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Method and device for producing carbon nano-tube or nitrogen doping carbon nano-tube with liquid phase forerunner article

A technology of carbon nanotubes and nitrogen-doped carbon, which is applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of inconstant material quantity, inability to achieve flow sampling, unfavorable and other problems, and achieve easy control of reaction conditions, Expanded range of options, easy-to-achieve effects

Inactive Publication Date: 2008-08-20
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] (1) The flow rate of the carrier gas is constant, but the amount of the substance actually entering the system is not constant, resulting in a large error;
[0011] (2) The products obtained under different seasons and temperatures have large deviations in yield, yield and product quality, which cannot be used to explore the real reaction situation well, and the repeatability is poor;
[0012] (3) It is impossible to accurately calculate the amount of precursors that enter the system, which is not conducive to the scale-up experiment
Peristaltic pumps generally cannot achieve flow rate injection, similar to human infusion, which is a static point, and the injection volume is too large and not uniform

Method used

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  • Method and device for producing carbon nano-tube or nitrogen doping carbon nano-tube with liquid phase forerunner article
  • Method and device for producing carbon nano-tube or nitrogen doping carbon nano-tube with liquid phase forerunner article
  • Method and device for producing carbon nano-tube or nitrogen doping carbon nano-tube with liquid phase forerunner article

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Using benzene as a precursor, 1.0mmol / g Fe-2.0mmol / g Co / γ-Al 2 o 3 As a catalyst, carbon nanotubes are prepared.

[0042] Weigh about 0.4g of catalyst, spread it in the quartz reaction tube, then place the quartz reaction tube in the central temperature zone of the tube furnace, and raise the temperature at a rate of 10°C per minute under an argon or nitrogen atmosphere with a flow rate of 100 sccm to 650°C, and then turn on the syringe pump to inject the benzene precursor into the furnace tube. The distribution coefficient of the syringe pump is 0.75ml / 3hour. g, the utilization of carbon atoms in the benzene precursor is greater than 65%. Transmission electron microscopy (TEM) characterization as figure 2 As shown, the diameter of the nanotube is about 20-30nm, and the length can reach the micron level.

Embodiment 2

[0043] Example 2 Using pyridine as a precursor, 1.0mmol / g Fe-2.0mmol / g Co / γ-Al 2 o 3 As a catalyst, nitrogen-doped carbon nanotubes were prepared.

[0044] Weigh about 0.4g of catalyst, spread it in the quartz reaction tube, then place the quartz reaction tube in the central temperature zone of the tube furnace, and raise the temperature to 650°C at a rate of 10°C per minute under argon or nitrogen atmosphere (100sccm). ℃, and then turn on the syringe pump (0.75ml / 3hour) to inject the pyridine precursor into the furnace tube. After the reaction, the furnace tube is protected by argon or nitrogen (100 sccm) and lowered to room temperature, and about 0.4 g of the carbon nanotube pyridine precursor is collected. The utilization rate of carbon atoms is greater than 70%. Transmission electron microscopy (TEM) characterization as image 3 As shown, the diameter of the nanotube is about 20-30 nm, and the length can reach the order of microns.

Embodiment 3

[0045] Example 3 Using benzylamine as a precursor, 1.0mmol / g Fe-2.0mmol / g Co / γ-Al 2 o 3 As a catalyst, nitrogen-doped carbon nanotubes were prepared.

[0046] Weigh about 0.4g of catalyst, spread it in the quartz reaction tube, then place the quartz reaction tube in the central temperature zone of the tube furnace, and raise the temperature to 650°C at a rate of 10°C per minute under argon or nitrogen atmosphere (100sccm). ℃, and then turn on the syringe pump (0.75ml / 3hour) to inject the benzylamine precursor into the furnace tube. After the reaction, the furnace tube is lowered to room temperature under the protection of argon or nitrogen (100sccm), and collect about 0.45g of benzylamine for carbon nanotubes The utilization rate of carbon atoms in the precursor is greater than 70%. Transmission electron microscopy (TEM) and photoelectron spectroscopy (XPS) characterizations are shown in Figure 4a) and Figure 4b), and the TEM images show that the diameter of the generated ni...

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Abstract

The invention provides a chemical vapor deposition method, which takes liquidoid organic precursor as the carbon source and the nitrogen source, adopts an injection pump to inject the precursor into a reaction chamber, regulates the variety and input of the precursor, the variety and load of catalyst, the flow speed of protective atmosphere, and the reaction temperature, so as to produce high-quality carbon nano-tubes of different sizes and appearances, or nitrogen-mixed carbon nano-tubes with different nitrogen contents, classes, sizes and appearances in large quantity. For the chemical vapor phase deposition method of the invention, the carbon atoms in the precursor are transformed into carbon nano-tubes or nitrogen-mixed carbon nano-tubes with the transformation rate up to more than 60%, and the nitrogen content in the obtained nitrogen-mixed carbon nano-tubes is comparatively high; the diameter of the obtained tubes is comparatively uniform and the purity is relatively high; by adopting the CVD method to produce carbon nano-tubes or nitrogen-mixed carbon nano-tubes, the chemical vapor deposition method in the invention has the advantages of easy feasibility, convenient control of the reaction conditions, and no special requirements on the physical properties of the precursor by adopting the injection pump to inject the precursor, and larger selectable range of the precursor.

Description

technical field [0001] The invention belongs to the technical field of carbon nanotube preparation, and specifically relates to a method and a device for preparing carbon nanotubes or nitrogen-doped carbon nanotubes with liquid phase precursors. Background technique [0002] Since the 1990s, carbon nanotubes have attracted extensive attention and research in the scientific and industrial circles due to their important scientific value and huge application prospects. Carbon nanotubes were first obtained by Ijima through the arc discharge method [S.Iijima, Nature, 1991, 354, 56.], followed by significant progress in the preparation of multi-walled carbon nanotubes by the arc method. P.M.Ajayan et al. purified graphite electrode arc discharge products for the first time High-purity multi-walled carbon nanotubes on the order of grams have been obtained [T.W.Ebbesen, P.M.Ajayan, Nature, 1992, 358, 220.]. In 1995, when R.E.Smally et al. [T.Guo,, R.E.Smalley.et.al., J.Phys.Chem., ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 蹇国强余乐书王喜章马延文胡征
Owner NANJING UNIV
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