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Preparation method of metal-doped nanometer black phosphorus

A technology of metal doping and black phosphorus, which is applied in the field of nanomaterials, can solve the problems of harsh conditions, damage to the crystal structure of materials, and needs, etc., and achieve the effects of low preparation cost, simple process and strong controllability

Inactive Publication Date: 2020-08-11
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, many methods have been reported for doping black phosphorus. Among them, 202010204887.1 discloses a method for electrochemically assisted preparation of doped nano black phosphorus. This method is an anode stripping method, and oxygen-containing free radicals will be generated during the experiment. Oxygen defects are caused in nano black phosphorus, and the experimental conditions are low temperature and inert gas atmosphere
In addition, the preparation of doped black phosphorus by high temperature and high pressure method is harsh and costly; the doping of black phosphorus by ball milling method will destroy the crystal structure of the material and affect the subsequent application; the mineralization method of doping black phosphorus takes a long time

Method used

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  • Preparation method of metal-doped nanometer black phosphorus
  • Preparation method of metal-doped nanometer black phosphorus
  • Preparation method of metal-doped nanometer black phosphorus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the method for preparing Al-doped nano black phosphorus is as follows:

[0026] Firstly, use an H-type electrolytic cell, separate the anode chamber and the cathode chamber with a cation exchange membrane, fix the black phosphorus on the platinum clip with a sealing film as the cathode electrode, and use the aluminum wire as the counter electrode, and use 0.01mol / L aluminum sulfate solution As the electrolyte, the counter electrode and the negative electrode are respectively connected to the positive and negative electrodes of the power supply; start the power supply, and react for 3 minutes under the action of a constant voltage of 30V; collect the reaction product, and then wash it with deionized water for 3 times, and the centrifugal speed is 12000r / min, each time is 5min, and finally the solid is vacuum-dried to obtain Al-doped nano black phosphorus;

[0027] The ultraviolet-visible absorption spectrum, transmission electron microscopy and XPS diagram...

Embodiment 2

[0028] Embodiment 2: the method for preparing Zn-doped nano black phosphorus is as follows:

[0029] Firstly, use an H-type electrolytic cell, separate the anode chamber and cathode chamber with a cation exchange membrane, fix black phosphorus on a platinum clip with a sealing film as the cathode electrode, and zinc wire as the counter electrode, and use 0.1mol / L zinc sulfate solution As the electrolyte, the counter electrode and the cathode electrode were respectively connected to the positive and negative electrodes of the power supply; start the power supply, and react for 10 minutes under the action of a constant voltage of 20V; collect the reaction product, and then wash it with deionized water for 3 times, and the centrifugal speed is 6000 r / min, each time is 30 min, and finally the solid is freeze-dried to obtain Zn-doped nano black phosphorus.

[0030] Figure 4 It is a scanning electron microscope image of Zn-doped nano black phosphorus. It can be seen from the figu...

Embodiment 3

[0031] Embodiment 3: the method for preparing Fe-doped nano black phosphorus is as follows:

[0032] Firstly, an H-type electrolytic cell is used, the anode chamber and the cathode chamber are separated by a cation exchange membrane, black phosphorus is fixed on a platinum clip with a sealing film as the cathode electrode, iron wire is used as the counter electrode, and 0.05mol / L ferric sulfate solution is used as the cathode electrode. Electrolyte, the opposite electrode and the negative electrode are respectively connected to the positive and negative electrodes of the power supply; start the power supply, and react for 30 minutes under the action of a constant voltage of 10V; collect the reaction product, then filter and wash it with deionized water for 5 times, and finally extract it by supercritical solid Dry to obtain Fe-doped nano black phosphorus;

[0033] Figure 5 It is a scanning electron microscope image of Fe-doped nano-black phosphorus. It can be seen from the f...

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Abstract

The invention discloses a preparation method of metal-doped nanometer black phosphorus. According to the method, an H-shaped electrolytic tank is adopted; an anode chamber and a cathode chamber are separated by a cation exchange membrane; black phosphorus is fixed on a platinum clamp to be used as a negative electrode; a metal to be doped is used as a counter electrode; a metal salt solution is used as an electrolyte; an electrochemical reaction is carried out under a constant voltage, elementary metal is oxidized into metal cations, the metal cations and H<+> penetrate through the cation exchange membrane and are inserted between cathode black phosphorus layers so as to peel off the black phosphorus and to form phosphide with the black phosphorus; a reaction product is collected, washed and dried to obtain the metal-doped nanometer black phosphorus. The method is simple in process, high in controllability and low in preparation cost, can be used for preparing nanometer black phosphorus doped with different metal elements according to application requirements, and has a good application prospect in the fields of energy storage, catalysis, chemical fertilizers and the like.

Description

technical field [0001] The invention relates to a method for preparing metal-doped nanometer black phosphorus, which belongs to the technical field of nanomaterials. Background technique [0002] Black phosphorus is a new type of two-dimensional material with many inherent excellent properties, such as directly adjustable band gap, high carrier rate, high anisotropy, biocompatibility, etc. The fields of materials, optoelectronics, biomedicine, catalysis and flame retardancy have shown good application prospects. However, there are still many defects in the current application of black phosphorus in various fields. Doping with metal ions can effectively regulate the crystal structure, electronic structure and magnetic properties of black phosphorus. Functional nano-black phosphorus can be prepared by doping metals according to the needs of the application. Promote the application of black phosphorus. So far, many methods have been reported for doping black phosphorus. Among...

Claims

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Application Information

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IPC IPC(8): C01B25/00C01B25/08C25B1/00B82Y30/00B82Y40/00
CPCC01B25/003C01B25/081C01B25/085C01B25/08C25B1/00B82Y30/00B82Y40/00C01P2002/84C01P2004/04C01P2002/85C01P2004/10C01P2004/20
Inventor 李雪梅侯冉冉廉培超梅毅刘岚君宋一帆
Owner KUNMING UNIV OF SCI & TECH
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