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Preparation method of Sn3P4 induced two-dimensional black phosphorus crystals

A technology of black phosphorus and crystals, which is applied in the field of efficient preparation of two-dimensional black phosphorus crystals induced by Sn3P4, can solve the problems of few reports on the growth of catalytic two-dimensional black phosphorus crystals, difficult to guarantee the controllability of the reaction process, difficult operation and high risk factor , to achieve the effect of less impurities, reduce energy consumption, and prevent tube explosion

Active Publication Date: 2020-06-16
HUBEI MOPHOS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires not only the SnCl 2 assistance, and the reactor at high temperature needs to be quenched in cold water instantly, the operation is difficult and the risk factor is high, and the controllability of the reaction process is difficult to guarantee
[0005] In summary, the current Sn 3 P 4 The preparation methods mainly focus on chemical synthesis and high-temperature sintering. The former often requires complex chemical synthesis processes, while the latter also requires the introduction of additives and quenching treatment with high risk and poor controllability.
and currently Sn 3 P 4 It 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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  • Preparation method of Sn3P4 induced two-dimensional black phosphorus crystals
  • Preparation method of Sn3P4 induced two-dimensional black phosphorus crystals
  • Preparation method of Sn3P4 induced two-dimensional black phosphorus crystals

Examples

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Comparison scheme
Effect test

Embodiment 1

[0047] A kind of Sn 3 P 4 The method for inducing the efficient preparation of two-dimensional black phosphorus crystals, the specific preparation steps are as follows:

[0048] 1) Under an inert atmosphere (argon), weigh 117.69 mg of red phosphorus raw material and 356.1 mg of tin powder into the bottom of a single-ended sealed quartz tube, and seal the opening with parafilm for later use.

[0049] 2) Remove the sealing film, quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube, and the vacuum condition pressure in the quartz tube is below 1 Pa.

[0050] 3) Put the sealed quartz tube in the tube furnace, and set the heating and cooling program to heat the quartz tube. The specific procedure is as follows: at room temperature, the temperature was raised to 450 °C for 1 hour, and then kept for 144 hours; then the temperature was lowered, and the heating process was stopped on the basis of the holding temperature, and the tube furnace...

Embodiment 2

[0057] A kind of Sn 3 P 4 The method for inducing the efficient preparation of two-dimensional black phosphorus crystals, the specific preparation steps are as follows:

[0058] 1) Under an inert atmosphere (argon), weigh 130.07 mg of red phosphorus raw material and 356.1 mg of tin bar at the bottom of a single-ended sealed quartz tube, and seal the opening with parafilm for later use.

[0059] 2) Remove the sealing film, quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube, and the vacuum condition pressure in the quartz tube is below 1 Pa.

[0060] 3) Put the sealed quartz tube in the tube furnace, and set the heating and cooling program to heat the quartz tube. The specific procedure is as follows: at room temperature, the temperature was raised to 520 °C for 2 hours, and then kept for 192 hours; then the temperature began to drop, and on the basis of the holding temperature, it was lowered to room temperature for 120 minutes. A...

Embodiment 3

[0067] A kind of Sn 3 P 4 The method for inducing the efficient preparation of two-dimensional black phosphorus crystals, the specific preparation steps are as follows:

[0068] 1) Under an inert atmosphere (argon), weigh 123.88 mg of red phosphorus raw material and 356.1 mg of tin foil to the bottom of a single-head sealed quartz tube, and seal the opening with parafilm for later use.

[0069] 2) Remove the sealing film, quickly use the vacuum sealing system to seal the reaction raw materials inside the quartz tube, and the vacuum condition pressure in the quartz tube is below 1 Pa.

[0070] 3) Put the sealed quartz tube in the tube furnace, and set the heating and cooling program to heat the quartz tube. The specific procedure is as follows: at room temperature, the temperature was raised to 500 °C for 1 hour, and then kept for 168 hours; then the temperature began to drop, and on the basis of the holding temperature, it was lowered to room temperature for 60 minutes. Aft...

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Abstract

The invention discloses a preparation method of Sn3P4 induced two-dimensional black phosphorus crystals. In an inert atmosphere, a red phosphorus raw material and metal elemental tin are placed at thebottom of a single-head sealed quartz tube, a vacuum tube sealing system is used for sealing a reaction raw material in the quartz tube, then the quartz tube is heated through optimized programmed heating and cooling to obtain a block Sn3P4 compound, and the block Sn3P4 compound is ground into powder for standby application. A red phosphorus raw material, the Sn3P4 powder and a transport agent are then weighed and added to the bottom of a single-head sealed quartz tube in an inert atmosphere, the reaction raw material is sealed in the quartz tube by using the vacuum tube sealing system, and the quartz tube is subjected to heating treatment through optimized programmed heating and cooling to prepare the high-purity and high-quality two-dimensional black phosphorus crystals. The intermediate product Sn3P4 of the reaction system is used as the 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, and the pressure intensity in the tube can be reduced.

Description

technical field [0001] The invention belongs to the technical field of two-dimensional materials, in particular to a Sn 3 P 4 A method for inducing the efficient preparation of two-dimensional black phosphorus crystals. Background technique [0002] Two-dimensional black phosphorus (BP) is a new type of semiconductor material that has come to the fore in recent years and has received extensive attention. With its excellent photonics and optoelectronics material properties, black phosphorus 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 properties of transistor devices, mobility and switch ratio, black phosphorus fills the gap between graphene (Graphene) and transition metal dichalcogeni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02C01B25/08B01J27/14
CPCC01B25/02C01B25/08B01J27/14
Inventor 喻学锋汪建南王佳宏
Owner HUBEI MOPHOS TECH CO LTD
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