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Black phosphorus and phosphinidene preparing methods

A technology of black phosphorus and red phosphorus, applied in the preparation of phosphorus and other directions, can solve the problems of extremely high requirements for experimental instruments and equipment, and achieve the effects of cheap raw materials, simple process and good repeatability

Inactive Publication Date: 2016-05-11
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the commonly used synthesis method is high temperature (1000°C) and high pressure (10kbar) method, but this method has extremely high requirements for experimental equipment.

Method used

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  • Black phosphorus and phosphinidene preparing methods
  • Black phosphorus and phosphinidene preparing methods
  • Black phosphorus and phosphinidene preparing methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 0.5g red phosphorus, 0.02g tin, 0.01g tin tetraiodide into the glass quartz tube, then vacuum the quartz tube, when the vacuum degree reaches 10 -3 Fill a certain amount of argon at mbar, and encapsulate a quartz tube (inner diameter 0.8cm, length 8cm). Then set the following heating program in the muffle furnace:

[0028] Room temperature-320min-650℃-60min-650℃-450min-500℃-100min-500℃-330min-room temperature.

Embodiment 2

[0030] Add the target product obtained in Example 1 to 100ml of C 7 H 8 In the solvent, a water bath heating method is used for purification at a temperature of 90°C for 2 hours. After the purification is completed, it is dried in a vacuum drying oven at 80°C to obtain high-purity black phosphorus.

Embodiment 3

[0032] Add 0.5g red phosphorus, 0.02g tin, 0.01g tin tetraiodide into the glass quartz tube, then vacuum the quartz tube, when the vacuum degree reaches 10 -7 Fill a certain amount of argon at mbar, and encapsulate a quartz tube (inner diameter 0.8cm, length 8cm). Then set the following heating program in the muffle furnace: room temperature-320min-650℃-60min-650℃-450min-500℃-100min-500℃-330min-room temperature.

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Abstract

The invention relates to black phosphorus and phosphinidene preparing methods. According to the black phosphorus preparing method, tin tetraiodide, tin and red phosphorus are used as raw materials to prepare black phosphorus through reaction. According to the phosphinidene preparing method, the prepared black phosphorus is treated in N-methyl pyrrolidone, absolute ethyl alcohol or N-cyclohexyl-2-pyrrolidone for a proper period of time under the stirring and ultrasonic condition at 20-50 DEG C. Reasonable preparing raw materials and reaction conditions are adopted, and synthesis can be achieved within 21-32 h only. Few-layer black phosphorus is prepared successfully by means of the liquid-phase stripping method. According to the preparing methods, the technology is simple, raw materials are cheap, and repeatability is high.

Description

Technical field [0001] The invention relates to the preparation and synthesis of materials, in particular to a preparation method of black phosphorus and phosphorene, belonging to the field of material synthesis. Background technique [0002] Black phosphorus is an allotrope of phosphorus. It is a two-dimensional crystal composed of a single layer of phosphorus atoms stacked. It has a similar structure to graphite, and the layers are combined by van der Waals forces. Black phosphorus has high electron mobility (~1000cm 2 / Vs) and switching ratio (10 5 ), has excellent mechanical, thermal, electrical, optical properties and wide application prospects. The biggest difference from graphene is that black phosphorus is a direct bandgap semiconductor. This feature allows its optical and optoelectronic properties to have huge advantages over other materials (including silicon and molybdenum sulfide), which makes black phosphorus a future optoelectronic device (Such as photodetectors, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02
CPCC01B25/02C01P2002/72C01P2002/82C01P2002/85C01P2004/03C01P2004/04
Inventor 胡晓云张国伟穆江龙樊君苗慧浦晨晨韩同信刘恩周
Owner NORTHWEST UNIV(CN)
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