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Method for rapidly preparing black phosphorus by crystal nucleus assisted high temperature difference manner

A black phosphorus, high temperature technology, applied in the field of nano two-dimensional material preparation, can solve the problems of complex process, harsh preparation conditions of black phosphorus, long time-consuming, etc., and achieve the effect of high energy consumption, long production cycle and reducing process energy consumption.

Inactive Publication Date: 2019-07-05
MINJIANG UNIV
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for rapidly preparing black phosphorus by crystal nucleus-assisted high-temperature difference method in view of the disadvantages of harsh preparation conditions, complicated process and long time-consuming for black phosphorus preparation

Method used

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  • Method for rapidly preparing black phosphorus by crystal nucleus assisted high temperature difference manner
  • Method for rapidly preparing black phosphorus by crystal nucleus assisted high temperature difference manner
  • Method for rapidly preparing black phosphorus by crystal nucleus assisted high temperature difference manner

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Embodiment 1

[0019] Red phosphorus (content: 99.999wt%) is used as raw material, tin powder (content: 99.99wt%) and tin iodide (content: 99.998wt%) are used as catalysts, and black phosphorus microcrystals (particle size: 50μm) are used as crystal formation materials. The nuclear agent is sealed in a quartz tube according to the mass ratio of 100:1:1:1, and placed in the middle of a dual-temperature zone tube furnace. The charged end of the quartz tube is located in the high temperature area, and the uncharged end is located in the low temperature area. The low-temperature zone of the tube furnace is not heated, and the high-temperature zone is heated at 10 ℃ min -1 Heating to 610 °C and keeping the temperature constant for 1 h, blocky black phosphorus crystals were obtained at the low temperature end of the quartz tube.

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Abstract

The invention belongs to the technical field of nano two-dimensional material preparation, and particularly relates to a method for rapidly preparing black phosphorus by crystal nucleus assisted hightemperature difference manner. The method includes sealing red phosphorus, stannum powder, stannic iodide and black phosphorus microcrystals in a mass ratio of 100:1:1:1 in a quartz tube; putting thequartz tube in the middle of a dual-temperature-zone heating tubular furnace, with a loaded end of the quartz tube being in a high-temperature zone, and an unloaded end being in a low-temperature zone; and heating to 610 DEG C in a speed of 10 DEG C / min in the high-temperature zone and maintaining the temperature for 1 h, with heating being not performed in the low-temperature zone, and then blackphosphorus crystals can be obtained at the low-temperature end of the quartz tube. The method utilizes nucleation of the black phosphorus microcrystals and the mechanism of high temperature difference rapid crystallization to rapidly prepare the black phosphorus crystals, shortens the preparation time of the black phosphorus from 24 h or above to 2h, and reduces energy consumption of steps. The black phosphorus crystals prepared by the method have great potential application value in the fields of biomedicine, electronic film, lithium batteries, infrared photoelectron technology and catalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanometer two-dimensional materials, and in particular relates to a method for rapidly preparing black phosphorus by a crystal nucleus-assisted high-temperature difference method. Background technique [0002] Black phosphorus is a black metallic luster crystal, which is converted from red phosphorus / white phosphorus under high pressure and high temperature. Black phosphorus is the least reactive of the phosphorus allotropes, and it does not ignite in air. Black phosphorus is a semiconductor with a density of 2.70g / cm 3 and a hardness of 2. Its crystal lattice is made up of diatomic layers, each of which is made up of tortuous chains of phosphorus atoms. [0003] Black phosphorus has an orthorhombic structure and is the least reactive phosphorus allotrope. Its lattice is an interlinked six-membered ring, with each atom connected to three other atoms. Black phosphorus is very similar to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02C01B25/00
CPCC01B25/00C01B25/02
Inventor 薛涵与林棋方润李心忠夏建荣
Owner MINJIANG UNIV
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