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Chemical vapor deposition method for continuously preparing carbon nanotubes with few walls under condition of no carrier gas
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A technology of chemical vapor phase and carbon nanotubes, applied in the direction of carbon nanotubes, nanocarbons, nanotechnology, etc., can solve safety problems and achieve the effects of safe operation, simple process, and uniform product morphology
Inactive Publication Date: 2013-10-16
TIANJIN UNIV
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At present, there are patents (CN101153413, CN101187094, CN 200910069120.6, CN 101696519A) disclosing methods for preparing carbon nanotube fibers using water sealing and water-assisted chemical gas phase reaction, but these methods all need to use hydrogen or inert gas (argon or nitrogen) as Carrier gas, which poses safety concerns for industrial mass production
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Embodiment 1
[0023] (1) Weigh 30 g of ethanol, 0.15 g of thiophene, and 0.60 g of ferrocene, mix them uniformly by ultrasonication for 30 min, and transfer them into a syringe.
[0024] (2) When the temperature of the reactor was raised to 1140° C. under an argon protective atmosphere, the argon flow to the reactor was stopped, and the precursor mixed solution and methanol in the step (1) were simultaneously mixed at a rate of 8ml / h and 50ml / h respectively. Inject into the reactor to continuously synthesize carbon nanotubes.
[0025] The few-walled carbon nanotube material prepared by the present invention has relevant characterization methods and characterization results as follows:
[0026] Morphological characterization: JSM-6700F EOL cold field emission scanning electron microscope and Dutch Tecnai G2F20 field emission transmission electron microscope were used to observe the morphology of the product.
[0027] figure 1 Scanning electron micrograph of the carbon nanotubes prepared in...
Embodiment 2
[0031] (1) Weigh 30 g of ethanol, 0.13 g of thiophene, and 0.45 g of ferrocene, mix them uniformly by ultrasonication for 30 min, and transfer them into a syringe.
[0032] (2) When the temperature of the reactor is raised to 1000° C. under an argon protective atmosphere, the argon gas flow to the reactor is stopped, and the precursor mixed solution and methanol in step (1) are simultaneously mixed at a rate of 20ml / h and 100ml / h respectively. Inject into the reactor to continuously synthesize carbon nanotubes.
Embodiment 3
[0034] (1) Weigh 30 g of ethanol, 0.03 g of thiophene, and 0.15 g of ferrocene, mix them uniformly by ultrasonication for 30 min, and transfer them into a syringe.
[0035] (2) When the temperature of the reactor is raised to 1200° C. under an argon protective atmosphere, the argon flow to the reactor is stopped, and the precursor mixed solution and methanol in the step (1) are simultaneously mixed at a rate of 2ml / h and 40ml / h respectively. Inject into the reactor to continuously synthesize carbon nanotubes.
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Abstract
The invention discloses a method for continuously preparing carbon nanotubes with a few walls under the condition of no carrier gas. The method comprises the following steps of: uniformly mixing a carbon source, a catalyst and a promoter through ultrasonic waves to obtain a precursor solution; and heating a reactor to the temperature of between 600 and 1,200DEG C in the inert atmosphere, stopping introducing gas, respectively injecting the precursor solution and methanol into the reactor, and continuously synthesizing a carbon nanotube material with a few walls at high temperature without carrier gas. The method has the advantages of safe operation, simple process, uniform product appearance and the like, and the carbon nanotube material with a few walls (n is less than or equal to 10) can be continuously synthesized.
Description
technical field [0001] The invention relates to the preparation of nanometer materials, in particular to a method for continuously preparing less-walled carbon nanotubes by chemical vapor deposition under the condition of no carrier gas. Background technique [0002] Carbon nanotubes are a typical one-dimensional nanomaterial. Due to their unique structure, high specific surface area, high electrical and thermal conductivity, and excellent mechanical and hydrogen storage properties, carbon nanotubes are widely used in composite materials and material preparation, Both energy and hydrogen storage fields have broad application prospects. For example: combining carbon nanotubes with metal oxides or compounds (TiO 2 , SnO 2 , MnO 2 , LiMn 2 o 4 、LiFePO 4 etc.) as electrode materials for lithium-ion batteries, solar cells, and supercapacitors, which can greatly enhance their electrical conductivity and thus improve specific capacity and cycle performance; as catalyst carrie...
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