and belongs to the technical field of nano material preparation. Background technique [0002] Black phosphorus is a new type of two-dimensional layered material developed in recent years. Similar to graphite, individual atomic layers are stacked together through van der Waals interaction. Therefore, the layered black phosphorus can be peeled off into nano black phosphorus (black phosphorene or black phosphorus quantum dots) under the action of external force. Studies have shown that nano-sized black phosphorus has good application prospects in fields such as energy storage, field effect transistors, solar cells, gas sensors, and biomedicine. However, the main factor restricting the application of nano black phosphorus is the inability to meet the requirements of fast, efficient, high qua...

Claims

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Application Information

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IPC IPC(8): C01B25/02B82Y30/00
CPCB82Y30/00C01B25/02C01P2004/62
Inventor 梅毅杨颖廉培超刘红红汤永威
Owner KUNMING UNIV OF SCI & TECH
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