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Method for preparing hollow carbon nano-cage through iodized thermal treatment

A hollow carbon and nano-cage technology, applied in the field of nano-materials, can solve the problems of loss, large loss, oxidation of graphite layer, etc., and achieve the effect of simple method, small loss and low cost

Inactive Publication Date: 2009-09-30
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chemical method usually consumes part of the carbon nanocage at the cost of serious damage to the structure of the carbon nanocage and a large amount of loss.
When the carbon nanocage has a good graphitized structure and the outer wall is thicker, the above oxidation treatment method cannot effectively remove the catalyst particles; and when the outer wall is thinner, the thinner graphite layer is easily completely oxidized, and the hollow space cannot be obtained. Carbon nanocage structure, severe loss
[0003] Searching the prior art literature found that Y.W.Ma et al published the article "A practical route to the production of carbonnanocages (method for preparing carbon nanocages)" in "Carbon" (carbon), 43 (2005) pages 1667-1672 , a method for removing carbon nanocage catalysts by acid washing is introduced in this paper. The specific process is as follows: firstly, the original sample is placed in 4mol / LHNO 3 Treat at medium room temperature for 5 hours, then raise the temperature to 120°C for 4 hours, and finally collect the sample by filtration and transfer it to 12mol / L HCl for dozens of hours, which can remove most of the iron particles inside the carbon nanocage; the disadvantages of this method are: The removal of iron particles inside the carbon nanocages obtained by this method is not complete, and the pores on the walls of the nanocages cause too many defects; "Thin-Walled Carbon Nanocages: Direct Growth, Characterization, and Applications (Thin-Walled Carbon Nanocages: Direct Preparation, Properties, and Applications)" describes a high-temperature treatment supplemented by magnetic separation and acid washing to remove catalyst particles , the specific process is: first place the sample in a corundum tube and fill it with argon protection, heat the corundum tube rapidly to 1000 ° C ~ 1350 ° C, and perform a high-temperature treatment on the carbon nanocage for 2 hours; then disperse the treated sample on the surface Ultrasonic vibration in the active agent aqueous solution for 0.5 hours, and then stand still on the external magnetic field for 3 hours, the carbon nanocages containing iron particles are deposited to the bottom and the hollow carbon nanocages are dispersed in the upper solution, and the samples in the upper solution are collected by filtration
The results show that the iron particles in the carbon nanocages are effectively removed and the graphite layer is not damaged. The disadvantage is that the method for removing the catalyst is too complicated, and most of the carbon nanocages containing the catalyst particles are separated and cannot be effectively used. very low output

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The nitrogen / acetylene mixed gas flows through the carbonyl iron liquid and then flows to the reactor. The temperature of the reactor is 1000°C, the flow rate of nitrogen is 120L / h, and the flow rate of acetylene is 50ml / min. carbon nanocages;

[0017] Mix the nanocages containing iron particles prepared in the previous step with iodine at a weight ratio of 1:8 and place them in the reactor, pass through the argon gas protection, and rapidly raise the temperature of the reactor to 600 ° C, and the holding time is 30 minutes;

[0018] The mixed sample after iodine heat treatment was placed in ethanol at 1g / 10ml, and ultrasonically oscillated for 20 minutes. The above mixed solution was filtered, washed, dispersed in a small amount of ethanol and dried at 80° C. for 3 hours to obtain a hollow carbon nanocage with catalyst particles removed.

[0019] Implementation effect: The solid carbon nanocage prepared by this group has an obvious hollow structure after iodine-added ...

Embodiment 2

[0021] The nitrogen / acetylene mixed gas flows through the carbonyl iron liquid and then flows to the reactor, and the reactor temperature is 1300°C. The flow rate of nitrogen is 160 L / h, and the flow rate of acetylene is 40 ml / min. Obtain carbon nanocages wrapped with iron particles in the reactor tail product collector;

[0022] Mix the carbon nanocages containing iron particles prepared in the previous step with iodine at a weight ratio of 1:10 and place them in the reactor, pass through nitrogen protection, and rapidly raise the temperature of the reactor to 1000°C, and hold the temperature for 35 minutes;

[0023] The mixed sample after iodine heat treatment was dispersed in acetone at 1g / 12ml, and ultrasonically oscillated for 10 minutes. The above mixed solution was filtered and washed, and the sample was dispersed in a small amount of ethanol again and dried at 80° C. for 3 hours to obtain a hollow carbon nanocage with iron particles removed.

[0024] Implementation e...

Embodiment 3

[0026] The nitrogen / acetylene mixed gas flows through the cobalt carbonyl liquid and then flows to the reactor, and the reactor temperature is 1100°C. The flow rate of nitrogen is 120 L / h, and the flow rate of acetylene is 60 ml / min. Obtain carbon nanocages wrapped with cobalt particles in the reactor tail product collector;

[0027] Mix the nanocages containing cobalt particles prepared in the previous step with iodine at a weight ratio of 1:8 and place them in the reactor, pass through argon protection, raise the temperature of the reactor to 800°C, and hold the temperature for 40 minutes;

[0028] The iodine-treated mixed sample was dispersed in ethanol at 1 g / 15 ml, and ultrasonically oscillated for 10 minutes. The above mixed solution was filtered and washed, and the sample was again dispersed in a small amount of ethanol and dried at 80° C. for 3 hours to obtain hollow carbon nanocages.

[0029] Implementation effect: After the solid carbon nanocage prepared by this gr...

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Abstract

The invention relates to a method for preparing a hollow carbon nano-cage through iodized thermal treatment, which belongs to the technical field of preparing nanometer materials and comprises the following steps: raising the temperature of a reactor to between 1,000 and 1,300 DEG C so that mixed gas of inert gas and acetylene flows through a metal carbonyl liquid and then flows towards the reactor so as to obtain a solid carbon nano-cage enwrapped with metal catalyst particles, wherein the flow rate of the inert gas is between 100 and 200 liters per hour and the flow rate of the acetylene is between 10 and 100 milliliters per minute; mixing iodine with the solid carbon nano-cage obtained in the step one according to the weight ratio of more than or equal to 2:1 and placing the mixture in the reactor, introducing the inert gas into the reactor, raising the temperature in the reactor to between 400 and 1,000 DEG C, and keeping the temperature for 10 to 60 minutes; and performing ultrasonic vibration on the mixture obtained in the step two in ethanol or acetone for 10 to 30 minutes, filtering the mixture, washing the mixture with deionized water, and drying the mixture at a temperature of 80 DEG C to obtain the hollow carbon nano-cage without the metal catalyst particles. The method can effectively remove the metal catalyst particles in the carbon nano-cage, and has smaller damage to the graphite structure of the carbon nano-cage in the process of the treatment.

Description

technical field [0001] The invention relates to a method for preparing a hollow carbon nanocage in the technical field of nanomaterials, in particular to a method for preparing a hollow carbon nanocage by iodine heat treatment. Background technique [0002] In recent years, more and more attention has been paid to the practical application value of carbon nanomaterials and their specific performance in applications. Due to its unique structural characteristics, carbon nanocages have broad application prospects. Its outer wall has a good graphitized structure, excellent thermal, chemical stability and electrical properties, and has great application potential. At present, the synthesis method of carbon nanocages is mainly based on chemical vapor deposition method. In this method, carbon source gas or liquid is decomposed into active carbon atoms at high temperature. Under the catalysis of transition metals, carbon nanocages are prepared by controlling the reaction conditions....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 王健农滕尚君
Owner SHANGHAI JIAO TONG UNIV