Method for efficiently preparing two-dimensional black phosphorus crystal by taking SnP3 as catalyst

A catalyst and black phosphorus technology, applied in the field of two-dimensional materials, can solve the problems of stability of tin-phosphorus compounds, poor controllability of the synthesis process of product purity, and few reports on catalyzing the growth of two-dimensional black phosphorus crystals. Accelerates the nucleation and growth process and promotes the effect of rapid generation

Pending Publication Date: 2020-07-24
深圳市中科墨磷科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, as in the patent CN109305661A, tin-iodine-phosphorus ternary compound is used as a catalyst. Although its catalytic efficiency is high, it needs to introduce extremely volatile iodine or iodide in the synthesis process, so the purity of the product and the controllability of the synthesis process Poor, far less stable than tin-phosphorus compounds
[0005] Current research status, tin phosphorus compounds (SnP 3 ) is only used in the field of batteries, and there are few reports on its catalytic growth of two-dimensional black phosphorus crystals.

Method used

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  • Method for efficiently preparing two-dimensional black phosphorus crystal by taking SnP3 as catalyst
  • Method for efficiently preparing two-dimensional black phosphorus crystal by taking SnP3 as catalyst
  • Method for efficiently preparing two-dimensional black phosphorus crystal by taking SnP3 as catalyst

Examples

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Effect test

Embodiment 1

[0043] A tin-phosphorous compound (SnP 3 ) is a method for efficiently preparing two-dimensional black phosphorus crystals as a catalyst, and the specific preparation steps are as follows:

[0044] 1) Weigh 86.7 mg of red phosphorus raw material and 118.7 mg of metal elemental tin into a ball mill jar, and perform high-energy ball milling under an inert atmosphere. The specific parameters are: the ball milling material (including ball milling pot and balls) is agate, the particle size of the balls is 0.5cm, the ball-to-material ratio is 90:1, the ball milling time is 36h, and the milling speed is 300r / min. After ball milling, get SnP 3 powder and take it out for later use.

[0045] 2) Under an inert atmosphere, weigh 3100 mg of red phosphorus raw material, SnP 3 210mg of powder and 60mg of transport agent I2 were placed at the bottom of a single-head sealed quartz tube, and the opening was sealed with parafilm for later use.

[0046] 3) Remove the sealing film, and quickly...

Embodiment 2

[0050] A tin-phosphorous compound (SnP 3 ) is a method for efficiently preparing two-dimensional black phosphorus crystals as a catalyst, and the specific preparation steps are as follows:

[0051] 1) Weigh 99.1 mg of red phosphorus raw material and 118.7 mg of metal elemental tin into a ball mill jar, and perform high-energy ball milling under an inert atmosphere. The specific parameters are: the ball milling material (including the ball mill jar and balls) is zirconia, the particle size of the balls is 1cm, the ball-to-material ratio is 100:1, the milling time is 60h, and the ball milling speed is 500r / min. After ball milling, get SnP 3 powder and take it out for later use.

[0052] 2) Under an inert atmosphere, weigh 3100 mg of red phosphorus raw material, SnP 3 Powder 210mg and Transport Agent SnI 2 60mg is placed at the bottom of a single-head sealed quartz tube, and the opening is sealed with parafilm for later use.

[0053] 3) Remove the sealing film, and quickly ...

Embodiment 3

[0057] A tin-phosphorous compound (SnP 3 ) is a method for efficiently preparing two-dimensional black phosphorus crystals as a catalyst, and the specific preparation steps are as follows:

[0058] 1) Weigh 92.9 mg of red phosphorus raw material and 118.7 mg of metal elemental tin into a ball mill jar, and perform high-energy ball milling under an inert atmosphere. The specific parameters are: the ball milling material (including ball milling pot and balls) is zirconia, the particle size of the balls is 0.8cm, the ball-material ratio is 95:1, the ball milling time is 48h, and the milling speed is 400r / min. After ball milling, get SnP 3 powder and take it out for later use.

[0059] 2) Under an inert atmosphere, weigh 3100 mg of red phosphorus raw material, SnP 3 Powder 210mg and Transport Agent SnI 4 60mg is placed at the bottom of a single-head sealed quartz tube, and the opening is sealed with parafilm for later use.

[0060] 3) Remove the sealing film, and quickly use...

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Abstract

The invention discloses a method for efficiently preparing a two-dimensional black phosphorus crystal by taking SnP3 as a catalyst. The method comprises the following steps: firstly, weighing a red phosphorus raw material and elemental metal tin, carrying out high-energy ball milling in an inert atmosphere to obtain SnP3 powder, and taking out the SnP3 powder for later use; and under an inert atmosphere, weighing the red phosphorus raw material, SnP3 powder and a transport agent, and carrying out heating treatment in a vacuum tube sealing system to finally prepare the high-purity and high-quality two-dimensional black phosphorus crystal. Compared with the traditional method for preparing the two-dimensional black phosphorus crystal by taking metal simple substance Sn as a catalyst, the intermediate product SnP3 of the reaction system is used as a catalyst so that the nucleation barrier required in the red phosphorus-black phosphorus conversion process can be remarkably reduced, the nucleation and growth processes of the reaction are accelerated, the reaction temperature and reaction time in the synthesis process can be reduced, the energy consumption is reduced, the pressure intensity in the pipe can be reduced and the pipe explosion is prevented. The black phosphorus crystal synthesized by the method has the advantages of few impurities, high purity and good quality and is more beneficial to realization of industrial large-scale preparation of the black phosphorus crystal.

Description

technical field [0001] The invention belongs to the technical field of two-dimensional materials, in particular to a tin phosphorus compound (SnP 3 ) is a method for efficiently preparing two-dimensional black phosphorus crystals as a catalyst. Background technique [0002] Since 2014, due to its excellent performance, black phosphorus has attracted widespread attention, and is even considered as a new two-dimensional atomic material comparable to graphene. The most special value of two-dimensional black phosphorus is reflected in three aspects that are different from other two-dimensional materials. (1) Optical properties. The bandgap of thin-layer black phosphorus can be adjusted by the thickness (0.3-1.5eV), and its bandgap is just between the zero bandgap connecting graphene and the wider bandgap (1.5-2.5eV) of transition metal sulfides. Gap-defective bridges. Studies have shown that thin-layer black phosphorus exhibits strong light transmission efficiency in the ran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02C01B25/08B01J27/14
CPCC01B25/02C01B25/08B01J27/14C01P2002/72
Inventor 王佳宏汪建南喻学锋
Owner 深圳市中科墨磷科技有限公司
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