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High nitrogen doped corrugated carbon nanotube material and its synthesis process

A carbon nanotube, synthesis method technology, applied in nanotechnology, nanotechnology, nanostructure manufacturing and other directions, can solve the problems of high cost, low nitrogen content, complex operation method, etc., and achieve mild synthesis conditions, cheap raw materials, and sources of wide range of effects

Inactive Publication Date: 2007-11-07
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the shortcomings of the existing nitrogen-doped bamboo-shaped carbon nanotubes, such as low nitrogen content, complicated operation methods, and high cost, the present invention proposes a high-nitrogen-doped bamboo-shaped carbon nanotube material and a synthesis method. Iron molecular sieves are used as catalysts, and organic amines with high nitrogen content are used as carbon and nitrogen sources at the same time, and the reaction temperature is controlled to obtain high-nitrogen-doped carbon nanotubes

Method used

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  • High nitrogen doped corrugated carbon nanotube material and its synthesis process
  • High nitrogen doped corrugated carbon nanotube material and its synthesis process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: 10.25g of SBA-15 molecular sieve roasted in 850°C high-temperature air was placed in a 5mL beaker; 0.1g Fe(NO) was weighed 3 9H 2 O was dissolved in 1.2mL of distilled water, then impregnated the solution on SBA-15 molecular sieves, stirred evenly, and left to stand for 12 hours; then dried in an oven at 150°C for 12 hours; In the tube furnace, the temperature was raised to 850°C, and 2mL of diethylamine was brought through the catalyst by the Ar protective gas, and the process was completed after 0.5 hours; then the heating was stopped, and the Ar protective gas was continued to drop to room temperature; the black sample was taken out as the high Nitrogen-doped bamboo-shaped carbon nanotube material, the molar ratio of C and N is 0.85:0.15.

Embodiment 2

[0021] Example 2: 1.0g of NaY molecular sieve calcined in 700°C high-temperature air is placed in a 5mL beaker; weigh 0.25gFe(NO) 3 9H 2 Dissolve O in 1.2mL of distilled water, then impregnate the solution on SAPO-11 molecular sieve, stir evenly, and let it stand for 12 hours; then put it in an oven at 150°C for 12 hours, bake it in the air at 300°C for 24 hours, and cool it down to room temperature naturally Then place in a tube furnace with a quartz tube with nitrogen protection gas, heat up to 700°C, 2g hexamethylenetetramine and 0.05mL ethylenediamine are brought through the catalyst by nitrogen protection gas, and complete this process in 0.5 hours process; then stop heating, continue to pass nitrogen protection gas until it drops to room temperature; take out the black sample which is the high nitrogen-doped bamboo-shaped carbon nanotube material containing catalyst, and the molar ratio of C to N is 0.62:0.38.

Embodiment 3

[0022] Example 3: 1.0g of SBA-15 molecular sieve roasted in 850°C high-temperature air was placed in a 5mL beaker; 0.5g of newly prepared Fe(OH) was weighed 2 Stir with 5mL of distilled water, then impregnate the emulsion onto SBA-15 molecular sieves and stir evenly, let it stand for 12 hours; then place it in an oven at 150°C for 12 hours, bake it in the air at 1000°C for 0.5 hour, and then cool it down to room temperature naturally; In a tube furnace with a quartz tube with an Ar protective gas, the temperature was raised to 900°C, 2mL of diethylamine was brought through the catalyst by the Ar protective gas, and this process was completed after 0.5 hours; then the heating was stopped, and the Ar protective gas was continued until Cool down to room temperature; take out the black sample, which is a high-nitrogen-doped bamboo-shaped carbon nanotube material, and the molar ratio of C to N is 0.88:0.12.

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Abstract

The present invention relates to high nitrogen doped corrugated carbon nanotube material and its synthesis process. The synthesis process includes the following steps: mixing Fe source and proper amount of distilled water, soaking porous molecular sieve to carry ferric oxide or ferrous oxide, stoving and roasting at 300-1000 deg.c for 0.5-24 hr to obtain catalyst; setting the catalyst inside a pipe furnace, leading organic amine into the furnace under the protection of Ar or N2 and reacting at 650-1000 deg.c for 0.2-4.0 hr to obtain high nitrogen doped corrugated carbon nanotube mixture containing the catalyst; soaking the mixture in proper amount of or excessive hydrofluoric acid, sulfuric acid, nitric acid or acid for 0.5-24 hr; and washing in distilled water, suction filtering and drying to obtain high nitrogen doped corrugated carbon nanotube material. The material has nitrogen content of 10-40 %, reinforced surface polarity, etc, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a high-nitrogen-doped bamboo-shaped carbon nanotube material and a synthesis method. Background technique [0002] Carbon nanotubes are a carbon structure discovered in 1991. Ideal carbon nanotubes are seamless, hollow tubes rolled up from graphene sheets formed by carbon atoms. Graphene sheets generally range from one layer to hundreds of layers. Those containing one graphene sheet are called single-walled carbon nanotubes (SWNTs), and those with more than one layer are called multi-walled carbon nanotubes (MWNTs). The diameter of SWNT is generally 1-6nm, and the minimum diameter is about 0.5nm, but when the diameter of SWNT is larger than 6nm, it is particularly unstable, and the collapse of SWNT tube will occur, and the length can reach hundreds of nanometers to several microns. The layer spacing of MWNT is about 0.34 nanometers, the diameter is several nanometers to tens of nanometers, the length is generally on the orde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00B01J23/745
Inventor 王利军
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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