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Preparation method of controllable nitrogen-doped carbon nanotubes

A technology of nitrogen-doped carbon and nanotubes, applied in the direction of carbon nanotubes, nanocarbons, chemical instruments and methods, etc., can solve the problems of high cost, complex process, difficult large-scale and extensive production, etc., to improve cycle life, process The effect of simple, good electrochemical performance

Active Publication Date: 2018-10-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method has various problems such as complex process, serious pollution, high cost and difficulty in large-scale and extensive production.

Method used

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  • Preparation method of controllable nitrogen-doped carbon nanotubes
  • Preparation method of controllable nitrogen-doped carbon nanotubes
  • Preparation method of controllable nitrogen-doped carbon nanotubes

Examples

Experimental program
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Embodiment 1

[0022] Dissolve 0.17mol urea in 50mL deionized water, then add 0.005mol citric acid and 0.008mol nickel acetate, add 150mL absolute ethanol after complete dissolution, and stir well. The mixed solution was vigorously stirred at 75° C. for 3 h until a sol-like form appeared. The sol samples were dried in an oven at 100 °C for 12 h. After drying, place the gel sample in a drying cabinet for 4-6 hours to completely dehumidify and dry it to obtain a precursor. The precursor was placed in a tube furnace, and the temperature was raised to 350 °C for 2 h at a heating rate of 5 °C / min, and then the temperature was raised to 750 °C for 5 h at the same heating rate. Natural cooling after heat preservation is completed to obtain nitrogen and metal carbon nanotubes, and then simple corrosion to obtain pure nitrogen-containing carbon nanotubes. SEM characterization as figure 1 As shown, the TEM characterization is as follows figure 2 As shown, the diameter of the nanotube is about 60-...

Embodiment 2

[0024] Dissolve 0.32 mol of urea in 50 mL of deionized water, then add 0.004 mol of citric acid and 0.004 mol of nickel acetate, and stir evenly. The mixed solution was vigorously stirred at 60° C. for 3 h until a sol appeared. The sol samples were dried in an oven at 120 °C for 12 h. After drying, place the sample in a drying cabinet for 4-6 hours to completely cool and dry to obtain a precursor. The precursor was placed in a tube furnace, and the temperature was raised to 350 °C for 4 h at a heating rate of 5 °C / min, and then the temperature was raised to 750 °C for 10 h at the same heating rate. Natural cooling after heat preservation is completed to obtain nitrogen and metal carbon nanotubes, and then simple corrosion to obtain pure nitrogen-containing carbon nanotubes.

Embodiment 3

[0026] Dissolve 0.12 mol of thiourea in 50 mL of deionized water, then add 0.006 mol of glucose and 0.012 mol of cobalt acetate, add 150 mL of absolute ethanol after complete dissolution, and stir well. The mixed solution was vigorously stirred at 75 °C for 3 h until a sol appeared. The sol samples were dried in an oven at 100°C for 10 h. After drying, place the sample in a drying cabinet for 4-6 hours to completely cool and dry to obtain a precursor. The precursor was placed in a tube furnace, and the temperature was raised to 650 °C for 4 h at a heating rate of 2 °C / min, and then the temperature was raised to 1000 °C for 10 h at the same heating rate. Natural cooling after the heat preservation is over, carbon nanotubes containing nitrogen and metal sulfides can be obtained, and then pure nitrogen-containing carbon nanotubes can be obtained through simple corrosion. SEM characterization as image 3 As shown, the diameter of the nanotube is about 150-200nm, and the length ...

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Abstract

The invention discloses a preparation method of controllable nitrogen-doped carbon nanotubes. The method comprises the following steps: dissolving a metal salt, a carbon source and a nitrogen source in an aqueous or ethanol solution, performing stirring at 60-80 DEG C until the solution volatilizes to form a sol, drying the sol at 80-120 DEG C to form a gel, carrying out high-temperature heat treatment carbonization on the above gel precursor, keeping the temperature at 350-650 DEG C for 2-4 h, keeping the temperature at 750-1000 DEG C for 5-10 h to obtain nitrogen-doped carbon nanotubes containing metal or metal sulfide, and simply corroding the nitrogen-doped carbon nanotubes containing metal or metal sulfide to obtain the nitrogen-doped carbon nanotubes. The above sol-gel technology canrealize the effective regulation of the caliber and the length of the nitrogen-doped carbon nanotubes and the adjustment of the nitrogen content, the pore structure and the conductivity of the nitrogen-doped carbon nanotubes. The nitrogen-doped carbon nanotubes can effectively prolong the cycle life of a battery when applied to the electrode material of the battery, has good electrochemical performances, and is hopeful to be applied to fields of electrochemical catalysis, energy transition and energy storage.

Description

technical field [0001] The invention relates to a controllable preparation method of nitrogen-doped carbon nanotubes, belonging to the technical field of material preparation. Background technique [0002] Carbon nanotubes are mainly composed of carbon atoms arranged in a hexagonal shape to form coaxial circular tubes with several to dozens of layers, and the interlayer spacing is 0.34nm. Curved carbon tubes exhibiting a hexagonal grid structure have attracted extensive attention due to their special electrical, chemical, and mechanical properties. Since carbon atoms in carbon nanotubes adopt SP 2 hybridized, compared to SP 3 Hybridization, SP 2 The S orbital composition in the hybridization is relatively large, so that the carbon nanotubes have high modulus and high strength. The P electrons of carbon atoms on carbon nanotubes form a large range of delocalized π bonds. Due to the significant conjugation effect, carbon nanotubes have some special electrical properties. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/16H01M4/62
CPCH01M4/62H01M4/625C01B2202/36C01B2202/22C01P2004/03C01P2004/04Y02E60/10
Inventor 夏晖郭秋卜杨梅翟腾
Owner NANJING UNIV OF SCI & TECH
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