Red phosphorus pre-treatment method for preparing black phosphorus

A pretreatment, red phosphorus technology, applied in the preparation of phosphorus, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of low selectivity, residual impurities, affecting the comprehensive performance of black phosphorus, etc., to achieve improved purity, particle size and shape. The effect of uniform appearance and high crystallinity

Inactive Publication Date: 2017-05-31
SHENZHEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, black phosphorus itself has certain instability and is easy to decompose in the environment of water and oxygen, while the raw material of red phosphorus is generally mixed with a certain amount of impurities such as water, oxides, and white phosphorus. If it is directly used in the synthesis of black phosphorus, it will reduce the Synthesis efficiency and quality of black phosphorus, some impurities will remain in black phosphorus
In addition, red phosphorus has a variety of sizes and shapes, which also have an important impact on the morphology of synthesized black phosphorus. If the morphology of red phosphorus is not controlled, the obtained black phosphorus may also have many morphology defects. Low, affecting the overall performance of black phosphorus

Method used

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  • Red phosphorus pre-treatment method for preparing black phosphorus

Examples

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Effect test

Embodiment 1

[0026] A kind of red phosphorus pretreatment method that is used for black phosphorus preparation comprises the following steps:

[0027] (1) Weigh 100g of red phosphorus powder raw material (purity 73%), loosely lay it in an alumina porcelain boat, and then load it into a tube-type heating furnace with a size of Φ100mm×1500mm; fill the tube-type furnace with a purity of 99.99% % argon, keep the flow rate at 1L / min, heat up to 180°C at a heating rate of 6°C / min, keep it for 2h and then cool down to room temperature naturally;

[0028] (2) Take out the heated red phosphorus from the tube furnace, put it into an agate mortar and grind it manually at a speed of 30 rpm for 30 minutes, then put it into a 325-mesh sieve for manual sieving, and obtain the preliminary The processed red phosphorus powder, its SEM picture is as follows figure 1 shown.

[0029] It can be seen from the figure that the red phosphorus powder obtained in this example is in the form of spherical particles, ...

Embodiment 2

[0032] A kind of red phosphorus pretreatment method that is used for black phosphorus preparation comprises the following steps:

[0033] (1) Weigh 200g of red phosphorus powder raw material (purity 85%), spread it loosely in an alumina porcelain boat, and then load it into a tube-type heating furnace with a size of Φ100mm×1500mm; fill the tube-type furnace with a purity of 99.99% % argon, keep the flow rate at 2L / min, heat up to 220°C at a heating rate of 8°C / min, keep it for 2.5h and then cool down to room temperature naturally;

[0034] (2) Take the heated red phosphorus out of the tube furnace, put it into an agate mortar and grind it manually for 40 minutes at a speed of 20 rpm, and then put it into a 400-mesh screen for manual sieving to obtain a preliminary Processed red phosphorus powder. After testing, it is known that the purity of the red phosphorus powder after pretreatment in this embodiment reaches 95.4%.

Embodiment 3

[0036] A kind of red phosphorus pretreatment method that is used for black phosphorus preparation comprises the following steps:

[0037] (1) Weigh 300g of red phosphorus powder raw material (purity 88%), loosely spread it in an alumina porcelain boat, and then load it into a tube-type heating furnace with a size of Φ100mm×1500mm; fill the tube-type furnace with a purity of 99.999% % argon, the flow rate is maintained at 2.5L / min, heated to 250°C at a heating rate of 12°C / min, kept for 3.5h and then naturally cooled to room temperature;

[0038] (2) Take out the heated red phosphorus from the tube furnace, put it into a planetary ball mill for ball milling, the speed is 200 rpm, and the ball milling time is 15min, then put it into a 500-mesh screen for manual sieving points to obtain the pretreated red phosphorus powder. After testing, it is known that the purity of the red phosphorus powder after pretreatment in this embodiment reaches 99.8%.

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Abstract

The invention provides a red phosphorus pre-treatment method for preparing black phosphorus. The red phosphorus pre-treatment method comprises the following steps: putting red phosphorus into a heating furnace; heating to 150 DEG C to 300 DEG C under a protective atmosphere or vacuum condition, and keeping for 1h to 4h; then naturally cooling to room temperature; carrying out manual grinding or ball milling on the red phosphorus subjected to the heating treatment to obtain pre-treated red phosphorus powder. The red phosphorus pre-treatment method provided by the invention has a simple process, and the treated red phosphorus powder has high purity and uniform granularity and shape; when the red phosphorus powder is used as a raw material for synthesizing the black phosphorus, the purity and conversion efficiency of the black phosphorus can be effectively improved, and high-quality and high-crystallization-degree black phosphorus single crystals or poly-crystals are obtained.

Description

technical field [0001] The invention relates to the technical field of red phosphorus processing, in particular to a red phosphorus pretreatment method for preparing black phosphorus and red phosphorus powder processed by the method. Background technique [0002] There are three main allotropes of phosphorus, white phosphorus, red phosphorus and black phosphorus, among which black phosphorus has relatively high thermodynamic stability, adjustable direct band gap, near-infrared light response characteristics and biodegradability. It has received more and more attention in fields such as optoelectronic devices. The traditional method of preparing black phosphorus is to convert white phosphorus into black phosphorus crystals under high temperature and ultra-high pressure conditions. The temperature used exceeds 1000°C and the pressure is as high as GPa. Therefore, this method has high technical threshold and great safety hazards. , high cost and other obvious shortcomings, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02C01B25/043
CPCC01B25/02C01B25/043C01P2004/03C01P2004/61C01P2004/62C01P2006/80
Inventor 张晗汤贤张家宜
Owner SHENZHEN UNIV
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