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Preparation method of nitrogen, sulfur and phosphorus heteroatom-doped carbon material

A carbon material and heteroatom technology, applied in the field of carbon material preparation, can solve the problem of small controllable range and achieve the effect of strong universality, easy operation, high efficiency and controllable doping

Inactive Publication Date: 2018-07-24
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in general, the content of phosphorus and sulfur in doped carbon materials reported so far is mostly in the range of 1wt%-4wt%, and the adjustable range is small, which is not conducive to further exploration of the effects of different concentrations of sulfur, phosphorus and other heteroatoms on the structure of carbon materials, Influence of physical and chemical properties and performance

Method used

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  • Preparation method of nitrogen, sulfur and phosphorus heteroatom-doped carbon material
  • Preparation method of nitrogen, sulfur and phosphorus heteroatom-doped carbon material
  • Preparation method of nitrogen, sulfur and phosphorus heteroatom-doped carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-6

[0031] Weigh 100 mg of carbon fluoride nanotubes and lay them flat on a porcelain boat, and place the porcelain boat in the center of the tube furnace until the temperature of the tube furnace rises to the target shown in Table 1 at a rate of 10°C / min under an argon atmosphere. Temperature: Inject thiophene into the high temperature area with a micro-injection pump at a rate of 1.5mL / h, and continue the injection for 2 hours. After the tube furnace is cooled to room temperature, take out the sample, wash it with ethanol and acetone three times, and measure it with an elemental analyzer. The sulfur content of doped carbon materials is shown in Table 1.

[0032] Table 1

[0033] Example

[0034] It can be seen from Table 1 that the sulfur doping content of fluorinated carbon nanotubes in the selected temperature range is above 4wt%, and the doping effect is the best at 800°C, and the sulfur content is 5.217wt%, which realizes the efficient doping of sulfur.

Embodiment 7-9

[0036] Weigh 100 mg of carbon fluoride nanotubes and lay them flat on a porcelain boat, and place the porcelain boat in the center of the tube furnace. The syringe pump injected thiophene into the high temperature area at the injection speed shown in Table 2, and continued to inject for 2 hours. After the tube furnace was cooled to room temperature, the samples were taken out and washed 4 times with ethanol and acetone respectively. The sulfur content is shown in Table 2.

[0037] Table 2

[0038] Example

[0039] It can be seen from Table 2 that when the injection speed of fluorinated carbon nanotubes is 1.5mL / h, a relatively ideal sulfur doping effect can be achieved.

Embodiment 10-11

[0041] Weigh 100 mg of carbon fluoride nanotubes and lay them flat on a porcelain boat, and place the porcelain boat in the center of the tube furnace. The syringe pump injects thiophene into the high-temperature area at a rate of 1.5mL / h, and continues the injection for the time shown in Table 3. After the tube furnace is cooled to room temperature, the sample is taken out, washed with ethanol and acetone for 5 times, and measured by an elemental analyzer. The sulfur content of the doped carbon materials is shown in Table 3.

[0042] table 3

[0043] Example

[0044] It can be seen from Table 3 that the ideal sulfur content can be achieved after thermal deposition of fluorinated carbon nanotubes for 2 hours, and the sulfur species on the surface decrease with the increase of the holding time.

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Abstract

The invention discloses a preparation method of a nitrogen, sulfur and phosphorus heteroatom-doped carbon material, and belongs to the technical field of carbon materials. The method comprises the following steps: adopting a perfluorocarbon material or a fluorinated carbon nanotube as a carbon substrate, doping one or more of liquid sources containing nitrogen, sulfur and phosphorus heteroatoms into the carbon substrate at the temperature of 400 to 800 DEG C by adopting a pyrolysis deposition method, or mixing a solid source containing the nitrogen, sulfur and phosphorus heteroatoms with the carbon substrate and grinding, and calcining at the temperature of 400 to 800 DEG C to realize doping, so as to obtain the nitrogen, sulfur and phosphorus heteroatom-doped carbon material. The liquid source contains pyridine, thiophene, triphenylphosphine solution and the like, and the solid source contains sublimed sulfur, dibenzyl disulfide and the like. The method has the advantage of simple operation and high universality; high-concentration vacancy is generated by utilizing the fluorinated carbon nanotubes to remove fluorine at high temperature, and further high-efficiency doping of heteroatom can be realized.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, and in particular relates to a preparation method of nitrogen, sulfur and phosphorus heteroatom-doped carbon material. technical background [0002] Heteroatom doping of carbon materials refers to the introduction of heteroatoms such as O, N, B, P, and S into the carbon skeleton, which can strengthen the inherent excellent properties of carbon materials and even endow them with new functions, so that carbon materials have higher electron density. Transmission rate, richer pore structure, stronger wettability, larger specific surface area, obvious surface acidity and alkalinity, etc., thus broadening the application of carbon materials in fuel cells, secondary batteries, supercapacitors, heterogeneous catalysis and other fields Applications. [0003] The preparation methods of heteroatom-doped carbon materials are generally divided into in-situ doping and post-treatment doping...

Claims

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Application Information

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IPC IPC(8): C01B32/05
Inventor 余皓王文丽彭峰王红娟曹永海
Owner SOUTH CHINA UNIV OF TECH
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