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Method for non-invasive efficient purification of single-wall carbon nano tube

A single-walled carbon nanotube, non-destructive technology, applied in nanotechnology and other directions, can solve the problems of excessive sample loss, impurity residue, fragmentation, etc., to achieve the effect of balanced oxidation environment, simple and easy process, and complete oxidation.

Inactive Publication Date: 2011-08-03
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Mainly use HNO 3 , HClO 4 , KMnO 4 / H 2 SO 4 As a strong oxidant, but during the purification process, the strong oxidant also destroys the wall structure of carbon nanotubes while removing impurities, and even breaks and breaks
lead to more sample loss, Wu (Wu C. X., Li J. X., Dong G. F., et al., Removal of Ferromagnetic Metals for the Large-Scale Purification of Single-Walled Carbon Nanotubes, J. Phys. Chem. C, 2009, 113, 3612-3616) and others reported a multi-step purification method for single-walled carbon nanotubes. The original sample of single-walled carbon nanotubes was subjected to air oxidation, high temperature treatment, HCl and HNO 3 The purified single-walled carbon nanotube samples were obtained after multiple processes. The original sample volume before treatment was 2.7g, and the sample obtained after multiple purification processes was only ~200mg. Most of the single-walled carbon nanotubes were in consumed during purification
[0004] The current problem of the above purification method is that the metal particles that act as catalysts after the growth of carbon nanotubes are tightly wrapped by graphitic carbon layers. These graphitized carbon layers exhibit very strong oxidation resistance. A large number of catalyst particles may not be removed after removal, or more hollow carbon layer structures remain after removal, which still remain in the sample as impurities
In order to obtain a better purification effect, a strong oxidizing environment is adopted, but in this case the destruction of the wall structure of carbon nanotubes and the loss of a large amount of samples cannot be avoided

Method used

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  • Method for non-invasive efficient purification of single-wall carbon nano tube
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  • Method for non-invasive efficient purification of single-wall carbon nano tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take a certain amount of original sample of single-walled carbon nanotubes (iron as a catalyst) and spread them in a quartz boat. The diameter of single-walled carbon nanotubes is about 5nm. Put the quartz boat of carbon nanotubes into the quartz tube. The end is open, in order to ensure that the air can enter the quartz tube to fully react, the air bubbler is used to continuously inject air from one end, and let the air flow out from the other end, so as to achieve continuous air supply, balanced oxidation environment, and complete oxidation. Effect. at 10 °C min -1 The furnace temperature was raised to 400°C at a rate of 1 hour. After the air oxidation is over, both ends of the quartz tube are closed and an inert gas argon is introduced as a protective gas. -1 The furnace temperature was raised to 800° C. for 1 h at a high rate. After the high-temperature heat treatment is finished, pass the protective gas argon until the furnace temperature is lowered to room temp...

Embodiment 2

[0029]Take a certain amount of original sample of single-walled carbon nanotubes (iron as a catalyst) and spread them in a quartz boat. The diameter of single-walled carbon nanotubes is about ~1nm. Put the quartz boat into the quartz tube. First, the two ends of the quartz tube are open. , in order to ensure that the air can enter the quartz tube to fully react, an air bubbler is used to continuously inject air from one end, and let the air flow out from the other end, so as to achieve continuous air supply, balanced oxidation environment, and complete oxidation. at 10 °C min -1 The furnace temperature was raised to 400°C at a rate of 1 hour. After the air oxidation is over, both ends of the quartz tube are closed and an inert gas argon is introduced as a protective gas. -1 The furnace temperature was raised to 800° C. for 1 h at a high rate. After the high-temperature heat treatment is finished, pass the protective gas argon until the furnace temperature is lowered to room ...

Embodiment 3

[0031] Take a certain amount of original sample of single-walled carbon nanotubes (iron as a catalyst) and spread them in a quartz boat. The diameter of single-walled carbon nanotubes is about ~1nm. Put the quartz boat into the quartz tube. First, the two ends of the quartz tube are open. , in order to ensure that the air can enter the quartz tube to fully react, an air bubbler is used to continuously inject air from one end, and let the air flow out from the other end, so as to achieve continuous air supply, balanced oxidation environment, and complete oxidation. at 10 °C min -1 Raise the furnace temperature to 500°C at a rate of 1 hour. After the air oxidation is over, both ends of the quartz tube are closed and an inert gas argon is introduced as a protective gas. -1 The furnace temperature was raised to 800° C. for 1 h at a high rate. After the high-temperature heat treatment is finished, pass the protective gas argon until the furnace temperature is lowered to room temp...

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Abstract

The invention belongs to the field of material synthesis, in particular relates to a method for non-invasive efficient purification of a single-wall carbon nano tube. The method comprises the following steps: laying original single-wall carbon nano tube samples in a quartz boat, and placing the quartz boat in a quartz tube; raising the temperature of a furnace to 400-500 DEG C at the speed rate of 10 DEG C. min<-1> and insulating for 1-3 hours; after an air oxidation reaction is finished, closing two ends of the quartz tube and introducing protective gas argon so as to exhaust the air in the quartz tube; then raising the temperature of the furnace to 750-1000 DEG C at the speed rate of 10 DEG C. min<-1> and insulating for 1-3 hours; after a high-temperature reduction reaction thermal treatment process is finished, introducing the protective gas, taking out the samples after the temperature of the furnace is reduced to room temperature, and removing catalyst particles and unreacted metal oxides, wherein the metals on the catalyst particles are reduced out; and filtering, washing and drying again, so as to obtain the purified single-wall carbon nano tube samples. In the method, the purification process is simple, the tube wall structure of the single-wall carbon nano tube is not destroyed in the whole purification process, the purification cost is low, environment is not polluted, and continuous operation can be realized, thus the method is suitable for large-scale purification of the single-wall carbon nano tube.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a method for efficiently purifying single-walled carbon nanotubes without damage. Background technique [0002] With its unique electrical, mechanical and chemical properties and unique quasi-one-dimensional tubular molecular structure, carbon nanotubes have become a research hotspot in many fields such as physics, chemistry and material science, and have shown their potential in the fields of energy materials and electronic devices. Broad application prospects. No matter the original samples of SWNTs prepared by arc method, laser method, or catalytic pyrolysis method contain a large amount of impurities, including metal catalyst particles, non-SWCNT carbon tissues mainly include fullerenes, amorphous Carbon, multi-wall carbon nanotubes, etc. The existence of these impurities hinders the further research and application of single-wall carbon nanotubes. The purificat...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y40/00
Inventor 马杰金路陈君红袁志文
Owner TONGJI UNIV
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