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Gradient oxidation purification method for single-walled carbon nanotube

A technology of single-walled carbon nanotubes and a purification method, which is applied in the field of carbon nanotube purification based on strong and weak oxidizing atmosphere gradient oxidation assisted acid treatment, which can solve the problems of lack of removal of metal particles, low product purity, and low purification efficiency. Achieve the effects of simple method, improved processing efficiency, improved purity and quality

Active Publication Date: 2019-04-19
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, among the above-mentioned purification techniques, some methods have low purification efficiency, complex operation, and lack of effective removal of metal particles coated in the crystalline graphite layer, resulting in low product purity; some methods sacrifice single-wall The quality and yield of carbon nanotubes to obtain relatively high purity products

Method used

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  • Gradient oxidation purification method for single-walled carbon nanotube
  • Gradient oxidation purification method for single-walled carbon nanotube
  • Gradient oxidation purification method for single-walled carbon nanotube

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The single-walled carbon nanotubes prepared by the arc method were placed on a quartz boat as it was, and the quartz boat was put into a tube furnace. The temperature was raised to 400° C. under a nitrogen atmosphere, and after the temperature stabilized, 20% of the total volume concentration of oxygen was introduced to react for 1 h. After the reaction was completed, the oxygen feed was cut off, and the temperature was raised to 800° C. under a nitrogen atmosphere. After the temperature was stabilized, carbon dioxide with a concentration of 50% of the total volume was introduced to react for 1 hour. After the reaction, the carbon dioxide feed was cut off, and the reactor was cooled down to room temperature under the protection of nitrogen. The sample was taken out and added to 100 mL of 6M hydrochloric acid solution and stirred at room temperature for 12 h, then filtered and dried to obtain the purified product, and the purified product and the original sample before p...

Embodiment 2

[0028] The single-walled carbon nanotubes prepared by the arc method were placed on a quartz boat as it was, and the quartz boat was put into a high-temperature tube furnace. The temperature was raised to 450° C. under a nitrogen atmosphere, and after the temperature was stabilized, 20% of the total volume concentration of oxygen was introduced to react for 0.5 h. After the reaction, the oxygen feed was cut off, and the temperature was raised to 800° C. under a nitrogen atmosphere. After the temperature was stabilized, carbon dioxide with a concentration of 100% of the total volume was introduced to react for 1 hour. After the reaction, the carbon dioxide feed was cut off, and the reactor was cooled down to room temperature under the protection of nitrogen. The sample was taken out and added to 50 mL of 12M concentrated hydrochloric acid and stirred at room temperature for 24 hours, then filtered and dried to obtain the purified product, and the purified product and the origin...

Embodiment 3

[0030] The single-walled carbon nanotubes prepared by the HiPco method were placed on a quartz boat as it was, and the quartz boat was put into a high-temperature tube furnace. The temperature was raised to 300° C. under an argon atmosphere, and after the temperature was stabilized, ozone with a concentration of 50% of the total volume was introduced to react for 2 hours. After the reaction was completed, the ozone feed was cut off, and the temperature was raised to 600° C. under an argon atmosphere. After the temperature was stabilized, carbon dioxide with a concentration of 20% of the total volume was introduced to react for 1 hour. After the reaction, the carbon dioxide feed was cut off, and the reactor was cooled down to room temperature under the protection of argon. The sample was taken out and added to 200 mL of 1M nitric acid solution, stirred at room temperature for 2 hours, then centrifuged and dried to obtain the purified product, and the purified product and the or...

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Abstract

The invention belongs to the field of carbon nanomaterials, and discloses a gradient oxidation purification method for a single-walled carbon nanotube. The method comprises steps that (1), an originalsingle-walled carbon nanotube sample is placed in a reactor, inert gas is introduced into the reactor, the reactor is heated to the lower temperature T1, after the temperature is stable, strong-oxidation gas is introduced in the reactor, and after the reaction is conducted for 0.1-5 h, the strong-oxidation gas stops being introduced; (2), under protection of the inert gas, the reactor is heated to the higher temperature T2, after the temperature is stable, weak-oxidation gas is introduced into the reactor, and after the reaction is conducted for 0.1-5 h, the weak-oxidation gas stops being introduced; T2-T1>=100 DEG C; (3), a sample obtained in the step 2 is dispersed in an acid solution, the stirring reaction is conducted or 0.1-24 h, and filtering and drying are conducted. The method notonly can improve the efficiency of treating carbon impurities on the premise of preventing the surface of the single-walled carbon nanotube from being damaged, but also can effectively damage outer-layer graphite impurity crystals of a carbon wrapping metal structure in the product, and solves the problem that metal particles wrapped in a graphite crystal layer are difficult to remove, and therefore the purity and quality of the single-walled carbon nanotube are improved.

Description

technical field [0001] The invention belongs to the technical field of carbon nanomaterials, in particular to a method for purifying carbon nanotubes based on strong and weak oxidizing atmosphere gradient oxidation assisted acid treatment. Background technique [0002] As the most representative one-dimensional nanomaterial, single-walled carbon nanotubes have many excellent mechanical properties, thermal properties, electrical properties and chemical properties. They have shown great promise in many fields such as electronic devices, composite materials, sensors and catalyst supports Broad application prospects. [0003] At present, there are three main methods for the preparation of single-walled carbon nanotubes, namely arc discharge method, laser evaporation method and chemical vapor deposition method. All of them contain more or less impurities, and the existence of these impurities has greatly hindered the performance research and practical application of single-walle...

Claims

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Application Information

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IPC IPC(8): C01B32/17
CPCC01B32/17C01B2202/02C01B2202/30
Inventor 邓顺柳汪凯范建标陈淼淼肖君谢素原
Owner XIAMEN UNIV