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Method for preparing nitrogen-containing carbon nano tube

A nanotube and nitrogen carbon technology is applied in the field of nitrogen-doped graphitized carbon nanomaterials and their synthesis, which can solve the problems of difficult control and low yield, and achieve the effects of easy control, low reaction temperature and uniform nitrogen distribution.

Inactive Publication Date: 2014-09-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of the present invention can effectively overcome the shortcomings of the existing preparation technology, such as high requirements for equipment, high energy consumption, difficult control, and low output.

Method used

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  • Method for preparing nitrogen-containing carbon nano tube
  • Method for preparing nitrogen-containing carbon nano tube
  • Method for preparing nitrogen-containing carbon nano tube

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Under the condition of stirring at room temperature, add dissolved metal ions Zn(NO 3 ) 2 , FeSO 4 The DMF solution was stirred at room temperature for half an hour, then transferred to a crystallization kettle and sealed, crystallized at 140°C for 48h, cooled to room temperature, centrifuged, and dried at 100°C for 24h to obtain an imidazole polymer material , SEM results show that it is a microsphere with uniform particle size and good dispersion ( figure 1 ); in a nitrogen atmosphere, put Zn-Fe-ZIFs spheres into a tube furnace, carbonize at 900°C for 4h; add the carbonized product into aqua regia, stir at room temperature for 4h and then centrifuge; wash with deionized water until neutral, 100 ℃ of drying 24h, thereby made product. SEM results show that the product obtained is a carbon nanotube ( figure 2 ). The XPS results of N1s of the obtained product show that nitrogen in carbon nanotubes contains three states: graphitized N (binding energy is 401.8eV), pyr...

Embodiment 2

[0042] Using the preparation process of Example 1, the difference is that before the imidazole polymer material is put into the tube furnace for carbonization, it is first dispersed in a DMF solution (1.5M) with dicyandiamine dissolved in it, and the dicyandiamine is adjusted. The amount that makes the mass ratio of dicyandiamide and imidazole polymer material is 2.5, stirred at room temperature for 2 hours, then spin-dried, and the solid obtained was put into a tube furnace for carbonization at 700°C for 3h under nitrogen atmosphere, carbonization The product was dispersed in aqua regia, stirred at room temperature for 20 min, washed with deionized water until neutral, and dried at 100° C. for 24 h to obtain the product. SEM results show that the product obtained is a carbon nanotube ( Figure 5 ). TEM results showed that the obtained product was bamboo-shaped and contained metal nanoparticles ( Figure 6 ), the XPS results of N1s of the obtained product show that nitrogen ...

Embodiment 3

[0044] Using the preparation process of Example 2, the difference is that the amount of dicyandiamine is adjusted so that the mass ratio of dicyandiamine to imidazole polymer material is 5, and the rest of the synthesis process is exactly the same. SEM results show that the obtained product is a carbon nanotube ( Figure 8 ). TEM results showed that the obtained product was bamboo-shaped and contained metal nanoparticles ( Figure 9 ), the XPS results of N1s of the obtained product show that nitrogen in carbon nanotubes contains three states: graphitized N (binding energy is 401.8eV), pyrrole N (binding energy is 400.1eV), pyridine N (binding energy Can be 398.7eV) ( Figure 10 ), the nitrogen content of the elemental analysis characterization product is 10.7%.

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Abstract

The invention relates to a nitrogen-containing carbon nano tube and a preparation method thereof. The preparation method specifically comprises the following preparation steps: by taking Zn<2+> and Fe<2+> as co-metallic ions in a solvothermal system, complexing the metal ions and imidazole organic ligands, and synthesizing imidazole polymer nanospheres; mixing the spheres with dicyandiamide of different amounts (a mass ratio of the dicyandiamide to the imidazole polymer nanospheres is adjustable in a range from 2.5 to 20) or carbonizing pure imidazole polymer nanospheres at the temperature of 700-900 DEG C in N2 atmosphere for 3-4 hours, and obtaining a solid material; removing metals Zn and Fe by using aqua regia and nitric acid, and further obtaining the nitrogen-doped multi-walled carbon nano tube of which the tube diameter is adjustable in a range from 30 to 800nm and the nitrogen doping amount is adjustable in a range from 4 to 12 percent. The method is simple in process, low in equipment requirement, low in energy consumption and simple and easily controlled in reaction process; the tube diameter of the carbon nano tube is adjustable; and the nitrogen is uniformly distributed in the carbon tube and is high in content.

Description

technical field [0001] The invention relates to a nitrogen-doped graphitized nano-carbon material and a synthesis method thereof, in particular to a nitrogen-containing carbon nanotube and a preparation method thereof. Background technique [0002] Nitrogen doping is a powerful means to change the properties of carbon materials, which extends the application of carbon materials from the field of catalysis to the microelectronics industry. Nitrogen-doped carbon nanotubes, as an important nitrogen-doped carbon material, have attracted extensive attention. Nitrogen-doped carbon nanotubes have good electron transport effects, and they are widely used in lithium-ion batteries, field emission materials, catalyst supports, supercapacitors, gas sensors, especially fuel cell cathode oxygen reduction reaction electrocatalysts and other fields. At present, the preparation methods of nitrogen-doped carbon nanotubes are mainly divided into: "chemical vapor deposition method" (CVD), "arc...

Claims

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Application Information

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IPC IPC(8): C01B31/02B82Y40/00C01B32/16
Inventor 杨启华李灿苏盼盼
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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