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How to prepare black phosphorus - a new material that is expected to exceed graphene

Release date:2018-08-23  source:粉体网  Browse times:825
     Phosphorus is one of the most abundant elements on earth, accounting for about 0.1% of the mass of all elements in the earth's crust. The allotropes of phosphorus are red phosphorus, white phosphorus, purple phosphorus and black phosphorus. Among them, black phosphorus has the most stable nature and the weakest reactivity, and it does not burn in the air. Black phosphorus is formed by conversion of white phosphorus at very high pressure and high temperature.
Figure 1: Schematic diagram of black phosphorus crystal and its unit cell structure

Physical properties of black phosphorus
Preparation method of black phosphorus

High pressure method

The high pressure method was first developed for the preparation of black phosphorus, developed by Bridgman in 1914. Experimental procedure: Firstly, white phosphorus is placed in a cylindrical steel container with a length of about 15 cm and an inner diameter of 1.5 cm, and then the container containing white phosphorus is placed in a high-pressure device equipped with kerosene, and pressurized to 0.6 × 109 Pa at room temperature. Subsequently, the apparatus was heated to 200 ° C and the pressure was raised to 1.2 × 109 Pa to obtain black phosphorus. The preparation of black phosphorus by high pressure method has good repeatability, and the conversion of red phosphorus to black phosphorus can be realized in a short time. However, the preparation method requires the use of ultra-high pressure equipment, which leads to a high production cost of black phosphorus to a certain extent, which is not conducive to large-scale commercial production.

Helium melting method

First, the red phosphorus and bismuth particles are placed on the left and right sides of the device under an argon atmosphere, and subjected to vacuum sealing treatment (as shown in Fig. 2a); then, the red phosphorus and bismuth powder are heated and the bottom of the right end is formed. In the block, white phosphorus is formed on the top, and the right end of the device is removed (as shown in Figure 2b). Finally, the crucible is heated at 300 ° C, and the liquid helium is poured onto the solid white phosphorus, and the device is placed at 400 ° C. After holding for 48 h, it was then cooled to room temperature, and the hydrazine was removed with nitric acid to obtain black phosphorus.

Figure 2: Schematic diagram of the preparation of black phosphorus by the enthalpy melting method


The mineralization method is a method of preparing black phosphorus developed in recent years. The Au, Sn, SnI4 and red phosphorus are mixed in a certain mass ratio, vacuum-packed in a quartz tube, heated to a certain temperature and kept for a certain period of time to obtain black phosphorus, but a small amount of unconverted red is present in the final product. Impurities such as phosphorus and metal phosphides formed by the reaction. But Au is expensive and SnI4 is toxic. Later, the researchers found that black phosphorus can be prepared directly under normal pressure by using I, Sn and red phosphorus as raw materials. The specific steps are as follows: Sn, I and red phosphorus are sealed under an argon atmosphere, and subjected to a program temperature rise and fall treatment. Black phosphorus was also prepared. The preparation method not only uses the expensive and toxic SnI4 as a mineralizer, but also eliminates the need for vacuum treatment, thereby simplifying the preparation process, greatly reducing the cost, and having a good industrial application prospect.

Comparison of preparation methods
Future prospects of black phosphorus

Black phosphorus can also be obtained by black phosphorus in a similar manner to the preparation of graphene. Compared with black phosphorus, black phosphorus has high specific surface area, good mechanical properties and electrical properties. Black phosphorus and black phosphorus have good application prospects in the fields of lithium ion batteries, sodium ion batteries and super capacitors. . But the fatal flaw of black phosphorus is the lack of stability. When exposed to water and oxygen, the black phosphorus sheet will oxidize and degrade in a very short time. This deficiency greatly limits the research and industrial application of black phosphorus. The successful preparation of high-stability black phosphorus can undoubtedly promote the industrial application of black phosphorus in photovoltaic devices and other fields, and will greatly promote its in-depth research in the fields of energy, catalysis, and biomedicine.

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