Method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction

A high-quality, black phosphorus technology, applied in the field of two-dimensional materials, can solve the problems of harsh reaction conditions of black phosphorus crystals, the inability to prepare in large quantities, and the difficulty of mass production, etc., to achieve industrial-scale preparation and accelerated nucleation Effects on growth process, reduction of reaction temperature and reaction time

Inactive Publication Date: 2020-03-13
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

However, due to the high temperature required for the reaction, it is difficult to achieve large-scale mass production
[0005] In short, the current seed crystal method to prepare black phosphorus crystals basically has a series of problems such as harsh reaction conditions, high reaction temperature, and inability to produce large-scale large-scale preparations.

Method used

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  • Method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction
  • Method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction
  • Method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction

Examples

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Effect test

Embodiment 1

[0049] A method for quickly preparing high-quality two-dimensional black phosphorus crystals by seed induction, the specific preparation steps are as follows:

[0050] 1) Under an inert atmosphere, weigh 310 mg of red phosphorus raw material, 6 mg of metal elemental tin, and 3 mg of iodine as a transport agent at the bottom of a single-head sealed quartz tube (raw material end, hot end); use a porous quartz gasket to separate, and weigh black Phosphorus seed crystal 8mg is placed on the top of the single-head sealed quartz tube (nucleation end, cold end); and the opening is sealed with a parafilm for later use;

[0051] 2) Remove the sealing film, and quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube.

[0052] 3) Put the sealed quartz tube in the muffle furnace, and set the heating and cooling program as follows: at room temperature, after the temperature rises to 440°C for 1 hour, keep it warm for 6 hours; then start to cool down,...

Embodiment 2

[0055] A method for quickly preparing high-quality two-dimensional black phosphorus crystals by seed induction, the specific preparation steps are as follows:

[0056] 1) Under an inert atmosphere, weigh 3100 mg of red phosphorus raw material, 100 mg of bismuth as a metal element, and 60 mg of iodine as a transport agent at the bottom of a single-head sealed quartz tube (raw material end, hot end); use alumina porous gaskets for separation, and weigh 160 mg of black phosphorus seed crystals are placed on the top of the single-head sealed quartz tube (nucleation end, cold end); and the opening is sealed with a parafilm for subsequent use;

[0057] 2) Remove the sealing film, and quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube.

[0058] 3) Put the sealed quartz tube in the muffle furnace, and set the heating and cooling program as follows: at room temperature, after the temperature rises to 520°C for 1 hour, keep it warm for 8 hour...

Embodiment 3

[0061] A method for quickly preparing high-quality two-dimensional black phosphorus crystals by seed induction, the specific preparation steps are as follows:

[0062] 1) Under an inert atmosphere, weigh 3100 mg of red phosphorus raw material, 105 mg of metal indium and 65 mg of tin tetraiodide as a transport agent at the bottom of a single-head sealed quartz tube (raw material end, hot end); use alumina porous gaskets for separation , take 100 mg of black phosphorus seed crystals on the top of a single-head sealed quartz tube (nucleation end, cold end); and seal the opening with a parafilm for subsequent use;

[0063] 2) Remove the sealing film, and quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube.

[0064] 3) Put the sealed quartz tube in the muffle furnace, and set the heating and cooling program as follows: at room temperature, after the temperature rises to 480°C for 1 hour, keep it warm for 7 hours; , down to 280°C for 7h, ...

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Abstract

The invention discloses a method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction. The method comprises the following steps: a red phosphorusraw material, a catalyst and a transport agent are weighed and are placed at the bottom (a raw material end and a hot end) of a single-head sealed quartz tube in an inert atmosphere, the internal ofthe single-head sealed quartz tube is separated by using a porous gasket, a black phosphorus seed crystal is weighed and is placed at the top (a nucleating end and a cold end) of the single-head sealed quartz tube, and the above reaction raw materials are sealed in the quartz tube by using a vacuum tube sealing system; and then the quartz tube is heated through optimized programmed heating and cooling, and the high-purity and high-quality two-dimensional black phosphorus crystal is finally prepared after the reaction is finished. Compared with a traditional preparation method without using crystal seeds, the method of the invention has the advantages of significant reduction of the reaction temperature and the reaction time in the synthesis process, reduction of the energy consumption, effective reduction of the introduction amounts of the catalyst and the transport agent required by the reaction, and cost saving. The black phosphorus crystals synthesized by the method have the advantages of few impurities, high purity, good quality, and facilitation of industrial large-scale preparation of the black phosphorus crystals.

Description

technical field [0001] The invention belongs to the technical field of two-dimensional materials, and in particular relates to a method for rapidly preparing high-quality two-dimensional black phosphorus crystals through seed crystal induction. Background technique [0002] Two-dimensional black phosphorus is a new two-dimensional semiconductor material that stands out in recent years and has received extensive attention. With its excellent optoelectronic properties, it shows excellent potential in various photonic and optoelectronic device applications. First, black phosphorus has a flexible and tunable direct bandgap, which provides an optoelectronic device with a wide-spectrum and high-efficiency photoelectric response spanning from the visible to the mid-infrared. Secondly, considering the two key performances of the mobility and the switching ratio of transistor devices, black phosphorus fills the gap between graphene and transition metal dichalcogenides, providing ide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/02C30B29/64C01B25/02C01B25/00
CPCC01B25/003C01B25/02C30B29/02C30B29/64
Inventor 喻学锋汪建南王佳宏
Owner 深圳市中科墨磷科技有限公司
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