Method for preparing nitrogen doping hollow carbon nanocages

A technology of nanocage and hollow carbon, which is applied in the direction of nanocarbon, nanotechnology, nanotechnology, etc., can solve the problems such as the preparation method of nitrogen-doped carbon nanocage that has not yet been seen, and achieve easy recycling and reuse, high specific surface area, mesoporous high rate effect

Inactive Publication Date: 2012-07-04
NANJING UNIV
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  • Abstract
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  • Claims
  • Application Information

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  • Method for preparing nitrogen doping hollow carbon nanocages
  • Method for preparing nitrogen doping hollow carbon nanocages
  • Method for preparing nitrogen doping hollow carbon nanocages

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Embodiment 1

[0042] Weigh basic magnesium carbonate and add it into the reaction tube, spread it evenly, put it into the central area of ​​the tube furnace, then repeatedly fill it with argon and evacuate it with a mechanical pump for 3-5 times. Under an argon atmosphere (50 sccm), the temperature was raised to 650 °C at a rate of 10 °C per minute, and 0.020 ml / min of pyridine was input with a convection pump, and the reaction was carried out for 60 min. ) protection down to room temperature, collect the powder from the reaction tube, soak in 1mol / L hydrochloric acid solution for 60min, filter, wash with deionized water until neutral, and dry to obtain nitrogen-doped hollow carbon nanocages. After testing, the nitrogen content is about 12%. The specific surface area is about 1800 m 2 ?g -1 , the pore volume can reach 4.20 cm 3 ?g -1 , the particle size is about 10~30 nm, and the mesoporosity is higher than 99.7%.

Embodiment 2

[0044] Weigh basic magnesium carbonate and add it into the reaction tube, spread it evenly, put it into the central area of ​​the tube furnace, then repeatedly fill it with argon and evacuate it with a mechanical pump for 3-5 times. Under an argon atmosphere (50 sccm), the temperature was raised to 700 °C at a rate of 10 °C per minute, and 0.020 ml / min of pyridine was input with a convection pump, and the reaction was carried out for 60 min. ) protection down to room temperature, collect the powder from the reaction tube, soak in 10mol / L hydrochloric acid solution for 60min, filter, wash with deionized water until neutral, and dry to obtain nitrogen-doped hollow carbon nanocages. After testing, the nitrogen content is about 11%. The specific surface area is about 1650 m 2 ?g -1 , the pore volume can reach 3.90 cm 3 ?g -1 , the particle size is about 10~40 nm, and the mesoporosity is higher than 99.5%.

Embodiment 3

[0046] Weigh basic magnesium carbonate and add it into the reaction tube, spread it evenly, put it into the central area of ​​the tube furnace, then repeatedly fill it with argon and evacuate it with a mechanical pump for 3-5 times. Under an argon atmosphere (50 sccm), the temperature was raised to 800 °C at a rate of 10 °C per minute, and 0.020 ml / min of pyridine was input with a convection pump, and the reaction was carried out for 60 min. ) protection down to room temperature, collect the powder from the reaction tube, soak in 1mol / L hydrochloric acid solution for 30min, filter, wash with deionized water until neutral, and dry to obtain nitrogen-doped hollow carbon nanocages. After testing, the nitrogen content is about 10%. The specific surface area is about 1100 m 2 ?g -1 , the pore volume can reach 2.50 cm 3 ?g -1 , the particle size is about 10~40 nm, and the mesoporosity is higher than 99.5%.

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Abstract

The invention relates to a method for preparing nitrogen doping hollow carbon nanocages, which comprises the following steps that: (1) basic magnesium carbonate or magnesium carbonate is taken to be added into a reaction tube and is uniformly dispersed, then the reaction tube is placed in a tube furnace, air in the tube furnace is extracted, inert gases are filled into the tube furnace, under the condition of 10-500sccm of inert gases, the temperature of the tube furnace is increased to 650-1,100 DEG C, then the inert gas flow is guided into steam which contains carbon (C) and nitrogen (N), and after reacting for 5-240min, the temperature of the tube furnace is reduced to a room temperature; and (2) powder in the reaction tube is collected, put into hydrochloric acid or sulfuric acid solution to be soaked for 5-720min, filtered, cleaned by deionized water and dried, so a nitrogen doping hollow carbon nanocage is obtained. The nitrogen doping hollow carbon nanocage which is produced by the method has the advantages of high specific surface area, large pore volume, high mesoporous ratio, good graphitization degree and the like, and is a metal-free oxygen reduction reaction catalyst with excellent performance.

Description

technical field [0001] The invention relates to a method for preparing a hollow carbon nanocage, in particular to a method for preparing a nitrogen-doped hollow carbon nanocage. Background technique [0002] Hollow carbon nanocages are usually a by-product formed during the preparation of carbon nanotubes and have been neglected for a long time. However, this unique hollow nanostructure has unique physical and chemical properties. Studies have shown that it is expected to be applied in many fields such as catalysis, energy, separation, and optical devices (Anvar A. Zakhidov, et al. science 1998, 282, 897.; S. Han, et al. Adv. Mater. 2003, 15, 1922.; Ajayan Vinu et al., J. Porous Mater. 2006, 13, 379.; J. J. Niu, et al. J. Phys. Chem. C 2007, 111, 10329.). So far, people have developed several technical routes to prepare hollow carbon nanocages, such as: arc method, laser evaporation method, plasma polymerization method, vapor phase chemical deposition method (CVD),...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y30/00B82Y40/00C01B32/15
Inventor 王喜章毕吉玉陈盛杨立军吴强胡征
Owner NANJING UNIV
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