Preparation method of nano black phosphorus

A black phosphorus and nano technology, applied in the field of preparation of nano black phosphorus, can solve the problem of not being the only one, and achieve the effect of high conductivity

Active Publication Date: 2017-06-06
深圳市来源新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that high temperature and high pressure are crucial to the synthesis of black phosphorus, but not the only

Method used

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  • Preparation method of nano black phosphorus
  • Preparation method of nano black phosphorus

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preparation example Construction

[0024] A preparation method of nano black phosphorus, the selected equipment is the invention patent "one-axis multi-cylinder multi-dimensional ball hammer type high-energy micro-nano ball mill, patent number 201410391780.7, including the following steps:

[0025] 1) Fill the grinding tank with raw material red phosphorus and spherical grinding medium, and complete the cover. The amount of raw material red phosphorus is 1 / 3 of the volume of the grinding tank, and the amount of spherical grinding medium is 1 / 3 of the capacity of the grinding tank; The composition is: 1 / 3 of 10 mm diameter, 1 / 3 of 8 mm diameter, 1 / 3 of 5 mm diameter; or 1 / 3 of 12 mm diameter, 1 / 3 of 10 mm diameter, and 1 / 3 of 8 mm diameter;

[0026] 2) Vacuumize to 0.08-0.1Pa, add argon or other inert gas to positive pressure of 0.08-0.1Pa, and then perform ultra-high energy ball milling at a frequency of 800 times / min to 1600 times / min;

[0027] 3) Continuous ball milling for 8-10 hours. After unloading the tan...

Embodiment 1

[0036] Put 100g of red phosphorus and 5g of red copper powder into a 0.5L copper mill jar, add 150g of red copper balls with a diameter of 10mm, 150g of red copper balls with a diameter of 8mm, and 150g of red copper with a diameter of 5mm. Argon Pa, then install the grinding balls on the wheel disc of the Nano Ferris Mill, fix it firmly, adjust it to 100 times / min after starting the machine, unload the tank for 10 hours of continuous ball milling, put the grinding tank in the vacuum glove box, put the glove box After evacuating and adding argon, open the lid of the grinding tank to sieve the ball material, pack and seal the material, and then take it out from the glove box to obtain crystalline black phosphorus of about 100-300 nanometers. The composition analysis shows that the phosphorus content is 90%. Contains 10% copper.

Embodiment 2

[0038] Add 100g of red phosphorus and 10g of boron nitride into the silicon nitride grinding tank, add 150g of silicon nitride balls with a diameter of 10mm, 150g of silicon nitride balls with a diameter of 8mm and 150g of silicon nitride balls with a diameter of 5mm, and vacuumize the tank to 0.08-0.1Pa, then add argon gas to 0.08-0.1Pa, then put the mill tank on the wheel of the Nano Ferris Mill, fix it firmly, turn it on and adjust it to 900 times / min, continue ball milling for 10 hours, unload the tank, and put the mill Put the tank into a vacuum glove box, vacuumize the glove box and add argon, open the lid of the grinding tank, sieve the ball material, put the material into the bottle and seal it, and then take it out of the glove box to obtain 100-300 Crystalline black phosphorus of about nanometers, composition analysis contains 90% phosphorus and 10% boron.

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Abstract

The invention discloses a preparation method of nano black phosphorus, and belongs to the field of novel materials. A novel technology for synthesizing the nano black phosphorus by a mechanical and physical method is adopted, and the technology is an ultrahigh-energy ball milling method comprising optimization of a ball-hammer type instantaneous high-frequency impact pressure and parameters, atmosphere control, and addition of a modified material, wherein red phosphorus is used as a raw material, a milling tank is vacuumized and filled with argon before ball milling, ball milling is performed for 8-10 hours at an impact frequency of 800-1600 times per minute to obtain crystal black phosphorus with an average size of 100-300 nanometers, and tank unloading, material taking and packaging needs to be completed in a vacuum glove box. According to a demand of oxidation resistance and high conductivity, during preparation of modified nano black phosphorus, a metal or metal alloy or metal oxide or nonmetal material is needed, and a high polymer material is used as a modifying material for grinding after being added with an added amount accounting for 0.1-10%.

Description

technical field [0001] The invention relates to the field of black phosphorus preparation, in particular to a method for preparing nanometer black phosphorus. Background technique [0002] In 1914, American scientist Bridgman prepared black phosphorus, the most stable of allotropes of phosphorus, through a high-pressure method. Bridgman also won the Nobel Prize in Physics in 1946, but the reason for the award was to recognize his outstanding contribution in the field of high-pressure physics, and black phosphorus itself did not attract much attention. In the 100 years since the first preparation of this material, there were only about 100 related literatures, with an average of only one paper a year. However, in 2014, the research on black phosphorus developed like a blowout, and many of its unique photoelectric properties were discovered. Among them, Chinese scientists have also made outstanding contributions, such as the research group of Professor Zhang Yuanbo from Fudan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02
CPCC01B25/02C01P2002/72C01P2004/03C01P2004/62C01P2006/40C01P2006/80
Inventor 曲莱曲少忠曾还相
Owner 深圳市来源新材料科技有限公司
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